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Process for preparing silane by magnesium silicide method

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

Active Publication Date: 2012-10-17
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

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Comparison scheme
Effect test

Embodiment 1

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

[0032] Before silane occurs, the entire reaction system is replaced with nitrogen to replace the oxygen in the reaction system;

[0033] After the oxygen replacement is completed, 80 parts per hour of liquid ammonia is injected from the buffer tank into the batching kettle 3, the vaporized ammonia is condensed by the condenser 4 and then returned to the batching kettle 3, and the ammonium chloride is passed through the high level tank 1 at 20 parts per hour. Screw feeder 2 adds in batching kettle 3, is mixed with 20% ammonium chloride liquid ammonia solution;

[0034] Ammonium chloride liquefied ammonia solution prepared is input first-stage silane generator 8 with 100 parts per hour through pump 5, simultaneously with the magnesium silicide in the magnesium silicide header tank 6 with 6.9 parts per hour (magnesium silicide and ammonium chloride) The molar ratio is 1: 4.1), and the mag...

Embodiment 2

[0039] Technological process is the same as embodiment 1, just changes 106.7 parts (being mixed with 15% ammonium chloride liquefied ammonia solution) into 106.7 parts (being mixed with 15% ammonium chloride liquid ammonia solution) of liquefied ammonia per hour add-on in embodiment 1, other conditions are constant. The yield of final product silane relative to magnesium silicide is 92.6%.

Embodiment 3

[0041] Technological process is the same as embodiment 1, just changes the per hour add-on of liquid ammonia into 64 parts (being mixed with 25% ammonium chloride liquid ammonia solution) by 80 parts in the embodiment 1, other conditions are constant. The yield of final product silane relative to magnesium silicide is 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 byall 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 multiplestages 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 silane preparation process, in particular to an improved silane preparation process using magnesium silicide as a raw material. Background technique [0002] Silane (SiH 4 ) is widely used in the epitaxial deposition of monocrystalline silicon films and the production of polycrystalline silicon films, the manufacture of photosensitive components for amorphous silicon solar cells and copiers, the replacement of traditional toner cartridges with silicon drums, and the production of brown glass in the glass industry. In the high-tech field, silane and ethylene can produce silicon carbide ultrafine powder under laser activation, and silane and ammonia can produce silicon nitride ultrafine powder under laser activation. At the same time, with the rapid development of the photovoltaic industry, the domestic demand for silane has increased rapidly. [0003] At present, the product...

Claims

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Application Information

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Patent Type & Authority Patents(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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