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Methyl MQ resin and preparation method thereof

A methyl and resin technology, applied in the field of methyl MQ resin and its preparation, can solve the problems of performance, application difference, narrow molecular weight distribution and high raw material cost, and achieve the effects of reducing service life, simplifying operation and avoiding pollution

Active Publication Date: 2019-04-02
济南雅达新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The silicate method can better control the M / Q molar ratio, and the molecular weight distribution is relatively narrow, but the process is more complicated and the cost of raw materials is high
[0004] There are also certain differences in the properties and uses of the final methyl MQ resin products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0064] The embodiment of the present application provides the preparation method of methyl MQ resin, the preparation method includes: (1) refined sodium silicate aqueous solution: add organic solvent 1 dropwise to the sodium silicate aqueous solution under stirring, stir at 25±2°C, Then stand still, the bottom of the sodium silicate aqueous solution generates a precipitate, the sodium silicate aqueous solution is taken out, and then water is added to obtain a refined sodium silicate aqueous solution; (2) in a three-necked flask, add acid, cool, and then Add refined sodium silicate aqueous solution under stirring, heat, continue to stir, then add organic solvent 2 and silicon ether, and then reflux reaction; (3) stand still, the reactant of step (2) is divided into upper and lower layers, and the lower layer of water phase Drain, the upper layer is the organic phase, the organic phase is heated, neutralized, dried, and filtered to obtain the silicon ether solution of the methyl ...

Embodiment 1

[0068] Refining of Sodium Silicate Aqueous Solution

[0069] 1000 g (SiO 2 The mass fraction is 10%) sodium silicate aqueous solution, add the organic solvent dropwise while stirring, mix and stir at 25±2°C for 3 hours, then let it stand for 12 hours, a precipitate is formed at the bottom of the sodium silicate aqueous solution, and the sodium silicate aqueous solution Take out, obtain about 910 grams of refined sodium silicate aqueous solution. Dilute this refined sodium silicate aqueous solution with distilled water to SiO 2 A quality score of 10% is spared.

[0070] The refined sodium silicate was measured by the Lentz method to measure the molecular weight of the trimethylated GPC (Gel Permeation Chromatography, Gel Permeation Chromatography). In 50 grams of distilled water and hydrochloric acid with a concentration of 13.9%, add 130 grams of isopropanol, mix well, then add 80 grams of silicon ether, stir and mix well, drop in 50 grams of 1mol at 20°C-25°C for about 10 ...

Embodiment 2

[0074] The synthesis of embodiment 2 methyl MQ resins

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Abstract

The invention discloses a methyl MQ resin preparation method, which comprises: adding an organic solvent 1 to a sodium silicate aqueous solution in a dropwise manner under stirring, stirring at a temperature of 25+ / -2 DEG C, standing, generating precipitate at the bottom portion of the sodium silicate aqueous solution, taking out the sodium silicate aqueous solution, and adding corresponding waterto obtain a refined sodium silicate aqueous solution; carrying out a reaction on an acid and the refined sodium silicate aqueous solution, adding an organic solvent 2 and silyl ether, and carrying out a reflux reaction; separating the reaction product, and purifying; and carrying out spray drying on the obtained purified product to obtain the methyl MQ resin. According to the present invention, the methyl MQ resin prepared from the refined sodium silicate aqueous solution has high molecular weight compared with the methyl MQ resin prepared from the non-refined sodium silicate aqueous solution, and further has narrow molecular weight distribution; the excess silyl ether can be used as both the reaction material and the extractant for the reaction product; and during the post-treatment, thewater washing is avoided so as to prevent the emulsification. The present invention further provides a high molecular weight methyl MQ resin having a molecular weight of greater than 10000 g / mol.

Description

technical field [0001] This application relates to but not limited to the field of material chemistry, in particular to but not limited to a methyl MQ resin and its preparation method. Background technique [0002] MQ resin is composed of a functional siloxane chain (M) and a four-tube energy chain (Q). Because of its different functional links, there are methyl vinyl MQ, methyl MQ resin, S-H-based MQ resin and other varieties, among which Methyl MQ resin is the most widely used, and the demand is also the largest. Methyl MQ resin can be used in silicone pressure sensitive adhesives, silicone coating materials, defoamers, cosmetics, powder hydrophobic treatment and other fields. [0003] There are sodium silicate method and silicate method for the preparation of methyl MQ resin, both of which have advantages and disadvantages. The sodium silicate method uses sodium silicate as the source of Q chains, and it is prepared by hydrolysis and condensation with triorganochlorosil...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/06
CPCC08G77/04C08G77/06C08G77/70
Inventor 赵秀华仇进华
Owner 济南雅达新材料科技有限公司
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