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Method for preparing methyl hydrocyclosiloxane

A technology of methylhydrogencyclosiloxane and hydrocarbylhydrohalosiloxane, which is applied in the field of preparation of methylhydrogencyclosiloxane, can solve the problems of many steps and not widely used, and achieve the effect of reducing production costs

Inactive Publication Date: 2012-03-14
江西多林科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] USP3714213 describes the method of preparing cyclosiloxane by pyrolyzing linear polysiloxane at high temperature in the presence of an alkali catalyst. Since the process needs to produce polysiloxane first, there are many steps and it is not widely used.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The hydrolysis experiment of hydrocarbyl hydrohalosilane was carried out in a 500ml three-neck beaker equipped with a thermometer, dropping funnel and reflux condenser (one end led out HCl gas). Under intense magnetic stirring, 72ml of methylhydrogendichlorosilane was evenly dropped into a reaction flask filled with 72ml of water, 26.6g of CaCl2 (template agent), and 72ml of petroleum ether (boiling range 30-60°C). The dropping speed and ice water cooling are controlled so that it does not exceed 15°C. After the dropwise addition, the reaction was continued at the same temperature for 1 hour, then poured into a separatory funnel, allowed to stand for layers, washed the organic phase with a small amount of water, and then washed with saturated NaHCO 3 The solution was neutralized to pH 7, and finally with Na 2 CO 3 After drying, the solvent was evaporated, and then rectified under reduced pressure to collect the fractions and analyze the composition of the fractions wi...

Embodiment 2

[0016] Methylhydrogen dichlorosilane consumption is 72ml, H 2 O 72ml, template agent CaCl 2 Dosage 7.3g

[0017] Solvent CH 2 Cl 2 72ml, reaction temperature 10-12 ℃, experimental apparatus and operation steps are the same as embodiment 1, and the results are shown in Table 1.

Embodiment 3

[0019] Each of methylhydrogendichlorosilane, water, and petroleum ether (boiling range 30-60°C) is 72ml, and the template agent is still CaCl 2 , but its consumption is reduced to 0.6g, 10-13 ℃ of temperature of reaction, other are the same as embodiment 1 results see table 1.

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Abstract

The invention provides a method for preparing methyl hydrocyclosiloxane. Methyl hydrochlorosilane is used as a raw material, low-boiling-point hydrocarbon compounds are used as solvents, the hydrolytic polycondensation reaction is carried out under the effect of template agents at the temperature lower than 15 DEG C, organic phases are washed by water and are neutralized after the standing lamination, the solvents are firstly distilled, then, the pressure-reduction rectification is carried out, and trimethyl hydrocyclotrisiloxane (D3H), tetramethyl hydrotetrasiloxane (D4H), pentamethyl hydrocyclopentasiloxane (D5H) and hexamethyl hydrohexasiloxane (D6H) are respectively prepared. The method has the advantages that alcohol is not used as the solvents, the low-boiling-point hydrocarbons are used as the solvents, the template agents with low price are used, the production cost is greatly reduced, and in addition, various products using methyl hydro-ring bodies can be prepared by adopting the solvents and the temperate agents with different properties.

Description

technical field [0001] The invention relates to a method for preparing methylhydrogen cyclosiloxane, in particular to a method for preparing methylhydrogen cyclosiloxane by using a template agent and low-boiling point hydrocarbons as solvents. Background technique [0002] Methylhydrocyclosiloxane is widely used in the preparation of various modified silicone oils and high-quality hydrogen-containing silicone oils. It can also be used as a crosslinking agent and anti-yellowing agent for silicone rubber. It is also a good sealing material and Preparation of hydrogen-containing siloxane [HSi(OSiH 2 )-O-SiH 3 ] Intermediates. [0003] There are two main methods for the preparation of alkylhydrocyclosiloxanes. One is to hydrolyze alkylhydrodihalosilanes in organic solvents, stand for stratification, and then distill. Polyalkyl hydrogen siloxane is obtained by cracking under the action of alkali catalyst and rectifying. [0004] James W. Carry et al. introduced in USP 3,484,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 李建勇李凤仪洪仁惠
Owner 江西多林科技发展有限公司