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Alkyl-substituted disilane and preparation method thereof

A disilane and alkyl technology, which is applied in the field of alkyl-substituted disilane and its preparation, can solve the problem of not being able to meet the requirements of long-term use under harsh conditions such as high temperature, acid and alkali, long-term use, and the increase in the viscosity of silicone oil, etc. problems, to achieve the effect of controllable product structure, obvious social and economic benefits, and outstanding heat resistance

Inactive Publication Date: 2013-09-11
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few studies and reports on silicone oils with other structures such as Si-C, silicate, etc.
In addition, although the performance of silicone oil as a heat transfer oil is better than that of other heat transfer oils, it can only be used at temperatures below 200°C, which cannot meet the requirements of long-term use under harsh conditions such as high temperature, acid and alkali; The molecular structure of silicone oil is different, and its rapid oxidation temperature range is 200-250°C; when the temperature exceeds the rapid oxidation temperature of silicone oil, the viscosity of silicone oil will increase rapidly until it forms a gel, which cannot meet the requirements of long-term use at high temperatures. Therefore, people have been looking for ways to improve the thermal oxidation resistance of silicone oil, so that it can be used for a long time under high temperature conditions

Method used

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  • Alkyl-substituted disilane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Grignard reaction prepares the method for phenyl-substituted disilane, main steps are as follows:

[0047] a. Raw materials and proportioning: Take high-boiling point chlorosilane waste liquid, bromobenzene, and magnesium powder as raw materials; take magnesium powder and bromobenzene according to the molar ratio of magnesium powder: bromobenzene is 1.2:1; use high-boiling point chlorosilane waste liquid The molar ratio of chlorine atom to Grignard reagent is 1:1.1 to take high-boiling point chlorosilane waste liquid; the content of chlorine atom in high-boiling point chlorosilane waste liquid is 13mol / L through acid-base titration;

[0048] b. Preparation of Grignard reagent: Add 1.2g (0.050mol) of magnesium powder into a reactor equipped with a constant pressure dropping funnel, vacuumize the reactor and pass nitrogen three times to remove oxygen and water in the reactor; Add 2ml ether and 40μg catalytic amount of iodine into the reactor, add bromobenzene (6.44g, 40.7...

Embodiment 2

[0054] Grignard reaction prepares the method for octyl-substituted disilane, and main steps are as follows:

[0055] a. Raw materials and raw material ratio: Take high-boiling point chlorosilane waste liquid, 1-bromooctane, and magnesium powder as raw materials; take magnesium powder and 1-bromooctane at a molar ratio of 1.2:1 for magnesium powder: 1-bromooctane Chlorine atoms in high-boiling point chlorosilane waste liquid: Grignard reagent is 1:1.1 molar ratio to take high-boiling point chlorosilane waste liquid, and the content of chlorine atoms in high-boiling point chlorosilane waste liquid is 13mol / L through acid-base titration ;

[0056] b. Preparation of Grignard reagent: Add 1.2g (0.050mol) of magnesium powder into a reactor equipped with a constant pressure dropping funnel, vacuumize the reactor and pass nitrogen three times to remove oxygen and water in the reactor; Add 2ml ether and 40μg catalytic amount of iodine into the reactor, add 1-bromooctane (7.85g, 40.7mm...

Embodiment 3

[0062] Grignard reaction prepares the method for decyl-substituted disilane, main steps are as follows:

[0063] a. Raw materials and proportioning: Take high-boiling chlorosilane waste liquid, 1-bromodecane, and magnesium powder as raw materials; take magnesium powder and 1-bromodecane at a molar ratio of 1.2:1 for magnesium powder: 1-bromodecane ;According to the high-boiling point chlorosilane waste liquid chlorine atom: Grignard reagent is 1:1.1 molar ratio to get the high-boiling point chlorosilane waste liquid, the content of chlorine atoms in the high-boiling point chlorosilane waste liquid is 13mol / L through acid-base titration;

[0064]b. Preparation of Grignard reagent: Add 1.2g (0.050mol) of magnesium powder into a reactor equipped with a constant pressure dropping funnel, vacuumize the reactor and pass nitrogen three times to remove oxygen and water in the reactor; Add 2ml ether and 40μg catalytic amount of iodine into the reactor, add 1-bromodecane (8.99g, 40.7mmo...

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Abstract

The invention discloses alkyl-substituted disilane expressed as Rn Si-Si(CH3)6-n (I) in a formula (I) and a preparation method thereof. The preparation method of the compound comprises: adding magnesium powder, diethyl ether and iodine in a reactor, dropwise adding a diethyl ether solution of brominated hydrocarbon into the reactor for initiation, dropwise adding the residual diethyl ether solution of brominated hydrocarbon into the reactor, and reacting for 2-3hours after the dropwise adding operation to prepare a Grignard reagent; putting the reaction system in ice water bath, dropwise adding a diethyl ether solution of chlorosilane liquid waste with high boiling point into the Grignard reagent, heating up to room temperature to react for 1.5-2hours after the dropwise adding operation, and heating up to 50-60 DEG C to react for 5-6hours; adding water to separate an organic phase from an aqueous phase, extracting the aqueous phase through petroleum ether, mixing the organic phase, drying, concentrating, performing silicagel column chromatography, and concentrating the leacheate to obtain the remaining material which is the product (alkyl-substituted disilane). Industrial waste is used as a raw material in the invention, and the product has good thermal stability and strong heat resistance, thereby being applied to hydraulic oil, diffusion pump oil and heat transfer oil.

Description

technical field [0001] The invention belongs to a silicon compound and a method for preparing the silicon compound by mainly using waste, and relates to an alkyl-substituted disilane and a preparation method thereof. The organosilicon compound obtained in the present invention—the alkyl-substituted disilane is suitable for use as heat-resistant and oxidation-resistant heat-conducting oil. Background technique [0002] Silicone monomers (methylchlorosilane, phenylchlorosilane, vinylchlorosilane, etc.) are the basis for the development of the entire silicone material industry, and the production of dimethyldichlorosilane is the backbone of the development of the silicone industry. At present, the industrial production of organosilicon mainly uses copper-catalyzed chloroform and silicon powder to directly synthesize methylchlorosilane, while organosilicon chemical industry produces organosilicon products by the direct method, and at the same time it is accompanied by a large nu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
Inventor 杨军校刘天洋曹克黄亚文
Owner SOUTHWEAT UNIV OF SCI & TECH
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