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Preparation method of reactive MQ silicon resin

A MQ silicone resin, reactive technology, applied in the field of additives, can solve the problems of white precipitation or foam, easy gelation, unstable product, etc.

Inactive Publication Date: 2011-09-14
ZHONGKAI UNIV OF AGRI & ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of reactive MQ silicone resin, to solve the problems of white precipitation or foam easily produced in the current preparation process of reactive MQ silicone resin, and the product is unstable and easy to gel, and to improve the reactive MQ silicone resin. Quality and performance for increased productivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0023] The preparation method of reactive MQ silicone resin of the present invention comprises the following steps:

[0024] 1) Hydrolysis-condensation polysiloxane, alkoxysilane and its homopolymer;

[0025] 2) After step 1) the product is formed and extracted with a weak polar or non-polar solvent;

[0026] 3) The water washing process, when washing, the solution is used to wash the non-pure water washing product to neutrality;

[0027] 4) Concentrating by distillation under reduced pressure to obtain the reactive MQ silicone resin;

[0028] The hydrolysis-polycondensation siloxane, alkoxysilane and homopolymer thereof in step 1) refers to adding deionized water, alcohol and acid to the reaction vessel equipped with thermometer, heater, stirrer and addition funnel. solution, at 30-50°C, add the M unit raw materials and Q unit raw materials into the solution composed of deionized water, alcohol and acid within 0.5-2h, stir and react for 0.5-5h, and the reaction temperature ...

Embodiment 1

[0058] Embodiment 1 methyl MQ silicone resin

[0059] 28g H 2 0. Add 8g of concentrated HCl and 5g of absolute ethanol into a three-necked flask equipped with a thermometer, an electric heating mantle, a mechanical stirrer and a dropping funnel, start stirring, and heat up to 50°C; then add 36.0g of hexamethyldisiloxane, Add 115.6g of ethyl orthosilicate dropwise to the above mixture within 1 hour, heat to 70°C after dropwise addition, and stir for 3 hours. After the reaction is over, cool the reaction system to 30°C, add 100g of toluene for extraction, let stand, separate layers, wash the product with deionized water until the pH is neutral; distill and concentrate the toluene resin solution under reduced pressure at 100°C and 0.09MPa , That is, a white MQ silicone resin toluene solution.

[0060] GPC research shows that the molecular weight of silicone resin is about 3000. A certain amount of MQ silicone resin toluene solution was dried to constant weight, which indicated...

Embodiment 2

[0061] Embodiment 2 methyl MQ silicone resin

[0062] The above implementation conditions are the same as in Example 1, the product is washed with 50% methanol solution until the pH is neutral, and the extract is concentrated by distillation at 100° C. and 0.09 MPa to obtain a transparent MQ silicone resin toluene solution. GPC research shows that the molecular weight of silicone resin is about 3500. A certain amount of MQ silicone resin toluene solution was dried to constant weight, which indicated that the product yield was 38.5%. When washing with 50% methanol solution, there is no white precipitate or foam between the acid water layer and the resin solution layer, and the system is divided into two layers: the acid water solution and the resin toluene solution.

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PUM

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Abstract

The invention discloses a preparation method of reactive MQ silicon resin. The method comprises the following steps of: (1) hydrolyzing and condensing siloxane, alkoxy silane and a homopolymer thereof; (2) leaching a product prepared in the step (1) with a weak-polar or non-polar solvent; (3) washing the product with an aqueous solution to a neutral state; and (4) distilling and concentrating at reduced pressure to obtain the reactive MQ silicon resin, wherein an M unit of the reactive MQ silicon resin in the step (1) contains hexamethyldisiloxane, divinyl tetramethyl disiloxane, tetramethyldisiloxane, 1,1,3,3-tetramethyl-1,3 diphenyldisiloxane, 1,3-diethyl-1,1,3,3-tetramethyldisiloxane or a mixture thereof; a Q unit of the reactive MQ silicon resin contains tetramethyl silicate, tetraethoxysilane, tetraisopropoxidesilane, tetrabutoxysilane, tetrakis(butoxyethoxy)silane and a mixture of homopolymers thereof; the solution in the step (3) consists of a methanol aqueous solution, an ethanol aqueous solution, an isopropanol aqueous solution, a normal butanol aqueous solution, an isobutyl alcohol aqueous solution or a mixed aqueous solution thereof; and the mass fraction of the solution is 30-80.

Description

technical field [0001] The invention relates to the technical field of additives such as electronic packaging materials, coatings, adhesives and cosmetics, in particular to a preparation method of reactive MQ silicone resin. Background technique [0002] MQ silicone resin is composed of monofunctional structural unit (R 3 SiO 1 / 2 , M) and tetrafunctional structural units (SiO 4 / 2 , Q) Silicone formed by covalent bonding. MQ silicone resin is due to the molar ratio of M and Q chain links, that is, n M / n Q Different values, different degrees of polymerization, different types of groups connected to M units, showing the state of viscous fluid to solid powder, physical properties such as light transmittance, viscosity, glass transition temperature, viscosity increasing, lipophilicity, and other Material compatibility, etc., and chemical reactivity will vary accordingly. [0003] At present, most of the existing technologies about MQ silicone resin and its preparation proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/20
Inventor 葛建芳向洪平崔少伟程少辉
Owner ZHONGKAI UNIV OF AGRI & ENG
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