Preparation method for branched silane and polyether alkyl co-modified silicone oil

A technology of polyether alkyl and branched chain, which is applied in the preparation of polyether alkyl co-modified silicone oil and the field of branched chain silane, which can solve problems such as skin hazards, pungent odor, and difficulty in achieving long-term stability, and achieve Good compatibility, increase washability, solve oil phase compatibility and stability problems

Active Publication Date: 2019-05-24
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the traditional synthesis method has the following problems: 1) toxic solvents such as toluene are used as solvents, and residues in products used in cosmetics will cause harm to the skin; 2) there are generally disadvantages such as backward synthesis technology, low product quality, and pungent odor. 3) As an emulsifier, it is difficult to achieve a long-term stable state for the mixed oil phase with a high silicone oil content

Method used

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  • Preparation method for branched silane and polyether alkyl co-modified silicone oil
  • Preparation method for branched silane and polyether alkyl co-modified silicone oil
  • Preparation method for branched silane and polyether alkyl co-modified silicone oil

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) prepare platinum catalyst: get 1g dry chloroplatinic acid (H 2 PtCl 6 ) was dissolved in 200 g of distilled isopropanol and sonicated, so that chloroplatinic acid was completely dissolved in isopropanol, and allowed to stand overnight to obtain a transparent orange-yellow liquid, which was kept in a brown bottle away from light for use. The effective platinum content of the prepared catalyst is: Pt 0.1875%.

[0032] (2) Add 15g of hydrogen-containing silicone oil (50cst, hydrogen content 1.8mmol / g) and 10ml of isopropanol into a three-necked flask, heat and reflux to 50°C in a constant temperature magnetic stirring water bath, then add 0.315ml of platinum catalyst .

[0033] (3) Slowly add 3.92 g of allyl polyether dropwise with a constant pressure funnel, heat to 85° C., and finish adding dropwise within 20 minutes.

[0034] (4) After reacting for 2 hours, start to drop a mixture of 1.66g dodecene and 3.12g vinyl tris(trimethylsiloxane) silane (allyl polyether, ...

example 1

[0042] Chemical titration method is measured Si-H bond content in the example 1, and conversion ratio calculation formula:

[0043]

[0044] Using the chemical titration method to measure the hydrogen content before and after the reaction, it is calculated that the conversion rate of the modified silicone oil product is as high as 94.32%, and the purity reaches 96.42%. The invention limits the operation process in the preparation process and improves the conversion rate of the co-modified silicone oil. During the preparation process, selecting sodium hydroxide solution and washing with water can remove unreacted silicon-hydrogen bonds and residual platinum catalyst, selecting hydrochloric acid solution and washing with water can remove odor impurities such as by-product aldehydes, so that the obtained product has a high purity.

[0045] figure 1 It is the total reflection Fourier transform infrared spectrogram of the obtained branched-chain silane and polyether alkyl co-m...

Embodiment 2

[0051] (1) prepare platinum catalyst: get 1g dry chloroplatinic acid (H 2 PtCl 6 ) was dissolved in 200 g of distilled isopropanol and sonicated, so that chloroplatinic acid was completely dissolved in isopropanol, and allowed to stand overnight to obtain a transparent orange-yellow liquid, which was kept in a brown bottle away from light for use. The effective platinum content of the catalyst is: Pt 0.1875%

[0052] (2) Add 15g of hydrogen-containing silicone oil (50cst, hydrogen content 3.8mmol / g) and 10ml of isopropanol into a three-necked flask, heat it in a constant temperature magnetic stirring water bath to reflux to 50°C, and then add 0.219ml of platinum catalyst .

[0053] (3) Slowly add 8.4 g of allyl polyether dropwise with a constant pressure funnel, heat to 85° C., and finish adding dropwise within 20 minutes.

[0054] (4) After reacting for 2 hours, start to drop a mixture of 3.53g dodecene and 6.73g vinyl tri(trimethylsiloxane) silane (allyl polyether, dodece...

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Abstract

The invention discloses a preparation method for branched silane and polyether alkyl co-modified silicone oil. According to the preparation method, a silicone oil emulsifier is prepared through three-radical co-modification, and the product obtained by using the method has no pungent smell and has no visible gel impurities, the emulsion prepared by using the method cannot become yellow after long-time storage, and the silicone oil is high in stability, high in compatibility with various types of oil and suitable for W/Si, W/O and W/Si+O emulsifying systems. The product prepared by using the method has a highly-branched silicon chain structure, can be used in make-up products and sunscreen and has the functions of improving washability and durability.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a preparation method of branched chain silane and polyether alkyl co-modified silicone oil. Background technique [0002] Silicone oil is a high and low temperature resistant, radiation resistant, physiologically inert polymer compound. It is neither soluble in water nor compatible with oil. By introducing functional groups through the hydrosilylation process under the platinum catalyst, various silicone oils with different properties can be prepared, which are widely used in cosmetics and personal care, textiles, petroleum and other fields. [0003] However, the traditional synthesis method has the following problems: 1) toxic solvents such as toluene are used as the solvent, and the residue in the product is used in cosmetics to cause harm to the skin; 2) there are generally disadvantages such as backward synthesis technology, low product quality...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38
Inventor 杨成何彤
Owner JIANGNAN UNIV
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