Method for synthesizing bromotrimethylsilane

A technology of trimethylbromosilane and synthesis method, which is applied in the field of chemical synthesis of trimethylbromosilane, can solve problems such as difficult separation, high reaction temperature, and many by-products, and achieve shortened reaction time, good catalytic effect, and reduced usage volume effect

Active Publication Date: 2011-08-17
扬州三友合成化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. Hexamethyldisilane method: Me 3 SiSiMe 3 +Br 2 → 2Me 3 SiBr, the product yield of this method is high, but the reaction is violent and difficult to control, and it is prone to explosion. In addition, the raw material hexamethyldisilane is expensive, and it has gradually lost the significance of industrial production
[0005] 2. Silicone ether—aluminum powder method: Me 3 SiOSiMe 3 +Br 2 + 2/3 Al → 2Me 3 SiBr + 1/3 Al 2 o 3 , the reaction temperature of this method is high, there are many by-products and it will solidify at about 120°C, which is difficult to handle. The product contains about 15% of dimethyldibromosilane, which is difficult to separate and affects the use of the product
[0006] 3. Silicon ether—triphenylphosphine method: Me 3 SiOSiMe 3 +Br 2 + Ph 3 P → 2Me 3 SiBr + Ph 3 PO, the raw material triphenylphosphine used in this method is expensive, and the by-pro

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0025] Example 1: Adopt iron tribromide to be the embodiment of catalyst

[0026] Pump 1800kg (6.65kmol) of phosphorus tribromide and 721kg (4.45kmol) of silicon ether into a dry 2000L enamel electric kettle with a condensing reflux system, and add 3kg (0.01kmol) of tribromide from the solid feeding port. Iron oxide, replace the closed system with nitrogen for 3 to 5 times, so that the entire material and its reaction process are under the protection of nitrogen atmosphere.

[0027] Turn on the stirring at one point, heat through the jacket steam, gradually increase the temperature to 100°C±5°C, and keep the temperature at reflux for 6±0.5 hours. 5m ordinary enamel rectification tower section), when the temperature in the kettle rises to 130-135 ℃, the rectification is stopped to obtain 1270kg (8.25kmol) of bromotrimethylsilane product with a content of more than 99%, and the yield of one rectification is 92.7% (calculated as silicon ether).

[0028] Recover excess phosphoru...

example 2

[0031] Example 2: Catalyst-free embodiment

[0032] Pump 1800kg (6.65kmol) of phosphorus tribromide and 721kg (4.45kmol) of silicon ether into a dry 2000L enamel electric kettle with a condensing reflux system in sequence, and replace the closed system with nitrogen for 3 to 5 times to make the whole The materials and their reaction process are under the protection of nitrogen atmosphere.

[0033]Turn on the stirring at one point, heat through the jacket steam, gradually increase the temperature to 100°C±5°C, and keep the temperature at reflux for 6±0.5 hours. 5m ordinary enamel rectification tower section), when the temperature in the kettle rises to 130-135 ℃, the rectification is stopped, and 1110kg (7.25kmol) of trimethylbromosilane product with a content of more than 99% is obtained, and the yield of one rectification is 81.5% (calculated as silicon ether).

[0034] Change to distillation to recover excess phosphorus tribromide, stop the distillation when the temperatur...

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PUM

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Abstract

The invention discloses a method for synthesizing bromotrimethylsilane, and relates to a synthetic production technology for a chemical product. The method comprises the following steps of: under oxygen-free conditions, stirring in a reaction kettle in which phosphorus tribromide and silyl ether are sequentially added, raising the temperature to 1005 DEG C, keeping the temperature, performing reflux reaction for 60.5 hours, rectifying under normal pressure to obtain the bromotrimethylsilane, and stopping to receive a finished product of the bromotrimethylsilane when the temperature in the kettle is raised to 135 DEG C. By the method, a silyl ether-phosphorus tribromide method is improved and innovated, side reactions are avoided, the obtained product has purity, and the finished product of the bromotrimethylsilane which has the content of about 99 percent can be obtained; and the stirring at normal temperature is changed into high-temperature reflux, so that the reaction time is greatly shortened.

Description

technical field [0001] The invention relates to the technical field of production of chemical products, in particular to a method for chemically synthesizing bromotrimethylsilane. Background technique [0002] Trimethylbromosilane is a new type of organosilicon synthesis reagent, which is mainly used in the synthesis of antiviral drugs. PMPA) is an essential raw material. [0003] There are several synthetic methods reported in the literature as follows: [0004] 1. Hexamethyldisilane method: Me 3 SiSiMe 3 +Br 2 → 2Me 3 SiBr, the product yield of this method is high, but the reaction is violent and difficult to control, and it is prone to explosion. In addition, the raw material hexamethyldisilane is expensive, and it has gradually lost the significance of industrial production. [0005] 2. Silicone ether—aluminum powder method: Me 3 SiOSiMe 3 +Br 2 + 2 / 3 Al → 2Me 3 SiBr + 1 / 3 Al 2 o 3 , the reaction temperature of this method is high, there are many by-pr...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 李明成张扬张众笑李辉宁
Owner 扬州三友合成化工有限公司
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