阅读说明：本技术 替代硅油的发用产品的制备方法 (Method for preparing hair product for replacing silicone oil ) 是由 曹玉华 秦志昂 于 2020-12-18 设计创作，主要内容包括：本发明涉及一种替代硅油的发用产品的制备方法。本发明通过使用双亲性无规聚合物与(C-(16)-C-(22))烷基三甲基季铵盐复配,制备得到替代硅油的发用产品。本发明使用的双亲性无规聚合物合成方法简单,过程易控制,安全无污染；双亲聚合物溶液采用直接溶解法,制备快速,成本低；复配体系具有刺激性低、稳定性好、梳理性强等特点；双亲聚合物通过静电作用在头发上吸附,解决了硅油在头发上的沉积问题,且梳理效果和含硅洗护用品相当。(The invention relates to a preparation method of a hair product for replacing silicone oil. The invention is achieved by using amphiphilic random polymers with (C) 16 ‑C 22 ) And compounding alkyl trimethyl quaternary ammonium salt to prepare the hair product for replacing silicone oil. The method for synthesizing the amphiphilic random polymer is simple, the process is easy to control, and the method is safe and pollution-free; the amphiphilic polymer solution is prepared quickly by a direct dissolution method, and the cost is low; the compound system has low irritation, good stability and strong carding propertyAnd the like; the amphiphilic polymer is adsorbed on the hair through electrostatic action, so that the problem of deposition of silicone oil on the hair is solved, and the combing effect is equivalent to that of silicon-containing washing and protecting products.)

1. A preparation method of a hair product for replacing silicone oil is characterized by comprising the following steps:

s1, mixing the hydrophobic monomer and the hydrophilic monomer according to a molar ratio of 4: 6-7: 3, and polymerizing by a solution free radical polymerization method under the action of an initiator to obtain an amphiphilic random polymer;

s2, dissolving the amphiphilic random polymer to prepare an amphiphilic random polymer solution;

s3, mixing (C)₁₆-C₂₂) And mixing the alkyl trimethyl quaternary ammonium salt solution and the amphiphilic random polymer solution at 70-80 ℃, and uniformly stirring to obtain the hair product replacing the silicone oil.

2. The method of claim 1, wherein the hydrophobic monomer is styrene.

3. The method according to claim 1, wherein the hydrophilic monomer is one or both of acrylic acid and methacrylic acid.

4. The method of claim 1, wherein the initiator is one or both of azobisisobutyronitrile and dimethyl azobisisobutyrate.

5. The method according to claim 1, wherein the solution radical polymerization is carried out in an organic solvent at 60-70 ℃ for 20-30 h.

6. The method according to claim 5, wherein the organic solvent is isopropyl alcohol.

7. The method according to claim 1, wherein in the step S2, the amphiphilic random polymer is dissolved in an alkaline solution, and the pH is adjusted to 8.5 to 9.5 after the dissolution is completed.

8. The method according to claim 1, wherein in the step S2, the concentration of the amphiphilic random polymer in the amphiphilic random polymer solution is 0.1 to 0.3 g/mL.

9. The method according to claim 1, wherein in the step of S3, (C)₁₆-C₂₂) The mass concentration of the alkyl trimethyl quaternary ammonium salt solution is 0.25-2.5%.

10. The method according to claim 1, wherein in the step of S3, (C)₁₆-C₂₂) When the alkyltrimethyl quaternary ammonium salt solution is mixed with the amphiphilic random polymer solution, the solution is mixed according to (C)₁₆-C₂₂) The molar ratio of the alkyl trimethyl quaternary ammonium salt to the amphiphilic random polymer is 0.8-1.8: 1.

Technical Field

The invention relates to the technical field of daily chemical industry, in particular to a preparation method of a hair product for replacing silicone oil.

Background

Shampoo and hair care products are necessary washing and caring products in daily life. The shampoo mainly plays a cleaning role and has excellent foamability; the hair care product can repair hair, improve combing property, resist static, repair damaged hair and the like. Along with the improvement of living standard of people, the requirements on safety and environmental protection are increased, and silicon-free washing products are increasingly favored by people. Most of the currently marketed washing products contain silicone oil, and the silicone oil products can be excessively accumulated on the scalp after long-term use, block pores, and hinder hair growth, so that the hair is unnatural, greasy, heavy, collapsed, frizzy and the like.

Silicon-free cleaning products have become a popular trend abroad, while the research on silicon-free cleaning products is started later in China. At present, researchers mostly search substitutes of silicone oil from natural products, soapnut saponin, tea saponin and the like are applied, but the natural products are complex in extraction process, long in time consumption, high in cost and the like, so that the silicon-free washing and nursing product is high in price. Therefore, it is necessary to develop a silicone oil substitute which is easy and fast to prepare, low in cost and good in combing property.

Disclosure of Invention

In order to solve the technical problems, the invention aims to provide a preparation method of a hair product for replacing silicone oil. Use of amphiphilic random polymers with (C)₁₆-C₂₂) And compounding alkyl trimethyl quaternary ammonium salt to prepare the hair product for replacing silicone oil.

The first purpose of the invention is to provide a preparation method of a hair product for replacing silicone oil, which comprises the following steps:

s1, mixing the hydrophobic monomer and the hydrophilic monomer according to a molar ratio of 4: 6-7: 3, and polymerizing by a solution free radical polymerization method under the action of an initiator to obtain an amphiphilic random polymer;

s2, dissolving the amphiphilic random polymer to prepare an amphiphilic random polymer solution;

s3, mixing (C)₁₆-C₂₂) And mixing the alkyl trimethyl quaternary ammonium salt solution and the amphiphilic random polymer solution at 70-80 ℃, and uniformly stirring to obtain the hair product replacing the silicone oil.

Further, the hydrophobic monomer is styrene.

Further, the hydrophilic monomer is one or two of acrylic acid and methacrylic acid.

Further, the initiator is one or two of azobisisobutyronitrile and dimethyl azobisisobutyrate.

Further, the solution free radical polymerization method is to react for 20-30 hours at 60-70 ℃ in an organic solvent.

Further, the organic solvent is isopropanol.

Further, in the step S2, dissolving the amphiphilic random polymer by using an alkaline solution, and adjusting the pH value to 8.5-9.5 after complete dissolution.

Further, in the step S2, the concentration of the amphiphilic random polymer in the amphiphilic random polymer solution is 0.1-0.3 g/mL.

Further, in step S3, (C)₁₆-C₂₂) The mass concentration of the alkyl trimethyl quaternary ammonium salt solution is 0.25-2.5%.

Further, in step S3, (C)₁₆-C₂₂) When the alkyltrimethyl quaternary ammonium salt solution is mixed with the amphiphilic random polymer solution, the solution is mixed according to (C)₁₆-C₂₂) The molar ratio of the alkyl trimethyl quaternary ammonium salt to the amphiphilic random polymer is 0.8-1.8: 1.

By the scheme, the invention at least has the following advantages:

the method for synthesizing the amphiphilic random polymer is simple, the process is easy to control, and the method is safe and pollution-free; the amphiphilic polymer solution is prepared quickly by a direct dissolution method, and the cost is low; the compound system has the characteristics of low irritation, good stability, strong carding property and the like; the amphiphilic polymer is adsorbed on the hair through electrostatic action, so that the problem of deposition of silicone oil on the hair is solved, and the combing effect is equivalent to that of silicon-containing washing and protecting products.

The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following description is made with reference to the preferred embodiments of the present invention and the accompanying detailed drawings.

Drawings

FIG. 1 shows a compounded system product obtained in example 1;

FIG. 2 is a comparison of the wet combing performance of the hair care products from example 1 compared to the wet combing performance of virgin, commercially available silicone-free conditioners, and commercially available silicone-containing conditioners;

fig. 3 is a comparison of the dry combing performance of the hair care products from example 1 compared to the dry combing performance of virgin, commercially available silicone-free conditioners, and commercially available silicone-containing conditioners.

Detailed Description

The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.

Preparation of amphiphilic random polymer solution:

(1) mixing hydrophobic styrene monomer and hydrophilic acrylic acid monomer in isopropanol at a ratio of 7:3, adding AIBN as initiator, removing air, sealing, reacting at 65 deg.C for 24 hr, polymerizing by solution free radical polymerization to obtain amphiphilic random polymer, recrystallizing the product, precipitating with petroleum ether, vacuum drying to obtain amphiphilic random polymer, and vacuum drying¹The ratio of the peak area of the hydrogen atom on the phenyl ring group to the peak area of the hydrogen atom on the carboxylic acid group in H NMR confirmed that the monomer ratio of the product substantially matched the charge ratio.

(2) Dissolution of amphiphilic random polymer: dissolving the amphiphilic random polymer obtained in the step (1) in a NaOH solution with the proper concentration, wherein the molar ratio of the acrylic acid monomer to the NaOH is controlled to be 1:1, adjusting the pH value to 9 by using 0.01mol/L HCl solution after complete dissolution, and filtering by using a 0.45 mu m water system filter membrane to prepare 0.2g/mL of amphiphilic random polymer solution for later use.

Example 1:

(1) 0.7g of behenyltrimethylammonium chloride with the content of 85 percent is weighed and added into 19.3g of deionized water, and the solution A is obtained after the solution is heated to 80 ℃ for dissolution.

(2) 10g of 0.2g/mL amphiphilic polymer solution was weighed and heated to 80 ℃ to obtain solution B.

(3) And mixing the solution A and the solution B to obtain a compound system (the molar ratio of the styrene to the behenyl trimethyl ammonium chloride is 1:1), as shown in figure 1.

Example 2:

(1) 0.88g of behenyltrimethylammonium chloride with the content of 85 percent is weighed and added into 16.6g of deionized water, and the solution A is obtained after the solution is heated to 80 ℃ for dissolution.

(2) 12.6g of 0.2g/mL amphiphilic polymer solution was weighed and heated to 80 ℃ to obtain solution B.

(3) And mixing the solution A and the solution B to obtain a compound system (the molar ratio of the styrene to the behenyl trimethyl ammonium chloride is 1: 1).

Example 3:

(1) 0.7g of behenyltrimethylammonium chloride with the content of 85 percent is weighed and added into 17.3g of deionized water, and the solution A is obtained after the solution is heated to 80 ℃ for dissolution.

(2) 12g of 0.2g/mL amphiphilic polymer solution was weighed and heated to 80 ℃ to obtain solution B.

(3) And mixing the solution A and the solution B to obtain a compound system (the molar ratio of the styrene to the behenyl trimethyl ammonium chloride is 1.2: 1).

The embodiment of the invention has the following effects:

(1) the above example 1 was selected to compare dry and wet combing performance with the original hair, as shown in figures 2 and 3. As can be seen from the figure, the dry combing performance and the wet combing performance of the example 1 are both better than those of the original hair, and the silicone oil is an effective substitute.

(2) The dry and wet combing performance of example 1 was compared to commercially available silicone-free conditioners and silicone-containing conditioners as shown in FIGS. 2 and 3. As can be seen from the figure, the wet combing performance of the example 1 is better than that of the commercial silicon-containing and silicon-free hair conditioner, the dry combing performance is better than that of the commercial silicon-free hair conditioner, and the combing performance is good.

The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.