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Preparation method of chloromethyl-methyl-dimethylsilane

A technology of chloromethylmethyldimethoxysilane and chloromethylmethyldichlorosilane, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc., and can solve the conditions Harshness, low reaction temperature, long reaction process cycle time, etc., to achieve the effect of easy operation

Active Publication Date: 2009-06-17
HANGZHOU ZHIJIANG SILICONE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above synthetic processes or the reaction temperature is too low, the reaction process cycle time is long, the conditions are harsh, or the experimental process involves problems such as low yield and complicated post-processing.

Method used

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  • Preparation method of chloromethyl-methyl-dimethylsilane
  • Preparation method of chloromethyl-methyl-dimethylsilane
  • Preparation method of chloromethyl-methyl-dimethylsilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] First, inject chloromethylmethyldichlorosilane (400mol) into the storage tank, then mix trimethyl orthoformate (800mol) and methanol (200mol) in the reaction kettle, and at 50°C, the chloromethyl Methyldichlorosilane was added to the reaction kettle for 1 hour; after atmospheric distillation, fractions were collected at 140-143°C to obtain 60.4 kg of chloromethylmethyldimethoxysilane with a yield of 98%. Purity 100% (GC). Chloromethane and methyl formate gases released during the reaction were collected by cryogenic cold traps.

Embodiment 2

[0026] First, chloromethylmethyldichlorosilane (51 liters) is injected into the storage tank, then trimethyl orthoformate (109 liters) and methanol (0.8 liters) are mixed in the reactor, and at 40 ° C, the Chloromethylmethyldichlorosilane was added to the reaction kettle for 4 hours; after atmospheric distillation, fractions were collected at 140-143°C to obtain 60 kg of chloromethylmethyldimethoxysilane with a yield of 97%, purity 99% (GC). Chloromethane and methyl formate gases released during the reaction were collected by cryogenic cold traps.

Embodiment 3

[0028] First, chloromethylmethyldichlorosilane (51 liters) is injected into the storage tank, then trimethyl orthoformate (91.5 liters) and methanol (3.2 liters) are mixed in the reactor, and at 90 ° C, the Chloromethylmethyldichlorosilane was added to the reaction kettle for 30 minutes; after atmospheric distillation, fractions were collected at 140-143°C to obtain 59 kg of chloromethylmethyldimethoxysilane with a yield of 96%, purity 100% (GC). Chloromethane and methyl formate gases released during the reaction were collected by cryogenic cold traps.

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Abstract

The invention relates to a method for preparing chloromethyl methyl dimethoxysilane. The current method has the problems of long cycle time of the reaction process, harsh conditions, and complicated reprocessing, and so on. In the invention, the method comprises the following steps: firstly, injecting the chloromethyl methyl dimethoxysilane into a storage tank; secondly, mixing methyl ortho formate and methanol in a reaction kettle, and adding the chloromethyl methyl dimethoxysilane into the reaction kettle at a temperature of between 40 and 90 DEG C for 0.5 to 4 hours; obtaining the chloromethyl methyl dimethoxysilane after atmospheric distillation; and collecting gas of methyl chloride and methyl formate released in the reaction process by a cryotrap. The method of the invention has the advantages of mild reaction condition, high yield, short reaction process, and easily operated feeding and post treatment, thereby easily realizing large scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a preparation method of a silane coupling agent intermediate, in particular to a preparation process of chloromethylmethyldimethoxysilane. Background technique [0002] In 2005, the new generation of organofunctional α-silanes launched by WACKER, Germany, replaced the traditional propylene bridges with methylene bridges, making the silanes very easy to undergo chemical reactions, thus promoting better than traditional commercial silanes. The hydrolysis and concentration process of silicon alkoxide, this super effect can be used to produce new fast curing sealants and adhesives. The relevant product brands are XL42, XL65, STP-E10, STP-E30, and the CAS registration numbers are 406679-89-8, 23432-65-7, 611222-18-5 and 611222-18-5 respectively. Chloromethylmethyldimethoxysilane (CAS Registry No. 2212-11-5) is a key intermediate for the above-mentioned α-silane product derivat...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 林旭锋李国亮陶小乐王彦广何永富
Owner HANGZHOU ZHIJIANG SILICONE CHEM
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