Method of preparing microemulsions

Microemulsion compositions comprising low amino content microemulsifiable silicones and a surfactant having a high phase inversion temperature, the microemulsions formed therewith, a means for preparing said microemulsions, and personal care products comprising said microemulsions.

FIELD OF THE INVENTION 
The instant invention comprises a method for preparing microemulsions. The 
process of the invention comprises blending a low amino content silicone 
oil with a surfactant having a high phase inversion temperature adding an 
approximately equal amount of water at a temperature approximately equal 
to the phase inversion temperature of the surfactant, acidifying, followed 
by rapidly adding water. The instant invention further comprises personal 
care products comprising the microemulsion prepared by the process of the 
invention. 
BACKGROUND OF THE INVENTION 
The instant invention is related to a method of making microemulsion blends 
having an average particle size of from about 0.001 microns to about 0.05 
microns whereby the blend comprises at least one low amino content 
silicone and a surfactant having a high phase inversion temperature. The 
instant invention is further related to personal care products comprising 
said microemulsion. 
Microemulsions containing silicone fluids have been found to be useful in a 
variety of personal care products. As defined herein, the term 
"microemulsions" refers to transparent, mechanically and thermally stable 
systems comprising small droplets having a mean or average particle 
diameter usually not more than 0.05 microns in diameter, preferably not 
more than 0.040 microns in diameter and most preferably not more than 
0.025 microns in diameter. The small size of the droplets imparts a high 
degree of transparency to the emulsion. 
The use of microemulsions is known in the art, see for example U.S. Pat. 
Nos. 4,797,272 (Linnet al.) and U.S. Pat. No. 4,620,878 (Gee). U.S. Pat. 
No. 4,797,272 to Linnet al. discloses water-in-oil microemulsion 
compositions having a mean droplet size ranging from about 0.001 microns 
to about 0.200 microns. U.S. Pat. No. 4,620,878 to Gee discloses a 
polyorganosiloxane emulsion that contains a polyorganosiloxane containing 
at least one polar radical such as an amino or ammonium radical attached 
to the silicon of the siloxane by Si-C or Si-O-C bonds or at least one 
silanol radical and at least one surfactant that is insoluble in the 
polyorganosiloxane. Water is added forming a translucent oil concentrate. 
The translucent oil concentrate is then rapidly dispersed in water to 
prepare emulsions with fairly low particle sizes. A drawback of Gee's 
teachings is that the oil concentrate must be diluted with very large 
quantities of water such that the final emulsion rarely contains more than 
about 5 wt. % silicone solids. The emulsions prepared by Gee typically 
have an average particle size of less than 0.14 microns. 
Microemulsions of volatile silicones are taught in the art, for example 
U.S. Pat. Nos. 4,782,095 and 4,801,447, however these microemulsions have 
required large amounts of surfactants. The high levels of surfactants 
required in the prior art applications are detrimental in many 
applications. 
Chrobaczek and Tschida in U.S. Pat. No. 5,057,572 teach the preparation of 
an aminoalkyl substituted polysiloxane where the silicone fluid, a 
water-soluble emulsifier, in contrast to Gee, water and an acid are 
combined and heated to 50.degree. C. The necessity for a specific sequence 
of process steps, such as order of addition, is not taught by Chrobaczek. 
While Chrobaczek teaches this procedure is applicable to silicone fluids 
with an amino content of 0.1 meq./gr., in practice microemulsions result 
only when the amino content is above a threshold of about 0.12 to 0.14 
meq./gr. Below this threshold level the particle size of the emulsion is 
such that the emulsion is hazy, and therefore not a true microemulsion, 
true microemulsions possess optical transparency to a greater or lesser 
degree. 
Breneman et al. in U.S. Pat. No. 5,234,495 teach the preparation of 
microemulsions through a process utilizing the blending of an organo 
modified polysiloxane, e.g. an aminofunctional polysiloxane, an organo 
modified polysiloxane emulsifier, water, and an alkaline metal salt. 
Heating such a blend above the cloud point of the mixture and 
simultaneously subjecting the mixture to high shear mixing produces a 
liquid phase that can be cooled to form a microemulsion. 
Microemulsions of aminofunctional silicones, particularly aminofunctional 
silicones having a low amino content, provide beneficial results when used 
in personal care product formulations. It continues to be desirable to 
provide alternative or improved methods for preparing microemulsions of 
small average particle size. 
SUMMARY OF THE INVENTION 
In one embodiment, the instant invention comprises a transparent 
oil-in-water microemulsion comprising: (a) a low amino content 
microemulsifiable silicone, (b) a surfactant having a high phase inversion 
temperature, and (c) water. 
In another aspect, the instant invention provides a method of preparing a 
transparent polyorganosiloxane microemulsion having a mean particle size 
of from about 0.001 to about 0.050 microns, preferably from about 0.010 to 
about 0.030 microns, and most preferably from about. 0.010 to about 0.025 
microns, comprising a low amino content microemulsifiable silicone and at 
least one surfactant having a high phase inversion temperature. 
Other aspects of the invention are microemulsions of polydimethylsiloxane, 
polymethylmethacrylates and the like, and personal care products 
comprising said microemulsion.

DETAILED DESCRIPTION OF THE INVENTION 
The instant invention is based upon the discovery that functionalized 
silicones such as amino functional silicones which are capable of forming 
microemulsions may be blended with surfactants having a high phase 
inversion temperature and the blend processed such that the mixture forms 
a microemulsion. Such microemulsions are generally transparent. By 
transparent applicants mean the absence of turbidity or haze wherein haze 
is defined by an ASTM test, specifically ASTM test number D871 using 
turbidity suspension standards and wherein said haze or turbidity is below 
an upper limit of about 150. At levels of the haze number above about 50 
the microemulsions of the present invention begin to gradually change from 
transparent to translucent. The haze numbers of the microemulsions of the 
present invention range from 0 to about 150, more preferably from about 0 
to about 80 and most preferably from 0 to about 50. The turbidity 
suspension standards used in the ASTM test D871 are available from Hellige 
Incorporated of Garden City, New York. Applicants note that pure distilled 
water is 0 on the haze scale. 
Polyorganosiloxane microemulsions prepared by the method of the instant 
invention have a mean particle size of from about 0.005 to about 0.050 
microns, preferably from about 0.010 to about 0.030 microns, and most 
preferably from about 0.010 to about 0.025 microns. Generally haze and 
average particle size correlate with one another but they are also 
affected by the relative amounts of the two major components of the 
emulsion, the silicone oil and the water. Thus while at a constant oil to 
water ratio the haze and average particle size might correlate, haze by 
itself is not both a necessary and sufficient criterion to be an indicator 
of average particle size in a microemulsion unless other constraints are 
specified. 
By microemulsifiable applicants define the term to mean capable of forming 
a microemulsion wherein the mean particle size of the emulsion ranges from 
0.0001 microns to about 0.050 microns. By microemulsifiable silicone 
applicants define a silicone or a mixture of silicones that can form a 
microemulsion as defined by applicants herein before. 
The phase inversion temperature is that temperature at which a given 
surfactant is equally soluble in a lipophilic and a hydrophilic phase that 
are co-extensive. Generally the hydrophilic phase of interest or use is 
water. At the phase inversion temperature, the surfactant, hydrophilic 
phase and lipophilic phase are in a thermodynamic state of minimum free 
energy. This thermodynamic state is characterized by a minimum in particle 
size of the emulsion formed therewith when the mixture is emulsified. Thus 
the phase inversion temperature has a tendency to be specific for a given 
composition of components. While the phase inversion temperature varies as 
a function of composition, when one of the two liquid phases is held 
constant e.g. water, the phase inversion temperature of a series of 
mixtures utilizing a given surfactant, water, and a variety of lipophilic 
phases that are immiscible with the water, the phase inversion temperature 
will tend to vary over a much narrower range of temperatures. 
In one embodiment of the instant invention an oil surfactant mixture is 
prepared by blending: 
(1) an amount ranging from 10 to 30 parts per hundred of the final 
composition of the microemulsion of a polyorganosiloxane that can be 
microemulsified, A(1), optionally having an amino content of from about 
0.06 to about 3.0 milliequivalents per gram and comprising a silicone of 
the formula: 
EQU M(R.sub.a Q.sub.b SiO.sub.(4-a-b)/2).sub.x (R.sub.c SiO.sub.(4-c)/2).sub.y 
M 
whereby in the formulas above R is a hydrocarbon or hydrocarbon radical 
having from 1 to about 6 carbon atoms, Q is a polar radical having the 
general formula --R.sup.1 HZ, wherein R.sup.1 is a divalent linking group 
bound to hydrogen and the radical Z, comprised of carbon and hydrogen 
atoms; carbon, hydrogen and oxygen atoms, or carbon, hydrogen and nitrogen 
atoms; and Z is an organic amino functional radical containing at least 
two amino functionalities; "a" assumes values ranging from about 0 to 
about 2, "b" assumes values ranging from about 1 to about 3, "a"+"b" is 
less than or equal to 3, and "c" is a number in the range of fiord about 1 
to about 3; and x is a number in the ,range of from 1 to about 20 
preferably from about 1 to 10 and most preferably about 8, and y is a 
number in the range from about 20 to about 800, preferably from about 100 
to about 500, and most preferably about 275, and M is any suitable 
silicone endstopping group known in the art. Non-limiting examples of 
radicals represented by R include alkyl radicals such as methyl, ethyl, 
propyl, isopropyl, butyl, isobutyl, amyl, isoamyl, hexyl, isohexyl, and 
the like; alkenyl radicals such as vinyl, halo vinyl , alkyl vinyl, allyl, 
haloallyl, alkylallyl, cycloalkyl radicals such as cyclobutyl, 
cyclopentyl, cyclohexyl and the like, phenyl radicals, benzylradicals, 
halohydrocarbon radicals such as 3-chloropropyl, 4-bromobutyl, 
3,3,3-trifluoropropyl, chlorocyclohexyl, bromophenyl, chlorophenyl and the 
like, and sulfur containing radicals such as mercaptoethyl, 
mercaptopropyl, mercaptohexyl, mercaptophenyl and the like; preferably R 
is an alkyl radical containing from 1 to about 6 carbon atoms; and most 
preferably R is methyl. Examples of R.sup.1 include methylene, ethylene, 
propylene, hexamethylene, decamethylene, --CH.sub.2 CH(CH.sub.3)CH.sub.2 
--, phenylene, naphthylene, --CH.sub.2 CH.sub.2 SCH.sub.2 CH.sub.2 --, 
--CH.sub.2 CH.sub.2 OCH.sub.2 --, --OCH.sub.2 CH.sub.2 --, --OCH.sub.2 
CH.sub.2 CH.sub.2 ; --CH.sub.2 CH(CH.sub.3)C(O)OCH.sub.2, 
--(CH.sub.2).sub.3 CC(O)OCH.sub.2 CH.sub.2 --, --C.sub.6 H.sub.4 C.sub.6 
H.sub.4 --, --C.sub.6 H.sub.4 CH.sub.2 C.sub.6 H.sub.4 --, and 
--(CH.sub.2).sub.3 C(O)SCH.sub.2 CH.sub.2 --. 
Z is an organic amino functional radical containing at least two amino 
functionalities. One possible formula for Z is --NH(CH.sub.2).sub.z 
NH.sub.2 where z is one or greater. Another possible formula for Z is 
--N(CH.sub.2).sub.z (CH.sub.2).sub.zz NH where both z and zz are 
independently one or greater, this structure encompasses diamino ring 
structures such as piperazinyl. Z is most preferably a --NHCH.sub.2 
CH.sub.2 NH.sub.2 radical. 
Q is most preferably an amine functional polar radical having the formula 
--CH.sub.2 CH.sub.2 CH.sub.2 NHCH.sub.2 CH.sub.2 NH.sub.2. 
In the formulas, "a" assumes values ranging from about 0 to about 2, "b" 
assumes values ranging from about 1 to about 3, "a"+"b" is less than or 
equal to 3, and "c" is a number in the range of from about 1 to about 3. 
The molar ratio of R.sub.a Q.sub.b SiO.sub.(4-a-b)/2 units to R.sub.c 
SiO.sub.(4-c)/2 units ranges from about 1:2 to about 1:65, preferably from 
about 1:5 to about 1:65, and most preferably from about 1:15 to about 
1:20. 
It is preferred to use amino functional silicone fluids A(1) in the instant 
invention having the formula: 
EQU (CH.sub.3)3SiO(CH.sub.3)(C.sub.3 H.sub.6 NH.sub.2 C.sub.2 H.sub.4 
NH.sub.2)SiO!.sub.x (CH.sub.3).sub.2 SiO!.sub.y Si(CH.sub.3).sub.3 
wherein x is a number in the range of from 1 to about 20 preferably from 
about 1 to 10 and most preferably about 8, and y is a number in the range 
from about 20 to about 800, preferably from about 100 to about 500, and 
most preferably about 275. 
(2) adding to the silicone blend from step (1), of from about 1 to 20 parts 
per hundred of the final composition of the microemulsion of at least one 
surfactant, A(3), wherein at least one of the surfactants has a high phase 
inversion temperature, said phase inversion temperature generally ranging 
from about 45.degree. to about 95.degree. C.; 
(3) heating the blend of silicone(s) and surfactant(s) to a temperature 
ranging from about 45.degree. C. to about 95.degree. C., which is a 
temperature below the phase inversion temperature of the surfactant(s), 
while stirring; 
(4) water, Part I water in the examples, in an amount equal in weight to 
the weight of the silicone(s) used in part 1 added slowly; 
(5) adding an amount of an acid such that the final pH of the microemulsion 
is between about 4 and 7; preferably steps (4) and (5) are accomplished 
simultaneously either by the separate addition of water and a suitable 
acid or by the addition of an aqueous solution of a suitable acid. A 
preferred acid is acetic acid, however other acids may also be used such 
as HCl, hypophosphorous, lactic, propionic, glycolic, formic, and nitric. 
(6) water, Part II water in the examples, in an amount ranging from 40 to 
about 90 parts, said part II water having a temperature ranging from 
0.degree. C. to about 95.degree. C. below the temperature of acidified 
emulsion such that by the addition of said cold water the temperature of 
said microemulsion is cooled rapidly. 
A(3) contains at least one surfactant, wherein at least one of the 
surfactants has a phase inversion temperature ranging from 50.degree. C. 
to about 95.degree. C., said surfactant hereinafter referred to as the 
primary surfactant. Other optional surfactants are referred to as 
secondary surfactants. 
The surfactant or blend of surfactants has a hydrophilic-lipophilic balance 
value of from about 10 to about 16, preferably from about 11 to about 16, 
and most preferably from about 12 to about 13. The preferred 
hydrophilic-lipophilic balance value may vary as a consequence of 
increasing the level of volatile silicone in the microemulsifiable 
silicone. 
The primary surfactant may be cationic, anionic, nonionic or amphoteric in 
nature. Examples of such surfactants are disclosed in U.S. Pat. No. 
4,620,878 to Gee which is hereby incorporated by reference. Generally, 
nonionic surfactants are preferred for use in the instant invention. 
Surfactants useful as the primary surfactant in the instant invention 
include the sorbitan esters of fatty acids having 10 to 22 carbon atoms; 
polyoxyethylene sorbitan esters of C.sub.10 to C.sub.22 fatty acids having 
up to 95% ethylene oxide; polyoxyethylene sorbitol esters of C.sub.10 to 
C.sub.22 fatty acids, polyoxyethylene derivatives of fatty phenols having 
6 to 20 carbon atoms up to 95% ethylene oxide; fatty amino and amido 
betaines having 10 to 22 carbon atoms, and polyethylene condensates of 
C.sub.10 to C.sub.22 fatty acids or fatty alcohols having up to 95% 
ethylene oxide. 
Preferred primary surfactants for the practice of the instant invention 
include, but are not limited to, the octylphenoxy polyethoxy ethanols, 
which are nonionic surfactants-possessing varying amounts of ethylene 
oxide units and are available from Union Carbide Corporation under the 
general TRITON.RTM. trade name; trimethylnonyl polyethylene glycol ethers 
and polyethylene glycol ethers of linear 11-15 carbon atoms containing 
alcohols, available from Union Carbide Corporation under the general trade 
name TERGITOL.RTM.; the nonionic ethoxylated tridecyl ethers, available 
from Emery Industries under the trade name TRYCOL.RTM.. 
The preferred surfactants for use as the primary surfactant of the instant 
invention are the trimethylnonyl polyethylene glycol ethers and 
polyethylene glycol ethers of linear 11-15 carbon atom containing 
alcohols, available from Union Carbide Corporation under the trade name 
TERGITOL.RTM.. A preferred surfactant for use as the primary surfactant of 
the instant invention is a trimethylnonyl polyethylene glycol ether. The 
most preferred primary surfactant is 
2,6,8-trimethyl-4-nonyloxypolyethylene oxide (TERGITOL.RTM. TMN-6). 
The optional secondary surfactants may be anionic, cationic, nonionic, or 
amphoteric and may either be soluble or insoluble in the preferred amino 
functional silicone of A(1). Nonionic surfactants are preferred. 
Non-limiting examples of surfactants that are soluble in the amino 
functional silicone include the alkyl phenol ethoxylates. 
Preferably, the optional secondary surfactant used in this invention is 
also insoluble in the silicone of A(1). The preferred surfactants for use 
as the secondary surfactants in the instant invention are polyethylene 
glycol ethers of linear 11-15 carbon atoms containing alcohols. 
The amount of A(3) is in the range of from about 1 to about 30, preferably 
from about 1 to about 20, and most preferably from about 5 to about 15, 
parts by weight per 100 parts by weight of the final microemulsion 
composition. 
The blend of silicones, surfactants and water is homogenized in a 
homogenizer or other suitable mixing equipment. The length of time 
necessary to form a homogeneous mixture or emulsion in this step will 
depend on mixing equipment parameters and can be determined by those 
skilled in the art without undue experimentation. High shear mixing, 
either at ambient pressure or under conditions where the reaction medium 
is pressurized are generally unnecessary in order to form the 
microemulsions of the instant invention. Because the blend contains a 
surfactant having a high phase inversion temperature, the temperature at 
which the microemulsion is formed must be carefully controlled. Thus the 
step of adding part I water is performed in a temperature range varying 
between 45.degree. C. and 95.degree. C., more preferably varying between 
55.degree. C. and 90.degree. C., and most preferably varying between 
65.degree. C. and 85.degree. C. 
In step (5) the microemulsion is acidified to bring the pH of the emulsion 
into a range varying between 4 and 7, more preferably between 5 and 6.5, 
and most preferably between 5.5 and 6.5. This step is particularly 
effective when combined with step (4) 
In order to change the pH of the reaction medium, it is necessary to 
consider the quantity of amino functional silicone or silicone present in 
the reaction mixture. The amount of acid needed to provide such pH values 
will depend on the amount of the amino functional silicone or silicone 
fluid (A)(1) and the amino content of the amino functional silicone fluid. 
For example, with the amino functional silicone fluid having an amino 
content of 0.6 milliequivalents per gram, the amount of acid sufficient to 
provide a pH within the desired range will be approximately 2.5 parts per 
weight per 100 parts per weight of the amino functional silicone fluid. 
With an amino functional silicone fluid having an amino content of 3.0 
milliequivalents per gram, the weight of acid will be about 12.5 parts per 
weight per 100 parts per weight of the fluid. While the weights of acid 
necessary to achieve a given pH may vary depending on the molecular and 
equivalent weights of the acid chosen to control the pH, control of pH to 
the desired value is the primary purpose of the acid addition. Further, it 
has been found that the addition of acid must be simultaneous with the 
addition of the part I water. 
Additionally, silicone fluids, particularly amino or ammonium. functional 
silicone fluids, having a viscosity ranging from 10 to 10,000 centistokes 
at 25.degree. C. are preferred for use with the process of the instant 
invention. Thus amino functional silicone fluids having an amino content 
ranging from about 0.10 meq./gr. to about 10.0 meq./gr. and viscosity 
ranging from about 10 to about 10,000 centistokes at 25.degree. C. are 
preferred for use with the process of the instant invention. 
The amino functional silicone microemulsions of the present invention are 
useful in a variety of personal care product applications such as hair 
conditioners, the so-called 2 in 1 shampoos, and hair fixative 
preparations such as styling gels mousses and the like. For purposes of 
personal care applications the conditioner formulations generally comprise 
an amino functional silicone microemulsion content ranging from about 5 
weight percent to about 15 weight percent, more preferably from about 5 
weight percent to about 10 weight percent, and most preferably from about 
6 weight percent to about 7 weight percent. For purposes of personal care 
applications the 2 in 1 shampoo formulations generally comprise an amino 
functional silicone microemulsion content ranging from about 2 weight 
percent to about 7 Weight percent, more preferably from about 2 weight 
percent to about 5 weight percent, and most preferably from about 3 weight 
percent to about 4 weight percent. For purposes of personal care 
applications the fixative formulations generally comprise an amino 
functional silicone microemulsion content ranging from about 2 weight 
percent to about 10 weight percent, more preferably from about 2 weight 
percent to about 6 weight percent, and most preferably from about 3 weight 
percent to about 5 weight percent. The personal care products utilizing 
microemulsions prepared by the process of the instant invention will 
typically exhibit haze numbers below about 100. Applicants note that the 
weight percent ranges herein before described constitute weight percent 
ranges for the finished microemulsions as a component of the personal care 
product. Thus a microemulsion prepared by the process of the present 
invention will have a silicone content varying from about 5 weight percent 
to about 25 weight percent, which will vary from about 0.1 weight percent 
to about 7 weight percent as a percentage of the final composition of the 
personal care product when the microemulsion is incorporated into the 
personal care product. Additionally, the microemulsions of the present 
invention may be formulated into textile treating products or skin care 
formulations including color cosmetics. 
EXPERIMENTAL 
The procedure outlined in the detailed description of the invention was 
utilized to prepare the following non-limiting examples, examples 1 
through 24, which are illustrative of the microemulsions of the instant 
invention. Uses of these microemulsions in personal care products are also 
demonstrated. Examples 25 and 26 are illustrative of personal care 
formulations. 
EXAMPLE 1 
While warming to 70.degree. C., 16 parts of an aminofunctional silicone 
(linear, trimethylsilyl terminated, --(CH.sub.2).sub.3 --NH--CH.sub.2 
--CH.sub.2 --NH.sub.2, viscosity of 150 to 400 csk, amine content of 0.12 
meq/gr.) was mixed with 8 parts TERGITOL TMN-6. Part I water (16 parts) 
was then added dropwise at 70.degree. C. After water addition was 
complete, 1 part of acetic acid was added. The mixture thickened and 
became translucent. Part II water (58 parts) was then added rapidly with 
good agitation. Upon cooling, a microemulsion having an ATM haze number of 
about 40 was obtained. 
COMATIVE EXAMPLE 1 
This example was prepared in the same fashion as Example 6 in U.S. Pat. No. 
5,057,572. While warming to 70.degree. C., 16 parts of an aminofunctional 
silicone (linear, trimethylsilyl terminated, --(CH.sub.2).sub.3 
--NH--CH.sub.2 --CH.sub.2 --NH.sub.2, viscosity of 150 to 400 csk, amine 
content of 0.12 meq/gr.) was mixed with 8 parts TERGITOL TMN-6 and 74 
parts water to form a homogeneous mixture. Lactic acid (1 part) was then 
added at 70.degree. C. After cooling a milky emulsion was obtained. The 
haze number of this preparation was greater than 200. 
EXAMPLE 2 
This example shows the effect of adding part II water slowly. While warming 
at 70.degree. C., 20 parts of an aminofunctional silicone (linear, 
trimethylsilyl terminated, --(CH.sub.2).sub.3 --NH.sub.CH.sub.2 --CH.sub.2 
--NH.sub.2, viscosity of 150 to 400 csk, amine content of 0.12 meq/gr.) 
was mixed with 12.5 parts TERGITOL TMN-6. Part I water was then added 
dropwise at 70.degree. C. After water addition was complete, 0.5 parts of 
acetic acid was added. The mixture thickened and became translucent. Part 
II water (53 parts) was then added dropwise with good agitation. The 
mixture slowly became thicker and then eventually thinned out towards the 
end of the water addition. Upon cooling, a microemulsion with a haze of 
about 200 was obtained. 
EXAMPLES 3-7 
These examples show the effect of different amounts of part I water (the 
amounts specified are in grams): 
______________________________________ 
Ex. Ex. Ex. Ex. Ex. 
Component 3 4 5 6 7 
______________________________________ 
Amino fluid 
65 65 65 65 65 
A1 
TERGITOL 40 40 40 40 40 
TMN-6 
Part I Water 
40 65 90 120 220 
Acetic Acid 
1 1 1 1 1 
Part II Water 
180 155 1130 100 0 
Haze 150 30 90 200+ 200+ 
pH 5.5 5.5 5.5 5.5 nm 
______________________________________ 
EXAMPLES 8-12 
These examples show the effect of different amounts of surfactant (the 
amounts specified are in grams): 
______________________________________ 
Ex. Ex. Ex. Ex. Ex. 
Component 8 9 10 11 12 
______________________________________ 
Amino fluid 
65 65 65 65 65 
A1 
TERGITOL 65 40 20 45 27.5 
TMN-6 
Part I Water 
65 65 65 65 65 
Acetic Acid 
1 1 1 1 1 
Part II Water 
130 155 175 150 167.5 
Haze 100 40 200 80 100 
pH 5.5 5.5 5.5 5.5 5.5 
______________________________________ 
EXAMPLES 13-17 
These examples show the effect of different temperatures of part II water 
and of using different amino fluids(the amounts specified are in grams): 
______________________________________ 
Ex. Ex. Ex. Ex. Ex. 
Component 13 14 15 16 17 
______________________________________ 
Amino fluid 
65 65 65 0 0 
A1 
Amino fluid 
0 0 0 65 65 
A2 
TERGITOL 40 40 40 40 40 
TMN-6 
Part I Water 
65 65 65 65 65 
Acetic Acid 
1 1 1 1 1 
Part II Water 
155 155 115 155 0 
Part II water 
Temperature 
25 0 75 25 25 
.degree.C. 
Haze 40 50 50 15 30 
pH 5.5 5.5 5.5 5.5 nm 
______________________________________ 
EXAMPLES 18-24 
These examples show the effect of using fluids with different amine 
concentrations at a low amine content (the amounts specified are in 
grams): 
______________________________________ 
Ex. Ex. Ex. Ex. Ex. Ex. Ex. 
Component 
18 19 20 21 22 23 24 
______________________________________ 
Amino fluid 
0 50 0 0 0 0 0 
A1 
Amino fluid 
65 15 25 15 0 0 0 
A3 
Amino fluid 
0 0 40 50 65 40 65 
A4 
Amino fluid 
0 0 0 0 0 25 0 
A5 
TERGITOL 40 40 40 40 40 40 40 
TMN-6 
Part I Water 
65 65 65 65 65 65 220 
Acetic Acid 
1 1 1 1 1 1 1 
Part II Water 
155 155 155 155 155 155 0 
Haze 200+ 100 80 50 40 60 60 
pH 5.5 5.5 5.5 5.5 5.5 5.5 5.5 
______________________________________ 
A3 = linear, trimethylsilylterminated, --(CH.sub.2).sub.3 --NH--CH.sub.2 
--CH.sub.2 --NH.sub.2 viscosity = 400 csk, amine content of 0.07 meq./gr. 
A4 = linear, trimethylsilylterminated, --(CH.sub.2).sub.3 --NH--CH.sub.2 
--CH.sub.2 --NH.sub.2 viscosity = 4500-5000 csk, amine content of 0.12 
meq./gr. 
A5 = linear, trimethylsilylterminated, --(CH.sub.2).sub.3 --NH--CH.sub.2 
--CH.sub.2 --NH.sub.2 viscosity = 4500-5000 csk, amine content of 0.07 
meq./gr. 
EXAMPLES 25 AND 26 
Personal Care Product Formulations 
The personal care products exemplified by examples 25 and 26 were prepared 
using a microemulsion prepared by the process of the present invention 
using a linear trimethylsilyl terminated amino functional silicone having 
an amino content of 0.55 meq./gr. and a viscosity of 150 centistokes at 
25.degree. C. prepared as described in example 1; the microemulsion had a 
silicone content of 20 weight percent. 
EXAMPLE 25 
A clear conditioner was prepared from the following components: 
______________________________________ 
Material Amount (wt. %) 
______________________________________ 
Deionized water 88.55 
Hydroxyethyl Cellulose 
1.0 
Cetrimonium Chloride 
3.5 
Silicone microemulsion 
6.0 
Glydant Plus .RTM. 
0.2 
Fragrance 0.75 
______________________________________ 
The preparative procedure employed was as follows: 
With good stirring the hydroxyethyl cellulose was added to the deionized 
water. The aqueous mixture was heated to 60.degree. C. When complete 
dispersion was achieved, the Glydant Plus.RTM. was added and stirred until 
the mixture was again clear. When the mixture was clear, the cetrimonium 
chloride and the silicone microemulsion prepared by the process of the 
present invention were added individually. The mixture was stirred while 
allowed to cool. When the temperature was below 40.degree. C., the 
fragrance was added. Stirring was continued for approximately 20 minutes 
after the addition of the fragrance. 
Generally, the optional components may be varied, substituted, or omitted 
according to the teachings of the art. For example, in order to prevent 
bacterial growth, preservatives may be added. Additionally fragrances, pH 
adjusting agents, antistatic or softening agents, cationic polymers, 
thickening agents, nonionic polymers such as acrylic acid polymers, 
neutralizing materials such as triethanolamine, sunscreens, antioxidants, 
proteins, vitamins, botanical extracts, and the like may be added. 
EXAMPLE 26 
A conditioning or 2 in 1 shampoo was prepared from the following 
components: 
______________________________________ 
Material Amount (wt. %) 
______________________________________ 
Deionized water 
33.89 
Hydroxyethyl Cellulose 
2.0 
Ammonium Lauryl Sulfate 
15.38 
(as 26% solution) 
Ammonium Laureth Sulfate 
21.43 
(as 28% solution) 
Cocamidopropyl Betaine 
11.43 
(as a 35% solution) 
Dowicil 200 .RTM. 
0.2 
Silicone microemulsion 
5.0 
Citric acid sufficient to adjust to desired pH 
Lauramide DEA 3.5 
Cetrimonium Chloride 
6.67 
Fragrance 0.5 
______________________________________ 
The preparative procedure employed was as follows: 
The hydroxyethyl cellulose was added to the water and stirred until the 
hydroxyethyl cellulose was thoroughly solvated. The Dowicil200.RTM. was 
added and the aqueous mixture was stirred and heated to 60.degree. C. The 
surfactants were added in the order listed, individually, followed by 
stirring until the mixture gave a homogeneous appearance. The Lauramide 
DEA was melted and added to the mixture. The mixture was then cooled with 
stirring continued during the cooling. When the temperature was below 
40.degree. C., the silicone microemulsion and fragrance were individually 
added followed by stirring. Mixing was continued for approximately 20 
minutes after the addition of the last component. 
Generally, the optional components may be varied, substituted, or omitted 
according to the teachings of the art. For example, in order to prevent 
bacterial growth, preservatives may be added. Additionally fragrances, pH 
adjusting agents, antistatic or softening agents, cationic polymers, 
thickening agents, nonionic polymers such as acrylic acid polymers, 
neutralizing materials such as triethanolamine, sunscreens, antioxidants, 
proteins, vitamins, botanical extracts, and the like may be added. 
While one of the benefits of using the microemulsions prepared by the 
process of the present invention is the ability to prepare clear personal 
care products having a haze number below about 100 to 150, opacifying or 
pearlizing agents may be incorporated into the personal care product 
formulations if desired. The microemulsions prepared by the process of the 
present invention provide conditioning benefits to a variety of personal 
care products including, but not limited to, hair coloring compositions, 
rinses, neutralizing lotions, creams, gels, mousses, aerosols, and pump 
sprays. 
It is apparent from the forgoing that many other variations and 
modifications may be made in the compositions and methods herein before 
described without deviating substantially from the process and 
compositions of the present invention. Accordingly, the embodiments of the 
present invention herein before described are exemplary only and are not 
intended to limit in any fashion or manner the scope of the claims 
appended hereto.