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Method for preparing chloromethyl trichlorosilane

A technology of monochloromethyltrichlorosilane and a condensing device, which is applied in the fields of compounds, chemical instruments and methods, organic chemistry, etc. , the reaction time is too long and other problems to achieve the effect of improving the conversion rate

Active Publication Date: 2015-12-30
山东时代新材料科技有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0009] In 2001, Jiang Biao, Xie Deliang and others reported "Method and device for preparing chloromethylchlorosilane by gas phase chlorination" (public number: CN1317488A), and provided a preparation method of chloromethylchlorosilane: the molecular formula is CH 3 Si(CH 3 ) m Cl 3-m The methyl chlorosilane as raw material, the Cl 2 It is directly passed into the reaction zone, mixed with the gasified raw material gas, and the gas-phase chlorination reaction is carried out only by indoor general visible light irradiation, so as to obtain higher yields of chloromethylchlorosilane. According to reports, the molar ratio of raw material gas to chlorine gas is 1: 0.1~0.75, the reaction temperature is 50~80℃, and the reaction time is 1~24h, but this method and equipment still face many problems: chlorine gas directly enters the reaction zone, and the amount of reactants is not easy to control; according to the patent description, a There is no distinction between chlorinated products and polychlorinated products, only the total conversion rate of chlorination reaction is pursued; the reaction time is too long; the surface of the reactor must be cleaned regularly to remove the generated polymer; in some cases it is possible Spontaneous combustion or explosion of the reactants occurs; after the reaction, the product needs to be moved to the still for difficult distillation separation

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  • Method for preparing chloromethyl trichlorosilane

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Embodiment 1

[0032] A glass tube with a wall thickness of 2-10mm made of quartz glass is used as the reactor 6; prepare a chlorine cylinder 1, a buffer tank 2, a flow meter 3, an evaporation kettle 4, and a rectification tower 5 (the number of plates is 9-15). ), condensing device 7 (condenser), alkali washing tower 8 and finished product tank 9; rectifying tower 5 is filled with glass spring or polytetrafluoroethylene silk wave packing, and the number of trays of rectifying tower 5 is 9-15 ; The outer surface of the evaporation kettle 4 is covered with opaque material, and the outer surface of the rectifying tower 5 is covered with an opaque heating layer (heating device 10). The chlorine gas bottle 1 is connected with the buffer tank 2, and the buffer tank 2 is connected with the evaporating kettle 4 through a vent pipe; the end of the vent pipe leads to the bottom of the evaporating kettle 4, and a flow meter 3 is installed on the vent pipe; , the top of the rectification tower 5 is con...

Embodiment 2

[0035] Gas-phase chlorination reaction device such as figure 1 As shown; a 500W incandescent lamp illuminates the reactor 6. The reflux condensing device is opened in advance, no cooling medium is required; Cl 2 The molar ratio to methyltrichlorosilane is 1:15 (Cl 2 The molar ratio to methyltrichlorosilane refers to the molar ratio of 5 kg of methyltrichlorosilane and the total amount of chlorine gas introduced). 5kg methyltrichlorosilane was added to the evaporating kettle 4, electromagnetic stirring was turned on, the evaporating kettle 4 was heated, and the heating device 10 of the rectifying tower 5 was opened simultaneously; Make chlorine pass into below the liquid level of methyltrichlorosilane through buffer tank 2; control the heating speed of evaporation kettle 4, make the backflow moderate, adjust the flow meter 3 to control the chlorine flow simultaneously, make the reaction speed not too violent, control the heating of the heating device 10 speed so that the tem...

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Abstract

The invention relates to a device for preparing chloromethyl trichlorosilane, belonging to the technical field of organic synthesis. The device is characterized in that an evaporation kettle is connected with a vent pipe; the tail end of the vent pipe is below the liquid level of a material in the evaporation kettle; a heating device is arranged outside a rectifying tower; a liquid return pipe of a condensing device is connected with the upper part of the rectifying tower and a finished product tank respectively; the evaporation kettle and the rectifying tower are lighttight; and a reactor is non-lighttight. The device has the beneficial effects that full mixing of chlorine and methyl trichlorosilane steam can be ensured as the tail end of the vent pipe is below the liquid level of the material in the evaporation kettle, and meanwhile, the mole ratio of Cl2 to CH3SiCl3 can be effectively controlled, thus increasing the conversion rate of methyl trichlorosilane; the rectifying tower is connected between the reactor and the evaporation kettle, the evaporation kettle can be directly heated to carry out distillation operation after reaction is completed, that is, the reaction device is a product separation device, so that the device is unnecessary to be replaced; and therefore due to existence of the rectifying tower, the danger occurrence probability is greatly reduced, the operation is simpler and the labor and time costs are reduced.

Description

technical field [0001] The invention relates to a device for preparing monochloromethyltrichlorosilane, belonging to the technical field of organic synthesis. Background technique [0002] Chloromethyltrichlorosilane is the most important raw material for the preparation of α-functional silane coupling agents. Compared with γ-functional silane coupling agents, α-functional silane coupling agents have the advantages of readily available raw materials, lively properties, and heat resistance. Good performance and other advantages, with a wider range of applications. [0003] Scholars from various countries have studied the synthesis of ClCH by chlorination 2 SiCl 3 A variety of methods have been tried, mainly liquid-phase chlorination, gas-phase photochlorination, and gas-phase thermal chlorination. [0004] When using azobisisobutyronitrile as the liquid phase method of the initiator, the product ClCH 2 SiCl 3 , Cl 2 CHSiCl 3 The chlorination rate is faster than that of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12
Inventor 马庆宇李建权杨冰雪关瑞芳
Owner 山东时代新材料科技有限公司
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