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Process for preparing silane by magnesium silicide method

A technology of magnesium silicide and silane, applied in the field of improved technology for preparing silane, can solve problems such as high labor intensity, poor safety, environmental pollution, etc., and achieve the effects of increasing production capacity, stabilizing silane gas volume, and reducing production costs.

Active Publication Date: 2010-08-11
JIANGSU YANGNONG CHEM GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a magnesium silicide method for continuous production of silane in order to solve the problems of high labor intensity, poor safety, low yield, high energy consumption, and serious environmental pollution in the existing small-scale batch production of silane in the existing magnesium silicide method. A method comprising the steps of:

Method used

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  • Process for preparing silane by magnesium silicide method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 Preparation of 3-stage silane generator in series and continuous silane

[0032] Before silane is generated, replace the entire reaction system with nitrogen gas, and replace the oxygen in the reaction system cleanly;

[0033] After oxygen replacement, liquid ammonia is pumped from the buffer tank into the batching tank 3 at 80 parts per hour, the vaporized ammonia is condensed by the condenser 4 and then returned to the batching tank 3, and ammonium chloride is passed through the high tank 1 at 20 parts per hour. The screw feeder 2 is added to the batching kettle 3 to prepare a 20% ammonium chloride liquid ammonia solution;

[0034] The prepared ammonium chloride liquid ammonia solution is fed into the first-stage silane generator 8 at 100 parts per hour through the pump 5, and at the same time, the magnesium silicide in the magnesium silicide high tank 6 is 6.9 parts per hour (magnesium silicide and ammonium chloride The molar ratio is 1:4.1) The magnesium silicid...

Embodiment 2

[0039] The process flow is the same as in Example 1, except that the amount of liquid ammonia added per hour in Example 1 is changed from 80 parts to 106.7 parts (prepared to 15% ammonium chloride liquid ammonia solution), and other conditions remain unchanged. The yield of the final product silane relative to magnesium silicide was 92.6%.

Embodiment 3

[0041] The process flow is the same as in Example 1, except that the amount of liquid ammonia added per hour in Example 1 is changed from 80 parts to 64 parts (prepared into a 25% ammonium chloride liquid ammonia solution), and other conditions remain unchanged. The yield of the final product silane relative to magnesium silicide was 95.2%.

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Abstract

The invention discloses a continuous production method for silane by a magnesium silicide method, which comprises the following steps of: preparing solid ammonium chloride and liquid ammonia into an ammonium chloride-liquid ammonia solution; carrying out addition or grading limit continuous addition of the solution and a magnesium silicide solid from the first stage of a multistage series connection silane generator; stirring and cooling all stages of the silane generator; leading the silane which is continuously generated by all stages of the silane generator to enter a silane buffer tank by all stages of washing tower and condensers for collecting; and returning the liquid ammonia formed by condensing the ammonia carried by a silane gas through a condenser to all stages of the silane generator by the washing towers and simultaneously washing impurities, such as borane in the silane and the like, by the returned liquid ammonia. The method continuously generates the silane at multiple stages by adopting continuous feed, and the reaction temperature at each stage is subjected to stepped type adjustment and control, therefore, the invention has stable silane gas quantity, mild reaction condition, high safety, high yield, few impurity and low cost and meets the requirement of green manufacturing.

Description

Technical field [0001] The invention belongs to the technical field of polysilicon, and relates to a preparation process of silane, in particular to an improved process for preparing silane using magnesium silicide as a raw material. Background technique [0002] Silane (SiH 4 ) It is widely used for epitaxial deposition of monocrystalline silicon film and production of polycrystalline silicon film, manufacturing of photosensitive parts for amorphous silicon solar cells and copiers, replacing traditional toner cartridges with silicon drums, and producing brown glass in the glass industry. In the high-tech field, silane and ethylene can generate ultrafine silicon carbide powder under laser activation, and silane and ammonia can generate ultrafine silicon nitride powder under laser activation. At the same time, with the rapid development of the photovoltaic industry, the domestic demand for silane is increasing rapidly. [0003] At present, the main methods of producing silane are: ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/04
Inventor 李群张晓薇顾克军祁宏祥吴海浪张晓谕蒋智慧殷恒志
Owner JIANGSU YANGNONG CHEM GROUP
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