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A kind of vinyl phenyl silicone resin synthesized by solvent-free method and preparation method thereof

A vinyl phenyl silicon, solvent-free technology, applied in the field of silicone resin materials, can solve the problems of solvent affecting product application, complex preparation process, uneven group distribution, etc., and achieve significant environmental protection benefits, simple process, and good fluidity. Effect

Active Publication Date: 2019-03-05
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) A large amount of organic solvents, such as toluene, ethanol, etc., are required to be used in the reaction system, the tail gas is difficult to handle, pollutes the environment, organic solvents are flammable and explosive, prone to safety accidents, and a small amount of residual solvents affect product applications;
[0005] (2) The different rates of hydrolysis of phenyl monomers and methyl monomers cause uneven distribution of groups, large differences in the refractive index of molecules, and incompatibility, thereby affecting the light transmittance of the product;
[0006] (3) The preparation process is complex, if the order of feeding needs to be strictly controlled, or the prepolymer of the reaction needs to be prepared in advance;
[0007] (4) Hydrolysis of chlorosilane produces a large amount of harmful gases and substances of hydrogen chloride, polluting the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Into a 1000ml glass kettle, add 20.8g of ethyl orthosilicate, 99g of phenyltrimethoxysilane, 54.6g of methylphenyldimethoxysilane, 13g of dimethylvinylethoxysilane, 1g of concentrated hydrochloric acid, Stir rapidly at 60°C, add 80m1 of deionized water dropwise, the dropwise addition is completed in 60 minutes, and the pH is 2; then raise the temperature to 75°C for 4 hours, let stand to separate the liquid, wash the lower layer of material with water until neutral, and then in the temperature of 100 ℃ and a vacuum of 0.096MPa to remove low boilers; raise the temperature to 160℃, add 0.1g of sodium hydroxide to react for 4 hours, and neutralize the product with phosphoric acid to obtain vinyl phenyl silicone resin (M 0.1 D. 0.3 T 0.5 Q 0.1 ). The resulting product has a refractive index of 1.5545 and a molecular weight of W w 7300, light transmittance > 98%.

Embodiment 2

[0036] Into a 1000ml glass kettle, add 15.2g of methyl orthosilicate, 59.4g of phenyltrimethoxysilane, 27.2g of diphenyldiethoxysilane, 12g of dimethyldimethoxysilane, dimethylvinyl 52g of methoxysilane, 1g of concentrated sulfuric acid, stir rapidly at 60°C, add dropwise 60m1 of deionized water, the dropwise addition is completed in 30 minutes, and the pH is 2; then heat up to 75°C for 4 hours, let stand to separate the liquid, and the lower layer material Wash with water until neutral, then remove low boilers at a temperature of 100°C and a vacuum of 0.096MPa; raise the temperature to 160°C, add 0.1g of potassium hydroxide to react for 5 hours, and neutralize the product with phosphoric acid to obtain Vinyl phenyl silicone resin (M 0.4 D. 0.2 T 0.3 Q 0.1 ). The resulting product has a refractive index of 1.5346 and a molecular weight of W w 1800, light transmittance > 98%.

Embodiment 3

[0038] Into a 1000ml glass kettle, add 26.4g of propyl orthosilicate, 39.6g of phenyltrimethoxysilane, 73.2g of diphenyldimethoxysilane, 44.4g of dimethyldiethoxysilane, divinyltetra Methyldisiloxane 9.3g, concentrated hydrochloric acid 1g, stir rapidly at 60°C, add dropwise 80m1 of deionized water, the dropwise addition is completed in about 60 minutes, and the pH is 2; then raise the temperature to 75°C for 4 hours, let stand liquid, the lower material was washed with water until neutral, and then the low boilers were removed at a temperature of 100°C and a vacuum of 0.096MPa; the temperature was lowered to 90°C, and 0.1g of tetramethylammonium hydroxide was added to react for 6 hours, and then Raise the temperature to 150°C and keep for 30min to decompose tetramethylammonium hydroxide to obtain vinylphenyl silicone resin (M 0.1 D. 0.6 T 0.2 Q 0.1 ). The resulting product has a refractive index of 1.5565 and a molecular weight of W w 8600, light transmittance > 98%.

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Abstract

The invention belongs to the technical field of silicone resin materials, and discloses vinyl phenyl silicone resin synthesized according to a solvent-free method, and a preparation method of the vinyl phenyl silicone resin. The preparation method comprises the following steps: adding a tetra-functional monomer, a tri-functional alkoxysilane monomer, a bi-functional alkoxysilane monomer, a mono-functional alkoxysilane monomer and one or more acid catalysts; dropwise adding deionized water while stirring the mixture; after the dropwise addition is finished, controlling the reaction system temperature to be 10-80 DEC and ensuring that the reaction lasts for 1-6 hours; neutralizing the reaction product I or removing the acid catalysts, removing low-boiling-point substances, and then adding one or more alkali catalysts for a 4-6 hours' reaction at 80-160 DEG C; neutralizing the reaction product II or removing the alkali catalysts, thereby obtaining the vinyl phenyl silicone resin. The preparation method has the advantages that no organic solvents is utilized, no toxic gas is generated, the refractive index and light transmittance of the prepared vinyl phenyl silicone resin are high, and high economic and environment-friendly benefits are achieved.

Description

technical field [0001] The invention belongs to the technical field of silicone resin materials, and in particular relates to a vinylphenyl silicone resin synthesized by a solventless method and a preparation method thereof. Background technique [0002] Phenyl silicone resin refers to the silicone resin material containing siloxane chain links in its structure, which is obviously superior to methyl silicone in terms of thermal elasticity, mechanical properties, adhesion, gloss, and compatibility with organic and inorganic fillers. Therefore, it is widely used as high temperature resistant insulating paint, high temperature resistant coating, high temperature resistant adhesive, high temperature resistant molding compound, and ablation material. [0003] Vinyl phenyl silicone resin refers to phenyl silicone resin containing vinyl end-capping, because it contains reactive vinyl groups, it can be widely used in addition-type phenyl silicone materials. 现有技术中,如专利CN101508776A、CN1...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/06C08G77/08
Inventor 王凌伟张宇丘集辉张利萍薛亮忠霍梦月杨思广
Owner GUANGZHOU TINCI MATERIALS TECH