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Preparation method of alkynyl bond-containing polyether modified organic silicon

An acetylenic bond polyether and organosilicon technology is applied in the field of preparation of acetylene bond-containing polyether modified organosilicon, which can solve the problems of many reaction by-products, low conversion rate, long reaction time, etc. The effect of shortening the reaction rate and reaction time

Active Publication Date: 2021-01-29
杭州崇耀科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process has the following disadvantages: long reaction time, low conversion rate, many reaction by-products under high temperature for a long time, etc.

Method used

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  • Preparation method of alkynyl bond-containing polyether modified organic silicon
  • Preparation method of alkynyl bond-containing polyether modified organic silicon
  • Preparation method of alkynyl bond-containing polyether modified organic silicon

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preparation example Construction

[0022] The invention provides a method for preparing polyether-modified organosilicon containing acetylenic bonds, comprising: S) carrying out pressurized heating reaction of hydrogen-containing polysiloxane, acetylenic polyether and transition metal catalyst in a closed container to obtain Alkyne bond-containing polyether modified silicone.

[0023] The invention improves the reaction rate through the pressurized reaction, thereby shortening the reaction time, and can effectively suppress the occurrence of side reactions and improve the conversion rate at the same time.

[0024] The present invention has no special limitation on the sources of all raw materials, which can be commercially available.

[0025] Wherein, the molecular weight of the hydrogen-containing polysiloxane is preferably 1000-5000, more preferably 1000-4000, more preferably 1000-3000, most preferably 2000; the hydrogen content in the hydrogen-containing polysiloxane is preferably 0.1%~0.5%; the hydrogen-co...

Embodiment 1

[0042] Add 100 parts of low hydrogen-containing polysiloxane A, 60 parts of acetylenic polyether B, and 20PPM chloroplatinic acid catalyst into the autoclave, and seal the autoclave.

[0043] Slowly fill high-purity nitrogen into the autoclave to pressurize to 0.3 MPa in the autoclave; slowly heat up to 140 °C at a heating rate of 4 °C / min, react for 2 hours, observe and record the temperature change; after the reaction, measure Hydrogen content, viscosity, etc., and the surface tension of its 0.1% aqueous solution was measured with a surface tensiometer, and the results are shown in Table 1.

Embodiment 2

[0045] Add 100 parts of low hydrogen-containing siloxane A, 32 parts of alkyne polyether B, and 20PPM chloroplatinic acid catalyst into the autoclave, and seal the autoclave.

[0046] Slowly fill high-purity nitrogen into the autoclave to pressurize to 0.3 MPa in the autoclave; then slowly heat up to 140 °C at a heating rate of 4 °C / min, react for 2 hours, observe and record the temperature change; after the reaction, Measure the hydrogen content, viscosity, etc., and measure the surface tension of its 0.1% aqueous solution with a surface tensiometer, and the results are shown in Table 1.

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Abstract

The invention provides a preparation method of alkynyl bond-containing polyether modified organic silicon. The method comprises the following step of: S) carrying out pressurization and heating reaction on hydrogen-containing polysiloxane, alkynyl bond polyether and a transition metal catalyst in a closed container to obtain the alkynyl bond-containing polyether modified organic silicon. Comparedwith the prior art, the method has the following advantages that: the reaction rate is increased through pressurization reaction, so that the reaction time is shortened, side reaction can be effectively inhibited, and the conversion rate is increased.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of polyether-modified organosilicon containing acetylenic bonds. Background technique [0002] The main chain of the silicone surfactant is a soft Si-O chain, and the branch chain is methyl, which is neither hydrophilic nor lipophilic. It can reduce the surface tension to about 20mN / m, and has excellent wetting performance. It is widely used in many fields such as coatings, leather, textiles, cosmetics and pesticides. [0003] Generally, polyoxyalkylene surfactants modified with polyether containing alkyne bonds are prepared by addition of polyether containing alkyne bonds and polysiloxane containing hydrogen through hydrosilylation. For example, the Chinese patent whose publication number is CN103191673A discloses a polyoxyalkylene surfactant modified with an acetylenic bond polyether and a synthesis method thereof: a transition metal cat...

Claims

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Application Information

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IPC IPC(8): C08G77/46
CPCC08G77/46
Inventor 汪瑜华黄涛杨雪忠张霄黄卓胡庆宋新锋邵斌林俊智
Owner 杭州崇耀科技发展有限公司
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