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Patent 2008387 Summary

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(12) Patent Application: (11) CA 2008387
(54) English Title: LIQUID DETERGENT PRODUCT
(54) French Title: PRODUIT DETERGENT LIQUIDE
Status: Deemed Abandoned and Beyond the Period of Reinstatement - Pending Response to Notice of Disregarded Communication
Bibliographic Data
(51) International Patent Classification (IPC):
  • C11D 3/10 (2006.01)
  • C11D 3/37 (2006.01)
  • C11D 3/386 (2006.01)
  • C11D 17/00 (2006.01)
(72) Inventors :
  • DONKER, CORNELIS B.
  • HO TAN TAI, LOUIS (France)
(73) Owners :
  • UNILEVER PLC
(71) Applicants :
  • UNILEVER PLC (United Kingdom)
(74) Agent: SMART & BIGGAR LP
(74) Associate agent:
(45) Issued:
(22) Filed Date: 1990-01-23
(41) Open to Public Inspection: 1990-07-30
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
8902011.9 (United Kingdom) 1989-01-30
8906836.5 (United Kingdom) 1989-03-23
8907877.8 (United Kingdom) 1989-04-07

Abstracts

English Abstract


ABSTRACT
A non-aqueous liquid detergent comprises a liquid
phase which preferably includes a nonionic surfactant and
a dispersed particulate phase which includes a carbonate,
or mixed carbonate/bicarbonate builder and a carboxylic
acid polymer, such as a maleic/acrylic copolymer, as a
calcium carbonate crystal growth inhibitor. The
compositions exhibit good physical stability and
performance. Other ingredients such as an oxygen bleach
system and lipase enzymes may also be present.


Claims

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


THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A substantially non-aqueous liquid detergent
composition comprising a liquid surfactant phase and a
solid particulate phase dispersed therein, the
particulate phase comprising a detergency builder which
is predominantly a water-soluble carbonate material,
characterised in that the composition further comprises a
calcium carbonate crystal growth inhibiting agent in the
form of a water soluble alkali metal salt of a carboxylic
acid polymer.
2. A composition according to Claim 1, wherein the
liquid surfactant phase comprises a nonionic surfactant.
3. A composition according to Claim 1, wherein the
liquid surfactant phase is present at a level of at least
10% by weight of the total composition.
4. A composition according to Claim 1, wherein the
water-soluble carbonate material comprises a mixture of
an alkali metal carbonate with an alkali metal
bicarbonate.
5. A composition according to Claim 1, wherein the
level of water-soluble carbonate material is at least 10%
by weight of the composition.

6. A composition according to Claim 1, wherein the
calcium carbonate crystal growth inhibiting agent is
selected from homopolymers derived from a monomer of the
formula (I)
<IMG> (I)
wherein R1 is hydrogen, hydroxyl, C1-C4 alkyl or alkoxy,
acetoxy or -CH2COOM, R2 is hydrogen, C1-C4 alkyl, or
-COOM and M is an alkali metal, copolymers thereof with
other monomers of formula (I) and copolymers thereof with
one or more non-carboxylic acid monomers.
7. A composition according to Claim 1, wherein the
level of polymer is from 0.5% to 15% by weight of the
composition.
8. A composition according to Claim 1, containing not
more than 5% by weight of calcite having a surface area
of more than 10m2/g.
9. A composition according to Claim 1, further
comprising a lipase enzyme.

10. The non-aqueous liquid detergent composition as
claimed in claim 1 and substantially as described herein.

Description

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


20(~8;~8~7
- 1 - C3291
LIOUTD DETERGENT PRODUCT
This invention relates to a liguid detergent
product, in particular to a non-aqueous product of the
type comprising a liquid surfactant phase and a
- particulate solid detergency builder suspended in the
liquid phase. Such products are suitable, for example,
for the washing of fabrics.
Non-aqueous liquid products have been described in
-~ the literature in which the suspended solid builder is a
phosphate material, such as sodium tripolyphosphate.
While technically such products can provide successful
cleaning results, there has been pressure in recent years
to reduce the level of phosphate in detergent products.
Crystalline aluminosilicates or zeolites have been
proposed as replacement materials for phosphate builders
: and their use in powder products has already been
wide-spread. The incorporation of zeolites in
non-aqueous liquids however is not without difficulties.
Many zeolite materials appear to be capable of
catalysing the breakdown of any bleach materials that may
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- 2 - 2 0 C83 ~t7
be present in the product. Since one of the major
advantages of non-aqueous liquids as a product form is
the possibility of including various water-sensitive
materials such as bleaches, this is a serious problem.
S :
Alkalimetal carbonates have also been proposed as
phosphate replacers. Their use in powders has
necessitated taking steps to avoid or suppress the effect
of calcium carbonate crystal growth inhibitors which
would otherwise act to retard the reaction between the
hardness ions of the wash liquor and the carbonate ions
from the alkalimetal carbonate, with a resulting loss in
detergency. Thus GB 14379SO, (Unilever Case C720)
teaches the use of high surface area calcite (ie. having
lS a surface area above ~Om /g) to suppress this effect and
encourage crystal growth. We have now surprisingly found
however, that in the case of such non-aqueous liquids in
which the liquid phase comprises a surfactant, improved
results can be obtained if the product contains an
inhibiting agent in the form of a water-soluble salt of a
carboxylic acid polymer.
Thus, according to the invention there is provided a
substantially non-aqueous liquid detergent composition
comprising a liquid surfactant phase and a solid
particulate phase dispersed therein, the particulate
phase comprising a detergency builder which is
predominantly a water-soluble carbonate material,
characterised in that the composition further comprises a
calcium carbonate crystal growth inhibiting agent in the
form of a water-soluble alkalimetal salt of a carboxylic
acid polymer.
The liquid phase of the product contains a
surfactant. The surfactant may make up all or only part
. .
.- . . .
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_ 3 _ 20~8~87
of the liquid phase, the remainder being constituted by a
liquid non-surfactant material such as a solvent.
In general, the surfactant may be chosen from the
liquid surfactants described "Surface Active Agents" Vol.
1, by Schwartz & Perry, Interscience 1949, Vol. 2 by
Schwartz, Perry & Berch, Interscience 1958, in the
current edition of "McCutcheon's Emulsifiers and
Detergents" published by Manufacturing Confectioners
Company or in "Tenside-Taschenbuch", H. Stache, 2nd Edn.,
Carl Hanser Verlag, 1981.
In this respect nonionic surfactants are especially
suitable, most preferably liquid polyalkoxylated nonionic
surfactants.
Nonionic detergent surfactants are well-known in he
art. They normally consist of a water-solubilizing
polyalkoxylene or a mono- or di-alkanolamide group in ~-
chemical combination with an organic hydrophobic group
derived, for example, from alkylphenols in which the
alkyl group contains from about 6 to about 12 carbon
atoms, dialkylphenols in which each alkyl group contains
from 6 to 12 carbon atoms, primary, secondary or tertiary
aliphatic alcohols (or alkyl-capped derivatives thereof),
preferably having from 8 to 20 carbon atoms, ;
monocarboxylic acids having from 10 to about 24 carbon
atoms in the alkyl group and polyoxypropylenes. Also
common are fatty acid mono- and dialkanolamides in which
the alkyl group of the fatty acid radical contains from
10 to about 20 carbon atoms and the alkyloyl group having
from 1 to 3 carbon atoms. In any of the mono- and
di-alkanolamide derivatives, optionally, there may be a
polyoxyalkylene moiety joining the latter groups and the
hydrophobic part of the ~olecule. In all polyalkoxylene
containing surfactants, the polyalkoxylene moiety
. ~ . , ,

' 20(~8~87
-- 4
preferably consists of from 2 to 20 groups of ethylene
oxide or of ethylene oxide and propylene oxide groups.
Amongst the latter class, particularly preferred are
those described in the applicants' published European
specification EP-A-225,654, especially for use as all or
part of the liquid phase. Also preferred are those
ethoxylated nonionics which are the condensation products
of fatty alcohols with from 9 to 15 carbon atoms
condensed with from 3 to 11 moles of ethylene oxide.
Examples of these are the condensation products of C11 13
alcohols with (say) 3 to 7 moles of ethylene oxide.
These may be used as the sole nonionic surfactants or in
combination with those of the described in the
last-mentioned European specification, especially as all
or part of the liquid phase.
Another class of suitable nonionics which may be
incorporated, preferably at most in minor quantities,
comprise the alkyl polysaccharides
(polyglycosides/oligosaccharides) such as described in
any of specifications US 3,640,998; US 3,346,558; US
4,223,129; EP-A-92,355; EP-A-99,183; EP-A-70,074, '75,
'76, '77; ~P-A-75,994, '95, '96.
Nonionic detergent surfactants normally have
molecular weights of up to about 11,000. When mixtures
of different nonionic detergent surfactants are used, it
is preferred that the mixture is liquid at room
temperature.
Mixtures of nonionic detergent surfactants with
other detergent surfactants such as anionic, cationic or
ampholytic detergent surfactants and soaps may also be
used.
.
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_ 5 _ 20~8387
:
Examples of suitable anionic detergent surfactants,
which may be used, preferably at most, in minor
quantities, are alkali metal, ammonium or alkylolamine
salts of alkylbenzene sulphonates having from 10 to 18
carbon atoms in the alkyl group, alkyl and alkylether
sulphates having from 10 to 24 carbon atoms in the alkyl
: group, the alkylether sulphates having from 1 to 5
ethylene oxide groups, olefin sulphonates prepared by
sulphonation of C10-C24 alpha-olefins and subsequent
neutralization and hydrolysis of the sulphonation
reaction product.
Other surfactants which may be used, preferably at
most in minor quantities, include alkali metal soaps of a
fatty acid, preferably one containing 12 to 18 carbon
atoms. Typical such acids are oleic acid, ricinoleic
acid and fatty acids derived from caster oil, rapeseed
oil, groundnut oil, coconut oil, palmkernal oil or
mixtures thereof. The sodium or potassium soaps of these
acids can be used. As well as fulfilling the role of
surfactants, soap can act as further detergency builders
or fabric conditioners, other examples of which will be
described in more detail hereinbelow. It can also be
remarked that the oils mentioned in this paragraph may
themselves constitute all or part of the liquid phase,
whilst the corresponding low molecular weight fatty acids
- (triglycerises) can be dispersed as solids or function as
structurants.
Yet again, it is also possible to utilise small
amounts of cationic, zwitterionic and amphoteric
surfactants such as referred to in the general surfactant
texts referred to hereinbefore. Examples of cationic
detergent surfactants are aliphatic or aromatic
alkyl-di(alkyl) ammonium halides and examples of soaps
are the alkali metal salts of C12-C24 fatty acids.

- 6 - 20~8387
Ampholytic detergent surfactants are eg. the
sulphobetaines. Combinations of surfactants from within
the same, or from different classes may be employed to
advantage for optimising structuring and/or cleaning
performance.
Non-surfactants which are suitable for inclusion in
the liquid phase include ethers, polyethers, alkylamines
and fatty amines, (especially di- and tri-alkyl- and/or
fatty- N- substituted amines), alkyl (or fatty) amides
and mono- and di- N-alkyl substituted derivatives
thereof, alkyl (or fatty) carboxylic acid lower alkyl
esters, ketones, aldehydes, and glycerides. Specific
examples include di-alkyl ethers, polyethylene glycols,
polyethylene oxides, ~lymes alkyl ketones (such as
acetone), glycerol, glycerol triacetate, propylene
glycol, and sorbitol.
The compositions of the invention may contain the
liquid phase in an amount of at least 10% by weight of
the total composition. The amount of the liquid phase
present in the composition may be as high as about 90%,
but in most cases the practical amount will lie between
20 and 70% and preferably between 35 and 50% by weight of
the composition. The dispersed particulate solid phase
preferably makes up the remainder of the composition.
The water-soluble carbonate material used is
preferably an alkali metal carbonate such as lithium,
sodium or potassium carbonate or a mixture thereof, for
reasons of cost and efficiency, although ammonium or
substituted aD onium carbonates can be used instead. The
amount of the carbonate material in the product can be
varied widely but the amount is desirably at least about
; 35 10% by weight, preferably not more than 65% by weight.
It should be mentioned within this range the hi~her
..... .. i: ............................. .
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-

2008;~87
- 7 -
levels tend to be required under conditions of use at low
product concentration, as is usually the practice in
North America, and the converse applies at higher product
concentrations as tend to be used in Europe. It may also
be desirable to limit the carbonate content to a lower
figure to decrease the risk of internal damage following
any accidental oral ingestion. Mixtures of carbonates
with the corresponding bicarbonates may advantageously be
used as a means of introducing more carbonate ions
without excessively raising the pH of the product when
added to a wash liquor. Compared with compositions which
contain only phosphate builders, the compositions of the
present invention show improved physical stability.
The compositions according to the present invention
preferably also contain one or more other functional
ingredients, for example selected from minor amounts of
other detergency builders, bleaches, non-building
electrolytes such as sodium sulphate and (for hard
surface cleaners) abrasives. -
The other detergency builders, like the
water-soluble carbonate material, are materials which
counteract the effects of calcium, or other ion, water
hardness, by precipitation, by an ion sequestering or
ion-exchange effect. They comprise both inorganic and
organic builders. They may also be sub-divided into the
phosphorus-containing and non-phosphorus types, the
latter being preferred in the present invention for
environmental reasons.
Inorganic builders comprise the various silicate-,
borate- and aliminosilicate-type materials, particularly
the alkali-metal salt forms. Mixtures of these may also
be used.
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2008;~87
- a
- Examples of other non-phosphorus-containing
inorganic builders, when present, include water-soluble
alkali metal borates, silicates, metasilicates, and
crystalline and amorphous alumino silicates. Specific
examples include sodium and potassium silicates and
zeolites.
Examples of organic builders include the alkali
metal, ammonium and substituted, citrates, cuccinates,
malonates, fatty acid sulphonates, carboxy~ethoxy
succinates, ammonium polyacetates, carboxylates,
polycarboxylates, aminopolycarboxylates, polyacetyl
carboxylates and polyhydroxsulphonates. Specific
examples include sodium, potassium, lithium, ammonium and
substituted ammonium salts of ethylenediaminetetraacetic
acid, nitrilotriacetic acid, oxydisuccinic acid, melitic
acid, benzene polycarboxylic acids and citric acid.
Other, less preferred, examples are organic phosphonate
type sequestering agents such as those sold by Monsanto
under the tradename of the Dequest range and
alkanehydroxy phosphonates.
';
It will be usual for the water-soluble carbonate
material to make up the major part of the total
detergency builder in the product.
'
The carboxylic acid polymer may be a homopolymer or
a copolymer having a molecular weight of at least 500 and
should be water-soluble. It may be derived from a
mono-carboxylic acid or from a di- or poly-carboxylic
acid. The polymer will be used in its water-soluble
alkali metal salt form. The level of polymer in the
composition is advantageously at least 0.5% by weight up
to 15% by weight, most preferably from 1% to 10% by
weight.
.
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2008;}87
g : .
one group of polymer materials found to be of value
in the present invention comprises homopolymers derived
from a monomer of the formula (I)
S R1 H
I
C C (I)
COOM 2
.:
where R1 is hydrogen, hydroxyl, Cl - C4 alkyl or alkoxy,
acetoxy or -CH2COOM, R2 is hydrogen , C1-C4 alkyl, or
-COOM and M is an alkali metal. Examples of this group
include the sodium and potassium salts of polyacrylic,
polymethacrylic, polyitaconic, polymaleic and
polyhydroxyacrylic acids and also the hydrolysis products
of the corresponding polymerised acid anhydrides. Thus
the polymer obtained by hydrolysis of maleic anhydride
falls within this group.
-
A second group of polymeric materials comprises the `
copolymers of two or more carboxylic monomers of the
above formula. Examples of this group include the sodium
and potassium salts of copolymers of maleic anhydride
with acrylic acid, methacrylic acid, crotonic acids,
itaconic acid and its anhydride, aconitic acid.
A third group of polymeric materials comprises the
copolymers of one or more carboxylic monomers of the
above formula with one or more non-carboxylic acid
monomers such as ethylene, propylene, styrene, ~ -methyl
styrene, acrylonitrile, acrylamide, vinylacetate, methyl
vinyl ketone, acrolein and esters of carboxylic acid
monomers such as ethyl acrylate and methacrylate.
~ - -- . .... , , . - i . ., . . , :

--` 2008~87
-- 10 --
In order to obtain maximum benefit from the presence
of the crystal growth inhibiting polymer, it is preferred
that no materials be present in the product which would
act as an absorbent for such pslymers. In particular
particulate calcium carbonate should be absent from the
product. More specifically the product should contain no
more than about 5%, preferably less than 2%, most
preferably less than 1% of high surface area calcite.
Suitable bleaches include the halogen, particularly
chlorine bleaches such as are provided in the form of
alkalimetal hypohalites, e.g. hypochlorites. In the
- application of fabrics washing, the oxygen bleaches are
preferred, for example in the form of an inorganic
persalt, preferably with an precursor, or as a peroxy
acid compound.
In the case of the inorganic persalt bleaches, the
precursor makes the bleaching more effective at lower
temperatures, i.e. in the range from ambient temperature
to about 60C, so that such bleach systems are commonly
known as low-temperature bleach systems and are well
known in the art. The inorganic persalt such as sodium
perborate, both the monohydrate and the tetrahydrate,
acts to release active oxygen in solution, and the
precursor is usually an organic compound having one or
more reactive acyl residues, which cause the formation of
peracids, the latter providing for a more effective
bleaching action at lower temperatures than the
peroxybleach compound alone. The ratio by weight of the
peroxy bleach compound to the precursor is from about
15:1 to about 2:1, preferably from about 10:1 to about
3.5:1. Whilst the amount of the bleach system, i.e.
peroxy bleach compound and precursor, may be varied
between about 5% and about 35% by weight of the total
liquid, it is preferred to use from about 6% to about 30%
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- 11 - 2008~87
of the ingredients forming the bleach system. Thus, the
preferred level of the peroxy bleach compound in the
composition is between about 5.5% and about 27% by
- weight, while the preferred level of the precursor is
between about 0.5~ and about 14%, most preferably between
- about 1% and about 5% by weight.
Typical examples of the suitable peroxybleach
compounds are alkalimetal peroborates, both tetrahydrates
and monohydrates, alkali metal percarbonates,
persilicates and perphosphates, of which sodium perborate
is preferred.
- Precursors for peroxybleach compounds have been
amply described in the literature, including in British
patent specifications 836,988, 855,735, 907,356, 907,358,
907,950, 1,003,310, and 1,246,339, US patent
~ specifications 3,332,882, and 4,128,494, Canadian patent
- specification 844,481 and South African patent -
specification 68/6,344.
. ~
The exact mode of action of such precursors is not
known, but it is believed that peracids are formed by
reaction of the precursors with the inorganic peroxy
compound, which peracids then liberate active-oxygen by
decomposition.
,
They are generally compounds which contain N-acyl or
0-acyl residues in the molecule and which exert their
activating action on the peroxy compounds on contact with
these in the washing liquor.
Typical examples of precursors within these groups
are polyacylated alkylene diamines, such as
N,N,Nl,Nl-tetraacetylethylene diamine (TAED) and
N,N,Nl,Nl-tetraacetylmethylene diamine (TAMD); acylated
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2008~}87
- 12 -
glycolurils, such as tetraacetylgylcoluril (TAGU);
triacetylcyanurate and sodium sulphophenyl ethyl carbonic
acid ester.
S A particularly preferred precursor is
N,N,N1,Nl-tetra- acetylethylene diamine (TAED).
The organic peroxyacid compound bleaches are
preferably those which are solid at room temperature and
most preferably should have a melting point of at least
50C. Most commonly, they are the organic peroxyacids
and water-soluble salts thereof having the general
formula
H0-0-C-R-Y
wherein R is an alkylene or substituted alkylene group
containing 1 to 20 carbon atoms or an arylene group
containing from 6 to 8 carbon atoms, and Y is hydrogen,
halogen, alkyl, aryl or any group which provides an
anionic moiety in aqueous solution.
Ano~her preferred class of peroxygen compounds which
can be incorporated to enhance dispensing/dispersibility
in water are the anhydrous perborates described for that
purpose in the applicants' European patent specification
EP-A-217,454.
If the liquid phase comprises an ester formed from
an organic acid and an alkoxylated alcohol nonionic
detergent, the ester can act as a precursor for a persalt
bleach included in the composition, thus obviating the
need for any other conventional precursor. These esters
can also lower the pour point of the compo ition.
.- . . : . . .,. ;
, . . . . : .~ :~
- :

Z008;~87
- 13 -
When the composition contains abrasives for hard
surface cleaning (i.e. is a liquid abrasive cleaner),
these will inevitably be incorporated as particulate
solids. They may be those of the kind which are water
insoluble. Water soluble abrasives may also be used.
.: .-
- The compositions of the invention optionally may
also contain one or more minor ingredients such as fabric
conditioning agents, enzymes, perfumes (including
lQ deoperfumes), micro-biocides, colouring agents,
fluorescers, soil-suspending agents (anti-redeposition
agents), corrosion inhibitors, enzyme stabilizing agents,
and lather depressants.
. '~
It has surprisingly been found that the activities
of enzymes and in particular lipase are well supported in
the use of such detergent formulations. Enzymes other
than lipase that may be present include protease,
amylase, oxidase and/or cellulase.
The lipolytic enzyme can usefully be added in the
- form of a granular composition of lipolytic enzyme with
carrier material (eg. as in EP 0258068 and Savinase and
Lipolase products of Novo).
-~
The added amount of lipolytic enzyme can be chosen
within wide limits, for example 50 to 30,000 LU/g of
detergent composition, eg. often at least 100 LU/g, very
usefully at least 500 LU/g, sometimes preferably above
1000, above 2000 LU/g or above 4000 LU/g or more, thus
very often within the range 50-4000 LU/g and possibly
within the range 200-1000 LU/g.
The lipolytic enzyme can be chosen from among a wide
range of lipases: in particular the lipases described in
for example the following patent specifications, EP
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2008387
- 14 -
0214761 (Novo), EP 0258068 (Novo) and especially lipases
showing immunological cross-reactivity with antisera
raised against lipase from Thermomyces lanuginosus ATCC
22070, EP 0205208 (Unilever) and EP 0206390 (Unilever),
and especially lipases showing immunological
cross-reactivity with antisera raised against lipase from
Chromobacter viscosum var lipolyticum NRRL B-3673, or
against lipase from Alcaligenes PL-679, ATCC 31371 and
FERM-P 3783, also the lipases described in specifications
WO 87/00859 (Gist-Brocades) and EP 0204284 (Sapporo
Breweries). Suitable in particular are for example the
following commercially available lipases preparations:
Novo Lipolase, Amano lipases CE, P, 9, AP, M-AP, AML,
CES, and Meito lipases MY-30, OF, and PL, also esterase
MM, Lipolzym, SP225, SP285, Saiken lipase, Enzeco lipase,
Toyo Jozo lipase and Diosynth lipase (Trade Marks).
Genetic engineering of the enzvmes can be achieved
by extraction of an appropriate lipase gene, eg. the gene
for lipase from Thermomyces lanuginosus or from a mutant
thereof, and introduction and expression of the gene or
derivative thereof in a suitable producer organism such
as an Aspergillus. The techniques described in WO
88/02775 (Novo), EP 0243338 (Labofina) and EP 0268452
(Genencor) may be applied and adapted.
Similar considerations apply mutatis mutandis in the
case of the other enzymes. Without limitation: Amylase
can for example be used when present in an amount in the
range about 1 to about 100 MU (maltose units) per gram of
detergent composition, (or 0.014-1.4, eg. 0.07-0.7, KNU/g
(Novo units)). Cellulase can for example be used when
present in an amount in the range about 0.3 to about 35
CEVU units per gram of the detergent composition.
Protease can for example be used when present in an
: :
- . : . : : -

20(~8~
- 15 -
'' "''' '.
amount in the range about 0.0002 to about 0.05 Anson
units per gram of the detergent composition.
In general, the solids content of the product may be
within a very wide range, for example from 10-90%,
usually from 30-80% and preferably from 50-65%, by weight
of the final composition. The solids should be in
particulate form and ideally should have an average
particle size of less than 300 microns, preferably less
than 200 microns, more preferably less than 100 microns,
especially less than 10 microns. The particle size may
even be of sub-micron size. The proper particle size can
be obtained by using materials of the appropriate size or
by milling the total product in a suitable milling
apparatus.
The solid phase may ba dispersed in the products of
the present invention by any means known in the art. ~-
. .
Preferably, the products of the present inYention
also contain one or more dispersants for modifying the -
rheology of the dispersion. Most preferred are the
deflocculants described in European patent specification
EP-A-266 199 (Unilever P~C), for example dodecyl benzene
sulphonic acid or lecithin.
Alternatively or additionally, other known
dispersants which may be used are the highly voluminous
inorganic carrier materials descri~ed in GB patent
specifications 1 205 711 and 1 270 040, chain
structure-type clays as described in EP-A-34 387 cationic
quaternary amine salt surfactants, urea, a
substituted-urea or -guanidine according to GB 2 179 346
or J 61 227 829, or substituted urethanes, according to J
61 227 830.
. ~
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- 16 - Z008~87
The compositions are substantially non-aqueous, i.e.
they little or no free water, preferably no more than 5%,
- preferably less than 3%, especially less than 1% by
; weight of the total composition. It has been found by
S the applicants that the higher the water content, the
more likely it is for the viscosity to be too high, or
even for setting to occur. However, this may at least in
part be overcome by use of higher amounts of, or more
effective deflocculants or other dispersants.
Since the objective of a non-aqueous liquid will
generally be to enable the formulator to avoid the
negative influence of water on the components, e.g.
causing incompatibility of functional ingredients, it is
clearly necessary to avoid the accidental or deliberate
addition of water to the product at any stage in its
life. For this reason, special precautions are necessary
in manufacturing procedures and pack designs for use by
the consumer.
Thus during manufacture, it is preferred that all
raw materials should be dry and (in the case of
hydratable salts) in a low hydration state, e.g.
anhydrous carbonate builder and sodium perborate
monohydrate, where the latter is employed in the
composition. In a preferred process, the dry,
substantially anhydrous solids are blended with the
liquid phase in a dry vessel. In order to minimise the
rate of sedimentation of the solids, this blend is passed
through a grinding mill or a combination of mills, e.g. a
colloid mill, a corundum disc mill, a horizontal or
vertical agitated ball mill, to achieve a particle size
of 0.1 to 100 microns, preferably 0.5 to 50 microns,
ideally 1 to 10 microns. A preferred combination of such
mills is a colloid mill followed by a horizontal ball
mill since these can be operated under the conditions
, .

- 17 - 20~8387
required to provide a narrow size distribution in the
final product. Of course particulate material already
having the desired particle size need not be subjected to
this procedure and if desired, can be incorporated during
a later stage of processing.
During this milling procedure, the energy input
results in a temperature rise in the product and the
liberation of air entrapped in or between the particles
of the solid ingredients. It is therefore highly
desirable to mix any heat sensitive ingredients into the
product after the milling stage and a subsequent cooling
step. It may also be desirable to de-aerate the product
before addition of these (usually minor) ingredients and -
optionally, at any other stage of the process. Typical
ingredients which might be added at this stage are
perfumes and enzymes, but miqht also include highly
temperature sensitive bleach components or volatile
solvent components which may be desirable in the final
composition. However, it is especially preferred that
volatile material be introduced after any step of
aeration. Suitable equipment for cooling (e.g. heat
exchangers) and de-aeration will be known to those
skilled in the art.
It follows that all equipment used in this process
should be completely dry, special care being taken after
any cleaning operations. The same is true for subsequent
storage and packing equipment.
The invention will now be illustrated by the
following non-limiting example.

- 18 - 20~8~87
EXAMPLE
The following liquid products were prepared.
Composition:
Inaredients (wt%) A B
Nonionic surfactant1 27.5 30.0
Glyceryl triacetate 12.5 13.0
ABS acid 4.0 4.0
Soap 2.0
Silica3 0.3 0.3
Sodium carbonate 27.5 18.0
Sodium bicarbonate - 12.4
Sodium disilicate 3.5
Sodium perborate monohydrate 11.0 10.5
4 4.0 3 0
CP5 polymer 4.0 4.0
Minor ingredients balance balance
Notes
1 - Such as PLURAFAC RA30 which is a C13/l5 fatty
alcohol alkoxylated with an average of 4 to 5 moles
ethylene oxide and 2 to 3 moles propylene oxide (ex
ICI) or LIALET 111 - 7E0 (ex Enichem, Italy) which
is approximately a Cll fatty alcohol alkoxylated
with an average of 7 moles ethylene oxide.
2 - Alkyl (ie. dodecyl) benzene sulphonic acid (as free
acid).
3 - Highly voluminous silica (Aerosil).
: . -~: : . . . ,, ,~, : : . . . : . . . -

- 19 - 20~8387
4 - SOKALAN CP5 which is an acrylic acid/maleic acid
copolymer in the sodium salt form with an average
molecular weight of 70,000 and an acrylic
acid : maleic acid ratio of 1:1 (ex BASF). This may
be successfully replaced by VERSA TL3 which is the
sodium salt of a 3:1 sulphonated styrene/maleic
anhydride copolymer with a molecular weight of
34'000-
':: '' .,- ~ ' ' . . ' ''- ' , ' . ' :
.. , , ~
- . ~ . , .. .-
- ~ : - . ~ :. .

Representative Drawing

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Administrative Status

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Event History

Description Date
Inactive: IPC from MCD 2006-03-11
Inactive: IPC from MCD 2006-03-11
Inactive: Adhoc Request Documented 1997-01-23
Inactive: Abandon-RFE+Late fee unpaid-Correspondence sent 1997-01-23
Application Not Reinstated by Deadline 1993-07-24
Time Limit for Reversal Expired 1993-07-24
Inactive: Adhoc Request Documented 1993-01-25
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 1993-01-25
Application Published (Open to Public Inspection) 1990-07-30

Abandonment History

Abandonment Date Reason Reinstatement Date
1993-01-25
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
UNILEVER PLC
Past Owners on Record
CORNELIS B. DONKER
LOUIS HO TAN TAI
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) 
Claims 1990-07-30 3 62
Cover Page 1990-07-30 1 22
Abstract 1990-07-30 1 16
Drawings 1990-07-30 1 7
Descriptions 1990-07-30 19 734
Fees 1991-12-17 2 59