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Method for producing phenyl chlorosilane by direct method

A phenylchlorosilane and direct method technology, applied in the field of direct method production of phenylchlorosilane, can solve the problems of low ratio of diphenyldichlorosilane to phenyltrichlorosilane, difficult industrial production, complex process, etc. Achieve the effects of improving reactivity, reducing dosage and improving production efficiency

Active Publication Date: 2021-07-02
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the method for present direct method production phenylchlorosilane, there are following shortcoming: (1) the consumption of copper powder as catalyzer and the cupric chloride of cocatalyst, cupric oxide are bigger, generally account for 30-50% of contact mass (2) the condition that reduces catalyst consumption in some methods is to need to adopt quaternary copper powder, and catalyst is comparatively strict in production preparation, and technique is very complicated, is difficult to be applied to industrial production; (3) diphenyl dichlorosilane and benzene in the product The proportion of trichlorosilane is generally not high, and it is not very stable

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  • Method for producing phenyl chlorosilane by direct method

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Experimental program
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Effect test

Embodiment 1

[0038] The method that the direct method of present embodiment produces phenylchlorosilane comprises the following steps:

[0039] (1) Activation step: add silicon powder, CuCl, and potassium bifluoride to the reactor, the mass ratio of silicon powder to CuCl is 4:1, the molar ratio of potassium hydrogen fluoride to CuCl is 0.05:1, and nitrogen is introduced into the reactor at 280°C Activation at lower temperature for 4h, to obtain activated silicon-copper contacts;

[0040] (2) Reaction step: Pass the vaporized chlorobenzene into the fluidized bed reactor, and react with the activated silicon-copper contact obtained in step (1), the space velocity of the reactor is 0.1m / s, and the reaction temperature is 600°C , the pressure is 0.1MPa to prepare phenylchlorosilane; the reaction is stopped, and the distillate is rectified to obtain diphenyldichlorosilane, phenyltrichlorosilane, chlorobenzene and by-products.

Embodiment 2

[0042] The method that the direct method of present embodiment produces phenylchlorosilane comprises the following steps:

[0043] (1) Activation step: add silicon powder, CuCl, and potassium bifluoride to the reactor, the mass ratio of silicon powder to CuCl is 4:1, the molar ratio of potassium hydrogen fluoride to CuCl is 0.05:1, and nitrogen and hydrogen chloride gas are introduced into the reactor. Activation at 280°C for 4 hours to obtain activated silicon-copper contacts;

[0044] Wherein, the volume ratio of nitrogen and hydrogen chloride is 1:1.5, and the proportioning of potassium bifluoride and hydrogen chloride gas is 1g:10ml / min;

[0045] Step (2) of this embodiment is the same as step (2) of Embodiment 1.

Embodiment 3

[0047] The method that the direct method of present embodiment produces phenylchlorosilane comprises the following steps:

[0048] (1) Activation step: add silicon powder, CuCl, and potassium bifluoride to the reactor, the mass ratio of silicon powder to CuCl is 4.5:1, the molar ratio of potassium hydrogen fluoride to CuCl is 0.3:1, and nitrogen and hydrogen chloride gas are introduced into the reactor. Activate at 380°C for 1 hour to obtain an activated silicon-copper contact; wherein, the volume ratio of nitrogen to hydrogen chloride is 1:3.5, and the ratio of potassium bifluoride to hydrogen chloride gas is 1g:30ml / min;

[0049] (2) Reaction step: Pass the vaporized chlorobenzene into the fluidized bed reactor, and react with the activated silicon-copper contact body obtained in step (1), the space velocity of the reactor is 0.1m / s, and the reaction temperature is 450°C , and the pressure is 1 MPa to prepare phenylchlorosilane; stop the reaction, and rectify the distillate ...

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Abstract

The invention relates to a method for producing phenyl chlorosilane by a direct method, which comprises the following steps of: (1) activating: activating silicon powder and a copper catalyst by using metal hydrofluoride to obtain an activated silicon-copper contact body; and (2) reaction: reacting the activated silicon-copper contact body with chlorobenzene to prepare phenyl chlorosilane. Metal hydrofluoride is used for activating the silicon-copper contact body formed by silicon powder and the copper catalyst, the contact condition of chlorobenzene and the silicon-copper contact body is improved, the metal hydrofluoride is decomposed into hydrogen fluoride and metal fluoride salt at the activation temperature, and the two compounds both have an etching effect on the silicon powder and the copper catalyst, the silicon powder can be subjected to surface modification, so that adhesion of the copper catalyst on the silicon powder is facilitated, and the high-activity silicon-copper contact body is formed. Meanwhile, silicon dioxide on the surface of the silicon powder is etched, and the reaction rate of chlorobenzene and the silicon powder is increased.

Description

technical field [0001] The invention belongs to the technical field of organosilicon preparation, and in particular relates to a method for producing phenylchlorosilane by a direct method. Background technique [0002] The direct method of producing phenylchlorosilane refers to the reaction of silicon powder, catalyst and chlorobenzene in a stirred bed, fluidized bed or rotary kiln to generate phenyltrichlorosilane, diphenyldichlorosilane and triphenylchlorosilane . At present, the industrial production process is to use chlorobenzene and metal silicon powder as raw materials, use copper as the main catalyst, add co-catalyst silicon tetrachloride or hydrogen chloride, the reaction temperature is 450-600 ° C, the reaction pressure is 0.2-0.5 MPa, the amount of copper catalyst The ratio of the product diphenyldichlorosilane to phenyltrichlorosilane is about 0.3:1. [0003] Patent CN85102880 discloses the direct synthesis of phenylchlorosilane. The amount of copper catalyst a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/16
CPCC07F7/16
Inventor 廖立颜岭王海栋黄晓辉冷江子
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD