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Synthesis method of methylhydro cyclo siloxane

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

Inactive Publication Date: 2005-05-25
蓝星安迪苏股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Synthesis method of methylhydro cyclo siloxane
  • Synthesis method of methylhydro cyclo siloxane
  • Synthesis method of methylhydro cyclo siloxane

Examples

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Effect test

Embodiment 1

[0021] Example 1 A method for preparing methylhydrocyclosiloxane with a high yield of tetramethylcyclotetrasiloxane, comprising silanes with the general formula RR'SiXX and alkanes in a volume ratio of 25-35 parts: 50 The ratio of -70 parts is mixed, gradually dropped into the mixed multiphase mixed solvent system, and stirred, and the hydrolysis reaction is carried out. The volume ratio of the multiphase 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 siloxane By-products, in the general formula RR'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.

[0022] The structural formula of RR'SiXX is

[0023]

Embodiment 2

[0024] Embodiment 2: The silane material of RR'SiXX general formula is methyl dichlorosilane. All the other are with embodiment 1.

Embodiment 3

[0025] Embodiment 3: The volume ratio composition of the mixed solvent is, alkane: alcohol: water=60-65 parts: 10-12 parts: 20-25 parts. All the other are with embodiment 1.

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Abstract

The present invention relates to a kind of preparation method of methylhydrogen cyclosiloxane, especially relate to tetramethyl cyclotetrasiloxane (being called for short D 4 H ) A method for the preparation of methylhydrocyclosiloxane with high yield. In this preparation method, the silane substance having the general formula RR'SiXX and the alkane are mixed in proportion, gradually dropped into the multi-phase mixed solvent system mixed with each other, and stirred, and the hydrolysis reaction is carried out, and the reaction time is 2-8 hours. Reaction temperature: 0-30°C, to obtain methylhydrocyclosiloxane products containing tetramethylcyclotetrasiloxane and linear siloxane by-products. The present invention has ring body and D 4 H The yield is high, and the molecular weight distribution is narrow, and the D in the mixed ring body 4 H The equilibrium concentration is high, the amount of methanol is small, the solvent is recovered, recycled, and pollution-free. The by-product line can also be recycled to hydrolysis for reuse. Therefore, this method basically has no by-products and has high economic benefits.

Description

technical field [0001] The present invention relates to a kind of preparation method of methylhydrogen cyclosiloxane, especially relate to tetramethyl cyclotetrasiloxane (being called for short D 4 H ) A method for the preparation of high-yield methylhydrocyclosiloxanes. Background technique [0002] Methylhydrocyclosiloxane is generally composed of methyldichlorosilane (M 1 H) Obtained by hydrolysis to generate mixed ring bodies and line bodies of various molecular weights. Sauer et al. published a paper in J.Am.Chem.Soc.Vol.68.962 in 1946, pointing out that diethyl ether and crushed ice were used as solvents to prepare methylhydrogencyclosiloxane (HMCS) by hydrolysis of methyldichlorosilane. The total yield of cyclic body is 56.7%, and the remaining linear body is 43.3%; in USP 3,484,468, Curry et al. introduced hydrolysis of M in tertiary alcohol and benzene 1 H, the total yield of the cyclic body is up to 66%, and the linear body is 34%; in USP3763212, EcEnee et al. ...

Claims

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Application Information

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Patent Type & Authority Patents(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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