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Method for preparing polyoxyethylene fatty alcohol ether-siloxane copolymer

A technology of alcohol polyoxyethyl ether and polysiloxane is applied in the field of non-ionic silicone emulsifier to achieve the effects of simple method, good compatibility and emollient effect

Active Publication Date: 2013-06-19
JIANGSU FEIXIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above prior art is mainly based on linking polyoxyethyl / polyoxypropyl ether, long-chain alkyl groups and other groups to the middle of the silicone segment to form a comb-shaped emulsifier or connecting to the end group of the silicone segment to form an emulsifier. Block-type structure emulsifiers can be adjusted by adjusting the ratio of hydrophilic and lipophilic groups in the molecule to obtain the required interfacial properties of the emulsifier. It can have a good emulsifying effect for the preparation of low-viscosity creams, but when high Viscosity cream emulsions have certain limitations

Method used

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  • Method for preparing polyoxyethylene fatty alcohol ether-siloxane copolymer
  • Method for preparing polyoxyethylene fatty alcohol ether-siloxane copolymer
  • Method for preparing polyoxyethylene fatty alcohol ether-siloxane copolymer

Examples

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example 1

[0046] Preparation of cetyl polyoxyethyl ether polysiloxane:

[0047] 1) under nitrogen protection, 34g hexadecyl decapolyoxyethyl alcohol C 16 h 33 O(CH 2 CH 2 O) 10 Add OH to a 250mL four-neck flask with a stirring reflux water separator, add 2.4g NaOH, and react at 130°C with 100mL toluene as a solvent. Hexadecyl polyoxyethylene sodium salt, then add propylene chloride dropwise and react at 50°C for 12 hours. The product is centrifuged to separate sodium chloride and unreacted sodium hydroxide, and the solvent and low boiling matter are removed under reduced pressure to obtain terminal allyl Hexadecyl polyoxyethyl ether intermediate. Its terminal double bond content is 95.2%.

[0048] figure 1 Is the terminal allyl hexadecyl polyoxyethyl ether intermediate nuclear magnetic spectrum, in the figure 1 H NMR (400MHz, CDCl 3 )(δppm): 0.84(t, 3H, CH 3 CH 2 -); 1.22(m, 26H, CH(CH 2 ) 13 -); 1.53(m, 2H, -(CH 2 ) 13 CH 2 CH 2 O-); 3.41(t, 2H, -(CH 2 ) 13 CH 2 CH ...

Embodiment 2

[0054] The preparation process of the fatty alcohol polyoxyethyl ether polysiloxane in this example is the same as in Example 1, and without changing other conditions in Example 1, only 40 g of low hydrogen-containing silicone oil (0.1% hydrogen content) is changed to low Hydrogen silicone oil (0.18% hydrogen content) 22.22g.

Embodiment 3

[0056] 1) Under nitrogen protection, 24.5g hexadecyl (polyoxyethyl) 6 Alcohol C 16 h 33 O(CH 2 CH 2 O) 6 Add OH to a 250mL four-neck flask with a stirring reflux water separator, add 2.4g NaOH, and react at 130°C with 100mL toluene as a solvent. Hexadecyl polyoxyethylene sodium salt, then add propylene chloride dropwise and react at 50°C for 12 hours. The product is centrifuged to separate sodium chloride and unreacted sodium hydroxide, and the solvent and low boiling matter are removed under reduced pressure to obtain terminal allyl Hexadecyl polyoxyethyl ether intermediate.

[0057] 2) Under the protection of nitrogen, add 21.2 g of the allyl cetyl polyoxyethyl ether intermediate obtained in step 1) and 40 g of low hydrogen-containing silicone oil (0.1% hydrogen content) into the four-port Add 20 mL of toluene to the flask, heat up to 90° C., and add 80 mg of 0.3% chloroplatinic acid in isopropanol. The reaction was initially exothermic, and the reaction was carried o...

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Abstract

The invention discloses a polyoxyethylene fatty alcohol ether-siloxane copolymer and its preparation method and use. The polyoxyethylene fatty alcohol ether-siloxane copolymer has a general structural formula shown in the patent specification. The preparation method comprises the following steps that 1, polyoxyethylene fatty alcohol ether and one or more alkali compounds are heated in toluene andundergo a reaction to produce an alkali metal salt of polyoxyethylene fatty alcohol ether; and the alkali metal salt of polyoxyethylene fatty alcohol ether and chloropropene undergo a reaction to produce allyl-terminated polyoxyethylene fatty alcohol ether; and 2, the allyl-terminated polyoxyethylene fatty alcohol ether and low-hydrogen content silicone oil undergo a reaction in the presence of one or more platinum catalysts to produce polyoxyethylene fatty alcohol ether-siloxane copolymer oil. The polyoxyethylene fatty alcohol ether-siloxane copolymer can be used as an emulsifier and is added into W / O cream and through the polyoxyethylene fatty alcohol ether-siloxane copolymer, an oil phase containing silicone oil or a complex of silicone oil and other oil can be effectively emulsified so that cream which has excellent stability under the conditions of a high temperature, freezing / unfreezing circulation, a long storage period and insolation is obtained and a W / O cream emulsion which has high viscosity and high stability is obtained. The cream and the W / O cream emulsion have good compatibility with the skin.

Description

technical field [0001] The invention relates to a nonionic silicone emulsifier, in particular to a fatty alcohol polyoxyethyl ether grafted polysiloxane water-in-oil emulsifier and a preparation method of the silicone emulsifier and its water-in-oil emulsifier. Application in cream. Background technique [0002] In order to prepare a stable water-in-oil emulsion, the emulsifier can usually be dissolved or dispersed in the oil phase and the HLB (Hydrophile-Lipophile Balance Number, hydrophilic-hydrophobic balance value) value is lower than 8. Traditional water-in-oil emulsifiers such as glycerin, polyglycerin, oleate or stearate of sorbitol or wool wax alcohol, such emulsifiers are usually used in large amounts in the preparation of stable water-in-oil (W / O) emulsions , accounting for 10-20Wt.% of the mass of the oil phase. And in the oil phase containing silicone oil and the composite oil phase of organic raw materials such as silicone oil and animal and vegetable oil, min...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00A61K8/894A61K8/92A61K8/02A61Q19/00
Inventor 侯腾腾庄东青
Owner JIANGSU FEIXIANG CHEM
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