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Preparation method of propyltriisoallyloxysilane

A technology of propyltriisopropenyloxysilane and propyltrichlorosilane is applied in the field of preparation of propyltriisopropenyloxysilane, and can solve the problems of long reaction time, poor filtration of triethylamine hydrochloride and the like

Active Publication Date: 2016-05-25
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Catalyst selection in most synthetic methods is cuprous chloride or metal carbonate etc., and hydrochloric acid sorbent is triethylamine, and the main problem of above-mentioned synthetic method is that reaction time is long, generally needs more than 20h, even under high pressure condition It takes 16 hours. In addition, the by-product triethylamine hydrochloride is not easy to filter

Method used

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  • Preparation method of propyltriisoallyloxysilane
  • Preparation method of propyltriisoallyloxysilane

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 232g (4mol) of acetone, 0.0004g of palladium trichloride, 105g (0.75mol) of hexamethylene tetrachloride into a four-necked flask connected with magnetic stirring, spherical condenser, nitrogen gas guide tube, and constant pressure dropping funnel. Amine, 2g trimethyl orthoformate, add 177.5g (1mol) propyltrichlorosilane to the constant pressure dropping funnel, turn on the nitrogen, raise the temperature to 80°C at a stirring speed of 100 rpm, add dropwise to the constant pressure funnel The propyltrichlorosilane in the solution was added dropwise in 6 hours. After the dropwise addition of propyltrichlorosilane was completed, the temperature was maintained for 2 hours. The whole reaction was protected by nitrogen gas. The reaction pressure was normal pressure. After the reaction was completed, propyltrichlorosilane was obtained. For the crude product of acryloxysilane, the crude product of propyltriisopropenyloxysilane is cooled to below 20°C, and then under the prot...

Embodiment 2

[0025] Add 812g (14mol) of acetone, 0.003g of palladium trichloride, and 420g (3mol) of hexamethylenetetramine into a four-necked flask connected with a magnetic stirrer, a spherical condenser, a nitrogen gas guide tube, and a constant pressure dropping funnel. , 6g trimethyl orthoformate, add 710g (4mol) propyl trichlorosilane in the constant pressure dropping funnel, turn on nitrogen, heat up to 90°C at a stirring speed of 120 rpm, add dropwise the Propyl trichlorosilane, the dropwise addition of propyl trichlorosilane is completed in 6 hours. After the dropwise addition of propyl trichlorosilane is completed, keep the temperature for 2 hours. The whole reaction is protected by nitrogen gas. The reaction pressure is normal pressure. The crude propyl silane, the crude propyl triisopropenoxy silane is cooled to below 20°C, and then under the protection of nitrogen, the by-generated hexamethylenetetramine hydrochloride is removed by filtration to obtain a transparent filtrate, a...

Embodiment 3

[0027] Add 1914g (33mol) of acetone, 0.006g of palladium trichloride, 1050g (7.5mol) of hexamethylene tetrachloride into a four-necked flask connected with magnetic stirring, spherical condenser, nitrogen gas guide tube, and constant pressure dropping funnel. Amine, 18g trimethyl orthoformate, add 1775g (10mol) propyl trichlorosilane to the constant pressure dropping funnel, turn on the nitrogen gas, raise the temperature to 85°C at a stirring speed of 110 rpm, drop into the constant pressure funnel Propyltrichlorosilane, after 6 hours of dropwise addition of propyltrichlorosilane, keep the temperature for 2h reaction, the whole reaction is protected by nitrogen, the reaction pressure is normal pressure, and propyltriisopropene is obtained after the reaction is completed The crude product of oxysilane, the crude product of propyltriisopropenoxysilane is cooled to below 20°C, and then under the protection of nitrogen, the by-generated hexamethylenetetramine hydrochloride is remo...

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Abstract

The invention relates to a preparation method of propyltriisoallyloxysilane, belonging to the technical field of fine chemical engineering. The preparation method comprises the following steps: by using propyltrichlorosilane and acetone as raw materials, hexamethylenetetramine as a hydrochloric acid adsorbent, palladium chloride as a catalyst and trimethyl orthoformate as a dehydrator, carrying out reaction at 70-90 DEG C to synthesize a propyltriisoallyloxysilane-containing reaction product, filtering, and carrying out reduced pressure distillation to obtain the propyltriisoallyloxysilane product. The method has the advantages of simple technique and high reaction efficiency, and is suitable for industrial large-scale production. Compared with the existing propyltriisoallyloxysilane preparation method, the method provided by the invention shortens the reaction time, enhances the reaction efficiency, reduces the side reactions due to the use of the dehydrator, and enhances the product quality and yield.

Description

technical field [0001] The invention relates to a preparation method of propyltriisopropenyloxysilane, which belongs to the technical field of fine chemicals. Background technique [0002] Propyltriisopropenyloxysilane is a crosslinking agent, mainly used in one-component room temperature vulcanized silicone rubber (RTV-1), which is one of the main products of condensation liquid silicone rubber, since the 1960s Since its inception, it has quickly become an important part of silicone products because of its characteristic of vulcanization without heating at room temperature. According to the by-products produced during vulcanization, RTV-1 silicone rubber can be divided into dealcoholization type, decarboxylation type, deketoxime type, deamination type, deamidation type and acetone removal type. The common feature of these types of RTV-1 silicone rubber is that after extrusion, the uniformly mixed rubber can be vulcanized into an elastomer when it meets moisture at room tem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07F7/20
CPCC07F7/1804C07F7/188C07F7/20
Inventor 刘明锋吴兵兵陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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