Method for preparing silane by disproportionating dichlorosilane

A technology for dichlorodihydrosilicon and silane, which is applied in the field of preparing silane by disproportionation of dichlorodihydrosilicon, can solve the problems of complex process and great difficulty, achieve simple system and equipment, improve production rate, improve production economic benefits and social effect of benefit

Active Publication Date: 2013-01-16
ZHEJIANG JINGGONG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process of this method is relatively complicated, and it is di...

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  • Method for preparing silane by disproportionating dichlorosilane

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Embodiment 1

[0024] The present invention adopts such as figure 1 The shown device carries out the disproportionation of dichlorodihydrosilane to prepare silane, and the device includes a dichlorodihydrosilane storage tank 1, a reaction kettle 2 and a rectification tower 3 which are successively connected by pipelines, and the reaction kettle 2 is successively the bottom of the kettle from bottom to top Section 21, heating section 22, a plurality of catalytic reaction sections 23 and kettle top section 24 arranged at intervals in the reactor, heating section 22 has 4-8 dichlorodihydrosilane inlets, and dichlorodihydrosilane storage tank 1 passes through The pipeline is connected with the inlet of dichlorodihydrosilane, the bottom of the bottom section 21 has an inlet at the bottom of the kettle, the top of the top section 24 has an outlet at the top of the kettle, the middle part of the rectifying tower 3 and the top of the first baffle at the bottom have a material inlet, and the top of th...

Embodiment 2

[0034] The device and method that adopt are with embodiment 1, and difference is:

[0035] Mixed chlorosilane raw material composition: monochlorosilane: dichlorodihydrosilane: trichlorosilane=35:70:1 (molar ratio). The feed rate of mixed chlorosilane is 9.6t / h. There are 4 catalytic reaction sections in the reactor, and the filling height of each section is 1200mm. The catalyst in this example is obtained by mixing a solid amine-based macroporous resin (Rohm and Haas IRA402) and an organic amine at a ratio of 2:1 (molar ratio). Composite catalyst, composite catalyst is more effective than single-component catalyst, reducing the activation energy of the reaction, thereby accelerating the disproportionation reaction of dichlorodihydrosilane. The average particle diameter of the loaded solid amine-based macroporous resin is 0.5-0.8mm.

[0036] The temperature in the reaction kettle is controlled at 60°C, and the operating pressure is 3.0MPa. The top of the reaction kettle is m...

Embodiment 3

[0039] The device and method that adopt are with embodiment 1, and difference is:

[0040] Mixed chlorosilane raw material composition: monochlorosilane: dichlorodihydrosilane: trichlorosilane=35:70:1 (molar ratio). The feed rate of mixed chlorosilane is 9.6t / h. There are many sections of catalytic reaction sections in the reactor, and the filling height of each section is 1000mm, and the catalyst is the same as in Example 2. The temperature in the reaction kettle is controlled at 60°C, and the operating pressure is 3.0MPa. The top of the disproportionation reaction kettle is mainly silane and monochlorosilane gas entering the rectification tower, and the middle part of the disproportionation reaction kettle is mainly unreacted dichlorodihydrosilane, a small amount of three Chlorosilane and a small amount of monochlorosilane enter the rectification tower.

[0041] The rectification tower is a plate tower with 70 layers of trays, the operating pressure is 2.9MPa, the temperat...

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Abstract

The invention relates to the technical field of preparation and purification of silane, in particular to a method for preparing silane by disproportionating dichlorosilane. The method comprises the following steps of: putting chlorosilane of which the main component is the dichlorosilane into a disproportionation reaction tower; and feeding a reaction product into a catalytic reaction and then fed into section rectification column for separating to obtain silane gas at the temperature of 30 to 100 DEG C, wherein macroporous anion exchange resins and organic amine composite catalyst are filled in the catalytic reaction section. By the method, the conversion rate of the dichlorosilane is greatly improved and up to over 25 percent; and a by-product, namely the dichlorosilane produced during polysilicon production is converted to the silane, so that the utilization rate of raw materials is increased, emission of waste water, waste residues and waste gas is reduced, and economic benefits and social benefits are improved during polysilicon production.

Description

technical field [0001] The invention relates to the technical field of silane preparation and purification, in particular to a method for preparing silane by disproportionation of dichlorodihydrosilane. Background technique [0002] Crystalline silicon materials (including polysilicon and monocrystalline silicon) are the most important photovoltaic materials. At present, the polysilicon production process of most enterprises in my country is the improved Siemens method. This process uses trichlorosilicon as raw material, and some secondary Chlorodihydrosilane and a large number of by-products of silicon tetrachloride. For silicon tetrachloride, it has been treated by cold hydrogenation and other methods to make it re-converted into trichlorosilane for reuse; for dichlorodihydrogen silicon, there is no mature technology to effectively utilize it in China at this stage, even if only The leaching process for the purpose of tail gas treatment also has a large material consumptio...

Claims

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Application Information

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IPC IPC(8): C01B33/04
Inventor 李波宫有圣汤川・理查德
Owner ZHEJIANG JINGGONG NEW MATERIAL TECH
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