High-molecular-weight MQ silicon resin and synthesis method and application thereof

A technology of MQ silicone resin and high molecular weight, which is applied in the field of high molecular weight MQ silicone resin and its synthesis, can solve the problems of low yield of MQ silicone resin, unreasonable purification method, and a large amount of waste water, etc. The effect of long retention time and high molecular weight

Active Publication Date: 2019-04-12
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] 3. The purification method is unreasonable, a large amount of waste water will be generated, and the production is not environmentally friendly;
[0014] 4. The yield of MQ silicone resin is low

Method used

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  • High-molecular-weight MQ silicon resin and synthesis method and application thereof
  • High-molecular-weight MQ silicon resin and synthesis method and application thereof
  • High-molecular-weight MQ silicon resin and synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] 1) Add 250 grams of deionized water, 50 grams of hydrochloric acid, 500 grams of ethanol, 70 grams of hexamethyldisiloxane, and 70 grams of divinyltetramethyldisiloxane into a four-necked flask with a condenser tube, a thermometer and a constant pressure dropping funnel. 5 grams of siloxane, start stirring, and raise the temperature to 30°C;

[0065] 2) Add 1055 grams of tetraethyl orthosilicate dropwise for 1 hour, and then heat-preserve and hydrolyze for 1 hour after adding;

[0066] 3) Heat up to 60°C, add a mixture of 650 grams of xylene, 350 grams of hexamethyldisiloxane and 24 grams of divinyltetramethyldisiloxane, and continue to keep warm for 4 hours; then add 650 grams of xylene, static separation;

[0067] 4) Add 30 grams of sodium bicarbonate to the organic phase, adjust the pH to 7, slowly raise the temperature to 150° C., remove low boilers at the same time, and then keep warm for 1 hour;

[0068] 5) Cool to room temperature, filter to remove insoluble ma...

Embodiment 2

[0070] 1) Add 250 grams of deionized water, 50 grams of acetic acid, 500 grams of isopropanol, 40 grams of hexamethyldisiloxane, and divinyltetramethyl to a four-neck flask with a condenser tube, a thermometer and a constant pressure dropping funnel. 5 grams of base disiloxane, start stirring, and heat up to 20-30°C;

[0071] 2) 771 grams of methyl orthosilicate was added dropwise, the dropwise addition time was 1 hour, and the temperature was kept at 20-30°C for 1 hour;

[0072] 3) Raise the temperature to 70°C, add a mixture of 650 grams of toluene, 350 grams of hexamethyldisiloxane and 24 grams of divinyltetramethyldisiloxane, and continue to keep warm for 3 hours; then add 650 grams of toluene and let stand Liquid separation;

[0073] 4) Add 30 grams of sodium bicarbonate to the organic phase, adjust the pH to 7, slowly raise the temperature to 110° C., remove low boilers at the same time, and then keep warm for 1 hour;

[0074] 5) Cool to room temperature, filter to rem...

Embodiment 3

[0076] 1) Add 200 grams of deionized water, 10 grams of trifluoromethanesulfonic acid, and 480 grams of methanol into a four-neck flask with a condenser, a thermometer and a constant pressure dropping funnel, raise the temperature to 45°C, and add hexamethyldisiloxane 30 grams, 5 grams of divinyltetramethyldisiloxane;

[0077] 2) Add 1340 grams of propyl orthosilicate dropwise, dropwise for 2.5 hours, and keep warm for 1 hour;

[0078] 3) Raise the temperature to 65°C, add a mixture of 750 grams of toluene, 360 grams of hexamethyldisiloxane and 24 grams of divinyltetramethyldisiloxane, and continue to keep warm for 4 hours; then add 750 grams of toluene and let stand Liquid separation;

[0079] 4) Add 30 grams of sodium bicarbonate to the organic phase, adjust the pH to 7.0, slowly raise the temperature to 120° C., remove low boilers at the same time, and keep the temperature for 3 hours;

[0080] 5) Cool to room temperature, filter to remove insoluble matter, and remove the...

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Abstract

The invention provides high-molecular-weight MQ silicon resin and a synthesis method and application thereof. The synthesis method of the MQ silicon resin comprises the steps that silicate ester and partial M unit silane monomers carry out a pre-reaction in a mixed solution composed of water, catalysts and cosolvents for a pre-reaction; then remaining M unit silane monomers and partial extractionagents are added in the mixed solution for a reaction under a heating condition, afterwards, remaining extraction agents are added, and an organic phase is obtained through extraction; the organic phase is adjusted to be neutral, and afterwards, the high-molecular-weight MQ silicon resin is obtained through distillation, wherein the mass ratio of the M unit silane monomers which are added twice is10:1-1:10. The synthesis method is simple in procedure, a large amount of washing is not needed, the product yield is high, and an extra curing agent is not needed to remove silicon hydroxyl and silicon alkoxy in the MQ silicon resin; meanwhile, the molecular weight of a target product can be controlled according to the ratio for adding the M monomers in batches and the ratio for adding the extraction agents in batches.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a high molecular weight MQ silicone resin and its synthesis method and application. Background technique [0002] MQ silicone resin is a very unique type of siloxane, a new type of silicone material with a three-dimensional (non-linear) structure composed of Si-O bonds as the skeleton, and a polycondensation link of four-functional siloxane ( Q) The silicone resin composed of monofunctional siloxane links (M) generally has a molar mass of 1000 to 8000 and has the following excellent characteristics: excellent heat resistance and low temperature resistance, and can be used at -60°C to 300°C ℃ temperature environment; good film-forming properties, moderate flexibility, and anti-aging, anti-ultraviolet radiation; good water repellency; good adhesion performance; excellent isolation performance, and durable, making a Permanent release agent. [0003] MQ silicone resin has the follo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06C08G77/08
CPCC08G77/06C08G77/08C08G77/20C08G77/70
Inventor 徐文远沈一平赖凤玲
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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