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Patent 1323278 Summary

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(12) Patent: (11) CA 1323278
(21) Application Number: 1323278
(54) English Title: FREE FLOWING ANIONIC DETERGENT AND A METHOD OF PRODUCTION THEREOF
(54) French Title: DETERGENT ANIONIQUE FLUIDE ET METHODE DE PRODUCTION
Status: Expired and beyond the Period of Reversal
Bibliographic Data
(51) International Patent Classification (IPC):
  • C11D 1/12 (2006.01)
  • C11D 11/04 (2006.01)
  • C11D 17/00 (2006.01)
  • C11D 17/06 (2006.01)
(72) Inventors :
  • MADEN, JOHN (United Kingdom)
  • LOUDIADIS, LYCOURGOS (United Kingdom)
(73) Owners :
  • CUSSONS (INTERNATIONAL) LIMITED
(71) Applicants :
  • CUSSONS (INTERNATIONAL) LIMITED (United Kingdom)
(74) Agent: OSLER, HOSKIN & HARCOURT LLP
(74) Associate agent:
(45) Issued: 1993-10-19
(22) Filed Date: 1989-07-31
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
8818613.5 (United Kingdom) 1988-08-05

Abstracts

English Abstract


ABSTRACT
A FREE FLOWING ANIONIC DETERGENT AND METHOD
OF PRODUCTION THEREOF
A method of producing a free flowing, high active, particulate
anionic detergent comprising the step of adsorbing an anionic surfactant
acid onto a powdered or granular material such as a phosphate,
carbonate, bicarbonate or silicate so as to form an agglomerate. No
water is added during the agglomeration stage. The agglomerate may
subsequently be coated with a silicate and/or an alkaline salt preferably
in a fluidised bed.


Claims

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


-12-
THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A method of producing a free flowing, high active, anionic
detergent comprising the step of adsorbing an anionic surfactant acid
onto a powdered or granular material to form an agglomerate without
the addition of water in the agglomeration stage.
2. A method of producing a free flowing, high active detergent as
claimed in claim 1, wherein said material is heated and is substantially
dry prior to adsorption of the anionic surfactant acid.
3 A method of producing a free flowing, high active detergent as
claimed in claim 1 or claim 2, wherein at least a part of the anionic
surfactant acid is adsorbed onto the powdered or granular material in
a fluidised bed.
4 A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein the anionic surfactant acid
comprises any of the following alone or in combination: alkyl aryl
sulphonic acids, fatty acid sulphonic acids, olefin sulphonic acids,
fatty alcohol ether sulphuric acid, fatty methyl ester sulphonic acid,
alkane sulphonic acids.
5. A method of producing a free flowing, high active detergent as claimed
in claims 1 or 2, wherein the anionic surfactant acid comprises any of the
following either alone or in combination: alkyl aryl sulphnic acids containing
an alkyl group with 9-20 carbon atoms and a sulphonic acid or sulphuric
acid ester group, fatty acid sulphuric acids obtained by sulphating
alcohols with 8-18 carbon atom chains and linear straight chain alkyl
benzene sulphonic acids in which the average number of carbon atoms
in the alkyl group is from 11 to 13.

-13-
6. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein the amount of anionic surfactant
acid is in the range from 12% to 40% by weight based on the weight of
the final product.
7. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein the amount of anionic surfactant
acid is in the range from 12% to 35% by weight based on the weight of
the final product.
8. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein the amount of anionic surfactant
acid is in the range from 12% to 30% by weight based on the weight of
the final product.
9. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein said powdered or granular
material comprises alkaline material.
10. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein said powdered or granular-
material comprises solely or in combination with other ingredients, a
phosphate, carbonate, bicarbonate, sulphate or silicate salt of an alkali
metal or an alkaline earth metal.
11. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein the amount of powdered or
granular material is in the range from 60 to 95% by weight based on
the weight of the final product.
12. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein said method further comprises
the coating of said agglomerate with a silicate.

-14-
13. A method of producing a free flowing, high active detergent as
claimed in claims 1 or 2, wherein said method further comprises
the coating of said agglomerate with an alkali, or an alkaline salt.
14. A free flowing, high active anionic detergent prepared by the
method as claimed in claims 1 or 2.
15. A free flowing, high active, anionic, powdered or granular
detergent composition comprising an anionic surfactant acid adsorped
onto a powdered or granular material wherein at least 96% by weight of
said detergent composition has a particle size distribution substantially
within the range from 250 microns to 1700 microns.
16. A free flowing, high active, anionic powdered or granular detergent
composition as claimed in claim 15, wherein the anionic surfactant acid
is present in the range from 12 to 40% by weight of the total composition
and the powdered or granular material is present within the range
from 20 to 50% by weight at the total composition.
17. A free flowing, high active, anionic, powdered or granular
detergent composition comprising an anionic surfactant acid adsorped
onto a powdered or granular material anionic surfactant acid being
present in the range from 12 to 40% by weight of the total composition
and the powdered or granular material being present within the range
from 20 to 50% by weight of the total composition.
18. A free flowing, high active, anionic powdered or granular detergent
composition as claimed in claim 17, wherein at least 96% by weight of
said detergent composition has a particle size distribution substantially
within the range from 250 microns to 1700 microns.
19. A free flowing, high active, anionic, powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein

-15-
said detergent composition has an average particle size substantially
in the range from 1100 to 1300 microns.
20. A free flowing; high active, anionic, powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said detergent composition has an untapped bulk density in the range
from 600 to 720 gm/ml.
21. A free flowing, high active, anionic powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said detergent composition has a tapped bulk density in the range
from 730 to 830 gm/ml.
22. A free flowing, high active, anionic, powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said detergent composition has a mositure content less than 4% by
weight of the total composition.
23. A free flowing, high active, anionic powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said detergent composition has an angle of repose within the range
from 36° to 41°.
24. A free flowing, high active, anionic, powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said detergent composition has a sliding angle in the range from 25°
to 28°.
25. A free flowing, high active, anionic powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said detergent composition has a flowrate in the range from 30 to 41
cc/sec.
26. A free flowing, high active, anionic, powdered or granular

-16-
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said detergent composition has a compressibility in the range from 7
to 15%.
27. A free flowing, high active, anionic powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein the
anionic surfactant acid is present in the range from 12 to 30% by
weight of the total composition.
28. A free flowing, high active, anionic, powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein
said powdered or granular material is present in the range from 30 to
40% by weight of the total composition.
29. A free flowing, high active, anionic powdered or granular
deter gent composition as claimed in any of claims 15, 16 or 17, wherein
said powdered or granular material comprises alkaline material.
30. A free flowing, high active, anionic, powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17 wherein
said powdered or granular material comprises any of the following
either alone or in combination: a phosphate, carbonate, bicarbonate,
sulphate, or silicate salt of an alkali metal or an alkaline earth metal.
31. A free flowing, high active, anionic, powdered or granular
detergent as claimed in any of claims 15, 16 or 17, wherein said anionic
surfactant acid comprises any of the following alone or in combination:
alkyl aryl sulphonic acids, fatty acid sulphonic acids, olefin sulphonic
acids, fatty alcohol ether sulphuric acid, fatty methyl ester sulphonic
acid, alkane sulphonic acids.
32. A free flowing, high active, anionic powdered or granular
detergent composition as claimed in any of claims 15, 16 or 17, wherein

-17-
said anionic surfactant acid comprises any of the following ether alone
or in combination: alkyl aryl sulphonic acids containing an alkyl group
with 9-20 carbon atoms and a sulphonic acid or sulphuric acid ester
group, fatty acid sulphuric acids obtained by sulphating alcohols with
8-18 carbon atom chains, and linear straight chain alkyl benzene
sulphonic acids in which the average number of carbon atoms in the
alkyl group is from 11 to 13.

Description

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


3 ~
A FREE FLOWING ANIONIC DETE~GENT AND METHOD
OF PRODUCTION THEREOF
This invention relates to detergents, and more particularly, to
free flowing, high active anionic detergents.
High active detergents, for the purposes of the present invention,
may be defined as detergents comprising more than 1 29d active matter .
Free flowing, for the purposes of the present invention, may be
defined as sufficiently mobile as to be capable of being poured or
dispensed reproducably as a measured quantity.
It is desirable that detergent powders exemplify certain
characteristics, namely, the detergent powder should be non-dusty,
free flowing, easily handled, easily dissolved and stable under normal
storage conditions.
A large proportion of the worldwide detergent market uses high
foaming powder surfactants, most of which are based on anionic active
lS matter ingredients.
It has hitherto been common practice to produce detergents in
powder form by making up a slurry of the various ingredients in
water and subsequently spray drying the slurry to yield a powder- of
typical bulk density 0 . 2 to 0 . 5 gms/ml . This method of manufacture
is expensive because heat is required to evaporate the water which
was ini~ialiy added and yet is not required in the final product.
A further method of manufacture of detergents in powder form is
by so called 'dry neutralisation'. Dry neutralisation and associated
agglomeration is normally regarded as a three part process:
1. Dry adsorption of an alkyl aryl sulphonic acid onto the
surface of an alkaline base.
.
:.... : , ,. ::: : :: -
~, ; .: ~ :. :, . :,
:-. ; : ,;:; :, ; :-:.
; -;: : :

1323278
--2--
2. Addition of water to affect the reaction of the alkali and
sulphonic acid to form an alkaline sulphonate which binds the
constituents to produce a neutralised de-tergent agglomerate and
3. Coating the outside of the agglomerate with a layer of dessicant
material such as sodium tripolyphosphate, sodium carbonate or silicate.
It has previously been assumed that: there is a reasonably well
described limitation on the amount of alkyl aryl sulphonic acid which
can be adsorpted onto the surface of various alkaline bases without
first causing over agglomeration or poor flow properties. For example
it has been claimed that the adsorptive characteristics of
tripolyphosphate or other adsorptive materials are a function of their
surface area. Therefore, sodium tripolyphosphate (STPP) in powder
form must have greater adsorptivity than in granular form. Definitive
tables of the adsorptivity of STPP and other alkalies have been published
in the past giving the adsorptivity of various powders with regard to
the uptake of alkyl aryl sulphonic acid, for example do decyl benzene
sulphonic acid (DDBSA . ) This, theoretically, limits the amount of
active matter which can be formulated into a detergent powder produced
by dry neutralisation.
The table (A) below shows commonly accepted limitations of the
adsorptlvity of various bases.
TABLE A
g DDBSA/1 OOg alkali salt
STPP Powder 32 . 5
STPP low density granular 2 . 0
STPP regular density granular 2 . l
soda ash ( powder ) 2 . 2
, : .. ,.. : .
: -
:~ .

lc~23278
--3--
soda ash (granular) 0.2
Sodium metasilicate anhydrous 0.1
Sodium metasilicate 5H20 0.1
It has previously been assumed that the addition of approximately
5 1-2 % of water was necessary to cause in situ neutralisation of sulphonic
acids with alkaline bases. The product was not thought to be stable
until this reaction had been completed. It has previously been assumed
that a dessicant should be used to coat the outside of the agglomerate
to adsorb free water, usually by hydration of the dessicant, to obtain
lO a free flowing product.
According to a first aspect of the present invention, there is
provided a method of producing a free flowing, high active, anionic
detergent comprising the step of adsorbing an anionic surfactant acid
onto a powdered or granular material to l`orm an agglomerate without
15 the addition of water in the agglomeration stage.
It has been discovered that the powdered or granular detergent
composition derived from this method suprisingly has a subs-tantially
uniform particle size and may comprise high levels of surfactant acid
successfully exceeding the maximum surfactant acid content of the
2 0 pr ior art .
According to a second aspect of the present inven-tion there is
provided a free flowing, high active, anionic powdered or granular
detergent composition comprising an anionic surfactant acid adsorped
onto a powdered or granular material, said detergent composition having
25 a particle size distribution substantially within the range from 248
microns to 1752 microns.
According to a third aspect of the present invention there is
.. . . , . . ~
. ' : ::. ' : :,:` '~ :
- . .,: , ..... . .

i 3~2~
--4--
provided a free flowing, high active, anionic, powdered or granular
detergent composition comprising a surfactant acid adsorped onto a
powdered or granular material the surfactant acid being present in the
range from 12 to 40% by weight of the total composition and the powdered
5 or granular material being present within the range from 20 to 50% by
weight of the total composition.
In a preferred embodiment of the invention, the anionic surfactant
acid is adsorbed onto heated, dry, powdered, or granular material.
In a preferred embodiment of the invention the anionic surfactant acid
lO is adsorbed onto heated dry powdered or granular form preferably in a
fluidised bed.
In a further preferred embodiment, the agglomerate so formed is
then coated by the application of a silicate and/or alkali, preferably in
a fluidised bed. The temperature of the inital part of the fluidised bed
15 is preferably above 50C and more preferably in the range from 85 to
95C
Any suitable anionic surfactant acid may be used. Suitable examples
of such are as follows: alkyl aryl sulphonic acids, fatty acid sulphonic
acids, olefin sulphonic acids, fatty alcohol ether sulphuric acid, fatty
20 methyl ester sulphonic acid, alkane sulphonic acids. More particularly
alkyl aryl sulphonic acids containing an alkyl group with 9-20 carbon
atoms and a sulphonic acid or sulphuric acid ester group (included in
the term alkyl is the alkyl portion of the aryl groups), or fatty acid
sulphuric acids obtained by sulphating alcohols with 8-18 carbon atom
25 chains. Especially valuable are linear straight chaln alkyl benzene
sulphonic acids in which the average number of carbon atoms in the
alkyl group is from 11 to 13. The amoun-t of anionic
. . . ,
:~ .. .. : , ~
:.,-: , .:,.
.. . :
,, . ~ ....... ..

~32~ 8
--5--
surfactant acid added is preferably in the range 12% to 40%, more
preferably from 12% to 35% and even more preferably from 12% to 30% of
the final product weight for weight .
We have discovered that we can adsorb up to at least 50gm
5 DDBDA/lOOgm STPP powder when operating under the conditions of
the invention thus significantly exceeding the amounts known to have
been adsorbed in previously published work, whilst still retaining the
free flowing na-ture of the end product.
The powdered or granular material may comprise any suitable alkali,
lO or alkalies, alone, or in combination with other additional ingredients.
Examples of suitable alkalies are as follows: Sodium phosphates, for
example sodium tripolyphosphate, sodium carbonate, sodium bicarbonate,
sodium silicate or other similar alkalies including potassium or magnesium
salts. The amount of alkali is preferably in the range 1096 to 95% and
15 more preferably 60% to 95% final product weight for weight.
Additional ingredients may include the following: bleaching agents
for example Sodium Perborate, corrosion inhibitors or alkaline additives,
for example, Sodium Silicates, inert fillers, for example Sodium Sulphate,
surfactants, optical brighteners, preventors of soil redeposition, (for
20 example, sodium carboxy-methyl cellulose, ) dedusting agents and
solubilisers, such as sodium xylene sulphonate, enzymes, chelating
agents, perfumes, softening agents, defoamers, bleach activators, soap,
and non ionic active material.
Any suitable apparatus may be used, but this may have to be
25 adapted to run under the appropriate conditions so as to maintain dry
conditions during the agglomeration stage. Examples of such apparatus

13'~f3278
-6--
are as follows:
l. Static or moving machines with dividers or blades or paddles to
mix the powders. These include twin shell blenders or V blenders,
baffled drums and ribbon or paddle blenders.
5 2. Air suspension machines which suspend the particles in air whilst
liquid is sprayed onto said particles. The particle size increases until
the particles are too heavy to be suspended at which time they fall
from the air stream.
3. Apparatus in which air is used to fluidise the particles making
lO them act in a similar manner to a liquid, for example, a fluidised bed.
Sample powdered or granular detergents derived from this method
exhibit the following characteristics:
Particle Size
no more than 3% by weight of the particles are larger than l700
15 microns
no more than l % by weigh-t of the particles are less than 250
microns
average particle size 1100 to 1300 microns
Bulk density: untapped 600-720 gm/ml
tapped: 730-830 gm/ml
moisture content: less than 4~ W/W
. . _ . . _ .
angle of repose average: 37 to 38C
with minimum 36 maximum 41
sliding angle: minimum 25 maximum 28
flowrate: 30-41 cc/sec through standard orifice.
compressibility: 7-15%
. . . _ _
;,
',.,

13 23S~7~
--7--
Composition of anionic detergent granulate:
The detergent composition comprises 5 to 40g~ preferably 10 to 35%
and more preferably 12 to 30% by weight of the final composition of an
anionic surfactant acid for example Sodium alkyl ar~yl sul~hate. The
5 detergent composition comprises 20 to 50% preferably 25 to 4S% and
more preferably 30 to 40% by weight of the final composition of the
powdered or granular material such as the alkaline material sodium
tripolyphoshphate. The detergent composition may also comprise any
of the optical ingredients listed on page 5 including for example any of
lO the following: soda ash, sodium sulphate, sodium carboxy methyl
cellulose, optical bleaches, sequestering agents, sodium silicates etc.
For the purpose of the present invention:-
the angle of repose is defined as the angle from the horizontal tothe line of slope of a heap of powder, the heap having been formed
15 by directing powder through a funnel into the centre of a circular
horizontal surface. The funnel is slowly raised to allow the heap to
form immediately beneath it.
The flow rate of the powder is de~ined as the rate in cubic
centimetres per second that will flow through a 1 . 25cm diameter orifice
20 with a smooth PVC funnel e~<panding at 10 to the vertical above the
or if ice .
The angle of slide is defined as the minimum angle between -the
horizontal and an inclined surface when a powder slides by gravity en
masse down that surface, the surface being a smooth, wooden unpolished
25 medium. The powder is scattered as a layer no more than 20mm deep
on the surface. The surface is raised slowly until the sliding condition
is achieved~
- . ;

13232~8
The compressibility of the powder is defined as the percentage
of initial volume lost when a sample is subjected to a compressive
load, the compressive load being provided by a 10Kg weight which is
applied to a cylinder of powder of 69mm diameter for a period of 3
5 minutes.
The invention will now be described further by the following
Examples:
EXAMPLE 1
The following mixture was prepared by dry blending and then
l0 fed at a rate of typically 1.83 kg per minute onto a horizontal fluidised
bed. No water was added. The inital part of the fluidised bed was
heated to above 80C and retained at this temperature during the
experiment .
Material ~6 W/W
15 Sodium Tripolyphosphate 44 . 8
Sodium Carbonate 23.4
Sodium Carboxy-Methyl Cellulose 2.40
Sodium Sulphate 29 . 00
Optical Brightener ~TINOPAL* CBS-X) 0.40
*TINOPAL is a Trade Mark of Ciba-Geigy.
Two liquids, as defined below, were sprayed sequentially along
the fluidising bed onto the fluidised powder.
LIQUID 1. Do Decyl Benzene Sulphonic Acid ~DDBSA) at a spray
rate of 390g/min.
25 LIQUID 2. A solution comprising
% WIW
a) Sodium Silicate ~2:1 Si02:Na20~ 40.00
~,. - ~ i
, , : '~

~32~2'~'~
g
b) Pigment blue 15:1 (46% Dispersion 0.18
c ) Tetra sodium sait of ethylene
diamine tetra acetic acid 3.66
d ) Water 56 .16
The solution was applied at a spray rate of 390g/min. The
combined addition of alkyl aryl sulphonic acid and silicate solution
equated to a 30.0% w/w combined percentage liquid additions.
After processing, chemical analysis indicated the powders had
the following chemical content.
% W/W
Active Detergent 15 . 6
(calculated as Sodium Alkyl Aryl
Sulphonate - Molecular Weight 322)
Sodium Tripolyphosphate 32.4
lS (calculated as P205)
Moisture 1 . 53
The product was a dust free, free flowing granular agglomerate.
EXAMPLE 2
The foliowing powder mixtures were prepared and used as in EXAMPLE
20 1,
% WlW
Sodium Tripolyphosphate 57 . 60
Sodium Carbonate 23 . 00
Sodium Carboxy-Methyl Cellulose 2 . 40
25 Sodium Sulphate 16.60
Optical Brightener (TINOPAL* CBS-X) 0.40
*TINOPAL is a Trade Mark of Ciba-Geigy.
.... .. . . .

~32`~278
--10--
The composition of the two liquids sprayed along the fluidised
bed was as in EXAMPLE 1.
LIQUID 1 was applied at a spray rate of 600g/min.
LIQUID 2 was applied at a spray rate of 390g/min
The combined addition of alkyl aryl sulphonic and silicate solultion
equated to a combined percentage liquid addition of 35.0% W/W.
After processing, chemical analysis indicated the powder had the
following chemical content.
% W.W.
10 Active Detergent 23 . 9
(calculated as Sodium Alkyl Aryl
Sulphonate - Molecular Weight 332 )
Sodium Tripolyphosphate 41.7
(calculated as P205)
Moisture 1 . 73
The powder produced was a dust free, free flowing granular
agglomerate.
The method enabled a liquid addition of 35.0% W/W to the fluid
bed which is comfortably in excess of the limit of 20% imposed by
20 known methods.
Active matter content was as high as 23.3%, which is almost
twice the maximum amount of 12% of active matter achieved by known
methods, utilising a fluid bed apparatus.
The amount of alkyl aryl sulphonic acid adsorped onto the
25 tripolyphosphate and other alkalies present was well in excess of the
previously know adsorptive figures quoted in literature as shown in
TABLE A.
,
,. : i : : .

13~327~
In EXAMPLE 1 the theoretical maximum for successful adsorption
of alkyl aryl sulphonic acid is calculated to be 15 . 0759 of sulphonic
acid per 100 9 of initial powder mixture. The practical result of use
of the claimed method is calculated to be 21 . 3119 of sulphonic acid
5 per 1009 of initial powder mixture which is well in excess of the
results from previously known methods.
Similarly in EXAMPLE 2 the figures for theoretical maximum and
practical results are 19.2269 and 32.3119 of alkyl aryl sulphonic acid
per l OOg of initial powder mixture.
Prior art methods of dry neutralisation in whatever apparatus
have always assumed the presence of added water and have always
restricted the ratio of the amount of alkyl aryl sulphonates -to the
amount of alkali to a limit which the invention successfully exceeds.
The present invention provides a cost efficien-t method of producing a
15 high active, non-dusty, free flowing, stable anionic detergent powder
which may be easily handled and easily stored.
: ~ . , .............. : . :: .
~ ~ '. , .`; . ',`.' ,' ' ', ''. .

Representative Drawing

Sorry, the representative drawing for patent document number 1323278 was not found.

Administrative Status

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Event History

Description Date
Inactive: Agents merged 2013-10-10
Inactive: IPC from MCD 2006-03-11
Inactive: IPC from MCD 2006-03-11
Time Limit for Reversal Expired 1997-10-20
Letter Sent 1996-10-21
Grant by Issuance 1993-10-19

Abandonment History

There is no abandonment history.

Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
CUSSONS (INTERNATIONAL) LIMITED
Past Owners on Record
JOHN MADEN
LYCOURGOS LOUDIADIS
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) 
Cover Page 1994-03-08 1 21
Claims 1994-03-08 6 177
Drawings 1994-03-08 1 11
Abstract 1994-03-08 1 17
Descriptions 1994-03-08 11 330
Fees 1995-10-11 1 46
Courtesy - Office Letter 1989-11-22 1 32
PCT Correspondence 1990-01-16 1 161
Courtesy - Office Letter 1990-02-02 1 17
PCT Correspondence 1993-07-20 1 47
Prosecution correspondence 1992-10-09 2 63
Examiner Requisition 1992-06-12 1 59
Prosecution correspondence 1990-01-17 2 35