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Method for producing trichlorosilane

一种三氯硅烷、制造方法的技术，应用在卤代硅烷、化学仪器和方法、硅化合物等方向，能够解决三氯硅烷转化率降低等问题，达到使用量降低、降低制造成本的效果

Active Publication Date: 2012-10-24
TOKUYAMA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0024] However, the above-mentioned method has the following fatal problem: since the two reactions with different reaction conditions must be carried out at the same time, it is impossible to avoid adverse situations such as the reduction of the conversion rate of trichlorosilane.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0098] Metallic silicon having a boron content of 0.03% by weight, an Fe content of 0.51% by weight, and an Al content of 0.32% by weight was prepared as a production raw material.

[0099] the first manufacturing process;

[0100] In a fluidized bed reactor made of stainless steel with an inner diameter of 298 mm, hydrogen chloride was reacted with the metal silicon to produce trichlorosilane.

[0101] That is, 18 kg of the above-mentioned metallic silicon was charged into the above-mentioned reactor, and then 17 kg (460 mol) / hr of hydrogen chloride and 0.91 kg (460 mol) / hr of hydrogen gas were mixed and supplied to the reactor. At this time, the reaction temperature was set at 350° C., and the above-mentioned metal silicon was supplied at a rate of 4.3 kg (150 mol) / hr under atmospheric pressure.

[0102] The reaction product gas discharged from the above-mentioned reactor was cooled by a heat exchanger, pressurized to 650 kPaG by a compressor, and further cooled to -30°C to...

Embodiment 2）

[0126] Metallic silicon having a boron content of 0.1% by weight, an Fe content of 0.51% by weight, and an Al content of 0.32% by weight was prepared as a production raw material.

[0127] In the same manner as in Example 1 except that the metal silicon described above was used, the first manufacturing step and the second manufacturing step were continuously implemented for 50 hours. The condensate of chlorosilanes obtained in each step was mixed and analyzed. As a result, the composition is shown below.

[0128] Dichlorosilane 0.3% by weight

[0129] Trichlorosilane 26.7% by weight

[0130] Tetrachlorosilane 73.0% by weight

[0131] In addition, the boron concentration was 1300 ppma, and no large fluctuation was observed in the experiment.

[0132] In addition, thereafter, high-purity trichlorosilane is obtained by distillation. The boron concentration is less than 1ppba.

reference example 1）

[0134] In the second production process, the first production process and the second production process were carried out in exactly the same manner as in Example 1 except that pure hydrogen gas was used instead of exhaust gas from the first production process as hydrogen gas.

[0135] As a result, the composition of the off-gas from which the chlorosilanes were condensed and removed from the reaction product gas discharged from the reactor in the first production step was as follows.

[0136] Hydrogen: 99.0% by volume

[0137] Chlorosilane: 1.0% by volume

[0138] Dichlorosilane 0.1% by volume

[0139] Trichlorosilane 0.8% by volume

[0140] Tetrachlorosilane 0.1% by volume

[0141] Furthermore, exactly the same as Example 1, the 1st manufacturing process and the 2nd manufacturing process were implemented continuously for 50 hours. The condensate of chlorosilanes obtained in each step was mixed and analyzed. As a result, the composition is shown below.

[0142] Dichlorosi...

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Abstract

Disclosed is a method for commercially producing trichlorosilane in an efficient manner by effectively re-using the exhaust gas which remains after trichlorosilane has been condensed and separated from reaction product gas, when trichlorosilane is produced by means of a reaction between metallic silicon and hydrogen chloride. The disclosed production method independently includes a first production process wherein trichlorosilane is generated by reacting hydrogen chloride in metallic silicon, and a second production process wherein trichlorosilane is generated by reacting trichlorosilane and hydrogen in metallic silicon, and is characterised in that trichlorosilane is condensed and separated from the trichlorosilane-containing reaction product gas obtained by means of the first production process, and the exhaust gas which remains after the trichlorosilane has been condensed and separated is supplied to the second production process as a hydrogen source.

Description

technical field [0001] The present invention relates to a process for the manufacture of trichlorosilane. More specifically, it relates to a method for producing trichlorosilane including two different production steps of reacting hydrogen chloride and metal silicon to produce trichlorosilane, and reacting tetrachlorosilane and hydrogen with metal The process of producing trichlorosilane by reacting silicon. Background technique [0002] Trichlorosilane (SiHCl 3 ) is a compound useful as a raw material for polysilicon production, and high-purity polysilicon is precipitated by reacting with hydrogen gas at a high temperature of 1000°C or higher. This reaction is mainly represented by the following formulas (1) and (2). [0003] 4SiHCl 3 →Si+3SiCl 4 +2H 2 (1) [0004] SiHCl 3 +H 2 →Si+3HCl (2) [0005] Such trichlorosilanes are generally produced by reacting metallic silicon with hydrogen chloride. For example, Patent Document 1 discloses a method of producing tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/107
CPCC01B33/10763C01B33/1071C01B33/10736
Inventor 秋吉彩生相本忠
Owner TOKUYAMA CORP