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Preparation method of arsine

A technology of arsine and arsenic trichloride, applied in chemical instruments and methods, arsenic compounds, inorganic chemistry, etc., can solve problems such as incomplete reaction, large water consumption, environmental damage of arsenic waste liquid, etc., and achieve the solution of arsine The effect of incomplete and efficient industrial production

Active Publication Date: 2020-04-03
紫石能源有限公司
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is to provide a method for preparing arsine to solve the problems in the prior art that the method for preparing arsine consumes a large amount of water, the reaction is not complete, and the arsenic-containing waste liquid produced causes damage to the environment

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preparation example Construction

[0020] As described in the background art, the preparation method of arsine in the prior art uses a large amount of water, the reaction is not complete, and the resulting arsenic-containing waste liquid causes damage to the environment. In order to solve the above technical problems, the present invention provides a method for preparing arsine, which includes the following steps: mixing and reacting raw materials including calcium hydride and arsenic trichloride in a vacuum environment with a water content of less than 100 ppm to obtain arsine.

[0021] The preparation process of arsine in the prior art makes it difficult to remove the water in arsine, and the present invention can effectively solve the above problems by using anhydrous n-hexane as the medium; and, the present invention uses calcium hydride and arsenic trichloride. The reaction can also effectively solve the problem of incomplete arsine generation in the arsine production process in the prior art. Further, in ord...

Embodiment 1

[0033] The preparation method of arsine in this embodiment includes the following steps:

[0034] Add 1300g calcium hydride to the reaction kettle and vacuum process the reaction kettle. When the vacuum degree of the reaction kettle is 1kpa, the pressure of the reaction kettle is reduced to 10pa by a molecular pump to ensure that a very small amount of air remains in the reaction kettle. Add 3000g n-hexane (moisture is less than 100ppm, no air treatment). The temperature of the reaction kettle is set to 30°C, and the condenser is set to 0°C. When the temperature of the reaction kettle and the condenser reach the set temperature, turn on the stirring and start to add 1815g of arsenic trichloride dropwise. After the dropwise addition is completed in 2 hours, the reaction kettle is adjusted. At a temperature of 50°C, calcium hydride reacts with arsenic trichloride to obtain arsine. The n-hexane and arsine evaporated in the reactor enter the condenser for cooling. The liquefied n-hex...

Embodiment 2

[0036] The preparation method of arsine in this embodiment includes the following steps:

[0037] Add 1300g calcium hydride to the reactor, and treat the reactor with vacuum. When the vacuum of the reactor is 1kpa, the pressure of the reactor is reduced to 10pa by a molecular pump to ensure that a very small amount of air remains in the reactor. 3500g n-heptane (moisture less than 100ppm, no air treatment) The temperature of the reaction kettle is set to 30°C, and the condenser is set to 0°C. When the temperature of the reaction kettle and the condenser reach the set temperature, turn on the stirring and start to add 1815g of arsenic trichloride dropwise. After the dropwise addition is completed in 2 hours, the reaction kettle is adjusted. At a temperature of 50°C, calcium hydride reacts with arsenic trichloride to obtain arsine. The n-hexane and arsine evaporated in the reactor enter the condenser for cooling. The liquefied n-hexane is refluxed to the reactor, and the reflux con...

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Abstract

The invention provides a preparation method of arsine. The preparation method comprises the following steps: carrying out a mixed reaction on raw materials including calcium hydride and arsenic trichloride in a vacuum environment under a condition of a water content of less than 100 ppm to obtain arsine. According to the method, the difficulty in water removal in purification is avoided, and the water content problem of the produced arsine is solved; calcium hydride reacts with arsenic trichloride, so that the problem of incomplete arsine generation in an arsine production process in the priorart can be effectively solved; preferably in order to further solve the problem of a large amount of arsenic-containing waste liquids generated in an arsine production process, a specific organic solvent is adopted, and is recycled through a distillation method, so that the generation of the arsenic-containing waste liquid is greatly reduced; and by adopting the preparation method provided by theinvention, the problems of incomplete reaction, damage of arsenic-containing waste liquid to the environment and the like in the traditional method are solved, and rapid and efficient industrial production can be realized.

Description

Technical field [0001] The invention relates to the technical field of electronic gas synthesis, and in particular to a method for preparing arsine. Background technique [0002] Electronic gases are indispensable raw materials for the production of electronic industries such as ultra-large-scale integrated circuits, flat display devices, compound semiconductor devices, solar cells, and optical fibers. They are widely used in processes such as thin film, etching, doping, vapor deposition, and diffusion. [0003] Arsine (AsH 3 ) Is a very important electron gas. As an n-type dopant, it plays a key role in epitaxial and ion implantation processes, such as the N-type doping of epitaxial silicon and the N-type diffusion in silicon. At the same time Arsine is also an important raw material for the synthesis of compound semiconductor gallium arsenide (GaAs) and gallium arsenide phosphorous (GaAsP). [0004] At present, the traditional arsine preparation method usually uses the reaction of...

Claims

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Application Information

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IPC IPC(8): C01G28/00
CPCC01G28/00C01B6/06
Inventor 宁红锋赵青松
Owner 紫石能源有限公司