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Method and device for continuously producing ultra-pure arsine

An arsine and ultra-pure technology, applied in chemical instruments and methods, arsenic compounds, inorganic chemistry, etc., can solve the problems of uncontinuous production of arsine products, unstable product quality, low production efficiency, etc., to achieve large output, The effect of mild reaction and low risk

Pending Publication Date: 2022-07-29
沧州渤海新区盛泰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method belongs to intermittent production and cannot produce arsine products continuously; the purification process implemented is a multi-stage adsorption device to remove impurity components one by one. In the process of large-scale production, there are many problems such as low production efficiency, unstable product quality, and large quality fluctuations. disadvantages

Method used

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  • Method and device for continuously producing ultra-pure arsine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0061] After the nitrogen replacement system was evacuated, 540Kg of deionized water was added to the first reactor A and the second reactor B in turn, and the stirring was turned on. Concentrated sulfuric acid, control the temperature of the first reaction kettle A and the second reaction kettle B not to exceed 40 ° C, then gradually add 180Kg of zinc arsenide, the sulfuric acid and zinc arsenide react with exothermic heat, control the rate of addition of zinc arsenide, and maintain the temperature of the reaction solution 40°C, rotating speed 120r / min, maintaining system pressure of 0.2MPa and producing crude arsine gas. No gas was generated after the reaction for 5 hours, the reaction was completed, and the reaction solution was discharged. When the reaction liquid is discharged, a small amount of the reaction liquid is left to act as a liquid seal to prevent the discharge of arsine gas. The first reactor A and the second reactor B are alternately fed in parallel to produc...

Embodiment example 2

[0065] After the nitrogen replacement system was evacuated, 360Kg of deionized water was added to the first reactor A and the second reactor B in turn, and the stirring was turned on. Sulfuric acid, control the temperature of the first reaction kettle A and the second reaction kettle B not to exceed 70 ℃, then gradually add 180Kg of zinc arsenide, the sulfuric acid and the zinc arsenide react with exothermic heat, control the rate of addition of the zinc arsenide, and keep the temperature of the reaction solution at 70 °C ℃, the rotation speed is 90r / min, the system pressure is maintained at 0.2MPa, and the crude arsine gas is produced. After the reaction for 3.5 hours, no gas was produced, the reaction was completed, and the reaction solution was discharged. When the reaction liquid is discharged, a small amount of the reaction liquid is left to act as a liquid seal to prevent the discharge of arsine gas. The first reactor A and the second reactor B are alternately fed in pa...

Embodiment example 3

[0069] After the nitrogen replacement system was evacuated, 400Kg of deionized water was added to the first reactor A and the second reactor B in turn, and the stirring was turned on. Sulfuric acid, control the temperature of the first reaction kettle A and the second reaction kettle B not to exceed 65 ℃, then gradually add 180Kg of zinc arsenide, the sulfuric acid and the zinc arsenide react with exothermic heat, control the rate of addition of the zinc arsenide, and keep the temperature of the reaction solution at 65 ℃, the rotation speed is 100r / min, the system pressure is maintained at 0.1MPa, and the crude arsine gas is produced. No gas was generated after the reaction for 4 hours, the reaction was completed, and the reaction solution was discharged. When the reaction liquid is discharged, a small amount of the reaction liquid is left to act as a liquid seal to prevent the discharge of arsine gas. The first reactor A and the second reactor B are alternately fed in parall...

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Abstract

The invention relates to a method and a device for continuously producing ultra-pure arsine. In a water environment, zinc arsenide is added into concentrated sulfuric acid under the control of a spiral feeder, and a plurality of reaction kettles are connected in parallel and alternately feed for production and discharge reaction liquid; crude arsine is obtained; high-boiling-point impurities of the crude arsine are frozen in a condenser through two-stage low-temperature freezing; arsine is alternately collected at low temperature, and is heated and gasified to provide a gas source for subsequent processes; after low-temperature cold trap collection is finished, crude arsine provided by heating passes through a two-stage low-temperature low-pressure rectifying tower to remove high-boiling-point and low-boiling-point impurities; the arsine obtained after rectification is adsorbed; the yield of arsine in the refining process is larger than or equal to 90%, and compared with a traditional process, the two-stage low-temperature low-pressure rectification process saves energy by larger than or equal to 25%. And filling the ultra-pure arsine product into a low-temperature negative-pressure steel cylinder group through a mass flow meter. The large-scale filling of the ultra-pure arsine is realized.

Description

technical field [0001] The invention belongs to the technical field of arsine preparation, purification and filling, and in particular relates to a method and a device for continuous production of ultrapure arsine. Background technique [0002] High-purity arsine is widely used in the semiconductor industry for n-type doping of epitaxial silicon, n-type diffusion in silicon, ion implantation, growth of gallium arsenide (GaAs), gallium arsenide phosphide (GaAsP) and formation with III / V elements compound semiconductors. Arsine is an important material for high-efficiency concentrating solar cells and semiconductor light-emitting components. The synthesis methods of arsine mainly include chemical method and electrolysis method, but any synthesis process will produce unnecessary impurities, which cannot be directly used in electronics, aviation, military and other fields. At present, the main purification methods of arsine mainly include molecular sieve adsorption method, low...

Claims

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Application Information

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IPC IPC(8): C01G28/00
CPCC01G28/00
Inventor 周桂明
Owner 沧州渤海新区盛泰化工有限公司
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