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Preparation method of acid-binding functional catalyst for synthesizing methyltris(methylethylketoxime)silane

A technology of methyl tributyl ketone oxime and base silane, which is applied in the field of preparation of acid-binding functional catalysts, and can solve problems such as limiting production capacity, increasing production costs, and large consumption

Active Publication Date: 2021-04-23
ZHEJIANG JINHUA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation of methyl tributylketoxime silane by the above technology is to directly react with vinyl trichlorosilane and butanone oxime, and its reaction yield is often about 85%, and using butanone oxime as an acid-binding agent consumes a lot. Limit the improvement of production capacity and increase the production cost of products

Method used

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  • Preparation method of acid-binding functional catalyst for synthesizing methyltris(methylethylketoxime)silane
  • Preparation method of acid-binding functional catalyst for synthesizing methyltris(methylethylketoxime)silane
  • Preparation method of acid-binding functional catalyst for synthesizing methyltris(methylethylketoxime)silane

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Effect test

Embodiment 1

[0029] A kind of preparation method of the acid-binding functional catalyst that is used for synthesizing methyl tributylketoxime base silane, its operating steps are:

[0030] Step 1: Add 80g of activated mesoporous solid powder and 400g of toluene into the reactor, stir and disperse evenly, then heat up to 90°C, then add 5g of 2,5-divinyl-pyridine into the reactor, stir and mix 30min, then 3g of 1,1`-bis(dimethylsilyl)iron, 0.1g of isopropanol solution of chloroplatinic acid with a mass percent content of 5-10%, were evenly added into the reaction kettle slowly , then control the temperature to 60°C, stir the reaction for 1h,

[0031] Step 2: Add 8g of vinyl sulfonamide, 1.2g of allyl polyoxyethylene ether, 0.5g of benzoyl peroxide, then control the temperature to 80°C, stir and react for 10h, and filter after completing the reaction to obtain a solid Slurry and purify with absolute ethanol for three times, and then vacuum dry to obtain the acid-binding functional catalyst ...

Embodiment 2

[0035] A kind of preparation method of the acid-binding functional catalyst that is used for synthesizing methyl tributylketoxime base silane, its operating steps are:

[0036] Step 1: Add 90g of activated mesoporous solid powder and 460g of toluene into the reactor, stir and disperse evenly, then heat up to 100°C, then add 7g of 2,5-divinyl-pyridine into the reactor, stir and mix 40min, then 5g of 1,1'-bis(dimethylsilyl)iron, 0.3g of 7% isopropanol solution of chloroplatinic acid by mass percent, evenly and slowly added to the reactor, and then Control the temperature to 604°C, stir and react for 1.5h,

[0037] Step 2: Add 11g of vinyl sulfonamide, 2.5g of allyl polyoxyethylene ether, 0.9g of benzoyl peroxide, then control the temperature to 90°C, stir for 17 hours, and filter after the reaction to obtain a solid Slurry and purify with absolute ethanol for 4 times, and then vacuum dry to obtain the acid-binding functional catalyst for synthesizing methyltributanoximinosilane...

Embodiment 3

[0041] A kind of preparation method of the acid-binding functional catalyst that is used for synthesizing methyl tributylketoxime base silane, its operating steps are:

[0042] Step 1: Add 140g of activated mesoporous solid powder and 500g of toluene into the reactor, stir and disperse evenly, then heat up to 110°C, then add 15g of 2,5-divinyl-pyridine into the reactor, stir and mix 60min, then 6g of 1,1'-bis(dimethylsilyl)iron, 0.5g of 10% isopropanol solution of chloroplatinic acid in mass percentage, evenly and slowly added to the reactor, and then Control the temperature to 67°C, stir the reaction for 3h,

[0043] Step 2: Add 12g of vinyl sulfonamide, 3.5g of allyl polyoxyethylene ether, 1.5g of benzoyl peroxide, then control the temperature to 100°C, stir and react for 20h, filter after the reaction is completed, and obtain the solid Slurry and purify with absolute ethanol for 5 times, and then vacuum-dry to obtain the acid-binding functional catalyst for synthesizing me...

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Abstract

The invention relates to the field of chemical engineering, and particularly relates to a preparation method of an acid-binding functional catalyst for synthesizing methyltris(methylethylketoxime)silane. The preparation method comprises the steps of compounding various metal chlorides, calcining at high temperature to prepare metal chloride solid powder with a mesoporous structure, and heating in concentrated hydrochloric acid to finish activation; then grafting a nitrogen-containing cyclic compound 1,1'-di(dimethylsilyl) iron to the surface of the mesoporous metal chloride solid powder through a siloxane hydrolysis reaction so as to enable the surface to have an active amino group, wherein the catalyst has an acid-binding function while catalyzing the reaction, can achieve the purpose of immobilizing the generated hydrogen chloride in the synthesis process of methyltris(methylethylketoxime)silane, promotes the reaction, increases the reaction efficiency and reduces the input amount of a butanone oxime reactant. The catalyst provided by the invention is simple in preparation method and good in catalytic effect, belongs to a mesoporous solid-phase catalyst, does not introduce impurities into a reaction system, and is a promising catalyst.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing an acid-binding functional catalyst used for synthesizing methyltributanoximinosilane. Background technique [0002] Methyl tributyl ketoxime silane is used as a vulcanizing agent and crosslinking agent for room temperature vulcanized rubber, and also as an accelerator for bonding plastics, nylon, ceramics, glass, etc. to silicone rubber. [0003] CN111018900A is specifically about a kind of preparation method of methyl tributyl ketoxime silane; a kind of preparation method of methyl tributyl ketoxime silane of the present invention, this method directly drops methyl trichlorosilane to butanone oxime In the solution, the raw material ratio of excess butanone oxime is used, and the excess butanone oxime can be used in the extrusion reaction process and can be used as an acid-binding agent without introducing other substances, and the product has less impurit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F7/08C08F283/06C08F230/04C08F228/02
Inventor 段仲刚周强徐碧涛茅志清张军良
Owner ZHEJIANG JINHUA NEW MATERIALS
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