JPS6025906A - Preparation of highly-concentrated dispersion of pearl agent - Google Patents

Abstract

PURPOSE:To obtain the titled dispersion capable of providing a preparation system such as a detergent containing a cationic active agent, etc. with improved pearly luster, by crystallizing a pearl agent of a glycol higher fatty acid ester system in a blend of specific components with a specified composition under specific conditions. CONSTITUTION:A raw material mixture containing (A) 10-40wt% glycolic acid higher fatty acid diester, (B) 5-30wt% ampholytic ionic copolymer, (C) 5- 30wt% cationic active agent, and (D) 30-80wt% water is heated to >= the melting point of the component a to give a uniform solution, which is cooled so that crystal with pearly luster is precipitated, to give highly-concentrated dispersion of pearl agent. The dispersion can provide a preparation system such as a cleaner, e.g., shampoo, rinse, lotion, cream, soap, etc. and cosmetic comprising a cationic active agent as a main component with pearly luster by adding 0.1- 5wt% pearl agent to the preparation system.

Description

DETAILED DESCRIPTION OF THE INVENTION Technical Field The present invention relates to a method for producing a highly concentrated pearl agent dispersion.

According to the method of the present invention, in order to increase the commercial value of detergents, cosmetics, etc. containing cationic activators, a higher fatty acid diester pearl agent of glycols is crystallized in a formulation containing a high concentration of the diester. , it is possible to obtain a burl agent liquid with a satisfactory pearlescent luster.

Background of the Invention Conventionally, a method of adding a pearlescent agent to impart pearlescent luster has been practiced with the main purpose of increasing the commercial value of cleaning products such as shampoos, conditioners, lotions, creams, and soaps, as well as cosmetics. It has been.

Recently, (poly)alkylene glycol dihigher fatty acid esters have been commonly used as the pearl agent.

Depending on the crystal shape of this (poly)alkylene glycol dihigher fatty acid ester, the burl luster varies significantly.
Usually, a compound containing a (poly)alkylene glycol dihigher fatty acid ester is heated to a temperature above the melting point of this diester,
When the crystals are precipitated by cooling after forming a homogeneous liquid, the crystallization conditions are selected so that flaky crystals are precipitated. Using (poly)alkylene glycol dihigher fatty acid ester as a pearling agent in the formulation system to give it a good pearlescent luster has not yielded satisfactory results using the conventionally known method of crystallizing it in the final composition. It was impossible to obtain. Also, even by crystallizing the diester in a formulation containing a high concentration, it was not possible to obtain a satisfactory pearlescent luster.

The present inventors have discovered that (poly)alkylene dalicold dihigher fatty acid ester, which is currently mainly used as a pearl agent, can be used in detergents and cosmetics containing cationic activators (e.g., rinse agents, etc.). The present invention was completed by conducting intensive research to achieve crystallization in this state.

Summary of the Invention The present invention provides (a) higher fatty acid diester of glycols: 10 to 40 wt%, (b) zwitterionic copolymer = 5 to 30 wt%, (
c) Cationic activator = 5-30 wt%, (d) Water = 3
A high-concentration pearl characterized by heating a raw material mixture containing 0 to 80'wt% above the melting point of component (a) to form a uniform solution, and then cooling to precipitate crystals with pearl luster. The present invention provides a method for producing a drug dispersion.

Effects of the Invention By using the method of the present invention, formulations such as detergents such as rinses and cosmetics containing cationic activators contain (poly)alkylene glycol dihigher fatty acid ester crystallized as a pearl agent. 'It became possible to produce a dispersion.

3. Detailed description of the invention (a) used as a pearling agent in the method of the present invention
As the component higher fatty acid diester of glycols, (poly)algylene glycol dihigher fatty acid ester is preferably used. Specifically, higher fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, etc., and (poly)alkylene glycols, ethylene glycol, diethylene glycol, triethylene glycol, and Pyrene gelylcol, dipropylene glycol, etc. are used, and diesters produced from these higher fatty acids and (poly)alkylene glycols by known esterification techniques are used in the present invention. Examples include ethylene glycol dinoculumitate, triethylene glycol distearate, etc., but these need to be single products.
The above pearling agent may be present in the composition in an amount of 10 to 40% by weight, preferably in a mixture.
It is used as an additive in the range of 0 to 35% by weight.

The zwitterionic copolymer of component (b) used in the present invention has (I) CHz-C(Rx)COARzNR3R4, (
It) C&-C (R5 coogs, (2) other monomers copolymerizable with monomer (1) and (It), (in the above formula, R1 and R5 are each a hydrogen atom or a methyl group) , R2 is a C1-4 alkylene group, Ra and good are 01-4
18 alkyl group, bird is C1-18 saturated or unsaturated alkyl group or cycloalkyl group, A is oxygen atom or N
(indicating an H group). Examples of the monomer represented by the above general formula (1) include dimethylaminoethyl (meth)acrylate, diethylaminopropyl (meth)acrylate, and dimethylethyl (meth)ac 1-noramide.

Monomers represented by the above general formula (") include stearyl (meth)acrylate, lauryl (meth)acrylate, methyl (meth)acrylate, and cyclohexyl (
Examples include meth)acrylate, 2-ethylhexyl (meth)acrylate, allyl (meth)acrylate, and the like.

Further, monomers represented by the above general formula ( ) include diaseptone acrylamide, (meth)acrylamide, vinyl acetate, N-vinylpyrrolidone, 4-vinylpyridine, styrene, polyethylene glycol (meth)acrylate, etc. .

A plurality of monomers can be used for each of these monomers (I), (II) and (rib).

The above monomers (1), (II) and (g) are each 2
5-80% by weight, 20-75% by weight and 0-20% arsenic
preferably 30 to 60% by weight, 4% by weight, respectively.
It is used as a copolymer with a composition of 0 to 70% by weight and 0 to 10% by weight.

The copolymer having the above composition contains monomers (1), (TI) and (
[IO can be obtained by solution polymerization in a hydrophilic solvent such as ethanol, ingropanol, ethylene glycol monoethyl ether, acetone, methyl ethyl ketone, dioxane, etc. according to known techniques.

The copolymer having the above composition obtained by solution polymerization is then modified by reacting with a haloacetate to obtain a zwitterionic conjugate of component (b) used in the method of the present invention. Specific examples of salts include ammonium salts and/or amine salts of monochloroacetic acid (e.g. 2-amino-
2-methyl-1-glopanol salt, triethanolamine salt, etc.), alkali gold 54 salt (e.g. J-ga salt, K salt, etc.)
etc.

The above denaturation was carried out by adding monoacetate for 4 to 10 hours.
The reaction can be achieved by heating to 0-90°C,
The solution of the zwitterionic copolymer obtained in this way is
If necessary, the by-product inorganic salt is removed, the solvent is removed, and the solvent is replaced with an aqueous solvent before use.

The cationic activator used as component (e) in the present invention includes trimethylstearylammonium chloride, dimethyldistearylammonium chloride, dimethyldistearylammonium chloride, triethyllauryl ammonium chloride, hexadecyldiethylbenzylammonium chloride, and stearyldimethylbenzylammonium chloride. Known tsunothione activators such as chloride are used.

In the method of the present invention, water is further added to the above-mentioned components (a), (b), and (C) as component (d), and component (a): 10 to 40 wt%, preferably 20 to 40% by weight.
35 wt%, component (b): 5 to 30 wt%, preferably 8 to 15 w
t%, component (e): 5 to 30 wt%, preferably 8 to 15
wt%, component (d): 30 to 80 wt, preferably 40 to 6
5 wt%, to form a raw material mixture. Next, the mixture is heated to a temperature higher than the melting point of component (a) and stirred to form a uniform liquid. Thereafter, this is cooled to precipitate crystals with a burl luster, thereby producing a highly concentrated burl agent dispersion.

The obtained high-concentration bur agent dispersion is added as a bur agent at a ratio of 0.1 to 5 wt% to a formulation system such as a rinse agent or a hair treatment agent that has a cationic activator as a main component, and is good for the formulation system. It is possible to impart a burl luster.

EXPERIMENTAL EXAMPLES "Parts" and "%" used in the following examples are by weight.

Zwitterionic copolymer production example A Dimethylamine ethyl methacrylate: 40 parts, methyl methacrylate: 25 parts, cyclohexyl methacrylate: 10 parts, tridecyl methacrylate: 25 parts, ethanol: 100 parts, α,α'-azo 1 part of bisisobutyronitrile was placed in a fourth flask equipped with a stirrer, a reflux condenser, and a nitrogen inlet tube, and after purging the system with nitrogen, the temperature was raised to 80°C in 30 minutes. The mixture was kept for about 4 hours to carry out copolymerization.

Next, tn-t', 2 monochloroacetic acid in 47 parts of ethanol.
4 parts to 2-amino-2-methyl-1-propanol 2
A solution obtained by neutralizing with 3 parts was added to the copolymerization reaction product obtained as described above, and a modification reaction was carried out at 80° C. for 6 hours. The solvent of the produced copolymer resin modified product solution was replaced with water to obtain a water bath solution of the copolymer resin modified product having a resin content of 30%. This resin aqueous solution is referred to as "copolymer resin modified solution A."

Zwitterionic copolymer production example B Dimethylamine ethyl methacrylate: 6 parts, Butyl methacrylate, 30 parts, Povinyl acetate: 10 parts, Ethanol: 100 parts, α,α'-azobisisobutyronitrile: 1 Copolymerization, modification, and solvent replacement were carried out in the same manner as in the above-mentioned amphoteric ionic copolymer production example A except that
An aqueous solution of a modified copolymer resin having a resin content of 30% was obtained. This is referred to as "copolymer resin modified product solution B". Zwitterionic copolymer production example C: 130 parts of dumeric amine ethyl acrylate, 25 parts of butyl methacrylate, 10 parts of 2-ethylhexyl acrylate, lauryl Methacrylate: 20 parts, 4
-Vinylpyridino: 15 parts, Improvil alcohol 1
6 parts, α, α'-Azobisinobutyronitrile: 1 part was placed in a four-bottle flask equipped with a stirrer, a reflux condenser, and a nitrogen inlet tube, and the system was purged with nitrogen. 8
The temperature was raised to 0° C. and maintained at this temperature for about 4 hours to carry out copolymerization.

Next, in the first step, sushily obtained by neutralizing 33.3 parts of monochloroacetic acid with 19.8 parts of potassium hydroxide in Improper Tool 3s and 4iNB was added to the copolymerization reaction product obtained by making the above paste. The denaturation reaction was carried out at 80° C. for 6 hours. After cooling, the produced potassium chloride was separated from each other, and water was added to the solution to obtain an aqueous solution of the modified copolymer resin having a resin content of 20%. This resin solution is called "copolymer resin modified solution C".
shall be.

Example 1 Ethylene glycol dipalmite): 9 H', B
, 21 parts of ethylene glycol distearate, 33 parts of modified copolymer resin J'M, A, 25 parts of trimethylstearylammonium chloride, 5 parts of trimethylhexadecyl ammonium chloride, and 27 parts of pure water. , and heated to 80° C. for about 1 hour while stirring to obtain a homogeneous solution. The solution was then heated to 30°C with gentle stirring.
The mixture was cooled down to precipitate pearl crystals.

The resulting high-concentration pearlescent agent dispersion was visually evaluated for pearlescent luster by the following method. That is, the concentration in the system to be evaluated is higher fatty acid diester of glycols: 1.0% and trimethylalkylammonium chloride (or dimethylalkylbenzylammonium chloride, where the alkyl group is stearyl group/hexadecyl group = so/so) = 1 After adjusting the dispersion uniformly so as to obtain a .5% aqueous dispersion, the degree of burl gloss was evaluated by visual judgment according to the following criteria.

5: Very good 4: Good 3: Normal 2: Defective 1: Extremely poor The results are shown in Table 1.

Example 2 Ethylene glycol dipalmitate: 9'f'15
, 21 parts of ethylene glycol distearate, 233 parts of copolymer resin modified solution A, 12 parts of dimethylstearylbenzylammonium chloride, and 25 parts of pure water were treated in the same manner as in Example 1 to obtain pearl crystals. was precipitated, and the same evaluation as in Example 1 was performed. The results are shown in Table 1.

Example 3 Ethylene glycol similystate: 2 parts, ethylene glycol dipalmitate: 13 parts, ethylene glycol distearate: 15 parts, copolymer resin modified product solution 82
A raw material mixture of 40 parts of trimethylstearylammonium chloride, 5 parts of trimethylhexadecyl ammonium chloride, and 20 parts of pure water was operated in the same manner as in Example 1 to precipitate pearl crystals. We conducted an evaluation. The results are shown in Table 1.

Example 4 Triethylene glycol dibehenate: 21 parts, triethylene glycol distearate: 4 parts, copolymer resin modified product solution C: 40 parts, trimethylstearylammonium chloride: 4 parts, trimethylhexadecyl ammonium chloride = 4 A raw material mixture containing 27 parts of pure water was operated in the same manner as in Example 1 to precipitate Burr crystals, and the same evaluation as in Example 1 was performed. The results are shown in Table 1.

Example 5 Glopylene glycol dipalmitate: 9 parts, propylene glycol distearate: 21 parts, copolymer resin modified product solution A: 40 parts, trimethylstearylammonium chloride = 6 parts, trimethylhexadecyl ammonium chloride 76 parts , pure water = 18 parts of the raw material mixture,
The same operation as in Example 1 was performed to precipitate Burl crystals, and the same evaluation as in Example 1 was performed. The results are shown in Table 1.

Comparative Example 1 A raw material mixture of 9 parts of ethylene glycol dipalmitate, 21 parts of ethylene glycol distearate, 5 parts of trimethylstearylammonium chloride, 5 parts of trimethylstearylammonium chloride, and 60 parts of pure water was stirred, Heat to 80° C. for about 1 hour to obtain a homogeneous solution. The solution was then heated to 30°C with gentle stirring.
The mixture was cooled down to precipitate Burl crystals.

The obtained high-concentration var agent dispersion was evaluated in the same manner as in Example 1. The results are shown in Table 1.

Comparative Example 2 Ethylene glycol civalmitate = 2 parts, nee y-v
A raw material mixture of y Glycol Civalmicy 113L ethylene dalicol distearate: 15 parts, trimethylstearylammonium chloride: 5 parts, trimethylhexadecyl ammonium chloride = 5 parts, and pure water: 60 parts was treated in the same manner as in Comparative Example 1 to obtain pearls. Crystals were precipitated and evaluated in the same manner as in Example 1. The results are shown in Table 1.

Comparative Example 3 Ethylene glycol civalmitate: o, part a, ethylene glycol distearate: 0.77+3. ) Limethylstearylammonium chloride = 0.8 part,
Trimethylhexadecyl ammonium chloride: 0.
8 parts, pure water: 97.4 parts of the raw material mixture is heated to 80° C. for about 1 hour while stirring to obtain a homogeneous solution. Next, the solution was cooled to 30° C. with gentle stirring to precipitate pearl crystals, and the same evaluation as in Example 1 was performed. The results are shown in Table 1.

Comparative Example 4 Ethylene glycol cyalmite): 0.3, -ethylene glycol distearate: 0.7 part, trimethylstearylammonium chloride: 0.8 part, trimethylhexadecyl ammonium chloride = 0.8
parts, copolymer resin modified solution A: 0.3 parts, pure water: 9
1 part of the raw material mixture was operated in the same manner as in Example 3 to precipitate pearl crystals, and the same evaluation as in Example 1 was performed. The results are shown in Table 1.

Table 1

Claims (2)

[Claims] (1) (a) Ri+): higher fatty acid diester of yl group: 10 to 40 wt%, (b) zwitterionic copolymer = 5 to 30 wt%, (c
) Cationic activator: 5 to 30 wt%, (d) water = 3
A high-concentration pearling agent characterized by heating a raw material mixture containing 0 to 8 wt% above the melting point of component (a) to form a uniform solution, and then cooling to precipitate crystals with pearl luster. Method for producing dispersion liquid. (2) The zwitterionic copolymer of component (b) has a copolymer composition such that (I) CH2<(Rx)COA&NRa&: 25
~80wt% (ff) Hz<'(1(s) COOR
a: 20 to 75 wt% ((2) monomer (1) and (
20 to 20 wt% of other monomers copolymerizable with W) (In the above formula, R□ and R5 are each a hydrogen atom or a methyl group, R2 is an alkylene group of 01 to 4, and R3 and R4 are C1 to 18 R6 is a C1-18 saturated or unsaturated alkyl group or cycloalkyl group, A is an oxygen atom or a Nu group) modified with a haloacetate. ゛ Patent Claim Range 1. Method described in ◎