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Patent 2073432 Summary

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(12) Patent Application: (11) CA 2073432
(54) English Title: LIQUID BLEACH COMPOSITION
(54) French Title: COMPOSITION DE 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 3/39 (2006.01)
  • C11D 17/00 (2006.01)
(72) Inventors :
  • VAN DE PAS, JOHANNES C.
  • FRANKENA, HIDDE
(73) Owners :
  • UNILEVER PLC
(71) Applicants :
  • UNILEVER PLC (United Kingdom)
(74) Agent: BERESKIN & PARR LLP/S.E.N.C.R.L.,S.R.L.
(74) Associate agent:
(45) Issued:
(86) PCT Filing Date: 1991-02-07
(87) Open to Public Inspection: 1991-08-09
Examination requested: 1992-11-26
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/EP1991/000260
(87) International Publication Number: EP1991000260
(85) National Entry: 1992-07-09

(30) Application Priority Data:
Application No. Country/Territory Date
90200290.6 (European Patent Office (EPO)) 1990-02-08
90202307.6 (European Patent Office (EPO)) 1990-08-28
PCT/EP90/01046 (Austria) 1990-06-27

Abstracts

English Abstract

2073432 9112309 PCTABS00006
A liquid detergent composition comprising an aqueous base, one or
more detergent active materials and a bleach material, said
composition comprising from 5 to 32 % by weight of solvent materials.


Claims

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


21
Claims
1. A liquid detergent composition comprising an aqueous
base, 10-60% by weight of detergent active material and
1-40% by weight of bleach material selected from
perborates and percarbonates, said composition comprising
from 5 to 32% by weight of solvent material comprising,
water or a mixture of water and a water-miscible solvent,
wherein the weight ratio of water to water-miscible
solvent is more than 1 : 1.
2. A liquid detergent composition according to claim 1
comprising from 1 to 40 % by weight of bleach materials.
3. A liquid detergent composition according to claim 1
wherein the bleach material is a perborate or a
percarbonate bleach.
4. A liquid detergent composition according to claim 1,
further comprising from 1 to 60 % of salting-out
electrolytes and from 0 to 50 % of builder non-soap
materials.
5. A liquid detergent composition according to claim 1
having a viscosity of less than 2,500 mPas at 21 s-1,
having a pH of 7.0 to 12.0 and being physically stable,
volume stable and having solid suspending properties.
6. A liquid detergent composition according to claim 1,
comprising a structure of lamellar droplets of detergent
active material.

22
7. Use of a compositions according to claim 1 for the
washing of fabrics.

Description

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


WO91/12309 PCT/EP91/00260
LIQUID BLEACH COMPOSITION 2 0 7 3 ~ 3 2
The present invention relates to a liquid detergent
composition comprising an aqueous base, detergent active
materials and a bleach material.
Liquid aqueous detergent compositions comprising one or
more bleach materials have been described in EP 293 040,
EP 2~4 904, EP 378 26i and EP 378 262 (P&G). A problem
of the formulations as disclosed in these patent
application is the relatively low level of activ~
materials. These low active levels generate tne n2ed o~
high dosages of li~uid detergent materials to be ~sed
per washing cycle.
Surprisingly it has now been found that stable liquid
detergent compositions can be formulated which do not
suffer from the above disadvantage, if specific levels
of solvent materials are used.
Accordingly the present invention relates to a liquid
detergent composition comprising an aqueous base, one or
more detergent active materials and a bleach material,
said composition comprising from 5 to 32 % by weight of
solvent materials.
For the purpose of the present invention the term
solvents is intended to cover water and water-miscible
solvents. Examples of water-miscible solvents are for
examp}e described in EP 293 040.
bleach material
.
Compositions according to the present invention
comprise a bleach material, whicn is preferably a
peroxygen bleach. This bleach component may be present
in the system in dissolved form, but preferred is that
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WO91/12309 'PCT/EP91/002~ .
2073`~32 2
no or only part of the peroxygen bleach is solubilized,
the remaining part preferably being present as solid
peroxygen particlQs ~hich are susp~nded in he s-~s~em.
Examples oF suit~ble bleach c^mpou.~', i-c'-.m~ e-
peroxide, the perborates, persul~ales, peroxy
disulfates, perphosphat2s, calciu~æ o~ld-s and 'h~
crystalline peroxyhydrates formed by reac~ing nydrogen
peroxide with urea or al~ali me~al czr~ona,e. ~lso
encapsulated bleaches ma~! be u~ed. ?r_~ L ~ed '~leaches
are only partially solubl- ln 'he sl~te~ ~,e~ial'~
preferr2d is the use of perbora`e or _e_~arbonate
bleaches.
Typical amounts of bleach will be between l and 40 % by
weight of the aqueous composition, more preferred from 7
to 30%, especially preferred from lO to 2S % by weight
of the composition.
The weight average particle size of the bleach particles
is preferably from more than 0.5, more préferably more
than 20 micrometer, especially preferably from 22-60
~j micrometer, even more preferably f,om 25 to 50
micrometer, most preferably from 30 to 45 micrometer. A
preferred method for determining the weight average
particle size involves the making of microscopy
Pictures of the li~uid detergent composition at a
magnification of between 50 and 600 (preîerably abcut
150~, followed by the manual or automatic counting of
the visible particles, measuring the particle diameter
for each particle and calculating the weight average
~` particle size for the visible particlPs.
-
.deteraent active materials
-` 35
Compositions of the present invention also comprise
detergent active materials. In the widest definition the
, . .
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WO91/12309 PCT/EP91/00260
3 2~73~32
detergent active materials in general, may comprise one
or more surfactants, and may be selected from anionic,
cationic, nonionic, zwitterionic and amphoteric species,
and (provided mutually compatible) mixtures th~reof. For
example, they ~ay be chosen from any of the classes,
sub-classes and specific materials described in "Surface
Active Agsnts" Vol. I, by Schwartz & Perry, Interscience
1949 and "Surface Active Agents" Vol. II by Schwartz,
Perry & Berch (Interscience 1958), in the current
edition of "`~lcCu~cheon's Emulsifiers & Detergents"
published by the McCutcheon division of ~anufac~uring
Confectioners Company or in Tensid-Taschenburch", H.
Stache, 2nd Edn., Carl Hanser Verlag, Munchen & '~ien,
1981.
Suitable nonionic surfactants include, in particular,
the reaction products of compounds having a hydrophobic
group and a reactive hydroge~ atom, for example
aliphatic alcohols, acids, amides or alkyl phenols with
; 20 alkylene oxides, especially ethylene oxide either alone
or with propylene oxide. Specific nonionic detergent
compounds are alkyl (C6-C18) primary or secondary
linl~ar or branched alcohols with ethylene oxide, and
products made by condensation of ethylene oxide with the
2S reaction products of propylene oxide and
ethylenediamine. Other so-called nonionic detergent
compounds include long chain tertiary amine oxides, long
chain tertiary phosphine oxides and dialkyl sulphoxides.
Also possible is the use of salting out resistant active
materials, such as for example described in EP 3?8 177,
especially the use of alkyl poly glycoside surfactants,
such as for example disclosed in EP 7 0 07 4 .
:,
35 Suitable anionic surfactants are usually water-soluble
alkali metal salts of organic sulphates and sulphonates
; having alkyl radicals containing from about 8 to about
, ., ' ' ' "

WO91/12309 PCT/EPgltOO~'~
2 07 3`a~ ~ 4
22 carbon atoms, the term alkyl being used to include
the alkyl portion of higher acyl radicals. Examples of
suitable synthetic anionic detergen~ psu~.ds 2~_
sodium and potassium alXyl sulp;~ates, .'s~25ialli' '-.lOSZ
5 obtained by sul~hating highar ~~3-~ 3; :_~h ~ d
for example from tallow or coconut oil, sodium and
potassium alXyl (Cg-C20) benz2rl2 sulp..3nat~s,
particularly sodium linear secondary a .{yl (C10-C1~)
benzene sulphonates; sodium alXyl glyc~-f~l e~,h2r
sulphates, especially those e~ers of ~ ig~.o~
alcohols derived ~rom t,2110-.~ Oi- _~c3a~ 3;:d
synthetic alcohols d~rived rrom _etrol2um i so~iu~
coconut oil fatty monoglyceride sulpha~as and
sulphonates; sodium and potassium salts of sulphuric
acid esters of higher (C8-C1~) fatty alcohol-alkylene
oxide, particularly ethylene oxide, reaction products;
the reaction products of fatty acids such as coconut
fatty acids esterified with isethionic acid and
neutralised with sodium hydroxide; sodium and potassium
salts of fatty acid amides of methyl taurine; alkane
monosulphonates such as those derived ~y reacting alpha-
olefins (C8-C20) with sodium bisulphite and those
derived from reacting paraffins ~ith S02 and Cl~ and
then hydrolysing with a base to produce a random
i~ 25 sulponate; and olefin sulphonates, which term is used to
describe the material made by reacting oleîins,
particularly C10-C20 alpha-olefins, with S03 and then
neutralising and hydrolysing the reaction product. The
preferred anionic detergent compounds are sodium (Cl1-
C15) alkyl benzene sulphonates and sodium or potassium
primary (C10-Cl8) alkyl sulphates.
It is also possible, and sometimes preferred, to include
an alXali metal soap of a ratty acld, especially a soap
of an acid having from 12 to 18 carbon atoms, for
example oleic acid, ricinoleic acid, and ratty acids
~ derived from castor oil, alXylsuccinic acid, rapeseed
:,'`'
.

WO91/12309 PCT/EP91/00260
2073~32
oil, groundnut oil, coconut oiI, palmkernel oil or
mixtures thereof. The sodium or potassium soaps of these
acids can be used.
The tocal detergent active material may be present at
from 5% to 70% by weight of the total composition, for
exampla from 10% to S0% and typically from 20% to 50% by
weight.
solv2nts
Compositions according to the invention comprise from 5
to 32 % by weight of solvent materials which are
selected from the group of water and water-miscible
solvents. Preferred levels of solvent materials are from
l0 to 30 % by weight of the compostion, more preferably
from 15 to 29 %, most preferably from 20 ~o 25 %.
Suitable water-miscible solvents are for exàmple lower
~Cl-C5) alcohols such as ethanol and iso-propanol, low
molecular weight (<l,000) Polyethyleneglycols,
alXyleneglycols for example propylene glycol etc. Other
suit2bls ~ater-miscible solvents are described in
EP 293 040. For the purpose of this invention glycerol
is not a solvent.
Preferably the solvent material comprises either water
alone or a mixture of water and one or more water-
miscible solvents. The preferred weight ratio of water
to water-miscible solvent is more than l : l, more
preferably from 2 : l to 500 : l, most preferabily from
3 : l ~o 50 : l.
o~tional inaredients
Compositions of the invention may be un-structured
(isotropic) but are preferably structured. Structured
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WO91/12309 PCT/~P9l/00~'~
- 2073~32 6
liquids of the invention may be intPrnally st.uctur~d
whereby the structure is formed ~y the detergent active
materials in the composition or P{t2rnally s-t ~c~ured,
whereby the structure is provided by an exter;lal
structuranc. Pref2ra~1y cs~positior.~ o. ~ n~ o.-
are internally structured. ~ost preferably compositions
of the invention comprise a structur2 of lamella r
droplets or detergent active matarials.
Some of the diffsrent kinds of a5tiVe-St'-''Ct''..i~ J 7h,ioh.
are possi~le are dascribed in tll2 reL~renc~ ~i.A. ~a. n~5,
"Detergents1', Ch.2. in K. Walters (~d), "~eome'_-ry:
Industrial Applications", J. ~iley & Sons, Le~chworch
1980. In general, the degree of ordering of such systems
increases with incrPasing surfactant and/or electrolyte
concentrations. At very low concentrations, the
surfactant can exist as a molecular solution, or as a
solution of spherical micelles, both of these being
isotropic. With the addition of further surfactant
` 20 and/or electrolyte, structured (antisotropic) systems
l can form. They are referred to respectively, by various
ter~s such as rod-micelles, planar lamellar structures,
! lamellar droplets and liquid crystalline phases. Often,
different workers have used different terminology to
refer to the structures which are really the same. For
instance, in European patent specification EP-A-151
884, lamellar droplets are called "spherulit2s".
The presence and identity of a surfactant structuring
system in a liquid may be determined by means known to
those skilled in the art for example, optical
techniques, various rheometrical measurements, x-ray or
neutron diffraction, and sometimes, electron microscopy.
When the compositions are of lamellar droplet str~cture
then in many cases it is preferrsd for the aq~eous
continuous phase to contain dissolved electrolyte. As

WO91/12309 PCT/EP91/00260
7 2~73432
used her~in, the term electrolyte means any ionic water
soluble material. However, in lamellar dispersions, not
all the electrolyte is necessarily dissolved but may be
suspended as particles of solid because the total
~lectroly~a concentration of the liquid is higher than
the solubility limit of the electrolyte. Mixtures of
21~c trolytes also may be used, with one or more of the
electrolytes being in the dissolved agueous phase and
one or mora being substantially only in the suspended
l~ solid phasa. ~o o more el~ctrolytes may also be
dlstributsd approximately proportionally, between these
~wo phases. In part, this may depend on processing, e.g.
the order of addition of components. On the other hand,
the term "salts" includes all organic and inorganic
; 15 materials which may be included, other than surfactants
and water, whether or not they are ionic, and this term
encompasses the sub-set of thè electrolytes (water
soluble materials).
`20 The selection of surfactant types and their proportions,
in order to obtain a stable liquid with the required
structure will be fully within the capability of those
skilled in the art. However, it can be mentioned that an
important sub-class of useful compositions is those
where the detergent active material comprises blends of
different surfactant types. Typical blends useful for
: fabric ~ashing compositions include those where the
primary surfactant(s) comprise nonionic and/or a non-
alkoxylated anionic and/or an alkoxylated anionic
surfactant.
,
In th2 cas2 of blends of surfactants, the precise
proportions of each component which will result in such
stability and viscosity will depend on the type(s~ and
amount(s) of the electrolytes, as is the case with
conventional structured liquids.
' '
.
'

WO91/12309 PCT/EP91/002~
2~73432
Preferably though, the compositions contain from 1~ to
60%, especially from 10 to 45% of a salting-out
electrolytPO Salting-out Plectrolyt2 has the ~Par.ing
ascribed to in specification ~-A-79 o~6~ that ls
salting-out electrolytos h~ve a l~ot_ 03i~ r~ 5e- o^ ~
than 9.5. Optionally, some salting-in electrolyte ~as
defined in the latter specification) ma~ also be
included, provided it is of a ~ind and in an amounc
compatible with the other components and th composltion
is still in accordance with the definitio~ o' the
invention clai~ed herein.
Some or all or the alectrolyte (whether salting-in or
salting-out), or any substantially water insoluble salt
which may be present, may have detergency builder
properties. In any event, it is preferred that
compositions according to the present invPntion include
detergency builder material, some or alI of which may be
electrolyte. The builder material is any capable of
reducing the level of free calcium ions in the wash
liquor and will preferably provide the composition with
other beneficial properties such as the generation of an
alkaline pH, the suspension of soil removed from the
fabric and the dispersion of the fabric softening clay
material. Preferably the salting-out electrolyte
comprises citrate.
Preferably the weight ratio of water to salting-out
electrolyte is from 10 : 1 to 1 : 1, more preferably
from 8 : 1 to 2 : 1. The weight ratio of water-miscible
solvent to salting out electrolyte is preferably from 1
: 1 to 1 : 20, more preferably 1 : 2 to 1 : lO, most
preferably 1 : 8 to l : 4.
;' .
Examples of phosphorus-containing inorganic detergency
builders, when present, include the water-soluble salts,
especially alkali metal pyrophosphates, orthophosphates,
:
, :

WO91/12309 PCT/EP91/00260
9 2073~32
polyphosphates and phosphonates. Specific examples of
inorganic phosphate builders include sodium and
potassium tripolYohosphates, phosphates and
hexametaphos~hat~s. Phosphonate sequestrant builders may
o ~ 2 '~
Exampl2s of non-phosphorus-containing inorganic
det2rg2ncy builders, when present, include-water-
soluble al'~ali m2tal carbonates, bicarbonates, silicates
and c~ys1-allino and ~morphous aluminosilicates. Specific
2~ampl es ' n~?uds sodium carbonate (with or without
calcite saeds), 2otassium carbonate, sodium and
potassi~m bicarbona-tes, silicates and zeolites.
Examples of organic detergency builders, when present,
include the alkaline metal, ammonium and substituted
ammonium polyacetates, carboxylates, polycarboxylates,
polyacetyl carboxyIates and polyhydroxysulphonates.
Specific examples include sodium, potassium, lithium,
ammonium and substituted ammonium salts of
ethylenediaminetetraacetic acid, nitrilitriacetic-acid,
oxydisuccinic acid, CMOS, TMS, TDS, melitic acid,
benzene ~olycarboxylic acids and citric acid.
Preferably the level of non-soap builder material is
from 0-50~ by weight of the composition, more preferred
from 5-40%, most preferred 10-35%.
In the context of organic builders, it is also desirable
to incorporate polymers which are only partly dissolved,
in the aqueous continuous phase as described in EP
. 301.882. This allows a viscosity reduction (due to the
polymer which is dissolved) whilst incorporating a
suffici~ntly high amount to achieve a secondary benefit,
especially building, because the part which is not
dissolved does not bring about the .instability that
would occur if substantially all were dissolved. Typical
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WO91/12309 PCT/EP9l/007'~
2~73~32 lo
amounts are from 0.5 to 4.5% by weight.
It is further 2ossible to include in the compositions of
the present in~ention, alternaiively, or in addition to
the 2artly dissolved polym~r, yet anocher pol~2r 7hish
-~ is substantially totally soluble in the aqueous phase
and has an electrolyte resistance of more than 5 grams
sodium nitrilotriacetat2 in 100ml of a 5~ by we1ght
aqueous solution of the polymer, said second pol~mer
also having a vapour pressure in 20% a~ueous solutlon,
equal to or less than the Yapour pressure of a ref eren.ce
.
2~ by weight or greater aqueous solution of po1yethylene
glycol having an average mol~cular ~elght of 6000; said
second polymer having a molecular weighl of at least
1000. Use of such polymers is generally described in our
EP 301,883. Typical levels are from 0.5 to 4.5% by
weight.
.
The viscosity of compositions according to the present
is preferably less than 2500 mPa.s, more preferred less
than 2000 mPas, most preferred less than 1500 mPa.s,
especially preferred between 30 and 900 mPa.s at 21 s~l.
, ` .
One way of regulating the viscosity and stability of
compositions according to the present invention is to
include viscosity regulating polymeric materials.
.i
Viscosity and/or stability regulating polymers which are
preferred for incorporation in compositions according to
the invention include deflocculating polymers having a
hydrophilic bac~bone and at least one hydrophobic side
chain. Such polymers are for instance described in our
copending European application E? 89201530.6
(EP 346 995). Preferably the amount of viscosity
regulating polymer is from 0.1 to 5% by ~eight of the
total composition, more preferred from 0.2 to 2%.
. ~
.: .
, .
,
.

WO91/12309 PCT/EP91/00260
11 2073432
Compositions o~ the invention may also comprise
materials ~or adjusting the pH. For lowering the pH it
is prere ~ed to use wPak acids, especially the use of
organic aci~5 is pre~rred, more preferred is the use of
5 C 1-3 _a~-bo:.1lic ~cids, most preferr2d is the use of
citric acid. The use of these pH lowering agents is
especiallv p eI2rrad whan the compositions of the
invention contain enz~m~s such as amylases, proteases
and lipGlases.
o
Apar_ ~-o.u '-h2 ing-~dients already mentioned, a number
of op~ional i~.gredi~nts may also be present, for example
lather boos'_rs such as al~anolamides, particularly the
monoethanolamides derived from palm kernel fatty acids
and coconut ~atty acids, fabric softeners such as clays,
amines and amine oxides, lather depressants, inorganic
salts such as sodium sulphate, and, usually present in
very minor amounts, fluorescent agents, perfumes,
germicides colourants and enzymes such as proteases,
cellulases, amylases and lipases (including Lipolase
(Trade MarX) ex Novo). Suitable examples of protease
enzymes are Savinase (ex Novo), Maxatal (gist-brocades),
Opticl2an (ex MXC) or ~P122 (ex Showa Den~o), Alcalase,
Maxatase, Esperase, Optimase, proteinase K and
subtilisin BPN. Suitable lipolases are for example
Lipolase (ex Novo), Amano lipases, Meito lipases,
Lipozym, SP 225, SP 285, Toyo Jozo lipase. Suitable
amylases are for example Termamyl (TM of Novo) and
Maxamyl. Suitable cellulases include Celluzym (ex Novo).
Liquid detergent compositions according to the invention
are preferably mhysically stable in that they show less
than 2% by volume phase separation upon storage for 21
days a~tor preparation at 25C.
Liquid detergent com~ositions according to the invention
are preferably volume stable in that they show less than
.
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WO91/12309 PCT/~P91/007~
207343~ 12
25~ preferably less than lO~, more preferably less than
5~ volume increase during storage at a temperature
between 20 and 37C for a period of thre~ months after
preparation.
Also preferably compositions according to the invention
have solid suspending properti~s, mo6t preferably the~
do not yield any visible sedimentation arter storage îor
three weeXs at 2l C.
~' 10
Compositions of the present invention may com~rise one
or more bleach precursor agents. A well-known example of
such an agent is T~ED. Preferably the bleach precursor
agent is preseni in the system in a-t least partly
undissolved form. One way of ensuring that the precursor
is present in undissolved form is to increase the amount
of electrolyte in the composition, therewith reducing
the solubility of the precursor in the system. Suitable
electrolytes for this purpose are for instance the at
least partially water soluble carbonate, sulphate and
halogenide salts.
Compositions of the invention may also advantageously
comp-ise one or more ingredients for the stabilization
of bleach materials. Suitable materials are for example
metaborate electrolytes and magnesium salts.
In use the detergent compositions of the inventention
will be diluted with wash water to form a wash liquor
for instance for use in a washing machine. The
concentration of liquid detergent composition in the
wash liquor is preferably from 0.05 to lO %, more
preferred from O.l to 3% by weight.
To ensure effective detergency, the liquid detergent
compositions prererably are alkaline, and it is
preferred that they should provide a pH within the range
:
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WO91/12309 PCT/EP91/00260
13 20734~2
of about 7.0 to 12, preferably about 8 to about 11, whenused in aoueous solutions of the composition at the
recommonded concentration. To meet this requirement, the
undiluted liquid composition should preferably be of a
~X a~o~;s ?, -~_ e,~ampl~ a~out ~H 8.0 io about 12.5. It
should b2 not~d that an excessively high pH, e.g. over
about pH 13, is less desirable for domestic safety.
Composltlons according to the invention may be prepared
by any m2thod for tne pro2aration of liquid detergent
compos'tl_ns. ~ p-efe_-ed ~ethod involYes the addition
of the wator-~iscible solvent and the salting out
elect-olytes (i~ any) to water, followed by the addition
of the ~ctives, the bleach ingredient and the remaining
ingrPdients.
The invention will now be illustrated by way of the
following Examples.
`
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2 0 7 3 ~ 3 2 PCT/EPg1/002~
! 14
Example I
The following compositions may be prepared by mixing the
ingrediants in the listed order:
5 Inarodi~n~ ~ ~t A 3
water 29 24
ethanOl __ 5
citrat~/citric acid1) 10 10
~BS 28 28
10 Synperonic A7 12 12
,: . pol ~m.Or2 )
; perborate.monohydrate 20 20
. ' 1
) this mixture is used to adjust the pH to 8.5
15 2) polymer A-11 as described in EP 346 995
. .
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.. . .
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.. : .

- WO91/12309 PCT/EP9l/00260
2 073 43 2
~ample II
The Collowing compositions were made by adding the
electrol1,7t2 tog2th~r with the minor ingredients except
5 ~or t:1e ~er~ e and _h~ en~l~es to wat-r of elevated
temperature, followed by the addition of the
deflocculating polymer and then the detergPnt active
mat rials as a prs-mix under stirring and thereafter
cooling tha mixture and adding the enzymes and the
10 perfl_mes.
Inqredient ?~ ~t~ a b c d
NaLas 21 24.5 21 21
Synperonic A7 9 10.5 9 9
15 Nametaborate.2aq 2.6 2.5 2.6 2.6
Nacitrate.2aq15.5 15.5 24.7 19.6
Dequest 2060S 0.4 0.4 O.4 o.4
Perborate.tetra 20 15 15 20
Alcalase 0.75 0.75 0.75 0.75
20 CaCl2.2aq 0.15 0.15 0.15 0.15
Tinopal CBS-X 0.1 0.1 0.1 0.1
Silicon DB1000.25 0.25 - 0.25 0.25
Perfume 0.3 0,3 0,3 0.3
polymer
25 water 28.95 28.95 28.95 28.95
pH g g g 9
Viscosity 1650 3730 1960 3580
` Volume stability 0% 0% 0~ o%
Phase separation stable stable stable stable
30 Bleach stability 95% 94% 98% 96%
`~ In the above table NaLAS refers ~o sodium linear C12
` alkyl benzene sulphonate, the polymer was a
deflocculating polymer as disclosed as A44 in EP 346
~, 35 995, the bleach was added as a 65 % dispersion in water
(Proxsol ex ICI), where necessary the pH was adjusted
~; with citric acid.
' '
~.
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: . . . .
. .
.. . .
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. ' .

WO91/12309 PCT/EP91/00~'~
æo73~32 16
The viscosity was measured in mPa.s at 21 5-1, the
volum~ st2bilit~ indicates the maximum volume increase
during storage fo. three months at ~mbient t~mperature,
Lhe blaach st.~bility indi-at2s th2 p2rc~ntage OI bl2ach
left after storage for 4 weeks at 37 oC. Compositions c
and d show2d some soIid sedimentation due to some
: crys-talli~ation of citrate.
The zbove results clearly show that pourable liquid
det2r~2n-t produrts can b2 made ~.~hich contain stable
bl2ach ingr~dien-ts, when only low levels of solvent
mat2rials ar2 us2d.
~ . .
:~
: ~ .
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, :
,
,
.

WO91/12309 PCT/EP91/00260
17 2073~32
Exam~le III
~;
The following composition was prepared by adding the
electrolyte together -~ith -the minor ingredients except
for the p2~ -. ~3_ ar.d '~ en~_~.es to water of elevat~d
temperatur , follo~ed by the addition of the detergent
active material as a premix under stirring and
thereaft r cooling the mix-ture and adding the enzymes,
perfumes and Lna bleach.
: INGRED~T~ r~ ~) A
Na-Do~s 2l
Synperonic A7 9
- Glycerol 3.5
. 15 Sodium-Metaborate 2.6
Nacitrate/Citric acid l) 9.8
Dequest 2060S ~as 100%) 0.4
Na-per~orate tetrahydrate 3) ` 20
Enzyme, Alcalase O.8
20 cacl2.2H2o 0.2
. Fluorescer, Tinopal CBSX O.l
Silicon, Dow Corning DBlOO 0.3
Perfume 0.3
Deflocculating polymer 4)
~:~ 25 Water balance
pH 9
l) This mixture is used to adjust the final pH.
2) Expressed as % of analyzed enzyme level in the fresh
` ~ 30 sample.
3) As 100% perborate, added as a dispersion (Proxsol ex
. ; ICI, ap~roximat2 65% per~orate dispersion in water
`~ ~ with an average perborate particle size of 40
micrometer).
~ 35 4) Deflocculating polymer oî formula I of EP 346 99S,
:: wherein x=50l y=O, R5=H, R6=CH3, Rl= -CO-O, R2 and R3
are absent, R4= -Cl2H25, mW=7,500.
;,
,
,~
- ~ "
:

2 a ~ 3 1 ~ 2 18 PCT/EP91/00?'~
5) wt~ -a~pro~imate- of total perborate, obtained by
removal of the undissolved bleach particles by mild
centriîugation.
The obtained mroduct had the following characteristics:
A
i lC Volum2 stabili'-y (~ volume 4
:~ increase, 3 molltns 25C)
claar l~y2~ sepa~ation no
(3 weeks 37C)
solld sedimentation - no
(3 wee~ 37C)
Viscosity 21 s-l 1,350
: Viscosity 10-4 s-l 200,000
dissolved perborates 5) 3
bleach activity 99
(2 months ambient T~
enzyme activity 65
(2 months ambient T)2)
:
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WO91/12309 PCT/EP91/00260
19 2~73~32
Example IV
The following rormula-tions may ba prepared by adding the
ingredient~ ;_o .ia~-r 1;~ t-~2 1 ' st2d 5rdr.
Inqredient Composition % wt
1 2
Na-Dobs . 9,1 17.3
10 Synperonic ~ 3 6 1.3
: Na Stearata -- o.g
Glyca.ol 8.1 3.0
NaOH 1.0 --
Na-metaborate ~.8 2.0
15 Na-perborate 20 10
Na-citrate -- 5.0
Citric acid 1.5 --
Zeolite A4 25.3 30.0
NaCMC -- 0.3
20 Tinopal CBS-X -- 0.13
Perfume -- - O.22
Alcalase 2.34~ -- 0.5
Polymer *) O.5 0.5
Water --to 100
*) polymer A-11 as described in EP 89201530.6
(EP 346 995).
'
. :
.
'
~, .
.
. . . . . . .

WO91/12309 PCT/EP91/002
207~32
E~ampl 2 V
.
The following det~rgent compositions may be prepared as
. 5 in example IV.
In~red~nr Composition ~ wt
l 2
~Ta-Dobs lO.2 --
lO ~lC-Dobs -- lO.7
Synperonic A7 19.3 19.3
Na Oleat~ lO.3 --
: ~ Oleate -- 10.3
Glycerol 5.0 5.0
15 Na-metabor2te 3.5 3.5
Na~perborate.4H2O lO.0 15.0
Na-citrate 2aq lO.0 --
2C3 -- 4.0
Sokolan CP5 2.5 --
`~ 20 Dequest 2066 0.4 --
~ Mg-silicate -- 0.4
: Silicon DB lO0 0.3 0.3
Tinopal CBS-X 0.5 0.5
Sa~inas2 O.l O.l
5 Amylase O.l O.l
., Perfume O.l O.l
Dye 0.3 0.3
Polymer *~ l.0 l.0
*) polymer A-ll 2S disclosed in EP 89201530.6
` (EP 346 995).
.
:
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,
'
.

Representative Drawing

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Administrative Status

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Event History

Description Date
Inactive: IPC from MCD 2006-03-11
Time Limit for Reversal Expired 1998-02-09
Application Not Reinstated by Deadline 1998-02-09
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 1997-02-07
Request for Examination Requirements Determined Compliant 1992-11-26
All Requirements for Examination Determined Compliant 1992-11-26
Application Published (Open to Public Inspection) 1991-08-09

Abandonment History

Abandonment Date Reason Reinstatement Date
1997-02-07
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
UNILEVER PLC
Past Owners on Record
HIDDE FRANKENA
JOHANNES C. VAN DE PAS
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) 
Abstract 1991-08-08 1 36
Drawings 1991-08-08 1 10
Abstract 1991-08-08 1 43
Cover Page 1991-08-08 1 19
Claims 1991-08-08 2 47
Descriptions 1991-08-08 20 675
Fees 1996-01-14 1 71
Fees 1995-01-15 1 58
Fees 1994-01-16 1 41
Fees 1993-01-14 1 41
International preliminary examination report 1992-07-08 15 471
Courtesy - Office Letter 1992-09-23 1 27
Prosecution correspondence 1992-11-25 1 25
Courtesy - Office Letter 1993-02-25 1 31
Prosecution correspondence 1995-07-12 5 222
Examiner Requisition 1994-12-12 2 86
Examiner Requisition 1996-07-08 2 74