Method for preparing side-chain modified polysiloxane

A polysiloxane, modification technology, applied in the field of synthesis of silicone polymers, can solve the problems of complex preparation process, long cycle, difficult operation, etc., and achieve the effect of simple operation steps, low cost and low condition requirements

Active Publication Date: 2017-11-21
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the deficiencies of the prior art, especially in the prior art, the synthesis process of modified polysiloxane requires the protection of modifiers, which leads to defects such as complicated preparation process, long period, and difficult operation. The present invention provides a method for preparing side chain modified The polysiloxane method

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  • Method for preparing side-chain modified polysiloxane
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  • Method for preparing side-chain modified polysiloxane

Examples

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Embodiment 1

[0046] A method for preparing side chain modified polysiloxane, comprising steps as follows:

[0047] (1) Under the protection of argon, add dry petroleum ether 120mL, methyl dichlorosilane (55.22g, 0.48mol) in the round-bottomed flask equipped with constant pressure dropping funnel, spherical condenser, thermometer and magneton. Add allyl alcohol (50.57g, 0.87mol) dropwise to the system at a rate of 2mL / min at -10°C, react at 35°C for 3h, distill under reduced pressure after the reaction, collect 40-45°C / 14- 15mmHg fraction, the alcoholysis product bisallyloxymethylsilane 47.37g was obtained, and the yield was 68.9%. The infrared spectrogram and proton nuclear magnetic spectrum spectrogram of alcoholysis product bis-allyloxymethylsilane are as follows figure 1 and figure 2 shown.

[0048] (2) Under argon protection, add dry toluene 60mL, chloroplatinic acid catalyst 30ppm and step (1) gained alcoholysis product (22.87g, 0.14mol ), stirred and reacted at 70° C. for 5 h, and...

Embodiment 2

[0051] A method for preparing side chain modified polysiloxane, comprising steps as follows:

[0052] (1) Under argon protection, add dry cyclohexane 60mL and methyldichlorosilane (25.31g, 0.22mol) into a round bottom flask equipped with a constant pressure dropping funnel, a spherical condenser, a thermometer, and a magnet, At -10°C, allyl alcohol (11.61g, 0.20mol) was added dropwise to the system at a rate of 2mL / min, and reacted at 35°C for 3h. ~15mmHg fraction, the alcoholysis product allyloxymethyl monochlorosilane 19.17g was obtained, and the yield was 70.2%.

[0053] (2) under argon protection, add dry toluene 80mL, chloroplatinic acid catalyst 30ppm and the alcoholysis product (19.17g, 0.14mol) of step (1) gained in the round bottom flask of spherical condenser, thermometer, magneton, The reaction was stirred at 60° C. for 4 h. After the reaction was completed, it was naturally cooled to room temperature. After removing the solvent, 18.21 g of the hydrosilylation pro...

Embodiment 3

[0056] A method for preparing side chain modified polysiloxane, comprising steps as follows:

[0057] (1) Under argon protection, add dry toluene 60mL and methyldichlorosilane (25.31g, 0.22mol) into a round-bottomed flask equipped with a constant pressure dropping funnel, a spherical condenser, a thermometer, and a magnet. Allyl alcohol (11.61 g, 0.20 mol) was added dropwise to the system at a rate of 2 mL / min at 10° C., and reacted at 35° C. for 3 h.

[0058] (2) After the alcoholysis is completed, use an oil pump to pump away the residual hydrogen chloride gas in the system, then add 30 ppm of chloroplatinic acid catalyst into the system, react at 80° C. for 6 hours, and naturally cool to room temperature after the reaction is completed. After removal of the solvent, 18.18 g of the hydrosilylation product was obtained with a yield of 95.7%.

[0059] (3) Add toluene 200mL, step (2) gained hydrosilylation product (8.55g, 0.06mol), hydrochloric acid solution 20mL and two Meth...

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Abstract

The invention relates to a method for preparing side-chain modified polysiloxane. The method comprises the following steps: (1) uniformly mixing dichlorohydrosilane with an organic solvent, dropping crylic acid or allyl alcohol or allyl amine into the mixed solution in ice bath, stirring to implement a reaction, after the reaction is completed, and performing vacuum distillation to remove the organic solvent so as to obtain a chlorosilane substituted product; (2) putting the chlorosilane substituted product and a catalyst into a solvent, performing a reaction for 4-20 hours at 30-90 DEG C, performing vacuum distillation to remove the organic solvent so as to obtain a silicon-hydrogen addition product; (3) performing co-hydrolysis on the silicon-hydrogen addition product with alkoxy silane or chlorosilane of bifunctionality, adding a proper amount of an end-capping reagent, and performing catalysis balance reaction, thereby obtaining side-chain modified polysiloxane. The raw methods are cheap and easy to obtain, the product yield is high, operation steps are simple and convenient, tedious steps of protection, deprotection and the like are not needed, and industrialization is easy to achieve.

Description

technical field [0001] The invention relates to a method for preparing functional polysiloxane, in particular to a method for preparing side-chain modified polysiloxane, which belongs to the technical field of organosilicon polymer synthesis. Background technique [0002] Polysiloxane has many unique properties and has been widely used in many industrial sectors of the national economy. But for special purpose of use, there are deficiencies again. In order to improve certain properties and uses of polysiloxane, functional polysiloxane has been researched and developed. Different modifying groups can endow polysiloxane with different functions, thereby broadening its application field. [0003] Modified polysiloxane is generally prepared by hydrosilylation reaction between hydrogen-containing polysiloxane and unsaturated hydrocarbon derivatives. Common modifying groups include hydroxypropyl, aminopropyl, carboxyl, etc., but during the hydrosilylation process, the Si-H bond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/16C08G77/14C08G77/06
CPCC08G77/06C08G77/14C08G77/16
Inventor 冯圣玉霍晓娟王灯旭张洁封玲珑
Owner SHANDONG UNIV
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