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Patent 2190739 Summary

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(12) Patent Application: (11) CA 2190739
(54) English Title: DETERGENT COMPOSITION
(54) French Title: COMPOSITION DETERGENTE
Status: Dead
Bibliographic Data
(51) International Patent Classification (IPC):
  • A61K 8/81 (2006.01)
  • A61K 8/36 (2006.01)
  • A61K 8/44 (2006.01)
  • A61K 8/46 (2006.01)
  • A61K 8/60 (2006.01)
  • A61Q 19/10 (2006.01)
(72) Inventors :
  • JOBLING, MARGARET (United Kingdom)
  • TSAUR, LIANG SHENG (United States of America)
  • SHEN, SHIJI (United States of America)
(73) Owners :
  • UNILEVER PLC (United Kingdom)
(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: 1995-07-18
(87) Open to Public Inspection: 1996-02-01
Examination requested: 1997-05-07
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/GB1995/001687
(87) International Publication Number: WO1996/002224
(85) National Entry: 1996-11-19

(30) Application Priority Data:
Application No. Country/Territory Date
9414575.2 United Kingdom 1994-07-19

Abstracts

English Abstract






An aqueous liquid cleansing and moisturising composition comprising a surface active agent, a skin benefit agent having a weight
average particle size in the range 50 to 500 microns and a structurant. The composition is substantially free of insoluble fatty acid soap
and has a viscosity of at least 5000 Pas at a shear stress of 0.01 Pa at 25°C.


French Abstract

Une composition nettoyante et hydratante liquide et aqueuse comprend un agent tensioactif, un agent adoucissant pour la peau dont la granulométrie moyenne pondérale est comprise entre 50 et 500 microns, et un agent structurant. La composition est pratiquement exempte de savon renfermant des acides gras insolubles et a une viscosité d'au moins 5 000 Pas à une contrainte tangentielle de 0,01 Pa à 25 ~C.

Claims

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






- 19 -
1. An aqueous liquid cleansing and moisturising composition
comprising: -

a) a surface active agent selected from anionic,
nonionic, zwitterionic, and cationic surface active
agents, and mixtures thereof;
b) a benefit agent having a weight average particle
size in the range 50 to 500 microns; and
c) at least one structurant;
wherein the composition is substantially free of insoluble
fatty acid soap and has a viscosity of at least 5,000 Pas at
a shear stress of 0.01 Pa at 25°C.
2. A composition according to claim 1 wherein the
structurant is selected from swelling clays; fatty acid and
derivatives thereof; cross-linked polyacrylates; acrylates
and copolymers thereof; polyvinylpyrrolidone and
copolymers thereof; polyethylene imines; salts; sucrose
esters; gellants; and mixtures thereof.
3. A composition according to claim 1 wherein the benefit
agent is selected from silicone oils; gums; fats; oils;
waxes: hydrophobic plant extracts; hydrocarbons; higher fatty
acids: higher fatty alcohols; esters; essential oils; lipids;
phospholipids; vitamins; sunscreens; and mixtures thereof.
4. A composition according to any one of the preceding
claims comprising 0.1 to 15 wt% of the benefit agent.

- 20 -
5. A composition according to any one of the preceding
claims wherein the benefit agent functions as a carrier to
deliver efficacy agents to skin treated with the composition.
6. A composition according to any one of the preceding
claims comprising 1 to 35 wt% of the surface active agent.
7. A process for preparing a composition according to claim
1 comprises:-
a) structuring the base formulation comprising at least one
surface active agent selected from anionic, nonionic,
zwitterionic and cationic surface active agents and mixtures
thereof; and
b) mixing the structured base formulation with the benefit
agent.
8. A method of depositing a benefit agent from an aqueous
liquid cleansing and moisturising composition, the method
comprising providing the benefit agent in a composition
comprising
a) a surface active agent selected from anionic, nonionic,
zwitterionic, and cationic surface active agents, and
mixtures thereof;
b) the benefit agent having a weight average particle size
in the range 50 to 500 microns; and
c) at least one structurant;
the composition being substantially free of insoluble fatty
acid soap and having a viscosity of at least 5,000 Pas at a
shear stress of 0.01 Pa at 25°C.

Description

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


21 90739
Wo 96l02224 PCT/GB95101687
-- 1 --
~ET~(-.~l`TT C~l`qPOST~ION
The present invention relates to detergent compositions
suitable for the care and personal washing of the skin. In
particular, it relates to compositions which are f~
to give mild cleansing and conditioning of the skin.
Compositions formulated to cleanse the skin are well known.
It is also known to formulate products which provide both a
cleansing and a moisturising benefit.
For example WO 90/13283 discloses a composition comprising an
acyl ester of an isethionic acid salt, a long chain fatty
acid, a moisturiser component and, optionally, soap.5
One of the problems which may be encountered with such dual
~urpose compositions is that, whilst cleansing may be
effective, there is an insufficient level of moisturising.
We have found a way of f~ tinsr such compositions such
that they can deliver effective moisturising, conditioning or
protection of the skin.
In WO 94/01085 and 94/01084 the advantage of depositing large
particles of petrolatum from soap based compositions to
moisturise the skin is recognised.
E~owever, according to Wo 94/03152, r~nrPrnP~l with shower gels
comprising a non-soap detergent, qi ~ i cnnp oil added to
3 o condition the skin and cationic polymers, the maximum average
droplet size of the q11 icr~nP oil that can be used is 2
microns, if product stabilicy is to be T--int~inPd
We have now f ound that larger particles, by particle is meant
a solid particle or licruid droplet, of benefit agenes such as

2 1 9073q
Wo 96/02224 ~ i687
-- 2
silicone oil can be incorporated in~o non-soap based
compositions and stable composi~ions formed by the use of
structurants .
Thus, i9rcor~li n~ to the invention there is provided an as[ueous
liquid cleansing and moisturising composition comprising:-
-
a3 a surface active agent selected rom anionic,
nonionic, zwitterionic, and cationic surface active
agents; and mixtures thereof;
b) a benefit agent having a weight average particle
size in the range 50 to 500 microns; and
c) at least one structur~nt;
wherein the composition is subst~nr;~lly free of ;nc~ hle
fatty acid soap and has a viscosity of at least 5, 000 Pas at
a shear stress of 0_ 01 Pa at 25C.0
The viscosity quoted is the minimum viscosity required to
suspend benef it agent having a welght average particle size
of 50 microns such that the composition has a separation rate
at 25C o less than l~n per year.5
As the weight average particle size o the benefit agent
increases much higher viscosities are re~uirsd to give a
composition with the same stability,
The comPositiOn is suitable for cleansing and ~moisturising",
"conditioning" or "protection~ of the skin. The benefit
agent is included in the composition to moisturise, condition

21 90739
W0 96/0222~ ,L. ~ 1687
-- 3
and/or.protect the skin. sy ~benefit agent~' is meant a
sUDstance that softens the skin (stratum corneum) and keeps
it soft by retarding the decrea3e of its water content or
protects the skin.
s

Preferred benefit agents include
a) silicone oils, gums and modifications thereof such
as linear and cyclic polydimethyl si ln~rAn~q; amino,
alkyl alkylaryl and aryl silicone oils:
b) fats and oils including natural fats and oils such
as jojoba, soyabean, rice bran, avocado, almond,
olive, sesame, persic, castor, coconut, mink oils;
cacao fat, beef tallow, lard; hardened oils
obtained by hydrogenating the af.,L~ rinn~-l oils;
and synthetic mono, di and triglycerides such as
myristic acid glyceride and 2-ethylhexanoic acid
glyceride;
cl waxes such as ~-~rn~llhA, spermaceti, beeswax,
lanolin and derivatives thereof;
d) hydrophobic plant extracts;
e) hydrocarbons such as liquid paraffins, petrolatum,
microcrystalline wax, ceresin, squalene, squalane,
and mineral oil;
f ~ higher fatty acids such as lauric, myristic,
palmitic, stearic, behenic, oleic, linoleic
linolenic, lanolic, isostearic and poly unsaturated
fatty acids (PUFA) acids,
g) higher alcohols such as lauryl, cetyl, steryl,
oleyl, behenyl, cholesterol and 2-
3 o alcohol;
h) esters such as cetyl octanoate, myristyl lactate,
cetyl lactate, isopropyl myristate, myristYl
myristate, isopropyl palmitate, isopropyl adipate,
butyl stearate, decyl oleate, cholesterol
isostearate, glycerol monostearate, glycerol
_ _ _ _ . . . . .

2l 90739
WO 96/02224 PCT/GB95/01687
-- 4 --
istearate, glycerol tristearate, alkyl lactate for
example lauryl lactate, alkyl citrate and alkyl
tartrate;
i) essential oils such as ~ish oils, mentha, jasmine,
camphor, white cedar, bitter orange peel, ryu,
turpentine, r; nni , b~L~Iw~t, citrus unshiu,
calamus, pine, lavender, bay, clove, hiba,
eucalyptus, lemon, starflower, thYme, porpPrmint,
rose, sage, menthol, cineole, eugenol, citral,
citronelle, borneol, linalool, geraniol, evening
primrose, camphor, thYmol~ q~irAntol~ pinene,
1 im~n~ne and ~erPenoid oils;
j ) lipids such as cholesterol, ceramides, sucrose
esters and pseudo-cPrRmi ~9PC as described in
European Patent Specification No. 556 957;
k) vitamins such as vitamin A and E, and vitamin alkyl
esters, including those vitamin C alkyl esters;
1) sunscreens such as octyl methoxyl rinnA---tP (Parsol
MCX) and butyl methoxy benzoylmP~hRn~ (Parsol
1789);
:n) Phosrhr~l i ri'lq; and
n) mixtures of any of the ~oregoing componen~s.
The benefit agent may be incorporated in a carrier in the
compositicns o~ the invention, particularly if it is likely
to suffer detrimental interactionS with other c ^~tq of
the composition. ~enefit agents for which such detrimental
interactions may occur include lipids; alkyl lactates;
sunscreens; esters such as isopropyl palmitate and isopropyl
myris~ate; and vitamins. The carrier can, for example, be a
silicone or hydrocArbon oil which is not solubilised~
mi rPl l; qed by the surface active phase and in which the
benef it agent is r~latively soluble .

2~ 90739
Wo 96/02224 PCr/GB95/01687
_ 5 _
Particularly preferred benefit agen~s include silicone oils,
gums and modifica~ions thereof; esters such as isopropyl
palmitate and myris~ate and alkyl lactates.
The benefit agent is preferably present in amount of from 0.1
to 15 wt%, most preferably from 0.2 to 10 wt96, more
preferably from 0 . 5 to 7 wt9s
An advantage of the composition according to the invention is
that, during use, it deposits benefit agent onto the skin at
a level which results in a perceivable benefit. Without
being bound by theory, it is believed the benefit agent is
dispersed into large pools during dilution of the composition
in use and these pools deposit readily onto the skin.
In WO 94/01084 and WO 94/01085 compositions comprising large
particles of petrolatum are structured by the presence of at
least 5wt% insoluble fatty acid soaP. ~owever, it is
believed such high levels of solid phase material may
adversely affect the amount of benefit agent deposited onto
the skin. Thus, in the present invention we require the
composition to be subs~ntl ~1 ly free of insoluble fatty acid
soap, by which is meant the level of insoluble fatty acid
soap is below 1 wt& based on the composition.
Structurants are an essential feature of the present
invention. Suitable structurants are those materials which
when added to a composition, will increase the zero shear
rate viscosity. They include swelling clays, for example
laponite: fatty acid and derivatives thereof, in particular
atty acid monoglyceride polyglycol ether: cross-linked
polyacrylates such as Carbopol (TM) (polymers available from
Goodrich): acrylates and copolymers thereof;

Wo96/02~24 2 1 90739 ~ C~ 7
-- 6 --
polyvinylpyrrolidone and copolymers thereof; polyethylene
imines; salts such as sodium chloride and ammonium sulphate:
sucrose esters; gellants; and mixtures thereof.
Of the clays particularly preferred are synthe~ic hectorite
( laponite) clay used in conjunction with an electrolyte salt
capable of causing the clay ~o thicken so as to suspend the
benefit agent. Suitable electrolytes include alkali and
AlkAl;n~ earth salts such as halides, ammonium salts and
sulphates.
Particularly preferred structurants include fatty acids and
derivatives thereof and cross-linked polyacrylates.
1~7hilst some materials can function as both a benefit agent
and structurant it will be a~preciated that the benefit and
s~ructuring function cannot be provided by the same
~nt, }Iowever, it will be understood that where the
composition comprises two or more benefit agents one of said
benefit aqents may also unction as a structurant.
The compositions according to the invention may also comprise
a thickening agent,~ i.e. a material which ~--int~;nq the
viscosity of the composition as the shear rate thereof is
increased during use. Suitable materials include cross-
linked polyacryla~es such as Carbopol (TM) ~polymers
available from Goodrich); fatty acid and derivatives thereof,
in particular, fatty acid monoglyceride polyglycol ether;
natural gums including alginates, guar, xanthan and
polysaccharide derivatives including car~oxy methyl ~ se
and hydroxypropyl guar; propylene glycols and propylene
glycol oleates; salts such as sodium chloride and ammonium
sulpha~e; glycerol tallowates; and mixtures thereof.


21 90739
Wo 96/02224 r~ ., 1687
-- 7
Further examples of s~ruc~uran~s and thickeners are given in
the International Cosmetic Ingredient Dictionary, Fifth
Edition, 1993, pllhli ~h~rl by CTFA (The Cosmetic, Toiletry &
Fragrance Association~, incorporated herein by reference.


The surface active agent can be selected from any known
surfactant suitable for topical application to the human
body. Mild surfactanes, i . e . surfactants which do not damage
the stratum corneum, the outer layer of the skin, are
particularly preferred.
One preferred anionic detergent is fatty acyl icethi~n~te of
formula:
RCO.CH.CH2503M
where R is an alkyl or alkenyl group of 7 to 21 carbon atoms
and M is a solubilising cation such as sodium, potassium,
ammonium or substituted ammonium. Preferably at least three
quarters of the RCO groups have 12 to 18 carbon atomS and may
be derived from coconut, palm or coconut~palm blends.
Anoeher preferred anionic detergent is alkyl ether sulphate
of formula:
RO (Cl~3CH20) nSO,M
where R is an alkyl group of 8 to 22 carbon atoms,
n ranges from 0 . 5 to 10, especially from 1. 5 to 8, and
M is a solubilising cation as defined above.
Other possible anionic detergents include alkyl glyceryl
ether sulphate, sulphosuccinates, taurates, sarcosinates,
s~lrhr~AC~otates, alkyl phosphate, alkyl phosphate esters and
acyl lacta~es, alkyl glutama~es and mixtures thereof.


21 90739
W0 96/02224 1 ~ ,., 5 1687
-- 8
5~ hnc~ ci n~t-~q may be monoalkyl sulphosuccinates having the
f ormula: RsOaCCH2C~I ( S03M ) CO~M; and amido-MEA s- 1 ~hn5~ ~ r~ i n :~ tes
of the formula: R;ceN~rT7-rFT~ (so3M)co~M; wherein Rs
ranges-from C8-C20 alkyl, preferably Cl2-CI5 alkyl, and M is a
sol--h; 1; qi "S cation.
Sarcnc;nAtPc are senerally i3}dicated by the fo_mula:
R5CON(C}I3~C~I2CO2M, wherein R5 ranges from C8-C20 alkyl,
preferably C,2-CI5 alkyl and M is a sol~hi 1 i 5; n~ cation.
Taurates are generally identified by the formula:
R5CoNR6C}}2CH,so,M, wherein Rs ranges from C8-C20 alkyl,
preferably Cl2-C,s alkyl, R6 ranges from C -C~ alkyl, and M is a
solubilising cation.

~Iarsh surfactants such as primary alkane sulphonate or alkyl
benzene sulphonate will generally be avoided.
Suitable nonionic surface active agents include alkyl
polysaccharides, lactobinnAl33~ q, ethyleneglycol esters,
glycerol monoethers, polyhydroxyamides (glucamide~, primary
and seconda3-y alcohol ethoxylates, especially the C8-20
aliphatic A1Cn~hnlq ethoxylated with an average of from 1 to
20 moles of ethylene oxide per mole of alcohol.
The surface active agent is preferably present at a level o~
from 1 to 35 wt%, preferably 3 to 30 wt%.
It is also preferable that the composition includes from 0.5
to 15 wt% of a cosurfactant with skin-mildness benefits.
Suitable materials are zwitterionic detergents which have an
alkyl or alkenyl group of 7 to 18 carbon atoms and comply
with an overall structural formula

21 9~739
Wo 96/02224 r~ 7
_ g _
O R;
11
R; - 1 -C -NH ( CH~ N' - X-Y
R~
where Rl i9 alkyl or alkenyl of 7 to 18 carbon atoms ~
R' and R3 are each independently alkyl, hydroxyalkyl or
carboxyalkyl of 1 to 3 carbon atoms;
m is 2 to 4 ~
n is 0 or l;
X is alkylene of 1 to 3 carbon atoms optionally
substituted with hydroxyl; and
Y is -CO2- or -SO,~
Zwitterionic deter~ents withirl the above general formula
include si.-nple bGtAin~oc of formula:-

Rl
R' r~--CH2C02
R3
and amido betaines of ~ormula:-

R2
- CONH(CH2~ CH2CO,
R~
~ 3 5 ~here m is 2 or 3 .
In both formulae R', R2 and R~ are as defined previously.
R' maY, in particular, ~e a mixture of C~2 and C" alkyl grou~s
derived from coconut so that at least half, pre~erably at
_ _ _ _ _ , ... . _ . _ . _ . . .

2l 90739
Wo 96/02Z24 PCr/GB95101687
-- 10 --
leas~ three quarters, of the group R1 has l0 to 14 carbon
a~oms. R2 and R' are pre~erably methyl.
A further possibility is a sulphobetaine of formula:-

R2
Rl-li'- ( CH2 ) ,S,03
0 r~3
or R2
R1-CONH ~CH2) m ~~ (CH3~ ,SO,
lS R'
where m is 2 or 3, or variants of these in which
-(C~2~3SO, is replaced by
OH
-f'T~2~ Q,
R;, Rl and R' in these formulae are as defined previously.

Furthermore, the benefit agent may also function as a carrier
to deliver efficacy agents to skin treated with the
compositions of the invention. ~his route is particularly
useful for delivering efficacy agents which are difficult to
deposit onto the skin or those which suffer detrimental
interactions with other components in the composition. In
such cases the carrier is a of ten a silicone or hydrocarbon
oil which is not sol1~hil j Sed/micellised by the surface active
phase and in which the efficacy agent is relatively soluble.
Examples o~ such efficacy agents include anti-viral agents;
hydroxycaprylic acias; pyrrolidone; carboxylic acids;
2,4,4~-trichloro-2'-hydroxydiphenyl ether (Irgasan DP300~;
3, 4, 4 ~ -trichlorocarbanilide; salicylic acid; benzoyl

- 2190739
WO 96/02224 P~l,~.. ,,c,~ 7
-- 11 --
peroxide; perfumes; essential oils; germicides and insect
repellants such as N,N-dimethyl m-toluamide (DEET~; and
mixtures thereof.
. .
Compositions of the inventlon may be formulated as products
for washing the skin, for example bath or shower gels, hand
washing compositions, facial,washing liquids; pre-and post-
shaving products; rinse-of f, wipe-of f and leave-on skin care
products .
The compositions of the invention will generally be pourable
liouids or semi-liguids for example pastes and will
preferably have a viscosity in the range 1000 to 100, 000 mPas
measured at a shear rate of lOs~l at 25C in a E~aake
Rotoviscometer RV20.
The compositions will exhibit a Newtonian viscosity at a
shear stress of 0.01 Pa at 25C of at least 5,000 Pas
preferably greater than 10, 000 Pas.
The abovo rionP~ characteristic viscosity mea~uL~ ~s may
be determined exactly (as in the case of the non-zero shear
viscosites) usin~, for example, a Carrimed CSL 100 low stress
rheometer, or o~t~inpd from an extrapolation according to the
Cross Model (see J of the Chemical Fn~inPPr, 1993, paper
entitled "Rheology for the Chemical Engineer~' by H Barnes ) as
in the case o~ the ero shear rate.
Other typical no"lrnnpnt~ of the compositions include opaci-
- 30 fiers, preferably 0.2 to 2.0 wt%; preservatives, preferably
0 . 2 to 2 . 0 wt% and perfumes, pre~erably 0 . 5 to 2 . 0 wt~ .
According to a further aspect Df the invention there is
provided a process for prepariny compositions according to
the invention comprising:-

21 90739
WO 96/02224 ~ 1, ~., 168
-- 12 --
a) struceuring the base ~ormulation comprising at least one
surface active agent selected ~rom anionic, nonionic,
zwitterionic, and cationic sur~ace active agents, and
mixtures thereo~ with a structurant; and


b) mixing the structured base ~r~r~ ti r~n with the benefit
a6e~t .
The invention-will be ~urther illustrated by reference to the
~ollowing non-limiting examples.
Ex~mnlGe
In the examples:-
Alkylpolyglucoside was Plantaren 2000 ex Xenkel
Coco amidopropyl betaine was Amonyl BA 380 ex Seppic.
Cross-linked polyacrylate was r~rhopol ETD 2020 ex Goodrich.
Fatty acid monoglyceride polyglycol ether was Rewoderm Ll580
ex Rewo.
Guar hydroxypropyl trimonium chloride was Jaguar C-13-S ex
Meyhall.
Silicone oil emulsion was BC 92/057 ex R~qi l~lnn,
ci 1 i C~nr~ oil was Dr200, a polydimethylsiloxane ex Dow Corninq
with a viscosity of 60000 mPas.
Sodium lauryl ether sulphate was Genapol ZRO ex EIoechst
Thickener was Antil 141 (a propylene glycol and propylene
glycol oleate) ex Goldschmidt
Fxr~lr,lr~q I-II
The following method was used to determine the amount of
benef it agent deposlted onto ~ull thickness porcine skin ( 5 x
15 cm) treated with compositions according to the invention.

2 1 90739
Wo 96/02224 ~ ,B _ 01687
-- 13 --
The skin was prehydraced and then 0 . 5 ml of the product
applied to it. The product was lathered for lO seconds and
then rinsed for lO seconds under running water.
Thereafter the skin was wiped once with a paper towel to
remove excess water.
2 minutes after drying a strip of adhesive tape was pressed
onto the skin for 30 seconds by applying a constant load of
lOOg.cm~2. The adhesive tape employed was J-Lar Superclear
(T~) tape having a width of 2 . 5cm. In total ten strips of
tape were applied to adjacent sites on the skin.
In this test procedure silicone which has deposited on the
skin will 5 lhses~ nt ly be transferred to the tape along with
some of the outer layer of the skin.
The amounts of silicon and skin ~dhering to the tape are
determined by means of X-ray ~luorescence spectroscopy. The
tape strips are placed in an X-ray fluorescence spectrometer
with the adhesive side facing the beam of this machine. A
mask is applied over the tape to define a standardised area
in the middle of the tape which is exposed to the X-ray beam.
The sample chamber of the machine is placed under vacuum
before making measurements and the spectrometer is then used
to measure the quantities of silicon and sulphur. The
sulphur is representative of the amount of skin which has
transferred to the tape.
The amounts of silicon and sulphur observed with a clean
piece of adhesive tape are subtracted from the experimental
measurements. The experimental mea~ , ~ s for the average
levels of sulphur and silicon are expressed as a ratio of
silicon to sulphur. From this ratio it is possible to
determine silicone oil deposition per unit area of skin.

21 90739
WO 96102224 PrL-r/GB95101687
-- 14 --
7~ mn i e
In this example deposition of silicon ~rom a composition
comprising a sili cnn~ oil with a weight average size o~ 80
microns was ~7lotorminec7 and compared with that from a similar
composition (composition A~ com7~7rising a sil; cnne oil
emulsion having a weight average size of O . 5 micron.
A base shower-gel ~ormulation Elaving the following
composition was prepared.
% 70v ~eir77~t
Sodium lauryl ether sulphate 13 . O
Coco amidopropyl betaine 2 . O
Sorbic acid O . 37
Sodium citrate dihydrate O . 49
Fatty acid monoglyceride 7,aolyglycol ether 3 . 00
Citric acid -O . 01'
Water + minors _ to 1000
~ This level ca~ be varied to obtain a p.; for the composition
of 5.~. ~
The v;scosity of the composition was 5500 mPas at 10s~l and
25C. ~
The base f orrn~ t i nn was prepared by mixing sodium lauryl
ether sulphate and betaine. Thereafter the l tnin~J
r~n~70nonts were added with mixing.0
Two .;arvard 44 syringe pumps were used to infuse the base
fnn-n-7i.o~tlnn and the benefit agent, silicone oil. silicone
oil was present at a level of 5 wt% based on the total
com7,70sit;on. One syringe was ~illed wi~h the base formu-
3 5 lation and the other with silicone oil . The syringes were

21 90739
WO 96/02224 ~ .~. ''01687
-- 15 --
then inserted into the syringe pum.p and the infusion rate set
at 5:95 oil:bage. The oil and base were forced through a
static in-line mixer and a composition with oil particles of
the required size obtained. The size of the particles can be
controlled by the ~;i t~r of the static mixer, the flow rate
and length of the mixer ~ube. The size of the particles can
be deteri~ined using a ~alver~ Mastersizer.
Comn~rative Comrosition (C~mnosition A)
1 0 %wt
Sodium lauryl ether sulphate 13 . 00
Coco amidopropyl betaine (CAP~) 2 . 00
Silicone oil emulsion 5 . oo
Guar hydroxypropyl trimonium 0.10
15 chloride
Sorbic acid o . 37
SodiLm citrate dihydrate 0 . 49
Sodium chloride- 2
Citric acid- 0 . 01
20 Water + minors to 100
# level can be varied ln order eo give the required
visco5ity of 5000 mPas at lOs~l and 25C.
level can be varied in order to give the rec~uired
25 pH.
Silicone deposition of these compositions were measured by
the test procedure described above and the following results
obtained .
si:s
Example I 25 . 6
Comparison (A) 2 . 2
The results demonstrate the improved deposition achieved when
the composition comprises large particle size silicone oil.

21 90739
W096/02224 r~ll~,~.s!Q1697
- 16
FxA~ e TI
A base shower gel formulation having the fQllowing
composition was prepared.
%wt
Sodium lauryl ether sulphate 4. 00
Sodium coco amido propyl betaine 1. 00
10 Alkyl~olyglucoside 5 . 00
Sorbic acid 0 . 37
Trisodium citrate dihydrate 0 . 49
Cross-linked polyacrylate 0. 9
Thickener~
15 5N NaOH- -1
Water + minors to 100
^ ^ Thickener was added to ~;ive the re~Iuired viscosity (-5000
mPas at 105-l and 25C)0
~ 5N NaOH was added to adjust the pH of the composition to
pH 5.3.
The bene~it agent used was si~ na oil with a viscosity of
25 60000 mPas.
The composition was prepared by dispersing the polyacrylate
in excess water. Thereafter sorbic acid and trisodium
citrate dihydrate were added to the resultin~ polymer
dispersion. The three sur~ace active agents were mixed and
the resulting mix added to the polymer dispersion.
Thereafter minors were added. The viscosity of the
resulting composition was measured a~ a shear rate of 10s~l at
25C and thickener ~dded until the re~uired viscosi~y
obtained.

21 90739
Wo 96/02224 PCT/GB95/01687
-- 17 --
The base formulation and silicone oil were infused using two
Harvard 44 syringe pumps as described above. me viscosity
of the final product was 5500 mPas.
Compositions comprising a number of different sized oil
particles were prepared. Silicone deposition from these
compositions was measured by the test ~rocedure described
above and _ ~d with that ~rom composition ~A).
The following results were obtained:-
Particle ~ize of Si: S ratio
silicone oil
0.5 0.8
24 1.4
52 3.7
88 8.3
130 16. 8
138 18 . 1
The results demonstrate the bene~it of using large particle
size bene~it agent.
The products were stored in a sealed glass vessel at 37C.
After 6 weeks they were still stable, i.e. there was no
visible separation.
F~c~mnle III
~ 30 In this examPle the stability o~ a composition acoording to
the invention structured with a cross-linked polyacrylate was
compared with an identical composition ~rom which ehe
structurant was absent.

2 3
WO 96/02224 1 9 0 7 9 PCrlGB95101687
-- 18 --
The composition comprised
wt
Sodium lauryl ether sulphate 4. 00
Sodium coco amido propyl betaine 1. 00
Alkylpolyglucoside 5 . 00
Sorbic aci~i 0 . 37
Trisodium citrate dihydrate 0 . 49
Cross-linked polyacrylate 0.9#
Thickener ~ 97
10 Water + minors to 100
5N NaOH was added to adjust the pH of the composition to
pH 5.3.
# absent from the comparative frrm ll ~t j on.
The benefit agent used was silicone oil present in an amount
of 5wt%.
The viscosity of the product ~crrr~l; nrJ to the invention and
o~ the comparison were, respectively, 4628 and 5500 mPas at
105-l and 25C and 22783 and 12.16 mPas at 0.01 Pa and 25C.
Both compositions were stored in sealed glass vessels and
placed in a oven at 37C.
Whereas the comparative composition separated after three
days the composition according to the invention was still
stable after 4 weeks.

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date Unavailable
(86) PCT Filing Date 1995-07-18
(87) PCT Publication Date 1996-02-01
(85) National Entry 1996-11-19
Examination Requested 1997-05-07
Dead Application 2000-07-18

Abandonment History

Abandonment Date Reason Reinstatement Date
1999-07-19 FAILURE TO PAY APPLICATION MAINTENANCE FEE

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1996-11-19
Maintenance Fee - Application - New Act 2 1997-07-18 $100.00 1996-11-19
Registration of a document - section 124 $100.00 1997-02-11
Request for Examination $400.00 1997-05-07
Maintenance Fee - Application - New Act 3 1998-07-20 $100.00 1998-06-15
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
UNILEVER PLC
Past Owners on Record
JOBLING, MARGARET
SHEN, SHIJI
TSAUR, LIANG SHENG
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) 
Description 1996-02-01 18 429
Claims 1996-02-01 2 46
Cover Page 1997-03-20 1 11
Abstract 1996-02-01 1 31
Assignment 1996-11-19 9 318
PCT 1996-11-19 15 438
Prosecution-Amendment 1997-05-07 1 53
Correspondence 1994-12-24 1 40