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Organopolysiloxane resin and preparation method thereof

A polysiloxane resin and organic technology, applied in the field of organopolysiloxane resin and its preparation, can solve the problems of salts, incomplete acid treatment, influence on application performance, complex solvent components, etc., and achieve environmental protection in the preparation process , good application performance, avoid the effect of local polycondensation

Inactive Publication Date: 2017-12-12
GUANGZHOU TINCI SILICONE TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The reaction system requires the use of a large amount of toxic solvents, such as toluene, xylene, etc., the tail gas is difficult to handle, pollutes the environment, and the solvent components are complex and difficult to recycle
[0006] (2) The reaction process is complicated, and operations such as extraction and water washing are often used. The yield is low, the energy consumption is large, and a large amount of waste water is generated, which is not environmentally friendly.
[0007] (3) The salt and acid treatment in the obtained product is not thorough, which affects the application performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation method of a kind of organopolysiloxane resin of the present embodiment comprises the following steps:

[0040] (1) Add 28.6g of concentrated hydrochloric acid, 40g of ethanol, 69g of water and 56.2g of hexamethyldisiloxane into a four-neck flask, and stir at 300 rpm and 25°C for 0.5h;

[0041] (2) Keep stirring, add 240g tetraethyl orthosilicate dropwise at room temperature, control the system temperature at 40°C, and complete the dropwise addition in 40 minutes; after the dropwise addition, polycondensate at 70°C for 3 hours;

[0042] (3) Then add saturated sodium bicarbonate solution to adjust the pH value of the system to 6.5-7.5;

[0043] (4) Stir and heat up to 120°C, first under normal pressure, then under vacuum, to remove alcohol and water in the system to obtain a salt-containing organopolysiloxane resin;

[0044] (5) adding 300g cyclohexane to dissolve the salt-containing organopolysiloxane resin;

[0045] (6) The reaction liquid obtained in ...

Embodiment 2

[0048] The preparation method of a kind of organopolysiloxane resin of the present embodiment comprises the following steps:

[0049](1) Add 28.6g of concentrated hydrochloric acid, 40g of ethanol, 69g of water and 56.2g of hexamethyldisiloxane into a four-neck flask, and stir at 300 rpm and 25°C for 0.5h;

[0050] (2) Keep stirring, add 240g tetraethyl orthosilicate dropwise at room temperature, control the system temperature at 40°C, and complete the dropwise addition in 40 minutes; after the dropwise addition, polycondensation reaction at 65°C for 4 hours;

[0051] (3) Then add saturated sodium bicarbonate solution to adjust the pH value of the system to 6.5-7.5;

[0052] (4) Stir and heat up to 100°C, first under normal pressure, then under vacuum, to remove alcohol and water in the system to obtain a salt-containing organopolysiloxane resin;

[0053] (5) Add 300g cyclohexane to dissolve the salt-containing organopolysiloxane resin, add 2g sodium carbonate, react at 90°C ...

Embodiment 3

[0057] The preparation method of a kind of organopolysiloxane resin of the present embodiment comprises the following steps:

[0058] (1) Add 28.6g of concentrated hydrochloric acid, 40g of ethanol, 72g of water and 75g of hexamethyldisiloxane into a four-necked flask, and stir for 0.5h at 300 rpm and 25°C;

[0059] (2) Keep stirring, add 240g tetraethyl orthosilicate dropwise at room temperature, control the temperature of the system at 40°C, and complete the dropwise addition in 40 minutes. After the dropwise addition, polycondensation reaction at 75°C for 2 hours;

[0060] (3) Then add saturated sodium bicarbonate solution to adjust the pH value of the system to 6.5-7.5;

[0061] (4) Stir and heat up to 120°C, first under normal pressure, then under vacuum, to remove alcohol and water in the system to obtain a salt-containing organosiloxane resin;

[0062] (5) adding 300g cyclohexane to dissolve the salt-containing organosiloxane resin;

[0063] (6) The reaction solution ...

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Abstract

The invention relates to an organopolysiloxane resin and a preparation method thereof. The general formula of the organopolysiloxane resin is (R13SiO0.5)m(R22SiO)n(R3SiO1.5)p(SiO2)q. The preparation method comprises the following steps: placing an end-capping reagent, deionized water, a cosolvent and acid into a reaction vessel and stirring; dropwise adding silane into the reaction vessel, raising the temperature of the reaction system to 60-80 DEG C and reacting for 2-4h; regulating pH value of the reaction solution to 7, stirring, raising the temperature to 80-120 DEG C and distilling till no fraction exists; dissolving the resin into an organic solvent, adding solid alkali, raising temperature to 70-140 DEG C and reacting for 2-4h; centrifuging the reaction solution and removing solid salt; and performing vacuum drying on the reaction solution, thereby acquiring the organopolysiloxane resin. The method has the advantages of high product yield, simple process, no pollution in a production process, less three-waste, energy-saving effect and environmental protection.

Description

technical field [0001] The invention relates to the technical field of organosilicon, in particular to an organopolysiloxane resin and a preparation method thereof. Background technique [0002] Organopolysiloxane resin is a kind of thermosetting polysiloxane system with highly cross-linked structure, which has the properties of both organic and inorganic materials, and presents many unique physical and chemical properties, such as non-toxic and tasteless, weather resistance, heat resistance, Electrical insulation, chemical resistance, hydrophobicity, adhesiveness and flame retardancy, etc. It has been widely used in the fields of national defense and military industry, energy development, light industry, food, textile, electronics, machinery, construction, transportation, medical medicine and daily life. [0003] The performance of organopolysiloxane depends on the type and proportion of raw material silane, the type and pH value of hydrolysis condensation medium, the natu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/20C08G77/12C08G77/06C08G77/34
CPCC08G77/04C08G77/06C08G77/12C08G77/20C08G77/34C08G77/70
Inventor 王凌伟饶磊张宇蔡华轮张利萍
Owner GUANGZHOU TINCI SILICONE TECHNOLOGY CO LTD
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