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Preparation technology of hydrophilic MQ silicone resin

A technology of MQ silicone resin and preparation process, applied in the field of organic synthesis, can solve the problems of wide molar mass distribution, easy generation of gel, difficult control of structure and M/Q value, etc., and achieves the effect of high refractive index and broadening the application field.

Inactive Publication Date: 2019-05-03
湖北新四海化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis of MQ silicone resin mainly adopts water glass method and silicate method at present; It is wide and easy to produce gel; compared with the sodium silicate method, the hydrolysis reaction activity of the silicate method is lower and the reaction is milder, so it is beneficial to the control of the reaction and the yield is higher. It is the current MQ silicone resin The main method of synthesis
However, the current literature reports and large-scale production are basically hydrophobic MQ silicone resins, and the literature on water-based or hydrophilic MQ silicone resins is still rare.

Method used

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  • Preparation technology of hydrophilic MQ silicone resin
  • Preparation technology of hydrophilic MQ silicone resin
  • Preparation technology of hydrophilic MQ silicone resin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] S1: To prepare modified alkoxysilane, add 0.55mol of unsaturated polyether and chloroplatinic acid catalyst into a flask, mix well, and heat up to 90°C for reaction. Slowly add 0.5 mol of trimethoxysilane into the flask dropwise, then keep the temperature for 2 hours, and remove the low boilers under reduced pressure to obtain modified alkoxysilane, that is, polyether modified trimethoxysilane.

[0029] In this embodiment, the unsaturated polyether structural formula is C 3 h 5 O-(C 2 h 4O ) m -(C 3 h 6 O) n -CH 3 , where m=0, n=2. The preparation method of the chloroplatinic acid catalyst is as follows: 1 weight part of chloroplatinic acid is dissolved in 10 weight parts of isopropanol to obtain the chloroplatinic acid catalyst. The dosage of chloroplatinic acid catalyst in this embodiment is 5 ppm of the total molar amount of trimethoxysilane and unsaturated polyether.

[0030] S2: Add the modified alkoxysilane obtained in step S1, 200 mL of isopropanol, 2.0...

Embodiment 2

[0033] S1: To prepare modified alkoxysilane, add 4 mol of unsaturated polyether and chloroplatinic acid catalyst into a flask, mix well, and heat up to 100°C for reaction. Slowly add 1 mol of trimethoxysilane into the flask dropwise, then keep the temperature for 1 hour, and remove the low boilers under reduced pressure to obtain modified alkoxysilane, that is, polyether modified trimethoxysilane.

[0034] In this embodiment, the unsaturated polyether structural formula is C 3 h 5 O-(C 2 h 4O ) m -(C 3 h 6 O) n -CH 3 , where m=8, n=5. The preparation method of the chloroplatinic acid catalyst is as follows: 1 weight part of chloroplatinic acid is dissolved in 30 weight parts of ethanol to obtain the chloroplatinic acid catalyst. The dosage of chloroplatinic acid catalyst in this embodiment is 20 ppm of the total molar amount of trimethoxysilane and unsaturated polyether.

[0035] S2: Add the modified alkoxysilane obtained in step S1, 200 mL of ethanol, 4 mol of tetra...

Embodiment 3

[0038] S1: To prepare modified alkoxysilane, add 2 mol of unsaturated polyether and chloroplatinic acid catalyst into a flask, mix well, and heat up to 60°C for reaction. Then slowly drop 2 mol of trimethoxysilane into the flask, and then keep the temperature for 3 hours, and remove the low boilers under reduced pressure to obtain modified alkoxysilane, that is, polyether modified trimethoxysilane.

[0039] In this embodiment, the unsaturated polyether structural formula is C 3 h 5 O-(C 2 h 4O ) m -(C 3 h 6 O) n -CH 3, where m=20, n=0. The preparation method of the chloroplatinic acid catalyst is as follows: 1 weight part of chloroplatinic acid is dissolved in 50 weight parts of tetramethyltetravinyl cyclotetrasiloxane to obtain the chloroplatinic acid catalyst. The dosage of the chloroplatinic acid catalyst in this embodiment is 50 ppm of the total molar amount of trimethoxysilane and unsaturated polyether.

[0040] S2: Add 400 mL of the modified alkoxysilane obtain...

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Abstract

The invention relates to the technical field of organic synthesis, and especially relates to a preparation technology of hydrophilic MQ silicone resin. The hydrophilic MQ silicone resin can be well applied to the fields of surfactants, defoaming, water-based coatings and the like. Raw materials of the hydrophilic MQ silicone resin mainly include 4-24 parts of tetraethoxysilane, 1-4 parts of unsaturated polyether or methyl acrylate, 1-7 parts of hexamethyldisiloxane, 1-4 parts of trimethoxysilane and 1-2 parts of an acid catalyst, and further comprise a chloroplatinic acid catalyst and dicyclohexyl phthalate, and the use amount of the chloroplatinic acid catalyst is 5-50 ppm of the sum of the use amounts of the trimethoxysilane and the unsaturated polyether or the sum of the use amounts ofthe trimethoxysilane and the methyl acrylate; and a molar ratio of dicyclohexyl phthalate to tetraethoxysilane is 0.1:1.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation process of hydrophilic MQ silicone resin. Background technique [0002] MQ silicone resin is an organopolysiloxane product with a special structure composed of tetrafunctional siloxane polycondensation chains (i.e. Q groups) and monofunctional siloxane chains (i.e. M groups). Excellent heat resistance, low temperature resistance, film-forming properties, flexibility, water resistance and adhesive properties, mainly used as fillers for silicone pressure-sensitive adhesives, tackifiers and reinforcing fillers for addition-type liquid silicone rubber, and Used in tackifiers, surface treatment agents, release agents, defoamers, anti-sticking agents, brighteners and other additives. The synthesis of MQ silicone resin mainly adopts water glass method and silicate method at present; It is wide and easy to produce gel; compared with the sodium silicate method, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46
Inventor 邵玲龚家全杨帆杨开柱
Owner 湖北新四海化工股份有限公司
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