U.S. patent number 3,829,563 [Application Number 05/311,035] was granted by the patent office on 1974-08-13 for emollient cleansing compositions.
This patent grant is currently assigned to Hoffman-La Roche Inc.. Invention is credited to Richard H. Barry, Meyer Matluck, Philip Orshitzer.
United States Patent |
3,829,563 |
Barry , et al. |
August 13, 1974 |
EMOLLIENT CLEANSING COMPOSITIONS
Abstract
Cleansing compositions for the hair and skin which deposit an
emollient, conditioning film thereon during washing are disclosed.
The compositions, which may be in a liquid or semi-solid form, are
oil-in-water emulsions characterized by a particular particle size
distribution of the oil phase and are comprised of from about 10 to
about 70 percent by weight petrolatum, from about 5 to about 30
percent by weight of one or more organic foaming detergents, from
about 1 to about 10 percent by weight of an emulsifier, from about
0.5 to about 5 percent weight of an organic foam stabilizer, from
about 0 to about 20 percent by weight of one or more emollient
substances other than petrolatum, and water.
Inventors: |
Barry; Richard H. (Bloomfield,
NJ), Matluck; Meyer (Flushing, NY), Orshitzer; Philip
(Staten Island, NY) |
Assignee: |
Hoffman-La Roche Inc. (Nutley,
NJ)
|
Family
ID: |
23205108 |
Appl.
No.: |
05/311,035 |
Filed: |
November 30, 1972 |
Current U.S.
Class: |
510/124; 514/846;
424/70.21; 424/70.24; 514/942; 510/121; 510/505; 510/480; 510/122;
510/125; 510/417; 510/159 |
Current CPC
Class: |
A61K
8/4946 (20130101); A61K 8/922 (20130101); A61K
8/062 (20130101); A61K 8/925 (20130101); A61Q
19/10 (20130101); A61Q 5/02 (20130101); A61K
8/31 (20130101); A61K 8/4973 (20130101); A61K
8/8176 (20130101); A61Q 5/12 (20130101); A61K
8/42 (20130101); Y10S 514/846 (20130101); Y10S
514/942 (20130101) |
Current International
Class: |
A61K
8/42 (20060101); A61K 8/81 (20060101); A61K
8/72 (20060101); A61K 8/31 (20060101); A61K
8/49 (20060101); A61K 8/92 (20060101); A61K
8/30 (20060101); A61K 8/04 (20060101); A61K
8/06 (20060101); A61Q 5/02 (20060101); A61Q
19/10 (20060101); A61Q 5/12 (20060101); A61k
007/06 (); A61k 027/00 () |
Field of
Search: |
;424/70,168 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Rosen; Sam
Attorney, Agent or Firm: Welt; Samuel L. Saxe; Jon S. Swope;
R. Hain
Claims
We claim:
1. A foaming, emollient composition suitable for the cleansing of
the skin and hair consisting essentially of an oil-in-water
emulsion wherein from about 95 to about 98 percent of the particles
of the oil phase thereof are smaller than about 5 microns at their
largest dimension, from about 2 to about 5 percent of said
particles are from about 5 microns to about 10 microns at their
largest dimension, from about 0.2 to about 1.0 percent of said
particles are between about 10 microns and 100 microns at their
largest dimension and substantially no particles are greater than
100 microns at their largest dimension, said emulsion
comprising:
a. from about 10 percent to about 70 percent by weight
petrolatum;
b. from about 5 percent weight to about 30 percent by weight of an
organic foaming detergent component comprising a mixture of one
part by weight sodium lauryl sulfate and from about one-half to
about 10 parts by weight of one or more amphoteric detergents
selected from those represented by the formula ##SPC2##
wherein R is an alkyl radical containing from nine to 11 carbon
atoms and X is hydroxyl or lauryl sulfate;
c. from about 1 percent by weight to about 10 percent by weight of
an emulsifier component having an HLB value of from 1 to 6 and
selected from the group consisting of sorbitan monooleate, sorbitan
sesquioleate, sorbitan trioleate, sorbitan monostearate, sorbitan
tristearate, polyoxyethylene (2) oleyl ether, polyoxyethylene (2)
stearyl ether, polyoxyethylene (2) cetyl ether, ethylene glycol
monostearate, diethylene glycol oleate, diethylene glycol stearate,
propylene glycol monostearate, propylene glycol distearate,
glyceryl monostearate, glyceryl monooleate, decaglyceryl
octaoleate, hexaglyceryl distearate and triglyceryl monooleate;
d. from about 0.5 percent by weight to about 5.0 percent by weight
of an organic foam stabilizer selected from the group consisting of
capric acid diethanolamide, stearyl trihydroxymethyl ammonium
chloride and lauric-myristic (70-30) monoethanolamide;
e. from about 0 percent to about 20 percent by weight of one or
more pharmaceutically acceptable emollient substances other than
petrolatum; and
f. from about 10 percent by weight to about 80 percent by weight
water, the percent by weight of said component b) in said
composition not exceeding two times the percent by weight of said
component a).
2. A composition in accordance with claim 1 wherein said component
a a) is present in from about 10 to about 55 percent by weight,
said component b) is present in from about 10 to about 30 percent
by weight, said component c) is present in from about 3 to about 8
percent by weight and said component d) is present in from about 1
to about 3 percent by weight.
3. A composition in accordance with claim 1 wherein said component
e) is present in from about 3 to about 15 percent by weight.
4. A composition in accordance with claim 1 wherein said component
b) comprises one part by weight sodium lauryl sulfate and from
about 1 to about 4 parts by weight of one or more of said
amphoteric detergents.
5. A composition in accordance with claim 1 wherein said component
c) is sorbitan sesquioleate.
6. A composition in accordance with claim 1 additionally containing
from about 0.5 by weight to about 1.5 percent by weight
polyvinylpyrrolidone.
7. A method of cleansing the hair and simultaneously depositing
thereon a palpable emollient film which comprises shampooing the
hair with the composition of claim 1.
8. A method of cleansing the skin and simultaneously depositing
thereon a palpable emollient film which comprises washing the skin
with the composition of claim 1.
9. A method of preparing a foaming emollient composition suitable
for the cleansing of the skin and hair said composition
comprising:
a. from about 10 by weight to about 70 percent by weight of
petrolatum;
b. from about 5 by weight to about 30 percent by weight of an
organic foaming detergent component comprising a mixture of one
part by weight sodium lauryl sulfate and from about one-half to
about 10 parts by weight of one or more amphoteric detergents
selected from those represented by the formula ##SPC3##
wherein R is an alkyl radical containing from 9 to 11 carbon atoms
and X is hydroxyl or lauryl sulfate;
c. from about 1 by weight to about 10 percent by weight of an
emulsifier component having an HLB value of from 1 to 6 and
selected from the group consisting of sorbitan monooleate, sorbitan
sesquioleate, sorbitan trioleate, sorbitan monostearate, sorbitan
tristearate, polyoxyethylene (2) oleyl ether, polyoxyethylene (2)
stearyl ether, polyoxyethylene (2) cetyl ether, ethylene glycol
monostearate, diethylene glycol oleate, diethylene glycol stearate,
propylene glycol monostearate, propylene glycol distearate,
glyceryl monostearate, glyceryl monooleate, decaglyceryl
octaoleate, hexaglyceryl distearate and triglyceryl monooleate;
d. from about 0.5 percent by weight to about 5.0 percent by weight
of an organic foam stabilizer selected from the group consisting of
capric acid diethanolamide, stearyl trihydroxymethyl ammonium
chloride and lauric-myristic (70-30) monoethanolamide;
e. from about 0 percent by weight to about 20 percent by weight of
one or more pharmaceutically acceptable emollient substances other
than petrolatum; and
f. from about 10 to about 80 percent water, the percent by weight
of said component b) being not greater than two times the percent
by weight of said component a) which comprises:
1. heating a mixture of said components a), c) and e) to a
sufficient temperature to form a melt thereof;
2. mixing together components b), d) and f);
3. heating the mixture of step 2) to a temperature approximating
that of said melt;
4. combining said melt and said mixture with agitation to form an
oil-in-water emulsion;
5. gradually cooling said emulsion to about 30.degree.C. while
maintaining agitation; and
6. continuing agitation of said emulsion at a temperature between
about 25.degree.C. and about 30.degree.C. until the particle size
of the oil phase of said emulsion is such that from about 95 to
about 98 percent of said particles are smaller than about 5 microns
at their largest dimension, from about 2 to about 5 percent of said
particles are from about 5 to about 10 microns at their largest
dimension, from about 0.2 to about 1.0 percent of said particles
are between about 10 microns and 100 microns at their largest
dimension and substantially no particles are greater than 100
microns at their largest dimension.
Description
BACKGROUND OF THE INVENTION
It is generally recognized by both laymen and dermatologists that
many of the commercially available skin cleansing preparations,
i.e., toilet soaps, detergents, foaming paste or cream type
cleansing compositions and the like, may remove oils from the skin
during use and thus cause skin dryness which manifests itself as
roughness, white scaling and, occasionally, itching. Such
preparations may also intensify existing dermatological conditions
which are characterized by such symptoms. In an effort to relieve
or prevent such symptoms, lotions and creams containing humectant
or emollient substances are widely used, particularly among women,
to help retard moisture loss from the skin and to plasticize and
soften the outer cellular layers thereof. Such preparations are
often inconvenient in that they must be carried from place to place
in the purse or pocket and additionally represent an unwelcome
expense to the user. As a result, many persons who suffer with dry
skin forego the use of such preparations.
There are a large number of soaps and other skin cleansing
preparations on the market which neither exhibit a softening effect
nor contain a residual emollient substance. However, even those
cleansing preparations containing emollient substances such as cold
creams, fats, oils and the like which are claimed to adhere to the
skin during use and leave an emollient film after washing generally
do not satisfactorily meet such claims. The failure of such
products to realize their claims results from the fact that most of
the mineral, animal or vegetable oils they contain possess poor
adhesion to the skin in the presence of the required amount of
detergent necessary to produce copious foam. In the case of
shampoos parallel situations exist with regard to the products
currently on the market many of which adequately clean the hair but
do not satisfactorily impart smoothness, body and manageability
thereto. The failure of such products to condition the hair during
use is evidenced by the substantial commercial success of
after-shampoo conditioning rinses and other conditioning
preparations for both men and women.
It can therefore be clearly seen that there exists a need for hair
and skin cleansing preparations which possess excellent cleansing
and foaming characteristics and which additionally act to condition
the hair and skin by depositing a palpable emollient film thereon
during the cleansing operation. Such unique preparations are
furnished in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to liquid or semi-solid compositions
suitable for the cleansing and "conditioning" of the hair and skin.
By "conditioning" is meant the deposition of a palpable emollient
film on the hair and/or skin during the cleaning operation. On the
skin, such a film works to retard moisture loss from the epithelium
and to maintain or restore the softness and smoothness of the skin
surface. On the hair, the emollient film deposited by the novel
preparations of this invention acts to impart combability and
manageability thereto. The aforementioned emollient film is
comprised principally of petrolatum which may be supplemented by
additional oily or fatty emollient substances such as are
recognized in the art.
The present invention is concerned with the discovery that
petrolatum can be formulated with certain organic detergents into
oil-in-water emulsions which are unique in that they possess
adequate foaming properties, cleanse exceptionally well and
simultaneously deposit a film of fine particles of petrolatum on
the skin or hair. This film, which acts to condition and soften the
hair or skin, adheres sufficiently well thereto to remain after the
latter is rinsed off with water.
It has been found that the particle size distribution of the oil
phase of the oil-in-water emulsions of the invention must be within
certain limits for maximum physical stability and functional
efficacy. Specifically, the great majority of these particles must
be smaller than five microns for maximum stability of the emulsion.
On the other hand, a minimal portion of the particles of the oil
phase, i.e. petrolatum and other optional emollient substances,
must be relatively large for functional efficacy. Therefore, the
particles of the oil phase of the novel oil-in-water emulsions of
the invention have the following approximate distribution by size:
up to about 98 percent are smaller than about five microns in their
largest dimension: about 2 percent are five microns or larger and
about 0.2 percent of the particles are 10 microns or larger. The
preferred particle size distribution by count is: from about 95 to
about 98 percent are smaller than five microns: from about 2 to
about 5 percent are between five and 10 microns; from about 0.2 to
about 1.0 percent are between 10 and 100 microns; and essentially
none are larger than 100 microns at their largest dimension.
The above specified size distribution of the oil phase particles of
the compositions of the invention can be achieved by continued
agitation of the emulsion after formation. Such agitation is
carried out at a temperature below 40.degree.C. i.e. from about
20.degree. to about 40.degree.C., preferably from about 20.degree.
to about 30.degree.C. Agitation of the emulsion at these
temperatures causes coalescence of the particles of the oil phase
with a resultant increase in the mean or average size of such
particles and an increase in the proportion by count of oil
particles in the five to 100 micron size range. The length of time
required to achieve the desired particle size distribution will
vary with the exact composition of the emulsion, the speed and type
of equipment utilized, the batch size and the like. Generally,
however, from about one-fourth to 4 hours preferably about 2 hours
is sufficient. Increasing the proportion of oil phase particles in
the five to 100 micron range increases the amount of oil phase
particles deposited on skin or hair during use of the preparations
of the invention for personal cleansing. The particle size
distribution of the oil phase may be determined by use of a Coulter
counter.
The compositions of the invention, in general, comprise from about
10 to about 70 percent, preferably from about 10 to about 55
percent by weight of petrolatum; from about 5 to about 30 percent
by weight, preferably from about 10 to about 30 percent by weight
of one or more organic foaming detergents; from about 1 to about 10
percent by weight, preferably from about 3 to about 8 percent by
weight of a suitable emulsifier; from about 0.5 to about 5 percent
by weight, preferably from about 1 to about 3 percent by weight of
an organic foam stabilizer; from about 0 to about 20 percent by
weight, preferably from about 3 to about 15 percent by weight of
one or more additional art-recognized emollient substances other
than petrolatum and the remainder water.
The amount of water to be included in the compositions of the
invention will vary depending on the desired consistency of the
final product. As the compositions of the invention are
oil-in-water emulsions, it is possible by varying the amount of
water present to formulate, for example, a thick-flowing liquid, a
semi-liquid thick creme, a paste and the like. Generally, the
compositions of the invention should not contain less than about 25
percent by weight nor more than about 80 percent by weight water if
a liquid form is desired and not less than about 10 percent by
weight nor more than about 50 percent by weight of water where a
paste preparation is desired. The compositions preferably contain
from about 20 to about 50 percent by weight water wherein a paste
composition is desired and from about 30 to about 80 percent by
weight water where a liquid formulation is desired. In compositions
containing from about 30 to about 50 percent by weight water, the
consistency will vary between liquid and semi-solid depending on
the characteristics of the non-aqueous ingredients.
The petrolatum suitable for use in the invention comprises any
grade of white or yellow petrolatum which is recognized as being
safe for application to the human skin or hair. The preferred types
are Petrolatum USP XVIII and NFXII. Also, any viscosity or
consistency grade of petrolatum recognized in the art can be used
in the invention. It is within the scope of the invention, however,
to partially replace petrolatum with mixtures of hydrocarbon
materials which can be formulated to resemble petrolatum in
appearance and consistency. For example, such a combination can be
formed by melting mineral oil in various proportions with
substances such as, for example, microcrystalline wax, paraffin
wax, ceresin and ozokerite. It is also within the purview of the
invention to augment the petrolatum in the compositions to be
utilized to cleanse the hair with one or more additional emollient
materials known in the art to impart sheen, luster, smoothness and
static charge reduction to the hair. It is, however, essential that
the compositions of the invention contain at least 10 percent
petrolatum by weight.
The above-mentioned emollient agents which can be utilized in
augmenting the emollient properties of petrolatum include one or a
mixture of art-recognized substances such as, for example, fatty
alcohols, liquid esters of mono- and di-basic fatty acids,
vegetable oils, modified fatty acid glycerides, silicone oils,
acetylated lanolin alcohols, esters of lanolin fatty acids,
cholesterol, lanolin, liquid lanolin, myristyl myristate, mineral
oil, squalene, squalane (perhydrosqualene), and the like. Such
additional emollient substances may be present in the compositions
of the present invention up to about 20 percent by weight.
The synthetic organic foaming detergents utilized in the
compositions of the invention may be of the anionic, non-ionic or
amphoteric types. An important consideration in the selection of a
suitable detergent ingredient is the relative irritant properties
of the individual detergents. Additional criteria to be met are the
ability of each detergent to stabilize the emulsion, produce
viscosity, achieve the desired foam level and remain stable at the
pH level of the formulation, i.e. a pH of from about 7 to about 9.
Examples of suitable detergents include the following:
Anionic: alkali and triethanolamine lauryl sulfates, lauryl ether
sulfates, sodium alkylbenzene sulfonate, secondary alkyl sulfates,
salts of higher acyl esters of isethionic acid, sodium salts of
higher acyl derivatives of taurine or methyl taurine, alkyl phenol
polyether sulfates, higher acyl derivatives of glycine and
methylglycine, di-higher alkyl sulfosuccinates, higher alkyl
alkanolamide ester sulfosuccinates, higher alkyl monoglyceride
sulfates, alpha-olefin sulfonates; Nonionic:
alkyl aryl polyether alcohols, alpha-hydro-omega-hydroxy-poly
(oxypropylene)polyoxyethylene block copolymers; and Amphoteric:
disodium salts of higher alkyl substituted imidazolinium
dicarboxylic acids wherein the connecting group linking said
carboxyl groups to the imidazolinium ring contains an ether
linkage, higher acyl beta-aminopropionates, higher acyl peptides,
higher alkyl amido betaines, and the like.
The preferred detergent ingredient in the compositions of the
invention is a combination of about one part by weight of an alkali
metal lauryl or lauryl ether sulfate and from about one-half to
about 10 parts, preferably from about 1 to about 4 parts by weight
of one or more disodium salts of higher alkyl substituted
imidazolinium dicarboxylic acids such as, for example, the Miranol
detergents which are manufactured by Miranol Chemical Co.,
Irvington, New Jersey and which have the following general formula
##SPC1##
wherein R is higher alkyl radical having, preferably, nine to 11
carbon atoms and X is an anion such as, for example, hydroxyl or
lauryl sulfate.
These detergents, when formulated into the compositions of the
invention, yield the ideal balance of low irritation, quality and
volume of foam and viscosity.
The detergent component of the compositions of the invention, as
stated above, comprises from about 5 to about 30 percent by weight,
preferably from about 10 to about 30 percent by weight thereof. In
no instance, however, does the percent by weight of the detergent
ingredient utilized exceed two times the percent by weight of the
petrolatum present in the composition.
The emulsifiers suitable for use in the compositions of the
invention include those amphiphilic organic emulsifiers recognized
in the art as being safe for the type of products contemplated
herein and of which the HLB values are from about 1 to about 19.
The preferred emulsifiers in accordance with the invention are
those with HLB values of from about 1 to about 6. It is also within
the practice of the invention to utilize more than one emulsifier
the cumulative HLB value of which falls within the desired range.
Examples of suitable types of emulsifiers in accordance with the
invention are the following: sorbitan fatty acid esters,
poly-oxy-ethylene sorbitan fatty acid esters, polyoxyethylene
sorbitol esters of fatty acids, lanolin, rosin, beeswax and tallow
acids, polyoxyethylene fatty acid esters, polyoxyethylene fatty
alcohol ethers, fatty acid mono- and di-glycerides, polyglycerol
fatty acid esters, polypropylene glycol fatty acid esters, fatty
alcohol phosphate esters, polyethoxylated fatty alcohol phosphate
esters and the like.
Specific emulsifiers which are preferred in the practice of the
invention include, for example, sorbitan monooleate, sorbitan
sesquioleate, sorbitan trioleate, sorbitan monostearate, sorbitan
tristearate, polyoxyethylene (2) oleyl ether, polyoxyethylene (2)
stearyl ether, polyoxyethylene (2) cetyl ether, ethylene glycol
monostearate, diethylene glycol oleate, diethylene glycol stearate,
propylene glycol monostearate, propylene glycol distearate,
glyceryl monostearate, glyceryl monooleate, decaglyceryl
octaoleate, hexaglyceryl distearate and triglyceryl monooleate.
Suitable organic foam stabilizers, which may additionally function
as thickening agents in the compositions of the invention, include
one or more of substances such as, for example, lauric, myristic
and coconut oil fatty acid di-ethanolamides, monoethanolamides and
isopropanolamides, stearyl trialkanol ammonium chlorides, fatty
acid dimethylamine oxides, fatty acid diethanolamine oxides and the
like. Preferred among this group are the coconut fatty acid
diethanolamides wherein the fatty acids are predominantly 12 and 14
carbon atom acids, capric acid diethanolamide, lauric-myristic
(70-30 ) monoethanolamide and stearyl trihydroxymethyl ammonium
chloride.
It is also within the purview of the present invention to include
in the emollient cleansing compositions thereof certain optional
ingredients which are recognized as being conventional in the art
for such preparations. These include, for example, organic or
inorganic acids for pH adjustment, dyes, perfumes, preservatives,
antioxidants, chelating agents and the like. Additionally, from
about 0 to about 3 percent by weight preferably from about 0.5 to
about 1.5 percent by weight polyvinyl pyrrolidone may be included
in the compositions of the invention for viscosity adjustment, and
irritancy reduction. Oil soluble medicinal agents such as are
recognized in the art for use in skin and hair cleansing
preparations e.g. antidandruff agents, may also be included in the
preparations of the invention to impart medicinal properties to the
emollient film deposited on the skin or hair thereby.
The compositions of the invention are prepared, generally, by first
melting together all the fatty ingredients and combining the melt
with agitation with the aqueous phase comprising a mixture of the
detergents, the foam stabilizer and water, both phases being at a
temperature of from about 60.degree. to 80.degree.C. The oily phase
may be added to the aqueous phase or vice versa. The mixture is
then cooled to a temperature of below about 30.degree.C. with
constant agitation. Perfume ingredients are added to the mixture
during the cooling process when the temperature thereof is at
between 50.degree. and 40.degree.C. After the temperature of the
mixture has reached about 30.degree.C., the emulsion is observed
under a microscope at 15 minute intervals while agitation is
continued, and the temperature is maintained between 25.degree. and
30.degree.C. Agitation is continued until a substantial proportion,
i.e. about 2 percent of the visible particles of the oil phase are
larger than 5 microns, about 90 percent of said large particles
being between 5 and 10 microns and the remainder between about 10
and 100 microns. At temperatures below 30.degree.C., the average
particle size of the oil phase of the emulsion increases rapidly as
the mixing time is extended and/or mixing speed increased.
The amount of oil phase deposited on the skin or hair during use of
the compositions of the invention is directly related to the
average particle size of the oil phase of the emulsion. Thus, the
oil deposition may be controlled within certain limits by the
duration and speed of agitation during mixing of the emulsion at a
temperature below about 30.degree.C. Washing tests on the skin and
hair, as will be described hereinafter, may be utilized to
determine standards whereby a termination point for the mixing may
be determined. As a general rule, the compositions of the invention
should be agitated on conventional equipment while cooling to below
30.degree.C. such as, for example, by agitating with an anchor type
stirrer running at 10-50 rpm for a period of from about one-half to
about 4 hours, preferably about 2 hours. These figures will vary
with the specific equipment utilized, the desired consistency of
the product, the amount of oil deposition desired and the like. The
manipulation of these variables is considered to be within the
purview of one skilled in the art utilizing the disclosure made
herein.
Additional adjustments of the characteristics of the composition to
yield the particular type desired may be made within the metes and
bounds of the invention. For example, the consistency of the
product may be varied by adjusting the relative proportions of
water, detergent, oil and thickener, and also by varying the
melting point of the oil phase. A water content of from about 20 to
about 40 percent by weight will, in general, yield a product with
the consistency of a thick paste whereas a water content above
about 40 percent will yield products of increasing liquidity. The
foam volume produced by agitation with water may also be varied by
varying the amount and kinds of foaming detergents utilized. For
example, sodium lauryl sulfate possesses a large foam capacity but
also a high irritancy. Its use in compositions of the type
contemplated herein is thus limited. It is, however, preferred in
the compositions of the invention to utilize at least 3 percent by
weight, more preferably between about 5 and about 10 percent by
weight sodium lauryl sulfate in combination with other foaming
organic detergents which are lower in both foam production and
irritancy.
The following tests demonstrate the amount of oil deposition during
use of the various compositions within the scope of the present
invention.
For the testing of hair cleaning compositions, a swatch of human
hair about 8 inches long, of average fineness and weighing about 5
grams was tied together at one end and was cleansed by immersion in
three 15 ml. portions of hexane, draining after each immersion. The
hair was towel-dried and then allowed to completely dry in the air.
The clean hair was thoroughly soaked in warm tap water, squeezed
dry and treated with exactly 1 gram of the test composition which
was spread over the swatch and worked vigorously with the fingers
to produce maximum foam. After about one minute, the cleansing
composition was removed by thoroughly rinsing the hair with warm
tap water. The excess water was squeezed from the swatch and it was
then dried with a towel, combed out and thoroughly dried in a
current of hot air. The dried swatch was then exhaustively
extracted with hexane. The extract was filtered through paper and
evaporated to dryness. The oily residue was than accurately weighed
and the milligrams of oil deposited per gram of product tested was
calculated.
To test the amount of oil deposited on the skin utilizing the
cleansing compositions of the invention, a rectangular area 5 cm.
.times. 10 cm. was marked along the flat, hairless, inner side of
the forearm with a pencil. The arm was held so that the marked area
was downward and a stream of hexane was sprayed on the area from a
wash bottle until about 25 ml. was used. The hexane washings were
then discarded. The dried, washed area, which appeared white and
scaly, was then thoroughly wetted with water. Exactly 0.25 gram of
test sample was distributed evenly over the test area. Using a
little water, the composition was worked up to maximum lather by
rubbing vigorously with the fingertips. The arm was thoroughly
rinsed with warm water until all slippery, soapy feel had
disappeared from the test area which was then patted dry with a
towel and allowed to dry in the air. The treated area was then
extracted with a stream of approximately 25 ml. of hexane
collecting the drainings in a 20 cm. diameter funnel held over a 50
ml. tared beaker. The solvent was then evaporated and the weight of
the oily residue determined and reported as mg. of oil deposited
per gram of product tested.
It has been demonstrated utilizing gas/liquid chromagraphic
analysis techniques of the hexane extracted fatty deposit obtained
in the above tests that the deposit contains the same ingredients
as are present in the oil phase of the test composition.
The following examples serve to further illustrate the invention.
All temperatures are given in degrees Centigrade.
EXAMPLE 1
A foaming emollient body cleanser for use in the bath or shower was
prepared from the following formulation:
Percent Ingredient by Weight ______________________________________
White Petrolatum 36.0 Acetylated lanolin alcohols, liquid
fraction.sup.1 2.0 Liquid lanolin 2.0 Polyolesters of short chain
fatty acids.sup.2 1.0 Sorbitan sesquioleate 5.0 Sodium lauryl
sulfate 9.0 2-Capryl-1-carboxymethyloxyethyl-
1-carboxymethylimidazolinium 1- hydroxide disodium salt 10.0 Capric
acid diethanolamide 1.2 Polyvinyl pyrrolidone 0.1 Perfume q.s.
Water Balance ______________________________________ .sup.1
Acetulan-American Cholesterol Products Division of CPC
International, Inc. .sup.2 Neobee-Drew Chemical Corp., Inc.
The first five ingredients (oil phase) were combined and heated in
a stainless container to about 80.degree. with stirring. The
remaining ingredients were combined in a separate jacketed
stainless steel kettle equipped with an anchor mixer and heated to
about 80.degree.. The sodium lauryl sulfate was added as a 42
percent aqueous paste and the imidazolinium salt was added as a 38
percent aqueous solution. The oil phase was then added slowly to
the aqueous phase while mixing rapidly (about 2,000 rpm) with an
inserted impeller mixer. After incorporation and emulsification of
the oil were complete, the impeller was removed and mixing was
continued by anchor blade rotating at about 30 rpms. The
temperature of the emulsion was lowered to 50.degree. by cold water
circulating through the kettle jacket. At 50.degree. the perfume
was added and the temperature of the emulsion was then gradually
lowered to 30.degree.. Mixing was continued for an additional two
hours during which the temperature of the emulsion cooled to about
25.degree.. Stirring was continued until microscopic observation of
the emulsion at 100 magnifications indicated proper particle size
distribution. Stirring was then discontinued and the product was
packaged into suitable containers.
The product was a stable, opaque, viscous yet pourable lotion. When
applied to the skin and lathered with water it provided very good
foam quality. When tested on the skin of the forearm as described,
the product deposited about 30 mg. of oil per gram applied and the
skin surface felt soft and supple.
EXAMPLE 2
A foaming emollient facial washing cream was prepared in accordance
with the method of Example 1 from the following formulation:
Percent Ingredient by Weight ______________________________________
White Petrolatum 27.0 Coconut Oil 1.5 Sesame Oil 2.5 Squalene 0.5
Squalene 0.5 Cholesterol 0.2 Lanolin sterols and alcohols.sup.1 1.5
Spermaceti 1.0 Myristyl myristate 1.0 Sorbitan sesquioleate 5.0
Sodium lauryl sulfate 7.5 1-Carboxymethyl-1-carboxymethyloxy-
ethyl-2-coco-imidazolinium 1- hydroxide disodium salt 4.7
1-Carboxymethyl-1-carboxymethyloxy- ethyl-2-coco-imidazolinium 1-
lauryl sulfate disodium salt 6.8 Stearyl trihydroxy methyl ammonium
chloride 1.5 Polyvinylpyrrolidone 0.5 Citric Acid q.s. to pH 7.2,
about 0.2 Water Balance ______________________________________
.sup.1 Amerchol-American Cholesterol Products Division of CPC
International, Inc.
As this preparation is to be applied to the face, the pH was
adjusted downward to about 7.2 to minimize eye-sting and irritancy.
Likewise, the oil content of this preparation was made higher than
the preparation of Example 1 to facilitate removal of makeup and to
deposit a heavier oil film on the face to combat dry skin. The
preparation was a soft cream which produced a moderate lather and
deposited a perceptible film on the skin. In the forearm test
described herein, the product was found to deposit about 40 mg. of
oil per gram applied and leave the skin soft and supple.
EXAMPLE 3
A grooming and conditioning shampoo for men's hair was prepared
from the following formulation in accordance with the method of
claim 1.
______________________________________ Percent Ingredient by Weight
______________________________________ White Petrolatum 25.0 Liquid
lanolin 3.0 Acetylated lanolin alcohols, liquid fraction (Acetulan)
1.0 Sorbitan sesquioleate 5.0 Sodium lauryl sulfate 5.0
1-Carboxymethyl-1-carboxymethyloxy- ethyl-2-coco-imidazolinium 1-
hydroxide disodium salt 16.0 1-Carboxymethyl-1-carboxymethyloxy-
ethyl-2-coco-imidazolinium 1- lauryl sulfate disodium salt 3.5
Lauric-Myristic (70-30) monoethanolamide 2.0 Water Balance
______________________________________
The product was a soft, stable cream with satisfactory foam and
superior conditioning effects of men's hair. Hair washed with the
preparation did not have the "squeaky" feel commonly experienced
with currently available soaps or shampoos but instead was smooth
and, after drying, had a light dressed appearance without feeling
or looking oily or greasy. The product was found by the hair test
described herein to deposit about 30 mg. of oil per gram.
EXAMPLE 4
A conditioning shampoo for women's hair was prepared in accordance
with the method of claim 1 from the following formulation:
Percent Ingredient by Weight ______________________________________
White Petrolatum 15.0 Light mineral oil 8.0 Liquid lanolin 5.0
Sorbitan sesquioleate 5.0 Sodium lauryl sulfate 9.0
1-Carboxymethyl-1-carboxymethyloxy- ethyl-2-coco-imidazolinium 1-
hydroxide disodium salt 16.0 Capric diethanolamide 2.5
Polyethyleneglycol 6000 Distearate 0.4 Water Balance
______________________________________
The product provided good foam and excellent conditioning
properties. Hair washed with this composition was free from
"squeakiness" and combed out with little or no tangling. There was
no need to treat the hair with an after-shampoo conditioning agent
except in some exceptional cases. The dry hair had good gloss, body
and hold and was free of frizziness and excessive fly-away. The
product, a soft, stable creme, provided a lighter dressing or
grooming effect (10 mg. of oil per gram by the hair test described
herein) than the men's shampoo of Example 3 in keeping with the
softer finish preferred by women.
* * * * *