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Preparation method for phenyl vinyl MQ silicone resin

A technology of MQ silicone resin and phenyl vinyl, which is applied in the direction of electrical components, circuits, adhesives, etc., can solve the problems of difficult purification treatment, easy to produce gel, unstable orthosilicic acid, etc., and achieve adjustable group content, Ease of separation and purification, stable product structure

Active Publication Date: 2013-01-16
CHANGZHOU INST OF CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Invention patents US7595113 and WO2004107458 disclose the preparation of high refractive index phenylvinyl silicone resins by hydrolysis and condensation of chlorosilanes, which is also the main method currently used abroad. The advantage of this method is that low-cost chlorosilanes are directly used to prepare benzene Vinyl silicone resin; the disadvantage is that the storage and transportation of chlorosilane is not easy, the reaction is violent and the process is difficult to control, a large amount of hydrochloric acid is produced, which corrodes the reactor, and there is a problem of post-treatment of a large amount of waste acid. Chinese invention patent CN101343365 also uses chlorosilane The hydrolysis route also has the same problems of reaction process control and post-treatment of a large amount of waste acid solution
Invention patent US7160972 discloses the preparation of methylphenyl vinyl silicone resin A and methylphenyl hydrogen-containing silicone resin B by cohydrolysis and condensation of chlorosilane and alkoxysilane, and its refractive index can reach 1.57, because it uses part of chlorosilane Monomer, still can not solve the problem in the process of hydrolysis and condensation with chlorosilane as mentioned above
[0007] Invention patent CN101717512 discloses a method for preparing methylphenyl vinyl silicone resin by hydrolyzing difunctional (D) and trifunctional (T) alkoxysilanes. The obtained product has not been deacidified, and the residual acid may reduce the Weather resistance and high and low temperature resistance of packaging materials
Invention patent CN101126010 uses alkoxysilane hydrolysis to prepare two-component silicone resin. The organometallic catalyst used is not removed in the reaction system, and there is still the possibility of reducing the weather resistance and thermal stability of the material after curing.
[0008] Invention patent CN101475689 prepares methylphenyl vinyl silicone resin by cohydrolysis condensation of monofunctional group (M) and D and T unit monomers, which overcomes the difficulty of controlling the above reaction process and the problem of waste liquid treatment, but the acidic cationic resin is in the alkoxy The alcohol solution generated by the hydrolysis of silane is easy to swell and disperse, making it difficult to purify in the later stage
[0009] Invention patent CN101323667 uses the method of sodium silicate hydrolysis condensation to prepare high refractive index, high light transmittance phenyl vinyl MQ silicone resin, but the disadvantage of this method that cannot be ignored is that a large amount of acid is used in the hydrolysis process, and sodium silicate is too much It is alkaline, and when the acidification process passes through pH=7.0, orthosilicic acid is extremely unstable, and it is easy to produce gel, and the process is difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In proportion by weight, 16.99 parts of ethyl orthosilicate, 4.15 parts of hexamethyldisiloxane and 1,3-divinyl-1,1,3,3-tetramethyldisiloxane were added to the reactor Add 0.25 parts of alkane, 32.70 parts of phenyltriethoxysilane and 15.50 parts of diphenyldiethoxysiloxane, and add hydrochloric acid aqueous solution dropwise under rapid stirring in a water bath at 10°C. The dropwise addition is completed in about 30 minutes, and the pH is 2; Start to heat up to 75°C and keep it for 8 hours, add 200 parts of toluene, adjust the pH value to 11 with sodium hydroxide solution, then start distillation in a water bath at 80°C, stop distillation when almost no distillate is distilled, and cool to room temperature naturally.

[0032] Wash the above cooled solution in a separatory funnel with deionized water until the pH is 6-7, then dry it in an Erlenmeyer flask with anhydrous calcium chloride until it is clear, filter, and then decompress under 10mmHg Distillation, the temper...

Embodiment 2

[0034] In proportion by weight, 16.80 parts of ethyl orthosilicate, 11.60 parts of hexamethyldisiloxane and 1,3-divinyl-1,1,3,3-tetramethyldisiloxane were added to the reactor 1.89 parts of alkane, 36.30 parts of phenyltriethoxysilane, rapidly stirring and dropwise adding hydrochloric acid aqueous solution in a 50°C water bath, the dropwise addition is completed in about 20 minutes, and the pH is 2; start to heat up to 75°C and keep it for 8 hours, add 200 parts toluene, and adjust the pH value to 11 with sodium hydroxide solution, then start distillation in a water bath at 80°C, stop the distillation when almost no distillate is distilled, and cool naturally to room temperature.

[0035] Wash the above cooled solution in a separatory funnel with deionized water until the pH is 6-7, then dry it in an Erlenmeyer flask with anhydrous calcium chloride until it is clear, filter, and then decompress under 10mmHg Distillation, the temperature starts from 30°C, at a rate of 3.5°C / min...

Embodiment 3

[0037] In proportion by weight, 16.03 parts of ethyl orthosilicate, 1.34 parts of hexamethyldisiloxane and 1,3-divinyl-1,1,3,3-tetramethyldisiloxane were added to the reactor 16.35 parts of alkane, 34.36 parts of phenyltriethoxysilane and 16.08 parts of diphenyldiethoxysiloxane, and rapidly stir and drop hydrochloric acid aqueous solution in a water bath at 30°C, the dropwise addition is completed in about 30 minutes, and the pH is 2; Start to heat up to 80°C and keep it for 8 hours, add 200 parts of toluene, adjust the pH value to 10 with sodium hydroxide solution, then start distillation in a water bath at 75°C, stop distillation when almost no distillate is distilled, and cool to room temperature naturally.

[0038] Wash the above cooled solution in a separatory funnel with deionized water until the pH is 6-7, then dry it in an Erlenmeyer flask with anhydrous calcium chloride until it is clear, filter, and then decompress under 10mmHg Distillation, the temperature starts fr...

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Abstract

The invention relates to a preparation method for a phenyl vinyl MQ silicone resin. The phenyl vinyl MQ silicone resin is prepared by the steps of co-hydrolysizing a mixture of silicate ester, phenyl alkoxy silane, vinyl alkoxy silane and methyl alkoxy silane with hydrochloric acid, extracting, drying an organic layer in a neutral condition and removing low-boiling-point substances. The method is mild in reaction condition, cheap and easily available in raw materials and simple in process. The phenyl vinyl silicone resin can be used as an LED packaging material, and also can be used as other reinforcing fillers, additives of personal care products, defoaming agents, brightening agents, other auxiliaries, etc.

Description

technical field [0001] The invention relates to a preparation method of organic silicon resin, in particular to a preparation method of phenylvinyl MQ silicone resin. The invention belongs to the technical field of preparation of silicone resin reinforced materials. Background technique [0002] With the increasingly severe energy situation, energy saving and new energy development are becoming more and more important. As a new light source for energy saving and environmental protection, LED has been widely used in tunnel lighting, automotive lighting, signal indication, decoration, indoor and outdoor lighting, and special fields lighting and other fields. [0003] The wide range of application fields of LED requires that its packaging materials must have high performance, such as: high light transmittance, high refractive index, UV resistance, high and low temperature resistance, low curing shrinkage, good bonding performance with the substrate, etc. Silicone materials ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/08C09J183/07H01L33/56
Inventor 刘白玲李茹张保坦陈修宁王公应何国锋
Owner CHANGZHOU INST OF CHEM
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