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Patent 2402653 Summary

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(12) Patent: (11) CA 2402653
(54) English Title: ANTISEPTIC COATING FOR THE PREVENTION OF DISEASE TRANSMISSION VIA BIOFILMS
(54) French Title: ENDUIT ANTISEPTIQUE POUR PREVENIR LA TRANSMISSION DE MALADIES PAR L'INTERMEDIAIRE DE FILMS BIOLOGIQUES
Status: Expired
Bibliographic Data
(51) International Patent Classification (IPC):
  • C09D 5/14 (2006.01)
  • A61K 38/43 (2006.01)
  • A61K 38/44 (2006.01)
  • A61K 38/45 (2006.01)
  • A61K 38/55 (2006.01)
  • C09D 5/18 (2006.01)
  • C09D 125/10 (2006.01)
  • C09D 151/00 (2006.01)
  • C09D 153/00 (2006.01)
  • C09D 193/02 (2006.01)
  • C08K 5/00 (2006.01)
(72) Inventors :
  • DORMON, JANE (Canada)
(73) Owners :
  • DORMON, JANE (Canada)
(71) Applicants :
  • DORMON, JANE (Canada)
(74) Agent:
(74) Associate agent:
(45) Issued: 2011-05-24
(22) Filed Date: 2002-09-26
(41) Open to Public Inspection: 2004-03-26
Examination requested: 2008-09-16
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data: None

Abstracts

English Abstract

The invention provides an improved means for creating a surface that strongly resists microbial colonization. The invention involves a process that can be instigated in the environment of an applied coating. Non-toxic microbicides and halogen-free flame retardants are added as components of the coating which is manufactured using traditional methods and then applied by traditional methods to the hard or soft surface that is to be protected.


French Abstract

Cette invention fournit un moyen amélioré de créer une surface qui résiste fortement à la colonisation microbienne. Cette invention fait appel à un procédé pouvant être provoqué dans l'environnement d'un revêtement appliqué. Des microbicides non toxiques et des ignifugeants sans halogènes sont ajoutés comme éléments du revêtement préparé selon les méthodes traditionnelles, puis ils sont appliqués au moyen des méthodes traditionnelles à la surface dure ou molle qui est alors protégée.

Claims

Note: Claims are shown in the official language in which they were submitted.




Claims

1. A coating composition comprising
i. a surface coating material,
ii. at least a first enzyme, and
iii. at least one flame retarding compound,
iv. at least one antimicrobial compound
wherein the first enzyme is capable of directly or indirectly inhibiting
attachment
and/or growth of microorganisms after applying the coating composition to a
surface and allowing it to form a film.


2. The composition according to claim 1, wherein the surface coating
material comprises a binder.


3. The composition according to claim 2, wherein the binder is a modified
rosin, maleic acid, or gloss oil.


4. The composition according to claim 2, wherein the binder is a shellac.

5. The composition according to claim 2, wherein the binder is an oxidised
rubber.


6. The composition according to claim 2, wherein the binder is a water-based
styrene butadiene latex system.


7. The composition according to claim 2, wherein the binder is a water-based
styrene acrylic.


8. The composition according to claim 2, wherein the binder is a chlorinated
polyolefin.


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SUBSTITUTE SHEET



9. The composition according to claim 2, wherein the binder is a modified
water-borne silicone.


10. The composition according to claim 2, wherein the binder is at least one
compound selected from a group consisting of modified sucrose, water-
borne polyvinylidene, chloride based latex terpopolymers, vinyl acetate,
polyvinyl alcohol, polyvinyl acetals, vinylidene fluoride, polyurethanes,
epoxides, and water soluble acrylics.


11. The composition according to any one of claims 1-10, wherein the surface
coating composition and the binder do not significantly inhibit the activity
of the enzyme.


12. The composition according to claim 11, wherein the antimicrobial
compound is a biocide selected from the group consisting of:
zinc oxide;
citrus oil, chili oil, cranberry extract, and/or seaweed extract;
2,4,4-trichloro-2-hydroxy-diphenyl ether, 5-chloro-2-phenol;
polyvalent glycosylated casein;
bismuth; and
carbamates with diethanolamide as a potentiator.


13. The composition according to claim 12 wherein the group further includes
vetiver oil, camphor oil, cedar oil, tea-tree oil, and citrus oil, each taken
alone or in any combination.


14. The composition according to claim 13 wherein the group further includes
honey, natural pine tree resins, natural elemi tree resins, copal, and
dammar.


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15. The composition according to claim 14 wherein the group further includes
sodium fluoride, dodecylamine, triclosan, and chlorhexidine, each taken
alone or in any combination.


16. The composition according to claim 15, wherein the group further includes
iodide salts, metal salts, cupric chloride, cupric sulphate, silver nitrate,
colloidal bismuth subcitrate, bismuth citrate, aluminum phosphate,
aluminum hydroxide hydrate, and gold chloride, each taken alone or in
any combination.


17. The composition according to claim 16, comprising 0.5% to 30% (w/v) of
biocide.


18. The composition according to claim 1 wherein the flame retarding
compound is selected from a group consisting of: macroplegmatic
compounds; a flame retardant mixture of melamine cyanurate, silica, and
phosphoric acid; a flame-retardant mixture of sodium carbonate,
pyrophosphate, ammonium salts, boric acid, phosphoric acid; a halogen-
based flame retardant, organic bromine compounds, brominated aromatic
epoxy compounds, brominated polycarbonates, brominated benzyl
acrylates, brominated polystyrene; phosphorous based flame retardants, ,
phosphate esters, nitrogen containing phosphorous compounds, and red
phosphorous; inorganic flame retardants; oxides of antimony; sodium
antimonate; aluminum hydroxide; and magnesium hydroxide.


19. The composition according to claim 18 wherein flame retarding compound
is non-toxic and/or does not release harmful amounts of toxic fumes.


20. The composition according to claim 18 wherein flame retarding compound
is present in an amount of 1% to 50% (w/v).


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21. The composition according to claim 18 further comprising up to 75% (w/v)
of an essentially non-combustible binder.


22. The composition according to any one of claims 1-21, wherein the
enzyme and/or a substrate for the enzyme are encapsulated in a material
selected from a group including mesoporous silicates, porous ceramic
particles, and porous glass spheres.


23. The composition according to claim 22 further comprising cellulosic
fibres.

24. The composition according to claim 23 wherein one or more of the
enzyme, enzyme substrate, and antimicrobial compound is bound to the
cellulosic fibres.


25. The composition according to any one of claims 1-25, further comprising
co-factors for the enzyme.


26. The composition according to claims 25 comprising 0.05%-60% (w/v) of
enzyme substrate for the enzyme.


27. The composition according to any one of claims 1-26 wherein hydrogen
peroxide is generated in an amount to prevent biofilm formation on the
surface of the composition.


28. The composition according to claim 17 being adapted to produce at least
5-10 mmol hydrogen peroxide in an overlying moisture film.


29. The composition according to claim 1 wherein the activity of at least one
enzyme is controllable by changes in environmental consideration
selected from a group consisting of: ambient humidity, ambient


64




temperature, ambient pH, and ambient oxygen levels, each taken alone or
in any combination.


30. The composition according to claim 29 wherein at least one enzyme has
an activity sufficient to inhibit biofilm formation when ambient humidity is
above 40%.


31. The composition according to claim 29 wherein at least one enzyme has
an optimum at in the interval between 5 - 40 °C.


32. The composition according to claim 29 wherein at least one enzyme has
an optimum in the interval between pH 4 and 11.


33. The composition according to claim 29 wherein at least one enzyme has
an optimum at 50 - 100% oxygen saturation.


34. The composition according to any one of claims 1-33 wherein the at least
one enzyme does not lose substantial activity when dried and rehydrated
repeated times.


35. The composition according to any one of claims 1-33 wherein the at least
one enzyme does not lose substantial activity when dried to below 20%
moisture content and rehydrated again.


36. The composition according to any one of claims 22-35 comprising a
combination of first enzyme and substrate selected from the group
consisting of mixture combinations including: malate oxidase - malic acid;
glucose oxidase - glucose; hexose oxidase - glucose; cholesterol oxidase
- cholesterol; arylalcohol oxidase - arylalcohol: galactose oxidase -
galactose; alcohol oxidase - alcohol; lathosterol oxidase - lathosterol;
aspartate oxidase - aspartic acid; L-amino-acid oxidase - L-amino acid;


65





D-amino-acid oxidase - D-amino acid; amine oxidase - amine; D-
glutamate oxidase - glutamine; ethanolamine oxidase - ethanolamine;
NADH oxidase - NADH; urate oxidase (uricase) - uric acid; superoxide
dismutase - superoxide radical; glucose - hexose oxidase; glucose -
glucose oxidase; L amino acid - L amino acid oxidase; galactose -
galactose oxidase; lactose - P-galactosidase - hexose oxidase; lactose -
galactosidase - glucose oxidase; 2-deoxyglucose - glucose oxidase; and
pyranose - pyranose oxidase; each mixture taken alone or in any
combination.


37. The composition according to any one of claims 1-36 comprising
0.0001%-5% (w/v) of enzyme.


38. The composition according to any one of claims 1-37 further comprising a
second enzyme capable of converting a compound into a substrate for the
first enzyme.


39. The composition according to claim 38 wherein the second enzyme is
selected from a group consisting of: an amylase, a fructase, a cellulase, a
ligninase, a proteinase, and a nuclease.


40. The composition according to claim 38 wherein the compound is a fructan.

41. The composition according to claim 40 wherein the fructan is inulin.


42. The composition according to any one of claims 1-41 comprising a
number of enzymes ranging from two to ten enzymes.


43. The composition according to claim 42 wherein the enzymes are selected
from a group consisting of: a protease, a lipase, an amylase, and an
oxidase, each taken alone or in any combination.


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44. The composition according to any one of claims 1-43 further comprising a
colored stain.


45. The composition according to any one of claims 1-44 comprising
enzymes, and optionally, substrate enough to ensure biofilm prevention
for a period of at least 6 months to 6 years.


46. Use of the composition according to any one of claims 1-45.


47. The use according to claim 46 for coating surfaces in an enclosed
habitable space.


48. The use according to claim 46 for coating surfaces in ventilation systems.


49. The use according to claim 46 for coating surfaces in an aeroplane.


50. The use according to claim 46 for coating surfaces in medical facilities.


51. The use according to claim 47 for coating surfaces in educational
facilities.

52. The use according to claim 47 for coating surfaces within vehicles
selected from a group consisting of: a bus, an ambulance, a mobile home,
a caravan, a watercraft, and a spacecraft


53. The use according to claim 47 for coating surfaces in sports facilities.

54. The use according to claim 47 for coating surfaces in public buildings.

55. The use according to claim 47 for coating sanitary surfaces in private
homes.


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56. The use according to claim 47 for coating surfaces in animal housings.

57. The use according to claim 47 for coating surfaces in pulp mills.


58. The use according to claim 47 for coating surfaces in food preparation
facilities.


59. The use according to claim 47 for coating surfaces in slaughterhouses.

60. The use according to claim 47 for coating surfaces in sanitation
facilities.

61. A method of controlling growth of microorganisms on coated surfaces
comprising:
applying to a surface a coating composition comprising a surface
coating material, at least one enzyme, and a substrate for the enzyme;
and
allowing the coating composition to dry;
whereby the coating composition upon subsequent exposure to
moisture releases an antimicrobially effective amount of hydrogen
peroxide as a consequence of a conversion of the substrate through the
enzyme.


62. Method of controlling growth of microorganisms on coated surfaces
comprising:
applying to a surface a coating composition comprising a surface
coating material, at least one enzyme; and
allowing the coating composition to form a film;
whereby the coating composition upon subsequent exposure to
moisture levels above 50% (RH) inhibits attachment of at least one


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species of microorganisms as a consequence of the action of the enzyme.

63. The method according to claim 61 or 62 wherein the coating composition
is a coating composition according to any one of claims 1 to 45.


64. The method according to claim 61 or 62 wherein the surface is a surface
in a spacecraft.


65. The method according to claim 61 or 62 wherein the surface is a surface
in a ventilation system.


66. The method according to claim 61 or 62 wherein the surface is a surface
in a watercraft.


67. The method according to claim 61 or 62 wherein the surface is a surface
in a vehicle selected from a group consisting of: an aeroplane, a bus, an
ambulance, a mobile home, and a caravan.


68. The method according to claim 61 or 62 wherein the surface is a surface
in a medical facility.


69. The method according to claim 61 or 62, wherein the surface is a surface
in a public building.


70. The method according to claim 61 or 62, wherein the surface is a sanitary
surface in a private house.


71. The method according to claim 61 or 62 wherein the surface is a surface
is a surface in animal housing.


69




72. The method according to claim 61 or 62 wherein the surface is a surface
in a food preparation facility.


73. The method according to claim 61 or 62 wherein the surface is a surface
in a sanitation facility.


74. The method according to claim 61 or 62 wherein the surface is a surface
in an industrial facility.

Description

Note: Descriptions are shown in the official language in which they were submitted.



CA 02402653 2002-09-26
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Antiseptic coating for the prevention of disease transmission via biofilms.
Technical field

The present invention relates to the formulation of an antiseptic interior
coating such
as a coating that uses enzymatic action to produce a biologically active
compound.
The invention also relates to the generation of a biologically active compound
that
has a short half-life and does not pollute the surrounding environment with
toxic
fumes, because it is broken down in the overlying condensation layer to
harmless
compounds. The invention also relates to the formulation of an antiseptic
coating
that is safe to touch. The invention further relates to the formulation of an
antiseptic
coating that will be fire retardant without the release of toxic fumes. The
invention
furthermore relates to the use of the inventive coating for coating specific
surfaces
and preventing biofilm formation on these.
Background
In all conditions where living animals including humans are crowded the air
becomes filled with bacteria and viruses, and humidity is elevated. Bacteria
released
from humans etc , into the air will attach to surrounding walls, and,
particularly in
conditions of increased humidity, will begin growth and division at a
logarithmic rate.
In order to adhere to surfaces, bacteria produce extracellular polymers which
not
only serve to attach and protect the bacteria, but also function to trap
moisture. The
network of extracellular polymers also serves to trap viruses and dirt
particles and
support growth of fungi.

In very enclosed conditions, such as a space capsule or station, this
bacterial
growth is very significant. Humans are crowded into a very small unventilated
area.
Added to the normal shedding of bacteria are the following problems: reduced
immune system efficiency as indicated by a seven-fold increase in shedding of
the
Epstein-Barr virus and presumed increased bacterial load caused by space-
sickness and the generally poor ability to maintain normal hygiene levels.
This is
further indicated by the bad smell associated with such vehicles. Astronauts
control
biofilm build-up by wiping accessible areas with antiseptic cloths, but
biofilms will
build up in the inaccessible areas, and become so thick and unstable that the
film


CA 02402653 2002-09-26
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sloughs off and small particles of biofilm float through the capsule and are
inhaled
by the astronauts causing negative effects on astronaut health.

The same conditions also apply although to a lesser degree in aeroplanes,
busses,
mobile homes, caravans, cars, and yachts. Especially in aeroplanes flying at
high
altitude the possibilities for exchanging air with the surroundings are very
limited due
to the low oxygen tension at high altitude. Most of the air in aeroplanes is
re-
circulated and thus during long flights, the germ count in the air constantly
increases
and biofilm may build up, especially in the ventilation systems and on contact
surfaces.

In ventilation systems, particularly in public buildings (sick building
syndrome),
hotels (legionnaires disease), hospitals and aeroplanes, the growth of
biofilms is
also associated with the transfer of disease. Thick bacterial mats can trap
viruses,
and as the mats become unstable and break up, particles of biofilm travel
through
the ventilation systems and are inhaled by others. Ventilation systems are
generally
not painted, and the current cleaning practise, physical removal of biofilm by
abrasion and cleaning compounds when health problems or legislation dictate
are
generally not sufficient. To many cleaning companies, cleaning of ventilation
systems is considered to be extremely hazardous because of the extremely high
bacteria and virus load, with extreme clothing and respiration protection
afforded to
workers.

Ventilation systems are believed to be associated with the spread of disease
in:
public buildings (hospitals, hospices, nursing homes, offices, hotels,
schools,
universities, sports facilities), private homes and transport vehicles
(aeroplanes,
submarines, ships, trains, busses) and buildings enclosing animals for human
use or
consumption, such as rabbits, mink, furred animals, poultry, goats, pigs,
sheep,
cattle, horses etc.
In hospitals and other medical care facilities, biofilms are believed to be a
factor
responsible for the spread of disease. Bacteria, which may be antibiotic
resistant,
cover the surfaces of wards, operating theatres etc , as well as being
transferred
through the ventilation system. Current cleaning practises are insufficient to
prevent


P 566 DKOO CA 02402653 2002-09-26
3
deaths due to drug resistant bacteria which readily infect patients due to
their
weakened state.

Biofilms are also readily found on most surfaces exposed to air and moisture.
Considered particularly risky are: public toilets, walls in all health care
institutions
(hospitals, hospices, nursing homes), walls in all public buildings
(hospitals,
hospices, nursing homes, offices, hotels, schools, nurseries, universities,
sports
facilities), surfaces in public transport vehicles (aeroplanes, submarines,
ships,
trains, busses), enclosures for farm animals also slaughterhouses, dairies,
abattoirs,
food preparation facilities and private homes. Current remediation practises
(cleaning products) do not control the health problems caused by biofilms, and
in
some cases may result in the generation of resistant bacteria due to
incomplete
disfection.

Generally in the case of most of the mentioned surfaces government regulations
require that the materials used fulfil certain requirement with relation to
flame
retardancy.

Generally in the art it is known to add enzymes to water based paints to
inhibit the
growth of microorganisms before the paint is applied to a surface. One group
of
examples of such compositions are disclosed in WO 00/68324 (Novo Nordisk AS).
However no reference is made to inhibiting the formation of biofilm on a
surface
coated with such a water based paint.

Enzyme base systems are also known that are capable of inhibiting biofilm
formation in coated surfaces permanently in contact with an aqueous
environment.
One example is a hexose oxidase based paint disclosed in WO 00/75293
(Danisco).
The disclosure mentions coating of the hull of a marine vessel as a possible
use of
the paint.
Another example of an enzyme based paint adapted for coating the hull of a
marine
vessel is disclosed in US 6,150,146 (Nippon Paint). The enzymes used in that
particular disclosure are lipase which releases butyric acid from tributyrin,
and
cholesterol oxidase which releases hydrogen peroxide through oxidation of
cholesterol.


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However the prior art does not teach that any of these paints are capable of
inhibiting biofilm formation, when the surface is not permanently in contact
with
water such as surfaces in enclosed environments. Furthermore, the prior art
does
not teach a paint which is simultaneously capable of inhibiting biofilm
formation and
possesses flame retarding properties.

Summary
According to a first aspect the invention relates to a coating composition
comprising
i. a surface coating material,
ii. at least a first enzyme, and
iii. at least one flame retarding compound,

wherein said first enzyme is capable of directly and/or indirectly inhibiting
attachment and/or growth of microorganisms when exposed to moisture after
applying said coating composition to a surface and allowing it to form a film.

By combining an enzyme based antimicrobial system with flame retardency, which
preferably conforms with fire regulations for public buildings and/or vehicles
it is
possible not only to inhibit the formation of biofilm but also to retard
flames.
Preferably, both the enzyme based system for inhibiting biofilm formation and
the
flame retardency system are not based on release of toxic fumes. This makes
the
composition especially adapted for used in an enclosed environment.
Ventilation systems present a particular problem in the present context.
Ventilation
shafts are normally non-coated and biofilms therefore form easily on the
surfaces of
these. Coating the surfaces of ventilation shafts with an antiseptic coating
solves or
reduces the problem of biofilm formation and the associated spread of
infectious
diseases and allergens. However, ventilation shafts also present a fire
hazard, since
fires often spread in buildings, ships and aircrafts through the ventilation
systems.
The coating compositions according to the present invention solve both
problems by
providing a coating, which reduces or eliminates biofilm formation and by
making
said coating composition flame retardant to reduce the fire hazard.


P 566 DKOO CA 02402653 2002-09-26
The at least one flame retardant compound may either be one that is added to
the
coating composition or the binder may be flame retardant in itself by being
essentially non-combustible at elevated temperatures.

5 According to a further aspect the invention relates to a coating composition
comprising
i. a surface coating material,
ii. at least a first enzyme, and
iii. at least one antimicrobial compound,
wherein said first enzyme is capable of directly and/or indirectly inhibiting
attachment and/or growth of microorganisms when exposed to moisture after
applying said coating composition to a surface and allowing it to form a film.

The inventive coating composition comprises both a passive system
(antimicrobial
compound) and an active system (the enzyme system) which are both directed to
inhibition of biofilm formation on the coated surfaces. The enzyme based
system is
"activated" by exposure to elevated moisture levels such as a relative
humidity
above 50%. Most microorganisms require the presence of a certain amount of
moisture to sustain growth; therefore it is only relevant to inhibit
attachment and/or
growth of the microorganisms when moisture levels increase.

Basically there are two different ways of inhibiting growth and/or attachment
of
microorganisms via an enzyme based system. Firstly, the enzyme can produce a
product, which has antimicrobial activity. Secondly the enzyme may be chosen
so
that it degrades compounds in the extracellular matrix of the microorganisms
such
as polysaccharides thereby predominantly inhibiting the attachment of the
microorganisms. A further enhancement of action may be obtained by including
an
enzyme which degrades substrates that the microorganisms metabolise and thus
"starve" the microorganisms.

According to a further aspect the invention relates to the use of a
composition
according to the invention, in particular for coating surfaces.


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By using the compositions according to the invention for coating surfaces,
biofilm
formation can be reduced or even eliminated while the risk that the coated
surfaces
catch or spread fire is reduced to a minimum due to the flame retardency.

According to a still further aspect the invention relates to a method for
controlling
growth of microorganisms on coated surfaces comprising

applying to a surface a coating composition comprising a surface coating
material,
at least one enzyme, and a substrate for said enzyme,
allowing said coating composition to form a film,

whereby said coating composition upon subsequent exposure to moisture levels
above 50% releases an antimicrobially effective amount of an antimicrobially
active
compound as a consequence of a conversion of said substrate through said
enzyme.

According to this aspect of the invention, it is possible to control biofilm
formation on
surfaces which are exposed to air. Known enzyme based antiseptic coating
compositions are designed for use on surfaces, which are more or less
permanently
in contact with water, such as the hull of a ship. In these cases the presence
of
water ensures that the enzymes are continuously active. On surfaces exposed to
air, the problems are very different.

By the method according to the invention, the at least one enzyme contained in
the
coating composition is automatically activated when moisture raises and
produces
an antimicrobially effective amount of a compound, which inhibits growth of
the
microorganism. Biofilm formation on such surfaces is mostly only a problem
when
the ambient humidity raises above a certain level.
According to a further aspect the invention relates to a method for
controlling growth
of microorganisms on coated surfaces comprising

applying to a surface a coating composition comprising a surface coating
material,
at least one enzyme,


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allowing said coating composition to form a film,

whereby said coating composition upon subsequent exposure to moisture levels
above 50% (RH) inhibits attachment of at least one species of microorganism as
a
consequence of a the action of said enzyme.

According to this aspect of the invention, it is possible to control biofilm
formation on
surfaces which are exposed to air. By the method according to the invention,
the at
least one enzyme contained in the coating composition is automatically
activated
when moisture raises and produces an antimicrobially effective amount of a
compound, which inhibits attachment of the microorganism, e.g. by degrading
compounds in the attachment matrix. Biofilrn formation on such surfaces is
mostly
only a problem when the ambient humidity raises above a certain level.
Definitions
The term "antiseptic" as used herein refers to the action of inhibiting
bacterial or
fungal or mycoplama growth on surfaces to the extent that it inhibits biofilm
formation.

The term "biofilm" used herein refers to the growth of bacteria that occurs on
surfaces exposed to living organisms especially where there is a high ambient
humidity. This bacterial growth if unchecked, results in the production of
extracellular
polymers which in turn create a water retaining matrix that supports fungi and
algae
as well as trapping viruses and air-borne particles.

The term "coating" as used herein in a preferred embodiment relates
specifically to
water-borne silicones, but generally does not exclude polyurethanes,
silicones,
epoxides, alkyds, latex vinyls, acrylics etc:. either water or solvent based,
1 or 2
component, so long as it conforms to the safety regulations for the purpose
for
which it is intended.

The term "surface" as used herein relates to any surface that may be covered
by a
biofilm, specifically, but not limited to: space ship interiors, ventilation
systems,


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medical care facility interiors, public building interiors, pulp mills, sports
facility
interiors, public transport interiors such as aeroplanes, ambulances, and
busses,
cars, mobile homes, caravans, private homes, ship interiors, abattoirs,
slaughterhouses food preparation facilities, dairies, and animal housing.
The term "moisture" as used herein refers to the moisture level as indicated
by the
relative humidity (RH).

The term "biocide" as used herein refers to a compound capable of inhibiting
the
growth of a microorganism and/or inhibiting the attachment of a microorganism
to a
surface.

The term "enzymes" as used herein refers specifically, but is not limited to
amylases
and oxidases, and can include oxidoreductases and hydrolytic enzymes as well
as
other enzymes including but not limited to oxidase, laccase, peroxidase,
haloperoxidase, amylase, lipidase, esterase, deaminase, urease, polysaccharide
hydrolase.

The term "accelerator" as used herein refers specifically to iodide salts, but
may also
include metal salts and thiocyanate ion further enhancing the action of
enzymes and
enzyme products.

The term "substrate" as used herein in connection with enzymes refers
preferably to
inulin or other fructans, but could include starches or other carbohydrates.
The term "flame retardancy" as used herein refers to compounds which act by
removing or replacing oxygen and so to stop combustion, e.g. by release of
halogen
gas or water vapour. Alternatively the coating may be non-flammable or non-
combustible in itself. The flame retardant may either be a compound that is
added to
the coating composition or it may be the binder, which is in effect non-
combustible.
Detailed description

Accordingly it is an object of the invention to provide improved methods for
controlling the growth of microorganisms, in particular the formation of
biofilms in


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enclosed habitats, ventilation systems etc.. For example, it is desired to
create a
coating that will inhibit the development of biofilms by controlled release of
an
environmentally friendly bioactive compound that does not accumulate in the
surroundings and cause discomfort.
It is desired to create a coating that contains or generates an antimicrobial
compound (e.g. H202) such that when humidity is elevated, the water film on
the
overlying surface is disinfected without causing build up of toxic fumes (e.g.
H202
breaking down into H2O and 02).
It is desired that the generation of H2O2 should ideally be reasonably
constant over a
period of 1 or more years depending on the intended use. It is therefore the
object of
the invention to combine the components of the composition in such a way as to
support this. For example, it is an object of this invention to select enzymes
whose
activity is in some way controlled by the presence of moisture and oxygen in
order to
control the activity of the enzymes.

It is an object of this invention that the generation of the antiseptic
compound (e.g
H202) is high enough to control bacterial growth over the working life of the
coating.
For example the level of H202 in a surface film preferably is >5mM, depending
on
the aggressiveness of the environment.

It is a further object of the invention that the coating should also conform
to fire
regulations for public buildings, but should also be possible to avoid flame
control by
release of toxic fumes where the coating is required for used in enclosed
environments (e.g. by using a water based silicone binder).

It is a further object of the invention that the coating or variations of the
coating
should be suitable for application on all typical surface materials (e.g. by
using a
water based silicone binder).

It is an object of the invention that the coating be safe for use in domestic
environments, i.e. the antiseptic ingredient for coatings exposed to humans
should
be non-toxic.


P 566 DKOO CA 02402653 2002-09-26
In accordance with these objectives there has been provided in accordance with
one
embodiment of the present invention a coating composition that includes an
example of an enzyme modulated generation of H202 over a 3 year working life,
preferably over a 3+ year working life, in a water based silicone system to
produce a
5 coating that has non-toxic antiseptic properties as well as non-toxic fire
retardant
properties.

Binder
10 The coating composition is based on a binder which determines the physical
properties and chemical resistance of the cured/dried film. The binder type or
possible binder types do not limit the effectiveness of the invention. Thus
the binder
may be of an oil-based type in an organic solvent or it may be a binder, which
is
dissolved or dispersed in water to reduce the requirements for VOCs (volatile
organic compounds).

The antimicrobial coating in question may be based on any type of binder
system,
including but not limited to such as epoxy, alkyd, acrylic, vinyl, urethane,
latex,
modified rubber, silicone, may be paint, lacquer, varnish or spray, and may be
applied using methods known to the art such as brush, roller, air-spray and
airless
spray.

The coatings may be water-borne or solvent-borne, but one particularly
preferred
embodiment is a water-borne silicone.
Preferably the binder is a binder, which is dissolved or dispersed in water
because
these binders are more environmentally friendly and because there is a great
demand in industry for such binders.

The binder may thus comprise a modified rosin such as rosin maleic acid or
gloss
oil. Alternatively the binder comprises a shellac, such as French polish.

Further examples of binder include but are not limited to an oxidised rubber,
a
water-based styrene butadiene latex system, a water based styrene acrylic, a
chlorinated polyolefin, a modified water-borne silicone,


CA 02402653 2002-09-26
P 566 DKOO
11
Among these the mostly preferred binder is the modified water-based silicone
binder, this being a naturally flame retardant binder.

Further examples of binder include modified sucrose, water-borne
polyvinylidene,
chloride based latex terpopolymers, vinyl acetate, polyvinyl alcohol,
polivinyl acetals,
vinylidene fluoride, polyurethanes, epoxides, water-soluble acrylics.

Preferably the binder and the other constituents of the coating composition do
not
do not inhibit the activity of the enzyme.

Anti-microbial compounds

The coating composition may comprise an additional antimicrobial such as a
biocide, although it is preferred that the coating does not contain a biocide.
When
the coating composition comprises an antimicrobial compound in addition to the
enzyme system this is preferably selected from the group consisting of: oxides
of
heavy metals, such as zinc oxide; organic compounds such as organic biocides
such as citrus oil, chilli oil, herbanero extract, cranberry extract, seaweed
extract
(e.g. from Gigartina stellata); non-leaching biocides such as 2,4,4-trichloro-
2-
hydroxy-diphenyl ether, 5-chloro-2-phenol; polyvalent carbohydrate molecules
such
as polyvalent glycosylated casein; class V metals such as bismuth; carbamates
with
diethanolamide as a potentiator.

Other examples of suitable biocides comprise oils selected from the group
consisting of vetiver oil, camphor oil, ceder oil, tea-tree oil. Still further
examples
include naturally occurring anti-bacterial compound selected from the group
consisting of honey, natural tree resins, preferably from pine trees or Elemi;
Copal;
Dammar. Furthermore compounds such as sodium fluoride and/or dodecylamine
and/or tricolsan and/or chlorhexidine may be added to the coating composition
according to the invention to act as antimicrobial compounds.

Still further examples of anti-microbial compounds include: an anti-microbial
salt
selected from the group consisting of iodide salts and/or metal salts, cupric
chloride,


P 566 DKOO CA 02402653 2002-09-26
12
cupric sulphate, silver nitrate, colloidal bismuth subcitrate, bismuth
citrate,
aluminium phosphate, aluminium hydroxide hydrate, gold chloride.

Preferably the antimicrobial compound comprises silver nitrate or a cupric
salt,
except in the case of acrylate based binders, which interfere negatively with
the
presence of such metals.

The amount of antimicrobial compound preferably is less than 40 % (w/v), such
as
less than 35%, more preferably less than 30 %, such as less than 25%, more
preferably less than 20%, such as less than 15%, more preferably less than
10%,
such as less than 7.5%, more preferably less than 5%, such as less than 4%,
less
than 3%, less than 2%, less than 1 %, or less than 0.5%.

Flame retardant
For this invention the coating also possesses non-toxic flame retarding/fire
resistant
properties. Flame resistance my be intrinsic to the binder system (silicones)
or
afforded through addition of macroplegmatic or other flame/fire resistant
compounds.
The at least one flame retardant compound is preferably selected from the
group
comprising: macroplegmatic compounds (for example as described in WO
98/03228); a flame retarding mixture comprising malamine cyanurate, silica,
and
phosphoric acid (as described in US 5,852,082); a flame retarding mixture
comprising sodium carbonate, pyrophosphate, ammonium salts, boric acid,
phosphoric acid (as described in US 6,066,198); a halogen-based flame
retardant
such as organic chlorine compounds, organic bromide compounds such as
brominated aromatic bisimide compounds, brominated aromatic epoxy compounds,
brominated polycarbonates, brominated benzyl arcylates, brominated
polystyrene;
phosphorous based flame retardents such as phosphate salts, phosphate esters,
nitrogen containing phosphorous compounds and red phosphorous; inorganic flame
retardents such as zinc borate ammonium borate, ammonium sulphamate,
ammonium bromide etc;


P 566 DKOO CA 02402653 2002-09-26
13
To further enhance flame-retardancy one or more oxides of antimony; sodium
antimonate; aluminium or magnesium hydroxide can be added to the coating
composition.

When the coating composition according to the invention is to be used in an
enclosed environment the flame retardency system should not be based on the
release of toxic fumes. One example of a preferred system for such enclosed
environments include a water based silicone binder or a composition comprising
a
macroplegmatic flame retardant or non-flammable compositions.
Flame retardents typically work by removing or replacing oxygen and so
stopping
combustion. In halide containing (5-25% by weight) paints, extreme heat breaks
down the coating releasing halogen gas which replaces oxygen at the surface
and
stops combustion. Macroplegmatic coatings contain high amounts of molecular
water which is released under conditions of extreme heat, replacing oxygen and
stopping combustion. Other coatings, such as a water based silicone binder,
require temperatures so far in excess of what could be experienced in a normal
fire
(e.g., they can withstand the heat from rocket exhausts) that they are, for
the
purpose intended, non-flammable/non-combustible. Finally, a coating
composition
may be rendered flame retardant by adding non-combustible filler, such as
clay,
silicon or glass.

The composition according to the present invention may comprise from 1 to 50%
(w/v) of flame retardant, preferably from 5 to 25%, such as from 5-10%, from
10-
15%, from 15-20%, or from 20-25%. When the flame retardancy is caused by the
binder, this may constitute up to 75% (w/v) of the coating composition, such
as up to
70 %, for example up to 65%, such as up to 60 %, for example up to 55 %, such
as
up to 50%, for example up to 45 %, such as up to 40%, for example up to 35%,
such
as up to 30%, for example up to 25%.
Preferably the compositions conform with fire regulations for public buildings
and/or
vehicles and/or ships.

Further additives


P 566 DKOO CA 02402653 2002-09-26
14
The coating composition may preferably further comprise pigments, fillers
additives
and solvents as mentioned in the examples (see below).

Apart from these additives, the composition may further comprise fibres such
as
cellulosic fibres. One purpose of adding fibres may be to increase the
physical
strength of the paint film. Another purpose may be to act as an "anchor" for
the
enzymes so that they do not migrate through the paint. A third purpose may be
to
act as substrates for the enzymes, such as may be the case when using
cellulosic
fibres for a coating comprising a cellulase. A further purpose of fibres may
be to give
a wall paint the desired texture.

Preferably the enzyme and/or substrate and/or a biocide is/are bound to said
fibres.
One effect of anchoring an enzyme to a fibre may be to (i) improve dispersion
of the
enzyme in the paint and/or to (ii) prevent migration of the enzyme through the
paint
(iii) and/or to increase the amount of substrate to increase performance
lifetime
(e.g., substrate added as filler and fibres), and/or (iv) one may possibly use
fibres to
control release of an organic biocide.

Malodour
Malodour is associated with certain compounds, such as sulphur containing
compounds, and short free fatty acids such as butyric acid. These are often
generated by micro-organisms growing on the surfaces of walls or by deposition
from the air (e.g. in kitchens). Different types of enzymes (peroxidases,
lipases,
proteinases, oxidoreductases), can be selected to breakdown the different
types of
compounds and reduce smell.

Hydrogen peroxide

In one preferred embodiment, the enzyme action results in the generation of
hydrogen peroxide, where the antimicrobial action may the result of H2O2
acting on
an enhancer such as thiocyanate, or alone. H2O2 may be generated for example
through the action of peroxidases, such as lactoperoxidase &/or of oxidases
such
alcohol oxidase; amine oxidase; arylalcohol oxidase; aspartate oxidase;
cholesterol
oxidase; D-amino acid oxidase; D-glutamate oxidase; ethanolamine oxidase;


P 566 DKOO CA 02402653 2002-09-26
glucose oxidase; galactose oxidase; hexose oxidase; L-amino acid oxidase;
lathosterol oxidase; malate oxidase; NADH oxidase; pyranose oxidase;
superoxide
dismutase; urate oxidase and so forth.

5 Hydrogen peroxide is produced through the action of an enzyme/enzymes on a
substrate. The substrates are not limited to, but can include:
carbohydrate/sugars,
cellulose, dextran, hexoses, galactose, glucose, lactose, 2-deoxyglucose,
fructose,
pyranose, pectin, inulin, starch or mixtures thereof. In one preferred
embodiment the
enzyme is hexose oxidase acting on glucose.
According to an especially preferred embodiment of the invention hydrogen
peroxide
is generated in an amount to prevent biofilm formation on the surface of the
composition. The advantages of enzyme systems based on hydrogen peroxide are
several. Hydrogen peroxide is highly reactive and therefore has a very short
half-life
in the presence of water, spontaneously degrading into water and oxygen.
Therefore
the compound is non-toxic and does not accumulate in the environment.
Furthermore hydrogen peroxide released from the surface coating may assist in
fighting unpleasant odours.

A high level of peroxide may also help by killing the bacteria whose activity
releases
smelly by-products (e.g., ammonia)

Preferably the composition and the enzyme system are adapted to produce at
least
5mM hydrogen peroxide in an overlying water film.
The enzymes and substrates should be added in an amount to ensure effective
prevention of biofilm formation for at least 1 year, preferably at least 2
years, more
preferably at least 3 years, such as at least 4 years, for example at least 5
years,
such as at least 6 years, for example at least 7 years, such as at least 8
years, for
example at least 9 years, such as at least 10 years.

Control of enzyme action

There are various ways of controlling the action of the at least one enzyme
contained in the coating composition. Examples include having the enzyme


P 566 DKOO CA 02402653 2002-09-26
16
activated by changes in ambient humidity and/or ambient temperature and/or
ambient pH and/or ambient oxygen levels.

By far the most preferred control system is simply control through increases
in
moisture level. It is to be understood that at least one enzyme may have an
activity
sufficient to inhibit biofilm formation, when ambient humidity is above 40%,
such as
above 45%, for example above 50%, such as above 55%, for example above 60%,
such as above 65%, for example above 70%, such as above 75%, for example
above 80%, such as above 85%, for example above 90%, such as above 95%.
Surprisingly, it has turned out that the enzymes in the compositions according
to the
present invention are active and effective even in the absence of a visible
water film
on the coated surfaces.

Preferably the enzymes are active in the temperature interval between 5-40 C,
such
as 5-10 C, 10-15 C, 15-20 C, 20-25 C, 25-30 C, 30-35 C, or 35-40 C.

The at least one enzyme may have an optimum in the interval between pH 4 and
11,
such as an optimum in the interval of pH 4-5, pH 5-6, pH 6-7, pH 7-8, pH 8-9,
pH 9-
10, pH 10-11. pH varies from paint to paint, tending to the acidic. The pH
optimum of
amylases tends to be acidic to neutral (e.g., 3.5 7.0) but amylases can be
active at
high pH's e.g., > 8. The pH optimum of oxidases depends on source. Hexose
oxidase from marine sources typically has an optimum around 8 and has been
shown to demonstrate adequate activity around pH 7, however glucose/glucose
oxidase (fungal) generating hydrogen peroxide has been shown to work between
pH
5 and 7.

Similarly, the at least one enzyme may have an optimum at 50-100 % oxygen
saturation.

Enzyme requirements

Preferably the at least one enzyme does not lose substantial activity when
repeatedly hydrated and de-hydrated. By absence of substantial loss of
activity is
meant a loss in activity after which the enzyme is still capable of preventing
biofilm
formation, such as a loss smaller than 90% compared to the initial activity,


P 566 DKOO CA 02402653 2002-09-26
17
preferably a loss smaller than 80 %, more preferably a loss smaller than 75%,
such
as smaller than 70%, for example smaller than 60%, such as smaller than 50%,
for
example smaller than 45%, such as smaller than 40%, for example smaller than
35%, such as smaller than 30%, for example smaller than 25%, such as smaller
than 20%, for example smaller than 15%, such as smaller than 10%, for example
smaller than 5%.

Preferably the at least one enzyme does not lose substantial activity when
dried to
below 20% moisture content and rehydrated again, preferably below 19%, such as
below 18%, for example below 17%, such as below 16%, for example below 15%,
such as below 14%, for example below 13%, such as below 12%, for example
below 11%, such as below 10%, for example below 9%, such as below 8%, for
example below 7%, such as below 6 %, for example below 5%, such as below 4%,
for example below 3%, such as below 2%, such as below 1.5%, for example below
1 %. This compares with the typical moisture content of a dried coating which
is in
the vicinity of 2-7%.

Enzymes
The antimicrobial activity may be the result of one or more enzymes, acting
independently (e.g., one-step: glucose/hexose oxidase; glucose/glucose
oxidase, L
amino acid/L amino acid oxidase, galactose/galactose oxidase, 2-
deoxyglucose/glucose oxidase, pyranose/pyranose oxidase and mixtures thereof,
or, cocktails of proteases, amylases, lipases, cutinases, cellulases etc..) or
step-
wise (the substrate for one enzyme is produced by the action of a precursor
enzyme
acting on substrates selected from polymers and oligomers of substrates for
oxidative enzymes such as: Starch, cellulose, dextrose, lactose, peptide,
inulin &
mixtures thereof).

The enzymes may act directly, to prevent attachment by bacteria, fungi or
algal
spores, or act by generating an antimicrobial compound such as hydrogen
peroxide.
The enzymes in question may be derived from microbial, plant or animal sources
and may be naturally occurring or modified and should be commercially
available.
Preferably, the enzymes are available for use for the food and beverage
industry.


CA 02402653 2009-07-31

The enzymes should ideally have at least 80% of optimal activity within
typical
accommodation temperatures, possibly 10 to 40 C, more ideally between 15 to
30 `C,
or more preferably between 20 and 25 C. But not be destroyed after
application by brief
exposure to temperatures between 1 and 50 'C. The enzymes should have within
80%
of optimal activity with the pH conditions experienced with the coating, such
that for
alkaline coatings, the optimal activity is between 7 and 12, whereas for more
acid
coatings, the pH optimum is between 4 and 7.

The enzymes may be added directly, or may be immobilized by spray coating on
fillers,
substrates, fibres, ceramic particles, glass particles or spheres, pigments or
thixotropic
agents; or may be immobilized in gels/capsules and may be added as part of a 1-

component or multi-component coating.

The enzymes may be the sole source of antimicrobial properties or may work in
conjunction with antimicrobial polymers such as polysiloxanes with propyl
pendant
groups or antimicrobial compounds, such as cranberry extract (US 6,210,681) or
other
antimicrobial compounds mentioned above.

Enzymes suitable for use according to the present invention include but are
not limited to
oxidases, and can include oxidoreductases and hydrolytic enzymes, laccases,
peroxidases, haloperoxidases, amylases, lipidases, esterases, deaminases,
ureases,
polysaccharide hydrolases, and nucleases.

Oxidoreductases
The oxidoreductase in the context of the present invention may be any
oxidoreductase
or combination of different oxidoreductases or combination of oxidoreductases
with other
enzymes. Accordingly, when reference is made to "an oxidoreductase " this will
in
general be understood to include combinations of one or more oxidoreductases.
It is to be understood that oxidoreductase variants (produced, for example, by
recombinant techniques) are included within the meaning of the term
"oxidoreductase".
18
SUBSTITUTE SHEET


P 566 DKOO CA 02402653 2002-09-26
19
The enzyme classification employed in the present specification with claims is
in
accordance with Recommendations (1992) of the Nomenclature Committee of the
International Union of Biochemistry and Molecular Biology, Academic Press,
Inc.,
1992.

Accordingly, the types of oxidoreductases which may appropriately be applied
for
the present invention include oxidoreductases (EC 1.-.-.-).

Preferred oxidoreductases in the context of the invention are any peroxidase
belonging to the classification group EC 1. 11. 1--, any laccase belonging to
EC
1.10.3.2, any catechol oxidase belonging to EC 1.10.3.1, any bilirubin oxidase
belonging to EC 1.3.3.5 or any monophenol monooxygenase belonging to EC
1.14.99.1 or any oxidases belonging to EC 1.1.3.-.
Laccase and laccase related enzymes

Preferred laccase enzymes and/or laccase related enzymes are enzymes of
microbial origin. The enzymes may be derived from plants, bacteria or fungi
(including filamentous fungi and yeasts).

Peroxidases and Compounds possessing Peroxidase Activity

Compounds possessing peroxidase activity may be any peroxidase enzyme
comprised by the enzyme classification (EC 1.11.1.7), or any fragment derived
therefrom, exhibiting peroxidase activity. In the context of this invention,
compounds
possessing peroxidase activity comprise peroxidase enzymes and peroxidase
active
fragments derived from cytochromes, haemoglobin or peroxidase enzymes.

Preferably, the peroxidase employed in the method of the invention is
producible by
plants (e. g. horseradish or soybean peroxidase) or microorganisms such as
fungi or
bacteria.

Also haloperoxidases such as chromo-, bromo-and/or iodoperoxidases are
suitable
for controlling biofilm formation according to the present invention.
Haloperoxidases


P 566 DKOO CA 02402653 2002-09-26
form a class of enzymes which are able to oxidize halides (Cl-, Br-, I-) in
the
presence of hydrogen peroxide or a hydrogen peroxide generating system to the
corresponding hypohalous acids according to: H202 + X-+ H+-- > H2O 4- HOX,
wherein X-is a halide and HOX is a hypohalous acid. If a convenient
nucleophilic
5 acceptor is present, a reaction will occur with HOX and a halogenated
compound
will be formed.

There are three types of haloperoxidases, classified according to their
specificity for
halide ions: Chloroperoxidases (E. C. 1.11.1.10) which catalyse formation of
hypo-
10 chlorit from chloride ions, hypo-bromit from bromide ions and hypo-iodit
from iodide
ions; Bromoperoxidases which catalyse formation of hypo-bromit from bromide
ions
and hypoiodit from iodide ions; and iodoperoxidases (E. C. 1.11.1.8) which
solely
catalyze the formation of hypoiodit from iodide ions. However, hypoiodit
undergoes
spontanous disproportionation to iodine and thus, iodine is usually the
observed
15 product of the reaction. These hypo-halit compounds may subsequently react
with
other compounds forming halogenated compounds.

Haloperoxidases have been isolated from various organisms: mammals, marine
animals, plants, algae, a lichen, fungi and bacteria. It is generally accepted
that
20 haloperoxidases are the enzymes responsible for the formation of
halogenated
compounds in nature, although other enzymes may be involved.

Haloperoxidases have been isolated from many different fungi, in particular
from the
fungus group dematiaceous hyphomycetes, such as Caldariornyces, e. g., C.
fumago, Alternaria, Curvularia, e. g., C. verruculosa and C. inaequalis,
Drechslera,
Ulocladium and Botrytis (see US Patent No. 4,937,192).

Another particularly preferred enzyme is hexose oxidase (D-hexose: 02-
oxidoreductase, EC 1.1.3.5), which catalyses the oxidation of D-glucose or D-
galactose to y-D-gluconolactone or y-D-galactolactone and hydrogen peroxide.

Specific examples of combinations of enzyme and substrate include but are not
limited to: malate oxidase-malic acid; glucose oxidase-glucose; hexose oxidase-

glucose; cholesterol oxidase-cholesterol; arylalcohol oxidase-arylalcohol:
galactose
oxidase-galactose; alcohol oxidase-alcohol; lathosterol oxidase-lathosterol;


P 566 DKOO CA 02402653 2002-09-26
21
aspartate oxidase-aspartic acid; L-amino-acid oxidase-L-amino acid; D-arnino-
acid
oxidase-D-amino acid; amine oxidase-amine; D-glutamate oxidase-glutamine;
ethanolamine oxidase-ethanolamine; NADH oxidase-NADH.; urate oxidase
(uricase)-uric acid; superoxide dismutase-superoxide radical; glucose/hexose
oxidase; glucose/glucose oxidase; L amino acid/L amino acid oxidase;
galactose/galactose oxidase; lactose/P-galactosidase/hexose oxidase; lactose/ -

galactosidase/glucose oxidase; 2-deoxyglucose/glucose oxidase;
pyranose/pyranose oxidase; and mixtures thereof.

The coating composition may comprise at least 0.0001 % (w/v) of enzyme, such
as
at least 0.001 %, for example at least 0.01 % such as at least 0.05, for
example at
least 0.1%, such as at least 0.5%, such as at least 1%, for example at least
1.5%,
such as at least 2%, for example at least 2.5%, such as at least 3%, for
example at
least 3.5%, such as at least 4%, for example at least 4.5%, such as at least
5%.
According to a further embodiment of the invention, the coating composition
comprises a second enzyme capable of converting a compound into a substrate
for
the first enzyme. Generally speaking the second enzyme will often be one that
is
capable of degrading a naturally occurring polymer (polysaccharide, lignin,
protein,
polyphenol etc.) into its monomer constituents. The second enzyme may be an
amylase, which converts starch into a substrate for a hexose oxidase or a
cellulase,
which converts cellulose into a substrate for a hexose oxidase, or a fructase,
which
converts a fructan such as inulin into hexoses, or a proteinase which converts
protein into amino acids, or a ligninase which converts lignin into monomers.
According to another embodiment, the composition may comprises at least a
third
enzyme, such as at least a fourth enzyme, such as at least a fifth enzyme. One
example of combinations of enzymes, which interact to improve the antiseptic
effect
of the coating composition is the combination of a proteinase, a lipase and an
amylase and/or an oxidase, which together may prevent the microorganisms from
attaching to the surfaces by degrading their attachment matrix, or which
degrade the
substrates the microorganisms can use for metabolism, such as short fatty
acids or
sulphur containing compounds.


P 566 DKOO CA 02402653 2002-09-26
22
The enzymes and substrates may simply be dissolved or dispersed in the coating
composition, but the may also preferably be encapsulated such as being
Oencapsulated in mesoporous silicates. By encapsulating the enzymes and
substrates you may control the movement of the enzyme (migration) andior may
control the activity of the enzyme by controlling access to active sites.

Uses
The coating compositions according to the present invention may be used for
coating any type of surface which is exposed to micro-organisms. An especially
preferred use is for coating surfaces in enclosed habits such as a spacecraft.
The
humidity levels in spacecrafts are high because the possibilities for
ventilation are
very limited. By providing the walls of the spacecrafts with a composition
according
to the invention, the formation of biofilm can be prevented, the need for
wiping walls
can be greatly reduced and the general health of the astronauts and cosmonauts
can be improved.

Another preferred use is for coating surfaces in ventilation systems. Such
surfaces
are normally inaccessible for cleaning and great saving are expected by
employing
the coating compositions according to the invention for such surfaces.
Important is
also the flame retardancy features of the compositions according to the
present
invention, since fires often spread through ventilation systems in buildings
and in
aeroplanes.

A further preferred use is for coating surfaces in medical and other health
care
systems such as operating theatres. The hygiene requirements.of such surfaces
are
very high and fire regulations also require that the coatings be flame
retardant. It is
of course possible to design the coating compositions to have stronger or
weaker
"anti-biofilm" action through adjustments of the concentrations of the
constituents. In
this way coating compositions especially adapted for surfaces in medical and
other
health care systems such as operating theatres can be made.

Generally the coating compositions according to the present invention are very
suitable for coating surfaces in public buildings and in buildings with high
hygiene
requirements and fire regulations. Such buildings include but are not limited
to


P 566 DK00 CA 02402653 2002-09-26
23
educational facilities, such as universities and schools, sports facilities,
offices, and
public sanitation facilities.

Another type of enclosed environment in which the use of the coating
compositions
according to the present invention is advantageous include vehicles, such as
aircrafts, ship interiors, particularly yachts, busses, mobile homes,
caravans. In
these vehicles the humidity levels are often high due to the presence of a
number of
passengers/patients/inhabitants and the limited possibilities for ventilation
(especially in aircrafts). This produces a high load of microorganisms in the
atmosphere and a potential risk for biofilm formation. In addition to this,
all of these
vehicles possess a high risk for catching fire. The use of the coating
compositions
according to the present invention at least for the interior surfaces of such
vehicles
solves both of these problems at the same time with the possibility of doing
this
without accumulation of toxic fumes.
The advantages of the coating compositions according to the present invention
are
also evident when used for coating surfaces in private homes, preferably in
bathrooms and/or kitchens; as well as when used for coating surfaces in animal
housings such as stables, and including slaughterhouses, abattoirs and food
preparation facilities.

Test of coated surfaces.

Coated panels are incubated at different atmospheric conditions with different
microorganisms. For example, the panels are exposed to wet/dry cycles; carbon
dioxide; and light/dark cycles which imitate the "worst-case-scenario"
condition-wise,
with an axenic innoculum of bacteria, algae, fungi or mixtures thereof.
Screening
tests will identify which formulations inhibit biofilm by examination of the
cultures
growing on the surface. Long-term tests can be done using accelerated ageing,
laboratory testing under controlled conditions and in-situ testing.

Examples
Example 1. Non-toxic antimicrobial, flame retarding water-borne silicone for
various applications


CA 02402653 2009-07-31
Example 1 a

Mix the following

20 parts approx. colloidal silica (e.g., Snowtex TM30 , Nissaq chemical
Industries Ltd.,
with min 30% effective component)

70 parts approx. of the following mixture (approx. 10 parts
dodecylbenzenesulphonic
acid dissolved in approx. 485 parts water, added to a mixture of approx.
500pts
octamethylcyclotetrasiloxane with approx. 5 parts phenyltriethosilane).

Neutralize the mixture with sodium carbonate

Add approx. 1 part of a mixture comprising approx. 30 parts dioctyltin
dilaurate with
approx. 5 parts polyoxyethylene nonyiphenylether;

Add approx. 0.5 parts silatrane D to make a silicone water-based emulsion
composition
To the mixture add: 0.001-200 mg/ml of starch which has been spray applied
with
amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1 AGU produces 1
mmol
glucose/min at 25 C), alternatively add 0.001 to 500 mg of glucose, galactose,
or
fructose/ml mixture 2. Also add 0.002 to 200 mg of starch which has been spray
applied
with hexose oxidase with an activity within 0.001 - 100 U (where 1 U produced
1 mmol
of H2O2/min at 25 C)
Example lb

Mix the following:

20 parts approx. colloidal silica (e.g., Snowtex TM30 , Nissaq chemical
Industries Ltd.,
with min 30% effective component)

70 parts approx. of the following mixture (approx. 10 parts
dodecylbenzenesulphonic
acid dissolved in approx. 485 parts water, added to

24
SUBSTITUTE SHEET


P 566 DKOO CA 02402653 2002-09-26
a mixture of approx. 500pts octamethylcyclotetrasiloxane with approx 5 parts
phenyltriethosilane)

Neutralise the mixture with sodium carbonate
5
Add approx. 1 part of a mixture comprising approx, 30 parts dioctyltin
dilaurate with
approx. 5 parts polyoxyethylene nonylphenylether.

Add approx. 0.5 parts Silatrane D to make a silicone water-based emulsion
10 composition.

To the mixture add a cocktail of enzymes such as:
Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
15 GIST-Brocades ) at the amount of 0.0001 - 0.5 % by weight of mixture 2.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 2,
Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 2.

Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor@,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 2..

Example 2. Non-toxic flame retarding antimicrobial coating for application to
cardboard for use in shanty towns


P 566 DKOO CA 02402653 2002-09-26
26
Fire retarding mixture with a silicone latex rubber binder, such as: a mixture
of the
following (weight percent) 15-20% phosphoric acid or disodic phosphate or
monosodic phosphate or sulphamic acid, 1 - 5% boric acid, 5 .. 10% ammonium
sulphate or ammonium chlorate, 1 - 5% sodium carbonate, 0.1 - 5%
pyrophosphate.
Alternatively, for some applications, phosphoric acid can be excluded and
replaced
by Boric acid.

Mix the following approximate amounts:
44 mis water
21 g phosphoric acid
13 g ammonium sulphate
4 g boric acid
1.4 g sodium carbonate
1 g pyrophosphate

Take 75 g of this mixture (mixture 1) and combine with 25 g silicone rubber
latex
(mixture 2).

To mixture 2 add 0.001 -200 mg/mi of starch which has been spray applied with
amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1 AGU produces
1 mmol glucose/min at 25 C), alternatively add 0.001 to 500mg of glucose,
galactose
or fructose/ml mixture 2. Also add 0.002 to 200mg of starch which has been
spray
applied with hexose oxidase with an activity within 0.001 - 100 U (where 1 U
produced 1 mmol of H2O2/min at 25 C).

Example 2b.

Alternatively to mixture 2 add a cocktail of enzymes such as:
Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapern from
GIST-Brocades ) at the amount of 0.0001 - 0.5% by weight of mixture 2.


CA 02402653 2009-07-31

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from the
fungus Hum icola, strain DSM 1800) at the amount of 0.00001 - 3% by weight of
mixture
2.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano" , AMANO Pharmaceutical Co. Ltd. Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also Lipomax from GIST-
Brocades and Lipolase from Novozymes. Alternatively a mixture of the named
type of
lipases combined with a cutinase at the amount of 0.0001 - 3% by weight of
mixture 2.
Amylase (e.g., a and b amylases such as Purefact Ox Am from Genencor,
Termamyl ,
Ban , Fungamyl and Duramyl from Novozymes) at the amount of 0.0002 - 2% by
weight of mixture 2.

Example 2c for various applications

Mix 75% by weight of mixture 1 with 25% vinyl resin to make a paint additive
(mixture 3)
For one kilo of paint mix 25 g of mixture 3 with 75 g of the following:
10-50% acrylic resin (e.g., Neocry 1727 (Zeneca resins), Synocryl 874 (Cray
Valley),
Acryloid B66 (Rohm & Haas)) or, a vinyl resin solution (e.g., UCAR VAGH ,
UCAR
VYHH , UCAR VMCC (Dow Chemical/Union Carbide), Hostaflex CM150 (Hoechst),
Laroflex MP25 (BASF)).
5 - 40% pigments (e.g., Titanium Dioxide (Ti-Pure R902 , DuPont), iron oxides,
carbon
black, graphite, metallic aluminum, zinc oxide, or other suitable pigments)

5 - 40% fillers (e.g., carbohydrates, zinc oxide, zinc phosphate, clay,
kaolin, silicates,
glass, ceramics (including spheres, fibres & powder), calcium carbonate,
barium
sulphate)

1 - 5% additives (e.g., thixatropic agents, f low control agents)
27
SUBSTITUTE SHEET


P 566 DKOO CA 02402653 2002-09-26
28
0.1 - 90% solvents (e.g., glycol ethers, alcohols, Solvesso 150, toluene,
acetates,
ketones)

To the mixture add 0.001 -200 mg/ml of starch which has been spray applied
with
amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1 AGU produces 1
mmol glucose/min at 25 C), alternatively add 0.001 to 500 mg of glucose,
galactose
or fructose/ml mixture 1. Also add 0.002 to 200 mg of starch which has been
spray
applied with hexose oxidase with an activity within 0.001 - 100 U (where 1 U
produced 1 mmol of H2O2/min at 25 C).

Example 2d

For one kilo of paint mix 25 g of mixture 1 with 75 g of the following:
10-50% acrylic resin (e.g., Neocryl 727 (Zeneca resins), Synocryl 874 (Cray
valley),
Acryloid B66 (Rohm & Haas)) or, a vinyl resin solution (e.g., UCAR VAGH, UCAR
VYHH, UCAR VMCC (Dow Chemical/Union Carbide), Hostaflex CM150 (Hoechst),
Laroflex MP25 (BASF)).
5 - 40% pigments (e.g., Titanium dioxide (Ti-Pure R902, DuPont), iron oxides,
carbon black, graphite, metallic aluminium, zinc oxide or other suitable
pigments)

5 - 40% fillers (e.g., carbohydrates, zinc oxide, zinc phosphate, clay,
kaolin,
silicates, glass, ceramics (including spheres, fibres & powder), calcium
carbonate,
barium sulphate)

1 - 5% additives (e.g., thixatropic agents, flow control agents)

0.1 - 90% solvents (e.g., glycol ethers, alcohols, Solvesso 150, toluene,
acetates,
ketones)

To the mixture add a cocktail of enzymes such as:


P 566 DKOO CA 02402653 2002-09-26
29
Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapern from
GIST-Brocades ) at the amount of 0.0001 - 0.5% by weight of mixture 1.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.
Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban(&, Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.

Example 3. An antimicrobial heat ablative water-borne silicone for extreme
applications (e.g., space)

Example 3a

Mix the following:
Part1
Approx. 2 g epoxy silane resin
Approx. 8 g xylene
Approx. 15 g epoxy resin
Approx. 4 g silicone intermediate
Approx. 1 g organotin
Approx. 0.5 g organozinc


P 566 DKOO CA 02402653 2002-09-26
Part 2

Approx. 66 g silicone modified polyether
Approx. 1 g thixotropic agent
5 Approx. 5 g ceramic fibre filer
Approx. 16 g clay filler

To this mixture add approx. 8 g xylene, approx. 2 g aminosilane, and 2 g amine
catalyst
Mix parts 1 & 2 together.

To this mixture add 0.001 -200 mg/ml of starch which has been spray applied
with
amyloglucosidase with an activity of 0.00001 to 10 AGU (where '1 AGU produces
1
mmol glucose/min at 25 C), alternatively add 0.001 to 500 mg of glucose,
galactose
or fructose/ml mixture 1. Also add 0.002 to 200 mg of starch which has been
spray
applied with hexose oxidase with an activity within 0.001 - 100 U (where 1 U
produced 1 mmol of H202/min at 25 C).

Example 3b.
Partl
Approx. 2 g epoxy silane resin
Approx. 8 g xylene
Approx. 15 g epoxy resin
Approx. 4 g silicone intermediate
Approx. 1 g organotin
Approx. 0.5 g organozinc
Part 2

Approx. 66 g silicone modified polyether
Approx. 1 g thixotropic agent
Approx. 5 g ceramic fibre filer


P 566 DKOO CA 02402653 2002-09-26
31
Approx. 16 g clay filler

To this mixture add approx. 8 g xylene, approx. 2 g aminosilane, and 2 g amine
catalyst
Mix parts 1 & 2 together.

To the mixture add a cocktail of enzymes such as:

Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades ) at the amount of 0.0001 - 0.5 % by weight of mixture 1.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.

Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.

Example 4. A flame retardant antimicrobial composition for housing and
industrial
use

Example 4a a thermoplastic vinyl or acrylic for industrial use
Mixture 1


P 566 DKOO CA 02402653 2002-09-26
32
10-50% acrylic resin (e.g., Neocryl 727 (Zeneca resins), Synocryl 874 (Cray
valley),
Acryloid B66 (Rohm & Haas)) or, a vinyl resin solution (e.g., UCAR VAGH, UCAR
VYHH, UCAR VMCC (Dow Chemical/Union Carbide), Hostaflex CM150 (Hoechst),
Laroflex MP25 (BASF)).
5 - 40% pigments (e.g., Titanium dioxide (Ti-Pure R902, DuPont), iron oxides,
carbon black, graphite, metallic aluminium, zinc oxide or other suitable
pigments)

5 - 40% fillers (e.g., particularly silicone, gypsum, lime)
1 - 5% additives (e.g., thixatropic agents, flow control agents,)

0.1 - 90% solvents (e.g., glycol ethers, alcohols, Solvesso 150, toluene,
acetates,
ketones)
To the above add 3 - 10% w/w macroplegmatic compound (Mc 30,000 to 50,000)
created by mutiprocessing polystyrene and coppolymers.

To the mixture add 0.001 -200 mg/mI of starch which has been spray applied
with
amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1 AGU produces
1 mmol glucose/min at 25 C), alternatively add 0.001 to 500 mg of glucose,
galactose or fructose/ml mixture 1. Also add 0.002 to 200 mg of starch which
has
been spray applied with hexose oxidase with an activity within 0.001 - 100 U
(where
1 U produced 1 mmol of H2O2/min at 25 C).
Example 4b
Mixture 1

10-50% acrylic resin (e.g., Neocryl 727 (Zeneca resins), Synocryl 874 (Cray
valley),
Acryloid B66 (Rohm & Haas)) or, a vinyl resin solution (e.g., UCAR VAGH, UCAR
VYHH, UCAR VMCC (Dow Chemical/Union Carbide), Hostaflex CM150 (Hoechst),
Laroflex MP25 (BASF)).


P 566 DKOO CA 02402653 2002-09-26
33
- 40% pigments (e.g., Titanium dioxide (Ti-Pure R902, DuPont), iron oxides,
carbon black, graphite, metallic aluminium, zinc oxide or other suitable
pigments)

5 - 40% fillers (e.g., particularly silicones, gypsum, lime)
5
1 - 5% additives (e.g., thixatropic agents, flow control agents,)

0.1 - 90% solvents (e.g., glycol ethers, alcohols, Solvesso 150, toluene,
acetates,
ketones)
To the above add 3 - 10% w/w macroplegmatic compound (Mc 30,000 to 50,000)
created by mutiprocessing polystyrene and coppolymers.

To the mixture add a cocktail of enzymes such as:
Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades ) at the amount of 0.0001 - 0.5% by weight of mixture 1.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.
Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.


P 566 DKOO CA 02402653 2002-09-26
34
Example 5. Composition based on a thermoplastic chlorinated rubber or
acrylated
rubber resin

Example 5a.
Mixture 1

Approx. 10-50 % chlorinated rubber resin solution e.g. Pergut S10 (Bayer),
Clortex
(Caffarro) or an acrylated rubber resin solution e.g. Pliolite AC4, AC80, AC-L
10 (Goodyear Chemicals)

Approx. 5 - 40% Pigments, preferably one or more of the following: Titanium
Dioxide
- Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminium, or
other suitable coloured pigments in the range
Approx. 5 - 40 % Fillers, preferably one or more of the following: talc,
calcium
carbonate, barium sulphate, silicones, gypsum, lime,zinc oxide, zinc
phosphate,
clay, kaolin, silicates, glass, ceramics, (including spheres, fibres & powder)
or
carbohydrates
Approx. 1-5% Additives, typically including: thixatropic agents, flow control
agents.
1-5%

Approx. 0.1 - 90% Solvents including xylene, hydrocarbons e.g. Solvesso 150;
toluene, alcohols, acetates, glycol ethers, ketones

Optional: antimicrobials in the range 0.1-10%
Approx. 3 - 10% macroplegmatic compounds
To the above add 0.001 -200 mg/ml of starch which has been spray applied with
amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1 AGU produces 1
mmol glucose/min at 25 C), alternatively add 0.001 to 500 mg of glucose,
galactose
or fructose/ml mixture 1. Also add 0.002 to 200 mg of starch which has been
spray


P 566 DKOO CA 02402653 2002-09-26
applied with hexose oxidase with an activity within 0.001 - 100 U (where 1 U
produced 1 mmol of H2O2/min at 25 C).

Example 5b.
5
Mixture 1

Approx. 10-50 % chlorinated rubber resin solution e.g. Pergut 310 (Bayer),
Clortex
10 (Caffarro) or an acrylated rubber resin solution e.g. Pliolite AC4, AC80,
AC-L
10 (Goodyear Chemicals)

Approx. 5 - 40% Pigments, preferably one or more of the following: Titanium
Dioxide
- Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminium, or
other suitable coloured pigments in the range
Approx. 5 - 40 % Fillers, preferably one or more of the following: talc,
calcium
carbonate, barium sulphate, silicones, gypsum, lime,zinc oxide, zinc
phosphate,
clay, kaolin, silicates, glass, ceramics, (including spheres, fibres & powder)
or
carbohydrates
Approx. 1-5% Additives, typically including: thixatropic agents, flow control
agents.
1-5%

Approx. 0.1 - 90% Solvents including xylene, hydrocarbons e.g. Solvesso 150;
toluene, alcohols, acetates, glycol ethers, ketones

Optional: antimicrobials in the range 0.1-10%
Approx. 3 - 10% macroplegmatic compounds
To the above add a cocktail of enzymes such as:

Protease (e.g., Esperase ; Alcalase. ; Durazym ; 8/or Savinase(D available
from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades) at the amount of 0.0001 - 0.5% by weight of mixture 1.


P 566 DKOO CA 02402653 2002-09-26
36
Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.
Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.

Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.

Example 6: Where the coating composition is based on a hydroxy functional
acrylic
or hydroxy functional polyester resin cured by an isocyanate for various uses

Example 6a.
Mixture 1

Approx. 10-60% hydroxy functional acrylic resin solution e.g. Desmophen A160
(Bayer) or a hydroxy functional polyester resin solution e.g. Setal 168 (Akzo
Nobel)
Approx. 5 - 30% isocyanate curing agent e.g. Desmodur N75 (Bayer) Tolonate
HDB75 (Rhodia) Desmodur N3390 Bayer

Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminium, or
other suitable coloured pigments

Approx 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, silicone, gypsum, lime,zinc oxide, zinc phosphate,
clay,

I I
CA 02402653 2009-07-31

kaolin, silicates, glass, ceramics (including spheres, fibres & powder), or
carbohydrates

Additives, typically including: thixatropic agents, flow control agents, 1-5%
Approx. 3-10% Fire retardant compounds, particularly macroplegmatic
compounds of multiprocessed polystyrene and copolymers

Approx. 10-50% Solvents including xylene hydrocarbons e.g. Solvesso 150 ;
toluene, alcohols, acetates, glycol ethers, ketones

To the above add 0.001-200 mg/ml of starch which has been spray applied with
amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1 AGU produces
1mmol glucose/min at 25 C); alternatively add 0.001 to 500 mg of glucose,
galactose or fructose/ml of mixture 1. Also add 0.002 to 200 mg of starch
which
has been spray applied with hexose oxidase with an activity within 0.001-100 U
(where 1 U produced 1 mmol of H2O2/min at 25 C).

Example 6b
Approx. 10-60% hydroxy functional acrylic resin solution, e.g., Desmophan
A160 (Bayer) or a hydroxy functional polyester resin solution e.g. Setal 168
(Akso Nobel)

Approx. 5-30% isocyanate curing agent e.g. Desmodur N75 (Bayer) Tolonate
HDB75 (Rhodia) Desmodur N3390 (Bayer);

Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide - Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite,
metallic
aluminum, or other suitable coloured pigments

Approx. 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, silicone, gypsum, lime, zinc oxide, zinc
phosphate,
clay, kaolin, silicates, glass, ceramics (including spheres, fibres & powder),
or
carbohydrates

37
SUBSTITUTE PAGE


P 566 DKOO CA 02402653 2002-09-26

Additives, typically including: thixatropic agents, flow control agents. 1-5%

Approx. 3-10% Fire retardant compounds, particularly macroplegmatic compounds
of multiprocessed polystyrene and copolymers
Approx. 10-50% Solvents including xylene, hydrocarbons e.g. Solvesso 150;
toluene, alcohols, acetates, glycol ethers, ketones

To the above mixture add a cocktail of enzymes such as:
Protease (e.g., Esperase ; Alcalase. ; Durazym(F ; &/or Savinase available
from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades) at the amount of 0.0001 - 0.5% by weight of mixture 1.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.
Amylase (e.g., a and b amylases such as Purafect Ox Amc from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.

Example 7
Where the coating is based on an aqueous dispersed polymer for various
uses

Example 7a

I I
CA 02402653 2009-07-31

Mixture 1

Approx. 5-50% emulsion polymer including a continuous aqueous phase and a
dispersed polymer phase, e.g. acrylic latex - Maincote HG54 (Rohm & Haas) or
similar;
Polyurethane dispersion - Neorez 960 (Zeneca resins), Styrene acrylic latex -
Haloflex
202S (Zeneca resins)

Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminum, or other
suitable coloured pigments

Approx. 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, silicone, gypsum, lime, zinc oxide, zinc
phosphate,
clay, kaolin, silicates, glass, ceramics, (including spheres, fibres & powder)
or
carbohydrates

Additives, typically including: wetting agents, surfactants, dispersants e.g.
Nopcosperse 44 , polyurethane thickeners, e.g., Acrysol RM8 (Rohm & Haas),
cellulosics and modified cellulosic thickeners, acrylic thickeners, matting
agents and
defoamers in the range 0.1-5.0%

Coalescing solvents, including alcohols, e.g. Texanol (Rohm & Haas), glycols,
glycol
ethers, ketoximes in the range 1-5%

Optional antimicrobials in the range 0.1-10%

Approx. 3-10% fire retardants - macroplegmatic compounds derived from
multiprocessing polystyrene and copolymers.

To the above mixture 1 add 0.001-200 mg/mL of starch which has been spray
applied
with amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1 AGU
produces 1 mmol glucose/min at 25 C), alternatively add 0.001 to 500 mg of
glucose,
galactose or fructose/ml of mixture 1. Also, add 0.002 to 200 mg of starch
which has
been spray applied with hexose oxidase with an activity within 0.001-100 U
(where 1 U
produced 1 mmol of H2O2/min at 25 C).

39
SUBSTITUTE PAGE


P 566 DKOO CA 02402653 2002-09-26
Example 7b

Mixture 1
5
Approx. 5 - 50% emulsion polymer including a continuous aqueous phase and a
dispersed polymer phase, e g. acrylic: latex - Maincote HG54 (Rohm & Haas) or
similar; Polyurethane dispersion - Neorez 960, (Zeneca resins), Styrene
acrylic latex
- Haloflex 202S (Zeneca resins)
Approx. 5 - 40% Pigments, preferably one or more of the following: Titanium
Dioxide
- Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminium, or
other suitable coloured pigments

Approx. 5 - 40% Fillers, preferably one or more of the following: talc,
calcium
carbonate, barium sulphate, silicone, lime, gypsum, zinc oxide, zinc
phosphate, clay,
kaolin, silicates, glass, ceramics, (including spheres, fibres & powder) or
carbohydrates

Additives, typically including: wetting agents, surfactants, dispersants e.g.
Nopcosperse 44, polyurethane thickeners, e.g. Acrysol RM8 (Rohm & Haas),
cellulosics and modified cellulosic thickeners, acrylic thickeners, matting
agents and
defoamers in the range 0.1-5.0 %

Coalescing solvents including alcohols, e.g. Texanol (Rohm & Haas), glycols,
glycol
ethers ketoximes in the range 1-5%

Optional antimicrobials in the range 0.1-10%

Approx. 3 - 10% fire retardants - macroplegmatic compounds derived from
multiprocessing polystyrene and copolymers.

To the above mixture 1 add a cocktail of enzymes such as:


P 566 DKOO CA 02402653 2002-09-26
41
Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades) at the amount of 0.0001 - 0.5% by weight of mixture 1.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.
Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2 % by weight of mixture 1.

Example 8: Where the coating is based on an aqueous dispersed polymer
containing active crosslinking groups for various uses.

Example 8a
Mixture 1

Approx 5 - 50% dispersed polymer including a continuous aqueous phase and a
dispersed polymer phase, e.g. Epoxy dispersion; Hydroxy functional acrylic
dispersion or Hydroxyl functional polyester i
Approx 1-40% water soluble or dispersed cross linking agent e.g. Amino resins,
polyamides polyamines, cycloaliphatic amines, mannich bases, isocyanates,
blocked isocyanates, aziridines or similar


P 566 DKOO CA 02402653 2002-09-26
42
Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminium, or
other suitable coloured pigments

Approx. 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, silicone, gypsum, lime, zinc oxide, zinc
phosphate, clay,
kaolin, silicates, glass, ceramics, (including spheres, fibres & powder) or
carbohydrates

Approx. 0.1-5.0% additives, typically including: wetting agents, surfactants,
dispersants e.g. Nopcosperse 44, polyurethane thickeners, e.g. Acrysol RM8
(Rohm
& Haas), cellulosics and modified cellulosic thickeners, acrylic thickeners,
matting
agents and defoamers

Approx. 1-5% Coalescing solvents including alcohols, e.g. Texanol (Rohm &
Haas),
glycols, glycol ethers ketoximes

Optional antimicrobials in the range 0.1-10%

Approx. 3 - 10% Fire retardants, for example macroplegmatic compounds
multiprocessed from polystyrene and copolymers.

To the above mixture 1 add 0.001 -200mg/ml of starch which has been spray
applied with amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1
AGU
produces 1 mmol glucose/min at 25 C), alternatively add 0.001 to 500mg of
glucose,
galactose or fructose/ml mixture 1. Also add 0.002 to 200mg of starch which
has
been spray applied with hexose oxidase with an activity within 0.001 - 100 U
(where
1 U produced 1 mmol of H202/min at 25 C).

Example 8b
Mixture 1


P 566 DKOO CA 02402653 2002-09-26
43
Approx 5 - 50% dispersed polymer including a continuous aqueous phase and a
dispersed polymer phase, e.g. Epoxy dispersion; Hydroxy functional acrylic
dispersion or Hydroxyl functional polyester

Approx 1-40% water soluble or dispersed cross linking agent e.g. Amino resins,
polyamides polyamines, cycloaliphatic amines, mannich bases, isocyanates,
blocked isocyanates, aziridines or similar

Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminium, or
other suitable coloured pigments

Approx. 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, silicone, gypsum, lime, zinc oxide, zinc
phosphate, clay,
kaolin, silicates, glass, ceramics, (including spheres, fibres & powder) or
carbohydrates

Approx. 0.1-5.0% additives, typically including: wetting agents, surfactants,
dispersants e.g. Nopcosperse 44, polyurethane thickeners, e.g. Acrysol RM8
(Rohm
& Haas), cellulosics and modified cellulosic thickeners, acrylic thickeners,
matting
agents and defoamers

Approx. 1-5% Coalescing solvents including alcohols, e.g. Texanol (Rohm &
Haas),
glycols, glycol ethers ketoximes
Optional antimicrobials in the range 0.1-10%

Approx. 3 - 10% Fire retardants, for example macroplegmatic compounds
multiprocessed from polystyrene and copolymers.
To the above mixture 1 add a cocktail of enzymes such as:

Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades ) at the amount of 0.0001 - 0.5% by weight of mixture 1.


P 566 DKOO CA 02402653 2002-09-26
44
Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.
Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.

Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.

Example 9 Where the coating is based on an aqueous hybrid binder composition
for
various uses

Example 9a.
Mixture 1

Combination of organic and inorganic polymers dispersible in water
Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminium, or
other suitable coloured pigments

Approx. 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, zinc oxide, zinc phosphate, clay, kaolin,
silicates, glass,
ceramics, (including spheres, fibres & powder) or carbohydrates

Approx. 0.1-5.0% additives, typically including: wetting agents, surfactants,
dispersants e.g. Nopcosperse 44, polyurethane thickeners, e.g. Acrysol RM8
(Rohm


CA 02402653 2009-07-31

& Haas), cellulosics and modified cellulosic thickeners, acrylic thickeners,
matting agents
and defoamers

Coalescing solvents including alcohols, e.g. Texanol (Rohm & Haas), glycols,
glycol
ethers, ketoximes in the range 1-5%

Optional antimicrobials in the range 0.1-10%

Approx. 3-10% fire retardant macroplegmatic compounds
To the above mixture 1 add 0.001 - 200mg/ml of starch which has been spray
applied with amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1
AGU
produces 1 mmol glucose/min at 25 C), alternatively add 0.001 to 500mg of
glucose,
galactose or fructose/ml mixture 1. Also add 0.002 to 200mg of starch which
has been
spray applied with hexose oxidase with an activity within 0.001- 100 U (where
1 U
produced lmmol of H202/min at 25 C).

Example 9b
Mixture 1

Combination of organic and inorganic polymers dispersible in water

Approx. 5-40% pigments preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminum, or other
suitable coloured pigments

Approx. 5-40% Fillers preferably one or more of the following: talc, calcium
carbonate, barium sulphate, zinc oxide, zinc phosphate, clay, kaolin,
silicates, glass,
ceramics, (including spheres, fibres & powder) or carbohydrates

Approx. 0.1-5.0% additives, typically including: wetting agents, surfactants,
dispersants e.g. Nopcosperse 44 , polyurethane thickeners e.g. Acrysol RM8
(Rohm &
Haas), cellulosics and modified cellulosic thickeners, acrylic thickeners,
matting agents
and defoamers

SUBSTITUTE PAGE

I I


P 566 DKOO CA 02402653 2002-09-26
46
Coalescing solvents including alcohols, e.g. Texanol (Rohm & Haas), glycols,
glycol
ethers ketoximes in the range 1-5%

Optional antimicrobials in the range 0.1-10%

Approx. 3-10% fire retardant macroplegmatic compounds
To the above mixture 1 add a cocktail of enzymes such as:
Protease (e.g., Esperase ; Alcalase. ; Durazym ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades ) at the amount of 0.0001 - 0.5% by weight of mixture 1.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.
Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.

Example 10 Where the coating composition is based on combined hybrid resin
system for various uses

Example 10a
Mixture 1

I I ~
CA 02402653 2009-07-31

Approx. 10-70% epoxy siloxane resin e.g. Silikoftal ED (Tego Chemie)

Approx. 5-25% amino functional silicone curing agent e.g. Dynasilan AMEO (3-
aminopropyl triethoxysilane, Degussa)

Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminum, or
other suitable coloured pigments)
Approx. 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, zinc oxide, zinc phosphate, clay, kaolin,
silicates, glass,
ceramics, (including spheres, fibres & powder) or carbohydrates

Approx. 1-5% additives, typically including: thixotropic agents, flow control
agents
Approx. 0.5-50% Solvents including xylene, hydrocarbons e.g. Solvesso 150 ;
toluene, alcohols, acetates, glycol ethers, ketones

Optional antimicrobials in the range 0.1-10%

This formulation is expected to be naturally flame resistant

To the above mixture 1 add 0.001-200mg/ml of starch which has been spray
applied with amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1
AGU
produces 1 mmol glucose/min at 25 C), alternatively add 0.001 to 500mg of
glucose,
galactose or fructose/ml mixture 1. Also add 0.002 to 200mg of starch which
has been
spray applied with hexose oxidase with an activity within 0.001- 100 U (where
1 U
produced 1 mmol of H202/min at 25 C).
Example 1 Ob
Mixture 1

Approx. 10-70% epoxy siloxane resin e.g. Silikoftal ED (Tego Chemie) in the
range
47
SUBSTITUTE PAGE


CA 02402653 2009-07-31

Approx. 5-25% amino functional silicone curing agent e.g. Dynasilan AMEO (3-
aminopropyl triethoxysilane, Degussa)

Approx. 5-40% Pigments, preferably one or more of the following: Titanium
Dioxide -
Ti-Pure R902 (DuPont), iron oxides, carbon black, graphite, metallic
aluminum, or other
suitable coloured pigments

Approx. 5-40% Fillers, preferably one or more of the following: talc, calcium
carbonate, barium sulphate, zinc oxide, zinc phosphate, clay, kaolin,
silicates, glass,
ceramics, (including spheres, fibres & powder) or carbohydrates

Approx. 1-5% additives, typically including: thixotropic agents, flow control
agents
Approx. 0.5-50% Solvents including xylene, hydrocarbons e.g. Solvesso 150 ;
toluene, alcohols, acetates, glycol ethers, ketones

Optional antimicrobials in the range 0.1-10%

This formulation is expected to be naturally flame resistant.
To the above mixture 1 add a cocktail of enzymes such as:

Protease (e.g., Esperase ; Alcalase ; Durazyme ; &/or Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocaades) at the amount of 0.0001-0.5% by weight of mixture 1.

Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001-3% by weight of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd. Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from
GIST-Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the
named
48
SUBSTITUTE PAGE


CA 02402653 2009-07-31

type of lipases combined with a cutinase at the amount of 0.0001-3% by weight
of
mixture 1.

Amylase (e.g., a and b amylases such as Purefact Ox Am from Genencor,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002-2% by weight of mixture 1.

Example 11 Where the coating composition is based on a combined hybrid resin
system for various uses
Example 11a
Mixture 1

Non aromatic epoxy e.g. Eponex 1510 (Resolution), Epodil 757 (Air Products)
in the
range 15-45%

Alkyl, aryl or alkoxy polysiloxane e.g. Dow Corning 3074 in the range 15-45%

Organooxysilane e.g. A163 Union Carbide/Dow Chemicals, Dow Corning 26070 , in
the range 1-10%.

Cured with an aliphatic amine or adduct thereof, polyamidoamide,
cycloaliphatic
amine or adduct thereof, Aromatic amine, mannich base, ketimine or amino
functional silane e.g. Al 100 Union Carbide/Dow Chemicals, Z6020 Dow
Corning,
in the range 10-20%

Pigments, preferably one or more of the following: Titanium dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminum, or other
suitable
coloured pigments in the range 5-40%

Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, silicone, lime, gypsum, zinc phosphate, clay, kaolin,
silicates,
glass, ceramics, (including spheres, fibres & powder) or carbohydrates in the
range
5-40%

49
SUBSTITUTE PAGE


P 566 DKOO CA 02402653 2002-09-26
bU

Additives, typically including: thixatropic agents, flow control agents and
organometallic catalysts in the range 1-5%

Solvents including xylene, hydrocarbons e.g. Solvesso 150; toluene, alcohols,
acetates, glycol ethers, ketones, in the range 5-40%

Optional antimicrobials in the range 0.1-10%

Macroplegmatic fire retarding compound in the range 3-10%

To the above mixture 1 add 0.001 200mg/ml of starch which has been spray
applied with amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1
AGU
produces 1 mmol glucose/min at 25 C), alternatively add 0.001 to 500mg of
glucose,
galactose or fructose/ml mixture 1. Also add 0.002 to 200mg of starch which
has
been spray applied with hexose oxidase with an activity within 0.001 - 100 U
(where
1 U produced 1 mmol of H2O2/min at 25 C).

Example 11 b
Mixture 1

Non aromatic epoxy e.g. Eponex 1510 (Resolution), Epodil 757 (Air Products) in
the
range 15-45 %
Alkyl, aryl or alkoxy polysiloxane e.g. Dow Corning 3074 in the range 15-45%
Organooxysilane e.g. A163 Union Carbide/Dow Chemical, Dow Corning Z6070, in
the range 1-10%.
Cured with an aliphatic amine or adduct thereof, polyamidoamide,
Cycloaliphatic
amine or adduct thereof, Aromatic amine, mannich base, ketimine or amino
functional silane e.g. A1100 Union Carbide/Dow chemical, Z6020 Dow Corning, in
the range 10-20%


P 566 DKOO CA 02402653 2002-09-26
51
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%

Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, silicone, lime, gypsum, zinc phosphate, clay, kaolin,
silicates,
glass, ceramics, (including spheres, fibres & powder) or carbohydrates in the
range
5-40%

Additives, typically including: thixatropic agents, flow control agents and
organometallic catalysts in the range 1-5%

Solvents including xylene, hydrocarbons e.g. Solvesso 150; toluene, alcohols,
acetates, glycol ethers, ketones, in the range 5-40%
Optional antimicrobials in the range 0.1-10%
Macroplegmatic fire retarding compound in the range 3-10%
To the above mixture 1 add a cocktail of enzymes such as:

Protease (e.g., Esperase ; Alcalase. ; Durazym ; 8Jor Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades ) at the amount of 0.0001 - 0.5% by weight of mixture 1.
Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.


P 566 DKOO CA 02402653 2002-09-26
52
Amylase (e.g., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.
Example 12 Where the coating composition is based on an alkyd resin
composition
for various uses.

Example 12a
Mixture 1

An alkyd or modified alkyd resin e.g. Synolac S31, Unithane 655W (Cray
Valley),
Uralac 390 (DSM Resins) in the range 10-50%
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%

Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%

Additives, typically including: thixatropic agents, flow control agents,
driers (aliphatic
carboxylic acid salts of metals such as cobalt, manganese, lead, zirconium,
calcium
and mixtures thereof) and antioxidants e.g. Methylethylketoxime or similar in
the
range 1-5%

Solvents including xylene, hydrocarbons e.g. Solvesso 150, white spirit;
toluene,
alcohols, acetates, glycol ethers, ketones, in the range 10-60%

Optional antimicrobials in the range 0.1-10%

Macroplegmatic Fire retarding compounds in the range 3 to 10%


P 566 DKOO CA 02402653 2002-09-26
53
To the above mixture 1 add 0.001 -200mg/ml of starch which has been spray
applied with amyloglucosidase with an activity of 0.00001 to 10 AGU (where 1
AGU
produces 1 mmol glucose/min at 25 C), alternatively add 0.001 to 500mg of
glucose,
galactose or fructose/ml mixture 1. Also add 0.002 to 200mg of starch which
has
been spray applied with hexose oxidase with an activity within 0.001 - 100 U
(where
1 U produced 1 mmol of H202/min at 25 C).

Example 12b
Mixture 1

An alkyd or modified alkyd resin e.g. Synolac S31, Unithane 655W (Cray
Valley),
Uralac 390 (DSM Resins) in the range 10-50%

Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%

Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%

Additives, typically including: thixatropic agents, flow control agents,
driers (aliphatic
carboxylic acid salts of metals such as cobalt, manganese, lead, zirconium,
calcium
and mixtures thereof) and antioxidants e.g. Methylethylketoxime or similar in
the
range 1-5%

Solvents including xylene, hydrocarbons e.g. Solvesso 150, white spirit;
toluene,
alcohols, acetates, glycol ethers, ketones, in the range 10-60%
Optional antimicrobials in the range 0.1-10%

Macroplegmatic Fire retarding compounds in the range 3 to 10%
To the above mixture 1 add a cocktail of enzymes such as:


P 566 DKOO CA 02402653 2002-09-26
54
Protease (e.g., Esperase ; Alcalase. ; Durazym ; Wor Savinase available from
Novozymes. Alternatively Maxatas ; Maxacal ; Properase or Maxapem from
GIST-Brocades ) at the amount of 0.0001 - 0.5% by weight of mixture 1.
Cellulase (e.g., commercially available cellulases from microbial origins,
e.g., from
the fungus Humicola, strain DSM 1800) at the amount of 0.00001 - 3% by weight
of
mixture 1.

Lipase (e.g., commercially available derived from bacterial or fungal origins,
such as
Lipase P "Amano", AMANO Pharmaceutical Co. Ltd., Nagoya, Japan) also AMANO-
CES NRRLB 3673 from Toyo Jozo Co., Tagata, Japan, also LIPOMAX from GIST-
Brocades and LIPOLASE from Novozymes. Alternatively a mixture of the named
type of lipases combines with a cutinase at the amount of 0.0001 - 3% by
weight of
mixture 1.

Amylase (e.g.., a and b amylases such as Purafect Ox Am from Genencor ,
Termamyl , Ban , Fungamyl and Duramyl from Novozymes) at the amount of
0.0002 - 2% by weight of mixture 1.
Example 13
Where the coating composition is based on an epoxy resin, crosslinked using an
amino functional curing agent comprising:

An epoxy resin obtained from the reaction of 2,2-bis(4-hydroxyphenyl)propane
with
epichlorhydrin e.g. Epikote 1001, Epikote 1003, Epikote 1004, Epikote 828
(Resolution); Araldite 7071, Araldite GY250(Vantico), DER 671, DER 331 (Dow
Chemical) or similar in the range 10- 50%.
An amino curing agent selected from the classes: Amino resins, polyamides
polyamines, cycloaliphatic amines, mannich bases, e.g. Versamid 115, Versamid
125, Versamid 140 (Cognis) Crayamid 115, Crayamid 125 (Cray Valley) Ancamine
1784 or similar, in the range 10-50%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%.


P 566 DKOO CA 02402653 2002-09-26
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: accelerators, e.g. 2,4,6-tris (dimethylamino
methyl)
5 phenol e.g. Ancamine K54 (Air Products), thixatropic agents e.g. Modified
Bentonites, fumed silicas, modified waxes, in the range 0.1-5%.
Solvents including xylene, butanol, hydrocarbons e.g. Solvesso 150; toluene,
alcohols, acetates, glycol ethers, ketones, ketimines. in the range 0.1-90%.
Enzymes or antimicrobials in the range 0.1-10%.
Example 14

Where the coating composition is based on a thermoplastic acrylic or vinyl
resin
comprising:
An acrylic resin solution e.g. Neocryl 727 (Zeneca resins) Synocryl 874 (Cray
Valley) Acryloid B66 (Rohm & Haas) or a vinyl resin solution e.g. UCAR VAGH,
UCAR VYHH, UCAR VMCC (Dow Chemical/Union Carbide), Hostaflex CM150
Hoechst, Laroflex MP25 (BASF) in the range 10-50%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: thixatropic agents, flow control agents. 1-5%.
Solvents including xylene, hydrocarbons e.g. Solvesso 150, toluene, alcohols,
acetates, glycol ethers, ketones, in the range 0.1-90%.
Enzymes or antimicrobials in the range 0.1-10%.
Example 15

Where the coating composition is based on a thermoplastic chlorinated rubber
or
acrylated rubber resin comprising:


CA 02402653 2009-07-31

A chlorinated rubber resin solution e.g. Pergut S10 (Bayer), Clortex 10
(Caffaro) or
an acrylated rubber resin solution e.g. Pliolite AC4 , AC80 , AC-L (Goodyear
Chemicals) in the range 10-50%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902 ,
(DuPont), iron oxides, carbon black, graphite, metallic aluminum, or other
suitable
coloured pigments in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: thixatropic agents, flow control agents: 1-5%.
Solvents including xylene, hydrocarbons e.g. Solvesso 150 , toluene, alcohols,
acetates, glycol ethers, ketones, in the range 0.1-90%.
Enzymes or antimicrobials in the range 0.1-10%.
Example 16

Where the coating composition is based on a hydroxy functional acrylic or
hydroxy
functional polyester resin cured by an isocyanate, comprising:

A hydroxy functional acrylic resin solution e.g. Desmophen A160 (Bayer) or a
hydroxy functional polyester resin solution e.g. Setal 168 (Akzo Nobel) in
the
range 10-60%.
An isocyanate curing agent e.g. Desmodur N75 (Bayer) Tolonate HDB75 (Rhodia)
Desmodur N3390 Bayer in the range 5-30%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminum, or other
suitable
coloured pigments) in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: thixatropic agents, flow control agents 1-5%.
Solvents including xylene, hydrocarbons e.g. Solvesso 150 , toluene, alcohols,
acetates, glycol ethers, ketones, in the range 10-50%.
Enzymes or antimicrobials in the range of 0.1-10%.

56
SUBSTITUTE PAGE


P 566 DKOO CA 02402653 2002-09-26
57
Example 17
Where the coating is based on an aqueous dispersed polymer comprising:

An emulsion polymer including a continuous aqueous phase and a dispersed
polymer phase, e.g. acrylic latex - Maincote HG54 (Rohm & Haas) or similar;
Polyurethane dispersion - Neorez 960, (Zeneca resins), Styrene acrylic latex -
Haloflex 202S (Zeneca resins) in the range 5-50%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: wetting agents, surfactants, dispersants e.g.
Nopcosperse 44, polyurethane thickeners, e.g. Acrysol RM8 (Rohm & Haas),
cellulosics and modified cellulosic thickeners, acrylic thickeners, matting
agents and
defoamers in the range 0.1-5.0 %.
Coalescing solvents including alcohols, e.g. Texanol (Rohm & Haas), glycols,
glycol
ethers ketoximes in the range 1-5%.
Enzymes or antimicrobials in the range 0.1-10%.
Example 18
Where the coating is based on an aqueous dispersed polymer containing active
crosslinking groups comprising:
A dispersed polymer including a continuous aqueous phase and a dispersed
polymer phase, e.g. Epoxy dispersion; Hydroxy functional acrylic dispersion or
Hydroxyl functional polyester in the range 5-50%.
A water soluble or dispersed cross linking agent e.g. Amino resins, polyamides
polyamines, cycloaliphatic amines, mannich bases, isocyanates, blocked
isocyanates, aziridines or similar in the range 1-40%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%.


P 566 DKOO CA 02402653 2002-09-26
58
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: wetting agents, surfactants, dispersants e.g.
Nopcosperse 44, polyurethane thickeners, e.g. Acrysol RM8 (Rohm & Haas),
cellulosics and modified cellulosic thickeners, acrylic thickeners, matting
agents and
defoamers in the range 0.1-5.0 %.
Coalescing solvents including alcohols, e.g. Texanol (Rohm & Haas), glycols,
glycol
ethers ketoximes in the range 1-5%.
Enzymes or antimicrobials in the range 0.1-10%.
Example 19
Where the coating is based on an aqueous hybrid binder composition:
Combination of organic and inorganic polymers dispersible in water.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: wetting agents, surfactants, dispersants e.g.
Nopcosperse 44, polyurethane thickeners, e.g. Acrysol RM8 (Rohm & Haas),
cellulosics and modified cellulosic thickeners, acrylic thickeners, matting
agents and
defoamers in the range 0.1-5.0 %.
Coalescing solvents including alcohols, e.g. Texanol (Rohm & Haas), glycols,
glycol
ethers ketoximes in the range 1-5%.
Enzymes or antimicrobials in the range 0.1-10%.
Example 20
Where the coating composition is based on combined hybrid resin system
comprising:

An epoxy siloxane resin e.g. Silikoftal ED (Tego Chemie) in the range 10-70%.


P 566 DKO() CA 02402653 2002-09-26
59
An amino functional silicone curing agent e.g. Dynasilan AMEO (3-amiriopropyl
triethoxysilane, Degussa) in the range 5-25%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: thixatropic agents, flow control agents, in
the range 1-
5%.
Solvents including xylene, hydrocarbons e.g. Solvesso 150; toluene, alcohols,
acetates, glycol ethers, ketones, in the range 0.5-50%.
Enzymes or antimicrobials in the range 0.1-10%.
Example 21

Where the coating composition is based on combined hybrid resin system
comprising:

Non aromatic epoxy e.g. Eponex 1510 (Resolution), Epodil 757 (Air Products) in
the
range 15-45 %.
Alkyl, aryl or alkoxy polysiloxane e.g. Dow Corning 3074 in the range 15-45%.
Organooxysilane e.g. A163 Union Carbide/Dow Chemical, Dow Corning Z6070, in
the range 1-10%.
Cured with an aliphatic amine or adduct thereof, polyamidoamide,
Cycloaliphatic
amine or adduct thereof, Aromatic amine, mannich base,, ketimine or amino
functional silane e.g. A1100 Union Carbide/Dow chemical, Z6020 Dow Corning, in
the range 10-20%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminium, or other
suitable
coloured pigments in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.


CA 02402653 2009-07-31

Additives, typically including: thixatropic agents, flow control agents and
organometal catalysts in the range 1-5%.
Solvents including xylene, hydrocarbons e.g. Solvesso 150 , toluene, alcohols,
acetates, glycol ethers, ketones in the range 5-40%.
Enzymes or antimicrobials in the range of 0.1-10%.
Example 22
Where the coating composition is based on an alkyd resin comprising:

An alkyd or modified alkyd resin e.g. Synolac S31 , Unithane 655W (Cray
Valley),
Uralac 390 (DSM Resins) in the range 10-50%.
Pigments, preferably one or more of the following: Titanium Dioxide - Ti-Pure
R902
(DuPont), iron oxides, carbon black, graphite, metallic aluminum, or other
suitable
coloured pigments in the range 5-40%.
Fillers, preferably one or more of the following: talc, calcium carbonate,
barium
sulphate, zinc oxide, zinc phosphate, clay, kaolin, silicates, glass,
ceramics,
(including spheres, fibres & powder) or carbohydrates in the range 5-40%.
Additives, typically including: thixatropic agents, flow control agents,
driers (aliphatic
carboxylic acid salts of metals such as cobalt, manganese, lead, zirconium,
calcium,
and mixtures thereof) and antioxidants e.g. Methylethylketoxime or similar in
the
range 1-5%.
Solvents including xylene, hydrocarbons e.g. Solvesso 150 , white spirit,
toluene,
alcohols, acetates, glycol ethers, ketones in the range 10-60%.
Enzymes or antimicrobials in the range of 0.1-10%.

SUBSTITUTE PAGE

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date 2011-05-24
(22) Filed 2002-09-26
(41) Open to Public Inspection 2004-03-26
Examination Requested 2008-09-16
(45) Issued 2011-05-24
Expired 2022-09-26

Abandonment History

Abandonment Date Reason Reinstatement Date
2006-09-26 FAILURE TO PAY APPLICATION MAINTENANCE FEE 2006-11-24
2007-09-26 FAILURE TO REQUEST EXAMINATION 2008-09-16
2009-09-28 FAILURE TO PAY APPLICATION MAINTENANCE FEE 2009-12-14
2010-08-02 FAILURE TO PAY FINAL FEE 2010-12-14

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $150.00 2002-09-26
Maintenance Fee - Application - New Act 2 2004-09-27 $50.00 2004-09-27
Maintenance Fee - Application - New Act 3 2005-09-26 $50.00 2005-09-08
Reinstatement: Failure to Pay Application Maintenance Fees $200.00 2006-11-24
Maintenance Fee - Application - New Act 4 2006-09-26 $50.00 2006-11-24
Maintenance Fee - Application - New Act 5 2007-09-26 $100.00 2007-08-08
Reinstatement - failure to request examination $200.00 2008-09-16
Request for Examination $400.00 2008-09-16
Maintenance Fee - Application - New Act 6 2008-09-26 $100.00 2008-09-16
Reinstatement: Failure to Pay Application Maintenance Fees $200.00 2009-12-14
Maintenance Fee - Application - New Act 7 2009-09-28 $100.00 2009-12-14
Maintenance Fee - Application - New Act 8 2010-09-27 $100.00 2010-07-13
Reinstatement - Failure to pay final fee $200.00 2010-12-14
Final Fee $150.00 2010-12-14
Maintenance Fee - Patent - New Act 9 2011-09-26 $100.00 2011-07-13
Maintenance Fee - Patent - New Act 10 2012-09-26 $125.00 2012-07-25
Maintenance Fee - Patent - New Act 11 2013-09-26 $125.00 2013-07-09
Maintenance Fee - Patent - New Act 12 2014-09-26 $125.00 2014-07-30
Maintenance Fee - Patent - New Act 13 2015-09-28 $125.00 2015-07-15
Maintenance Fee - Patent - New Act 14 2016-09-26 $125.00 2015-07-15
Maintenance Fee - Patent - New Act 15 2017-09-26 $225.00 2017-07-06
Maintenance Fee - Patent - New Act 16 2018-09-26 $225.00 2017-07-06
Maintenance Fee - Patent - New Act 17 2019-09-26 $225.00 2017-07-06
Maintenance Fee - Patent - New Act 18 2020-09-28 $225.00 2020-11-20
Late Fee for failure to pay new-style Patent Maintenance Fee 2020-11-20 $150.00 2020-11-20
Maintenance Fee - Patent - New Act 19 2021-09-27 $225.00 2020-11-20
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
DORMON, JANE
Past Owners on Record
None
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Maintenance Fee Payment 2020-11-20 1 33
Cover Page 2011-04-26 1 30
Claims 2002-09-26 10 357
Description 2002-09-26 60 2,436
Abstract 2003-12-19 1 12
Cover Page 2004-03-01 1 27
Claims 2009-07-31 10 278
Description 2009-07-31 60 2,380
Assignment 2002-09-26 3 110
Correspondence 2003-12-19 1 29
Correspondence 2004-09-29 1 19
Correspondence 2004-10-06 1 14
Correspondence 2002-10-22 1 20
Assignment 2002-09-26 1 39
Prosecution-Amendment 2011-01-05 1 27
Fees 2004-09-27 1 48
Correspondence 2004-01-05 1 15
Prosecution-Amendment 2003-12-19 1 29
Correspondence 2003-12-19 3 83
Correspondence 2004-01-19 1 14
Maintenance Fee Payment 2017-07-06 1 33
Correspondence 2004-05-05 1 18
Correspondence 2004-05-27 1 12
Fees 2005-09-08 1 47
Fees 2006-11-24 1 43
Correspondence 2007-09-10 2 60
Fees 2007-08-08 1 49
Fees 2011-07-13 1 55
Prosecution-Amendment 2008-09-16 1 28
Correspondence 2008-09-16 1 28
Prosecution-Amendment 2009-02-03 5 220
Prosecution-Amendment 2009-07-31 24 774
Fees 2009-12-14 1 25
Fees 2010-07-13 1 51
Prosecution-Amendment 2010-11-01 6 245
Prosecution-Amendment 2010-12-14 1 31
Correspondence 2010-12-14 1 31
Prosecution Correspondence 2002-09-26 71 2,886
Correspondence 2011-03-17 1 19
Fees 2012-07-25 1 163
Fees 2013-07-09 1 163
Fees 2014-07-30 1 33
Fees 2015-07-15 1 33