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Method for removing trace phenyl trichloride in methyl phenyl dichlorosilane

A technology of methylphenyldichlorosilane and phenyltrichloride, which is applied in the direction of chemical instruments and methods, silicon organic compounds, compounds of group 4/14 elements of the periodic table, etc., can solve problems such as secondary pollution, and achieve The effect of reducing the generation of waste liquid, easy realization, and overall energy consumption reduction

Inactive Publication Date: 2022-08-09
熵联节能科技(江苏)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Under these conditions, phenyltrichlorosilane will preferentially react with water to produce silanol, and finally form high-boiling oligomers, which will not be distilled out during rectification, so as to achieve the goal of purifying methylphenyldichlorosilane by rectification. purpose, the disadvantage is that a large amount of solvents are used to cause secondary pollution to the materials, and toxic acetonitrile and other substances are used at the same time

Method used

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  • Method for removing trace phenyl trichloride in methyl phenyl dichlorosilane
  • Method for removing trace phenyl trichloride in methyl phenyl dichlorosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Add 1KG of 98% methylphenyldichlorosilane to a 2000ml three-necked flask, insert a glass capillary, connect the capillary to the conical flask, open two holes in the flask stopper, insert a glass tube, and add an appropriate amount to the conical flask. Methanol, insert the gas inlet glass tube below the liquid level, turn on nitrogen gas, pass nitrogen gas into the three-necked flask, and discharge the tail gas after washing with water. Timing 2 hours. After weighing, methanol was reduced by 2.2 g. Through simple rectification in a laboratory glass rectification tower, 900 g of methylphenyldichlorosilane was obtained, and the purity was 99.2% through gas chromatography analysis. The calculated yield was 90%.

Embodiment 2-4

[0036] In embodiment 2-4, except changing nitrogen feeding time, operate in the same way as embodiment 1, and specific process conditions and relative product yield are shown in the following table:

[0037] serial number Nitrogen passing time Distillation product purity yield 1 (Example 2) Pass nitrogen for 3 hours 99.4％ 93％ 2 (Example 2) Passing nitrogen gas for 4 hours 99.5％ 95％ 3 (Example 2) Pass nitrogen for 5 hours 99.5％ 90％

Embodiment 5

[0039] Add 1KG of 98% methylphenyldichlorosilane to a 2000ml three-necked flask, insert a glass capillary, connect the capillary to the conical flask, open two holes in the flask stopper, insert a glass tube, and add an appropriate amount to the conical flask. pure water, insert the gas inlet glass tube below the liquid level, turn on nitrogen gas, pass nitrogen gas into the three-necked flask, and discharge the exhaust gas after washing with water. Timing 2 hours. After weighing, pure water was reduced by 1.8g. Through simple rectification in a laboratory glass rectifying tower, 910 g of methylphenyldichlorosilane was obtained, and the purity was 99.0% by gas chromatography analysis. The calculated yield was 91%.

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Abstract

The invention relates to a method for removing trace phenyl trichloride in methyl phenyl dichlorosilane, which utilizes the characteristic that one chlorine of the phenyl trichloride is substituted or the reaction activity is higher than that of other chlorine in a system, and the phenyl trichloride can be subjected to esterification reaction preferentially in the presence of trace methanol. According to the method, phenyl methoxy dichlorosilane is generated after one chlorine is esterified, the boiling point difference between the formed product and methyl phenyl dichlorosilane is large, the methyl phenyl dichlorosilane can be purified through a conventional rectification method, and the purity of the methyl phenyl dichlorosilane can be increased to 99% or above through a common rectification device.

Description

Technical field: [0001] The invention relates to a method for removing trace amounts of phenyltrichloride in methylphenyldichlorosilane, and further relates to a method and a device for removing trace amounts of phenyltrichloride in methylphenyldichlorosilane by chemical method. Background technique: [0002] When using the thermal shrinkage method to synthesize methylphenyldichlorosilane, a by-product phenyltrichlorosilane will be produced, both of which are important raw materials of organosilicon monomers, but due to their similar boiling points, they are 205.0°C (101.3KPa) respectively. and 201.0°C (101.3KPa), it is quite difficult to obtain high-purity methylphenyldichlorosilane by separating the components with high boiling point temperature and such close boiling point by ordinary distillation separation. The above-purity methylphenyldichlorosilane has relatively high requirements on the tower, the theoretical plate number of the tower is greater than 160 and the refl...

Claims

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Application Information

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IPC IPC(8): C07F7/12C07F7/20
CPCC07F7/12C07F7/20
Inventor 朱恩俊匡玉根莘振东单学凌邓柱明
Owner 熵联节能科技(江苏)有限公司
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