Preparation method of novel MQ silicon resin

A resin and a new type of technology, applied in the field of MQ silicone resin preparation, can solve problems such as production waste, separation difficulties, and corrosion equipment, and achieve the effects of reducing production costs, eliminating cumbersome operations, and reducing raw material composition

Active Publication Date: 2014-04-16
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using tetraethyl orthosilicate as raw material to synthesize MQ silicone resin is expensive, which limits the popularization and application of this method; using water glass as raw material to prepare MQ silicone resin, although the cost is relatively low, but due to raw material ratio, condition temperature, hydrolysis time and solvent The restriction of many factors such as the selection of the method makes the performance of MQ silicone resin prepared by this method unstable.
No matter which method is used above, a large amount of acidic catalyst used in the reaction will not only corrode the equipment, but also need to be removed by water washing or neutralization after the reaction is completed, the separation is more difficult, resulting in waste of production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 500g of toluene and 244g of anhydrous sodium silicate powder with a modulus of 3.1 and a particle size of 20-90 mesh into a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel, and start stirring at a speed of 300 RPM, maintain the temperature at 20°C, add 216g of trimethylchlorosilane dropwise from the dropping funnel, raise the temperature to 110°C, and continue the reflux reaction for 1h. Stand still after the reaction, cool down to room temperature, remove solid NaCl by filtration, distill off toluene and low boilers under reduced pressure, and continue vacuuming for 0.5 h to obtain methyl MQ silicone resin in the form of white powder.

[0026] The M / Q molar ratio of the methyl MQ silicone resin obtained in this example is 0.75, and the yield is 94.5%, which is much higher than the 85% yield of the silicic acid method. The Si-OH group mass fraction of the above-mentioned MQ silicone resin is 0.1 after detection. %~1...

Embodiment 2

[0028] Add 550g of toluene, 267g of anhydrous sodium silicate powder with a modulus of 3.5 and a particle size of 20-100 mesh into a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel, and start stirring at a speed of 350 Rotate per minute, maintain the temperature of 25°C, add 324g of trimethylchlorosilane dropwise from the dropping funnel, raise the temperature to 110°C, and continue the reflux reaction for 1.5h. Stand still after the reaction, cool down to room temperature, remove NaCl solid by filtration, evaporate toluene and low boilers under reduced pressure, and continue vacuuming for 0.5 h to obtain white powdery methyl MQ silicone resin.

[0029] The yield of methyl MQ silicone resin obtained in this example is 95%, the M / Q molar ratio is 0.70, and the weight-average molar mass measured by GPC method is 7600 grams per mole, and the resin structure does not contain Si-OH group, which can be directly It is used in occasio...

Embodiment 3

[0031] Add 470g of xylene, 246g of anhydrous sodium silicate powder with a modulus of 3.3 and a particle size of 20-100 mesh in a four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel, and start stirring at a speed of 400 rpm, maintain the temperature of 22°C, drop the mixture of 175g trimethylchlorosilane and 30g dimethylvinylchlorosilane from the dropping funnel, raise the temperature to 100°C, and continue the reaction for 2h. Stand still after the reaction, cool down to room temperature, remove NaCl solid by filtration, distill off xylene and low boilers under reduced pressure, and continue vacuuming for 1 h to obtain transparent block-shaped methyl vinyl MQ silicone resin.

[0032] The yield of the methyl vinyl MQ silicone resin obtained in this example is 95%, the number-average molar mass is 3975 grams per mole after detection and analysis, the vinyl content is 5.3 mol / kg, and the resin structure does not contain Si-OH groups....

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Abstract

The invention relates to a preparation method of novel MQ silicon resin. The method comprises the following steps: (1) adding 400-800 parts by mass of organic solvent to a reaction vessel with a stirrer, and adding 180-280 parts by mass of solid sodium silicate powder under high-speed agitation, so that a turbid liquid system is formed in the reaction vessel; (2) slowly dropwise adding 190-350 parts by mass of R1R2R3SiX halogenosilane at 15-35 DEG C; (3) heating to 80-120 DEG C keeping agitating, and reacting for over 0.5 hour; and (4) stewing, cooling, filtering, and removing a solvent by vacuum distillation, carrying out condensation polymerization to obtain liquid or solid MQ silicon resin. The method has the advantages of low raw material cost, fewer by-products, and simple and feasible preparation technology. No catalyst is used in the preparation process, and complicated post-treatment process is not needed, so that the synthesis time of the MQ silicon resin is greatly shortened, and the method can be widely applied to the field of synthesis of a plurality of MQ silicon resins containing different groups.

Description

technical field [0001] The invention discloses a novel preparation method of MQ silicone resin, and particularly relates to a method for preparing various MQ silicone resins with a low-cost raw material and a simple process. Background technique [0002] As we all know, MQ silicone resin is a kind of special silicone resin composed of monofunctional siloxane chain (M) and tetrafunctional siloxane chain (Q). Due to its special structure, MQ silicone resin has excellent heat resistance, low temperature resistance, film-forming properties, flexibility, water resistance and adhesive properties, and is widely used in silicone pressure-sensitive adhesives and anti-adhesive release agents , release agent, waterproofing agent, cosmetics and other important aspects. The synthesis of MQ silicone resin has always been a hot spot in the silicone field. [0003] At present, the synthesis of MQ silicone resin at home and abroad usually adopts the method of hydrolysis and polycondensatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/20C08G77/12
Inventor 宋振虎吴国相涂世俭
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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