CN113185710A - Amino silicone oil emulsion and preparation method thereof - Google Patents
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- A61K8/89—Polysiloxanes
- A61K8/896—Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate
- A61K8/898—Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate containing nitrogen, e.g. amodimethicone, trimethyl silyl amodimethicone or dimethicone propyl PG-betaine
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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Abstract
The invention discloses an amino silicone oil emulsion and a preparation method thereof. The invention firstly mixes the emulsifier and the stabilizing agent of the amino silicone oil, and then adds the auxiliary emulsifier and the water to obtain the emulsion with the bicontinuous phase structure between O/W and W/O, and the emulsification process is simple and is beneficial to popularization and production. The amino silicone oil emulsion obtained by the emulsification process has higher stability, can be uniformly dispersed in a system when being applied to shampoo and hair conditioner products, and effectively maintains the softness and the moisture of hair.
Description
Technical Field
The invention relates to the technical field of amino silicone oil, and particularly relates to an amino silicone oil emulsion and a preparation method thereof.
Background
The amino silicone oil is polydimethylsiloxane containing amino in a side chain or a terminal group, the structure of the amino silicone oil is special, the amino silicone oil has good adsorbability, compatibility, low surface tension and other properties, and the amino on the side chain has strong polarity and positive charge. The amino silicone oil can be used in various hair washing and caring products, can interact with the surface of hair with negative electricity, and is firmly adsorbed on the surface of hair, and the oily group can make the hair hydrophobic and easy to dry, can increase the luster and anti-static performance of the hair, improve and repair the hair quality, reduce the friction coefficient between the hair, and endow the hair with good smoothness, flexibility and washability. However, when the amino silicone oil with high molecular weight is used for preparing shampoo and hair conditioner products, the viscosity is high, the amino silicone oil is difficult to emulsify and uniformly disperse in a system, and the stability problem of the products is easily caused or the using effect of the products is easily influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of an amino silicone oil emulsion, which has higher stability, can be uniformly dispersed in a system when being applied to shampoo and hair conditioner products, and effectively maintains the softness and the moisture of hair.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing amino silicone oil emulsion, which is characterized by comprising the following steps:
(1) weighing amino silicone oil, an emulsifier, an auxiliary emulsifier, a stabilizer, a pH regulator and water;
(2) adding amino silicone oil, an emulsifier and a stabilizer into a reaction vessel, stirring for 50-100min at the temperature of 50-70 ℃ at the rotation speed of 1000-plus 5000rpm, then adding an auxiliary emulsifier, continuously stirring for 30-60min, adding water, and stirring for 30-60min at the rotation speed of 500-plus 1000 rpm;
(3) adding a pH regulator into the system obtained in the step (2) to regulate the pH to 5.0-7.0, and uniformly stirring at the rotating speed of 300-500rpm to obtain the amino silicone oil emulsion; wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 20-35% of amino silicone oil, 1-10% of emulsifier, 2-6% of co-emulsifier, 0.1-1% of stabilizer, 0.1-0.5% of pH regulator and the balance of water.
In the emulsification process, the emulsifier and the stabilizing agent amino silicone oil are mixed firstly, and then the auxiliary emulsifier and the water are added to obtain the emulsion with the bicontinuous phase structure between O/W and W/O.
The amino silicone oil emulsion obtained by the emulsification process has higher stability, can be uniformly dispersed in a system when being applied to shampoo and hair conditioner products, and effectively maintains the softness and the moisture of hair.
Preferably, the amino silicone oil comprises at least one of amino-terminated polydimethylsiloxane, bis-aminopropylpolydimethylsiloxane, and aminoethylaminopropylpolydimethylsiloxane.
Preferably, the emulsifier is at least one of an anionic emulsifier, a cationic emulsifier and a nonionic emulsifier.
Specifically, the anionic emulsifier can be sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and the like; the cationic emulsifier can be hexadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, dodecyl trimethyl ammonium chloride and the like; the nonionic emulsifier can be sorbitan monopalmitate, alkylphenol polyoxyethylene ether series, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, alcohol ether glycoside, glucosamide, etc.
Preferably, the emulsifiers are alcohol ether glycosides and glucose amides. Compared with other emulsifiers, the emulsifier selects the alcohol ether glycoside and the glucosamide to be compounded as the emulsifier, has better emulsifying capacity on amino silicone oil such as amino-terminal polydimethylsiloxane and the like, and can obtain uniform and stable amino silicone oil emulsion.
More preferably, the weight ratio of the alcohol ether glucoside to the glucose amide is 2-4:1, and the emulsifying effect of the amino silicone oil is better within the range of the mixture ratio.
Preferably, the coemulsifier is at least one of ethylene glycol monobutyl ether and diethylene glycol monobutyl ether.
Preferably, the stabilizer is at least one of cetearyl alcohol, trifluoromethyl maleic anhydride and fatty alcohol polyoxyethylene ether carboxylate, and contributes to further improving the stability of the amino silicone oil emulsion. .
Preferably, the pH adjusting agent is acetic acid.
Preferably, in the step (2), the amino silicone oil, the emulsifier and the stabilizer are added into a reaction vessel, stirred for 60-90min at the temperature of 50-60 ℃ and the rotation speed of 2000-4000rpm, then the co-emulsifier is added and stirred for 40-60min, water is added, and stirred for 40-50min at the rotation speed of 500-600rpm, and the stability of the amino silicone oil emulsion is further improved by optimizing the emulsification process parameters.
Preferably, the amino silicone oil emulsion comprises the following components in percentage by weight: 20-35% of amino silicone oil, 3-8% of emulsifier, 2-4% of co-emulsifier, 0.1-1% of stabilizer, 0.1-0.5% of pH regulator and the balance of water, and is beneficial to further improving the emulsification effect of the amino silicone oil emulsion.
The invention also provides the amino silicone oil emulsion prepared according to the method.
The invention also provides the application of the amino silicone oil emulsion in preparing hair conditioner and/or shampoo. The amino silicone oil emulsion provided by the invention and other conventional auxiliary materials are used for preparing shampoo and hair conditioner products, and the amino silicone oil emulsion can be uniformly dispersed in a system, so that the softness and the moisture of hair can be effectively maintained.
Compared with the prior art, the invention has the beneficial effects that:
the amino silicone oil emulsion has simple emulsification process, is beneficial to popularization and production, is uniform and stable, and can be uniformly dispersed in a system when being used for preparing shampoo and hair conditioner products, thereby effectively maintaining the softness and the moistening degree of hair.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Example 1
A method of making an amino silicone oil emulsion comprising the steps of:
(1) weighing ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, glucosamide, ethylene glycol monobutyl ether, trifluoromethyl maleic anhydride, acetic acid and water;
(2) adding ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, glucosamide and trifluoromethyl maleic anhydride into a reaction vessel, stirring at 60 ℃ for 90min at the rotating speed of 4000rpm, then adding ethylene glycol monobutyl ether, continuing stirring for 60min, adding water, and stirring at the rotating speed of 500rpm for 45 min;
(3) adding acetic acid into the system obtained in the step (2) to adjust the pH value to 5.0-7.0, and uniformly stirring at the rotating speed of 300rpm to obtain the amino silicone oil emulsion;
wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 35% of amino-terminated polydimethylsiloxane, 4% of alcohol ether glucoside, 2% of glucose amide, 4% of ethylene glycol monobutyl ether, 0.15% of trifluoromethyl maleic anhydride, 0.3% of acetic acid and the balance of water.
Example 2
A method of making an amino silicone oil emulsion comprising the steps of:
(1) weighing ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, glucosamide, ethylene glycol monobutyl ether, trifluoromethyl maleic anhydride, acetic acid and water;
(2) adding ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, glucosamide and trifluoromethyl maleic anhydride into a reaction vessel, stirring at 60 ℃ for 90min at the rotating speed of 4000rpm, then adding ethylene glycol monobutyl ether, continuing stirring for 60min, adding water, and stirring at the rotating speed of 500rpm for 45 min;
(3) adding acetic acid into the system obtained in the step (2) to adjust the pH value to 5.0-7.0, and uniformly stirring at the rotating speed of 300rpm to obtain the amino silicone oil emulsion;
wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 35% of ammonia-terminated polydimethylsiloxane, 4.8% of alcohol ether glucoside, 1.2% of glucose amide, 4% of ethylene glycol monobutyl ether, 0.15% of trifluoromethyl maleic anhydride, 0.3% of acetic acid and the balance of water.
Example 3
A method of making an amino silicone oil emulsion comprising the steps of:
(1) weighing ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, glucosamide, ethylene glycol monobutyl ether, trifluoromethyl maleic anhydride, acetic acid and water;
(2) adding ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, glucosamide and trifluoromethyl maleic anhydride into a reaction vessel, stirring at 60 ℃ for 90min at the rotating speed of 4000rpm, then adding ethylene glycol monobutyl ether, continuing stirring for 60min, adding water, and stirring at the rotating speed of 500rpm for 45 min;
(3) adding acetic acid into the system obtained in the step (2) to adjust the pH value to 5.0-7.0, and uniformly stirring at the rotating speed of 300rpm to obtain the amino silicone oil emulsion;
wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 35% of amino-terminated polydimethylsiloxane, 5% of alcohol ether glucoside, 1% of glucose amide, 4% of ethylene glycol monobutyl ether, 0.15% of trifluoromethyl maleic anhydride, 0.3% of acetic acid and the balance of water.
Example 4
A method of making an amino silicone oil emulsion comprising the steps of:
(1) weighing ammonia-terminated polydimethylsiloxane, lauryl sodium sulfate, glucose amide, ethylene glycol monobutyl ether, trifluoromethyl maleic anhydride, acetic acid and water;
(2) adding ammonia-terminated polydimethylsiloxane, lauryl sodium sulfate, glucosamide and trifluoromethyl maleic anhydride into a reaction vessel, stirring at 60 ℃ for 90min at the rotating speed of 4000rpm, then adding ethylene glycol monobutyl ether, continuing stirring for 60min, adding water, and stirring at the rotating speed of 500rpm for 45 min;
(3) adding acetic acid into the system obtained in the step (2) to adjust the pH value to 5.0-7.0, and uniformly stirring at the rotating speed of 300rpm to obtain the amino silicone oil emulsion;
wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 35% of amino-terminated polydimethylsiloxane, 5% of sodium dodecyl sulfate, 1% of glucose amide, 4% of ethylene glycol monobutyl ether, 0.15% of trifluoromethyl maleic anhydride, 0.3% of acetic acid and the balance of water.
Example 5
A method of making an amino silicone oil emulsion comprising the steps of:
(1) weighing ammonia-terminated polydimethylsiloxane, lauryl sodium sulfate, fatty alcohol-polyoxyethylene ether, ethylene glycol monobutyl ether, trifluoromethyl maleic anhydride, acetic acid and water;
(2) adding ammonia-terminated polydimethylsiloxane, lauryl sodium sulfate, fatty alcohol-polyoxyethylene ether and trifluoromethyl maleic anhydride into a reaction vessel, stirring for 90min at 60 ℃ at the rotating speed of 4000rpm, then adding ethylene glycol monobutyl ether, continuing stirring for 60min, adding water, and stirring for 45min at the rotating speed of 500 rpm;
(3) adding acetic acid into the system obtained in the step (2) to adjust the pH value to 5.0-7.0, and uniformly stirring at the rotating speed of 300rpm to obtain the amino silicone oil emulsion;
wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 35% of amino-terminated polydimethylsiloxane, 5% of lauryl sodium sulfate, 1% of fatty alcohol-polyoxyethylene ether, 4% of ethylene glycol monobutyl ether, 0.15% of trifluoromethyl maleic anhydride, 0.3% of acetic acid and the balance of water.
Example 6
A method of making an amino silicone oil emulsion comprising the steps of:
(1) weighing aminoethyl aminopropyl polydimethylsiloxane, alcohol ether glucoside, glucose amide, ethylene glycol monobutyl ether, trifluoromethyl maleic anhydride, acetic acid and water;
(2) adding aminoethyl aminopropyl polydimethylsiloxane, alcohol ether glucoside, glucose amide and trifluoromethyl maleic anhydride into a reaction vessel, stirring for 90min at the rotating speed of 4000rpm at 60 ℃, then adding ethylene glycol monobutyl ether, continuing stirring for 60min, adding water, and stirring for 45min at the rotating speed of 500 rpm;
(3) adding acetic acid into the system obtained in the step (2) to adjust the pH value to 5.0-7.0, and uniformly stirring at the rotating speed of 300rpm to obtain the amino silicone oil emulsion;
wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 30% of aminoethyl aminopropyl polydimethylsiloxane, 9% of alcohol ether glucoside, 1% of glucose amide, 2% of ethylene glycol monobutyl ether, 0.15% of trifluoromethyl maleic anhydride, 0.3% of acetic acid and the balance of water.
Example 7
A method of making an amino silicone oil emulsion comprising the steps of:
(1) weighing ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, sorbitan monopalmitate, ethylene glycol monobutyl ether, trifluoromethyl maleic anhydride, acetic acid and water;
(2) adding ammonia-terminated polydimethylsiloxane, alcohol ether glucoside, sorbitan monopalmitate and trifluoromethyl maleic anhydride into a reaction vessel, stirring at 70 ℃ for 100min at the rotating speed of 1000rpm, then adding ethylene glycol monobutyl ether, continuing stirring for 60min, adding water, and stirring at the rotating speed of 1000rpm for 60 min;
(3) adding acetic acid into the system obtained in the step (2) to adjust the pH value to 5.0-7.0, and uniformly stirring at the rotating speed of 300rpm to obtain the amino silicone oil emulsion;
wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 35% of amino-terminated polydimethylsiloxane, 4% of alcohol ether glucoside, 2% of sorbitan monopalmitate, 4% of ethylene glycol monobutyl ether, 0.15% of trifluoromethyl maleic anhydride, 0.3% of acetic acid and the balance of water.
The stability tests were carried out on the amino silicone oil emulsions prepared in the above examples and comparative examples, as follows: 8ml of the emulsion was placed in a 10ml centrifuge tube and centrifuged at 4000, 6000 and 8000rpm for 30min, and the emulsion was observed for delamination, the results of which are shown in Table 1.
TABLE 1 centrifugal stability
| Group of | 4000rpm | 6000rpm | 8000rpm |
| Example 1 | Uniform and stable | Uniform and stable | Uniform and stable |
| Example 2 | Uniform and stable | Uniform and stable | Uniform and stable |
| Example 3 | Uniform and stable | Uniform and stable | Slightly delaminated |
| Example 4 | Uniform and stable | Uniform and stable | Slightly delaminated |
| Practice ofExample 5 | Uniform and stable | Uniform and stable | Slightly delaminated |
| Example 6 | Uniform and stable | Uniform and stable | Slightly delaminated |
| Example 7 | Uniform and stable | Slightly delaminated | Slightly delaminated |
As can be seen from the results in Table 1, the present invention can obtain a uniform and stable amino silicone oil emulsion by optimizing the type of emulsifier and the emulsification process parameters.
Shampoos were prepared using the amino silicone oil emulsions prepared in the above examples and comparative examples, respectively, and the content of the amino silicone oil emulsion in the shampoo was 5 wt%.
The shampoo is subjected to performance test, and the specific test method comprises the following steps:
(1) 35 volunteers were selected, 7 groups of 5 persons each, and were shampooed using the shampoos prepared with the aminosilicone emulsions of the above examples or comparative examples, and scored according to table 2, and the average values for each group were calculated, the results being shown in table 3.
TABLE 2 sensory evaluation scores for wet and dry combing and wet and dry hair hand
TABLE 3 scoring results
| Group of | Dry and wet combing property | Dry and wet hair feel |
| Example 1 | 5 | 4.8 |
| Example 2 | 5 | 4.8 |
| Example 3 | 4.4 | 4.4 |
| Example 4 | 4 | 4 |
| Example 5 | 4.8 | 4.4 |
| Example 6 | 4.4 | 4 |
| Example 7 | 4 | 4.8 |
From the above results, it is understood that when the amino silicone oil emulsion of the present invention is used for preparing shampoo products, the amino silicone oil emulsion can be uniformly dispersed in the system, and the softness and the moisturization of hair can be effectively maintained.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method for preparing amino silicone oil emulsion, which is characterized by comprising the following steps:
(1) weighing amino silicone oil, an emulsifier, an auxiliary emulsifier, a stabilizer, a pH regulator and water;
(2) adding amino silicone oil, an emulsifier and a stabilizer into a reaction vessel, stirring for 50-100min at the temperature of 50-70 ℃ at the rotation speed of 1000-plus 5000rpm, then adding an auxiliary emulsifier, continuously stirring for 30-60min, adding water, and stirring for 30-60min at the rotation speed of 500-plus 1000 rpm;
(3) adding a pH regulator into the system obtained in the step (2) to regulate the pH to 5.0-7.0, and uniformly stirring at the rotating speed of 300-500rpm to obtain the amino silicone oil emulsion; wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 20-35% of amino silicone oil, 1-10% of emulsifier, 2-6% of co-emulsifier, 0.1-1% of stabilizer, 0.1-0.5% of pH regulator and the balance of water.
2. The method of claim 1, wherein the amino silicone oil comprises at least one of amodimethicone, bis-aminopropyldimethicone, and aminoethylaminopropyldimethicone.
3. The method for preparing amino silicone oil emulsion according to claim 1, characterized in that the emulsifier is at least one of anionic emulsifier, cationic emulsifier, and nonionic emulsifier.
4. The method of claim 1, wherein the co-emulsifier is at least one of ethylene glycol monobutyl ether and diethylene glycol monobutyl ether.
5. The method of claim 1, wherein the stabilizer is at least one of cetearyl alcohol, trifluoromethyl maleic anhydride, fatty alcohol polyoxyethylene ether carboxylate.
6. The method of claim 1, wherein the pH adjusting agent is acetic acid.
7. The method for preparing amino silicone oil emulsion as defined in claim 1, wherein in step (2), amino silicone oil, emulsifier and stabilizer are added into a reaction vessel, stirred at 2000-4000rpm at 50-60 ℃ for 60-90min, then co-emulsifier is added and stirring is continued for 40-60min, water is added and stirring is continued for 40-50min at 500-600 rpm.
8. The method for preparing amino silicone oil emulsion according to claim 1, wherein the amino silicone oil emulsion comprises the following components in percentage by weight: 20-35% of amino silicone oil, 3-8% of emulsifier, 2-4% of co-emulsifier, 0.1-1% of stabilizer, 0.1-0.5% of pH regulator and the balance of water.
9. An aminosilicone emulsion prepared according to any of claims 1 to 8.
10. Use of an aminosilicone emulsion according to claim 9 for the preparation of a hair conditioner and/or shampoo.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02284959A (en) * | 1989-04-27 | 1990-11-22 | Shin Etsu Chem Co Ltd | Production of emulsion of aminosilicone fine particle |
| CN101130634A (en) * | 2007-08-08 | 2008-02-27 | 浙江大学 | Amino silicone oil microemulsion with high solid content and preparation method thereof |
| CN101497744A (en) * | 2008-07-29 | 2009-08-05 | 浙江传化股份有限公司 | Amino silicon oil emulsion and preparation thereof |
| CN110615898A (en) * | 2019-11-07 | 2019-12-27 | 常州市宁河新材料科技有限公司 | Preparation method of high-temperature-resistant alkali-type amino silicone oil emulsion |
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| CN101130634A (en) * | 2007-08-08 | 2008-02-27 | 浙江大学 | Amino silicone oil microemulsion with high solid content and preparation method thereof |
| CN101497744A (en) * | 2008-07-29 | 2009-08-05 | 浙江传化股份有限公司 | Amino silicon oil emulsion and preparation thereof |
| CN110615898A (en) * | 2019-11-07 | 2019-12-27 | 常州市宁河新材料科技有限公司 | Preparation method of high-temperature-resistant alkali-type amino silicone oil emulsion |
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