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New technology of synthesizing dimethyldichlorosilance

A technology of dimethyldichlorosilane and methyltrichlorosilane, applied in the field of synthesizing dimethyldichlorosilane, can solve the problems of difficult large-scale utilization, direct discharge or incineration, immature technology, etc., and achieve production efficiency Improved, reduced emissions, simple process operation

Active Publication Date: 2014-04-09
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Low boilers are mixtures of by-products with a boiling point below 40°C, of ​​which the useful components are mainly Me 4 Si and Me 2 SiHCl, but it is difficult to be used on a large scale due to the close boiling points and difficult separation of the components
At present, there are few patents and literature reports on the utilization of low boiling substances. Foreign countries mainly use low boiling substances to produce fumed silica, but the domestic technology is immature, so they can only be directly discharged or incinerated.

Method used

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  • New technology of synthesizing dimethyldichlorosilance

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Experimental program
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Effect test

Embodiment 1

[0034] Add methyltrichlorosilane and trimethylchlorosilane to the raw material tank, and feed them to the preheating section of the fixed bed reactor with nitrogen gas. The temperature in the preheating section is 150°C. After the raw materials are vaporized, they enter the fixed bed reaction section with a diameter of φ25mm , the reaction section is filled with AlCl 3 Immobilized γ-Al 2 o 3 Immobilized catalyst, the temperature of the reaction section is 250°C, the reaction pressure (gauge pressure) is 0 Mpa; the residence time is 40s, the product after the reaction is cooled by the condenser, collected, sampled, analyzed and weighed, and a small amount of tail gas is absorbed with alkali solution. The samples were analyzed by gas chromatography, and the data are shown in Table 1.

[0035] The molar ratio of methyltrichlorosilane to trimethylchlorosilane is methyltrichlorosilane:trimethylchlorosilane=1:1;

[0036] The AlCl 3 Immobilized γ-Al 2 o 3 The dosage of the immo...

Embodiment 2

[0038] Add methyltrichlorosilane and trimethylchlorosilane to the raw material tank, and feed them to the preheating section of the fixed bed reactor with nitrogen gas. The temperature in the preheating section is 150°C. After the raw materials are vaporized, they enter the fixed bed reaction section with a diameter of φ25mm , the reaction section is filled with AlCl 3 Immobilized γ-Al 2 o 3 Immobilized catalyst, the temperature of the reaction section is 300°C, the reaction pressure (gauge pressure) is 0.6 Mpa; the residence time is 30s, the product after the reaction is cooled by the condenser, collected, sampled, analyzed and weighed, and a small amount of tail gas is absorbed with alkali solution. The samples were analyzed by gas chromatography, and the data are shown in Table 1.

[0039] The molar ratio of methyltrichlorosilane to trimethylchlorosilane is methyltrichlorosilane:trimethylchlorosilane=1.5:1;

[0040] The AlCl 3 Immobilized γ-Al 2 o 3 The dosage of the ...

Embodiment 3

[0042]Add methyltrichlorosilane and trimethylchlorosilane or methyltrichlorosilane and low boilers into the raw material tank, and at the same time add the mixture of zinc chloride and tin chloride, and feed it to the fixed-bed reactor with nitrogen to preheat Section, all the other are with embodiment 2;

[0043] The mass ratio of each component in the mixture of zinc chloride and tin chloride is zinc chloride:tin chloride=1.15:1, and the amount of the mixture of zinc chloride and tin chloride is methyltrichlorosilane and 10ppm of the total amount of trimethylchlorosilane.

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Abstract

The invention relates to a new technology of synthesizing dimethyldichlorosilance with methyl chlorosilane byproducts through disproportionation. The method comprises the following steps: by taking gama-Al2O3 immobilized AlCl3 as a catalyst, simultaneously adding the mixture of zinc chloride and stannic chloride, or adding methyl trichlorosilane and trimethylchlorosilane in a raw material tank at a low-boiling point, feeding to a preheating section with nitrogen, gasifying raw materials to enter a reaction section, keeping the temperature of the reaction section to be 200-400 DEG C, wherein the reaction pressure is 0-0.6 MPa; standing for 10-40s, cooling products through a condenser after reaction, feeding monomers after being cooled in a collection tank, and absorbing tail gas with alkali liquor. The new technology has the advantages that the content of dimethyldichlorosilance synthesized through the technology is higher than the level of existing patents and related articles; and moreover, the technology is simple in operation, can effectively reduce the emission of three wastes, and can continuously process methyl chlorosilane by products in a large scale.

Description

technical field [0001] The invention relates to a new process for synthesizing dimethyldichlorosilane, in particular to a new process for synthesizing dimethyldichlorosilane by disproportionation of by-products of methylchlorosilane. Background technique [0002] Methyl chloride and silicon powder can directly synthesize methylchlorosilane crude monomer under the catalysis of copper powder, but in the direct method, besides dimethyldichlorosilane, other by-products will be generated, such as 7-8% high boilers (boiling point over 70°C), 4-5% low boilers (boiling point below 40°C) of the total crude monomer, 5-15% of the crude product Chlorosilane, and trimethylchlorosilane and methylhydrochlorosilane with a content of less than 1%. Due to the limited application market of the above-mentioned by-products, and it is very easy to react with water in the air to form hydrogen chloride, which seriously pollutes the environment and greatly restricts the development of the methylchl...

Claims

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Application Information

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IPC IPC(8): C07F7/12B01J27/125
Inventor 谢谋证周俊刘达波邱玲白丽娜
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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