Synthesis method of methylhydro cyclo siloxane

A technology of methylhydrogencyclosiloxane and silanes, which is applied in the field of preparation of methylhydrogencyclosiloxane, can solve problems such as insecurity, and achieve the effects of less methanol consumption, high economic benefits, and high yield

Inactive Publication Date: 2003-04-16
蓝星安迪苏股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the amount of methanol, which is the most harmful to the human body, is as high as 50%, which constitutes a relatively large unsafe factor for production, life, and social environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 A method for preparing methylhydrocyclosiloxane with high yield of tetramethylcyclotetrasiloxane. The silane substance with the general formula of RR'SiXX and the alkane are in a volume ratio of 25-35 parts: 50 -70 parts are mixed, gradually dripped into the mixed multi-phase mixed solvent system, and stirred for hydrolysis reaction. The volume ratio of the multi-phase mixed solvent is composed of alkane: alcohol: water = 50-70 parts: 10 -15 parts: 20-36 parts, reaction time: 2-8 hours, reaction temperature: 0-30°C, to obtain methylhydrocyclosiloxane products containing tetramethylcyclotetrasiloxane and linear siloxanes By-product, in the general formula of R R'SiXX, R=C 1 -C 5 , Preferably R=CH 3 ; R'= H, C 1 -C 5 , Preferably, R'=H; X=Cl, Br, I, OMe, OEt, preferably X=Cl. The structural formula of RR'SiXX is

Embodiment 2

[0020] Example 2: The silane substance of the general formula RR'SiXX is methyldichlorosilane. The rest is the same as in Example 1.

Embodiment 3

[0021] Example 3: The volume ratio of the mixed solvent is composed of alkane: alcohol: water = 60-65 parts: 10-12 parts: 20-25 parts. The rest is the same as in Example 1.

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PUM

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Abstract

A process for synthesizing methyl hydrocyclosiloxane, especially tetramethyl cyclotetrasiloxane (D4H) includes such steps as proportionally mixing silanes with paraffins, dropping it to multi-phase solvent mixture while stirring, and hydrolytic reaction at 0-30 deg.c for 2-8 hr. Its advantages are high output rate, and no pollution and by-product.

Description

Technical field [0001] The invention relates to a preparation method of methyl hydrogen cyclosiloxane, in particular to tetramethyl cyclotetrasiloxane (abbreviated as D 4 H ) Preparation method of methylhydrocyclosiloxane with high yield. Background technique [0002] Methyl hydrogen cyclosiloxane is generally composed of methyl dichlorosilane (M 1 H) It is obtained by hydrolysis to generate mixed ring bodies and linear bodies of various molecular weights. Sauer et al. published a paper in J.Am.Chem.Soc.Vol.68.962 in 1946, and pointed out that using diethyl ether and crushed ice as solvents, methyldichlorosilane was hydrolyzed to prepare methylhydrocyclosiloxane (HMCS), The total yield of the ring body is 56.7%, and the remaining linear body is 43.3%. In USP 3,484,468, Curry et al. introduced the hydrolysis of M in tertiary alcohol and benzene. 1 H, the total yield of the ring body is up to 66%, and the linear body is 34%; in USP3763212, EcEnee et al. believe that hydrolysis in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 谢谋政章淑娥贺志江
Owner 蓝星安迪苏股份有限公司
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