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Method and device for circulating hydrogen repurification

A hydrogen and tail gas technology, applied in hydrogen separation, using solid contact hydrogen separation, etc., can solve the problem that impurities are difficult to effectively remove, and achieve the effect of thorough impurity removal process, breaking through technical blockade, and improving quality

Active Publication Date: 2016-02-03
YICHANG CSG POLYSILICON CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The impurities in circulating hydrogen mainly include small molecular impurities such as boron and phosphorus, such as B 2 h 6 、PH 3 、BCl 3 , PCl 5 etc., the above-mentioned impurities are difficult to be effectively removed by traditional processes

Method used

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  • Method and device for circulating hydrogen repurification

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Effect test

Embodiment 1

[0024] A method for repurifying circulating hydrogen. The circulating hydrogen comes from the recovered hydrogen in the dry recovery process of reducing tail gas. The circulating hydrogen is first passed into the hydrogen cooler 1 for cooling, the hydrogen is cooled to 20°C, and the cooled circulating hydrogen is passed through into the primary adsorption reaction column 2 to remove impurities mainly containing boron elements; the circulating hydrogen after the primary adsorption reaction is passed into the hydrogen deep cooler 3 to cool the hydrogen to -80°C, and the cooled circulating hydrogen enters the secondary The first-stage adsorption reaction column (4) removes impurities mainly containing phosphorus elements, and the adsorption temperature is -80°C. Hydrogen cooler 1 is a tube-and-tube heat exchanger, and the tube side uses circulating hydrogen, and the cooling medium on the shell side is frozen brine at a temperature of -10°C; hydrogen cryocooler 3 is a tube-and-tube...

Embodiment 2

[0026] A method for repurifying circulating hydrogen, the circulating hydrogen comes from the recovered hydrogen in the dry recovery process of reducing tail gas, the circulating hydrogen is first passed into the hydrogen cooler 1 for cooling, the hydrogen is cooled to 0°C, and the cooled circulating hydrogen is passed through into the primary adsorption reaction column 2 to remove impurities mainly containing boron elements; the circulating hydrogen after the primary adsorption reaction is passed into the hydrogen deep cooler 3 to cool the hydrogen to -70°C, and the cooled circulating hydrogen enters the secondary The first-stage adsorption reaction column 4 removes impurities mainly containing phosphorus elements, and the adsorption temperature is -88°C. Hydrogen cooler 1 is a tube-and-tube heat exchanger, and the tube side uses circulating hydrogen, and the cooling medium on the shell side is frozen brine at a temperature of -12°C; hydrogen cryocooler 3 is a tube-and-tube he...

Embodiment 3

[0028] A device for repurifying circulating hydrogen. The top of the hydrogen cooler 1 is connected to the bottom of the primary adsorption reaction column 2 through the feeding pipe, and the top of the primary adsorption reaction column 2 is connected to the bottom of the hydrogen deep cooler 3 through the feeding pipe. The top of the cooler 3 is connected to the bottom of the secondary adsorption reaction column 4 through a feed pipe. Both the primary adsorption reaction column 2 and the secondary adsorption reaction column 4 are of fixed bed structure.

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Abstract

The invention provides a method and a device for circulating hydrogen repurification and relates to the field of polysilicon production. According to the method and device, the circulating hydrogen is subjected to adsorption and impurity removal to reduce the content impurities of boron and phosphorus in hydrogen from 10 ppba to 0.1 ppba. The specific steps are as below: first introducing circulating hydrogen into a hydrogen cooler for cooling; cooling the hydrogen to 0 to 30 DEG C; introducing hydrogen into a first-stage adsorption reaction column to adsorb and remove impurities mainly containing boron; introducing the circulating hydrogen after the first-stage adsorption into a hydrogen cryogenic device, cooling the hydrogen to -88 to -68 DEG C; and introducing the hydrogen to a second-stage adsorption reaction column to adsorb and remove impurities mainly containing phosphorus element. According to the invention, the circulating hydrogen adsorption reaction is employed for removal of harmful impurities of boron and phosphorus elements, so as to dramatically reduce the content of impurities including boron and phosphorus in hydrogen, and upgrade the quality of circulating hydrogen. The invention makes it possible to improve Siemens method for stable production of electronic grade polysilicon, and breaks the blockade of foreign technology. The process is simple, easy to operate, and has obvious effect of impurity removal.

Description

technical field [0001] The invention relates to the field of electronic-grade polysilicon production, in particular to the removal of boron and phosphorus element impurities in hydrogen gas (circulating hydrogen gas) recovered in the dry recovery of reduced tail gas by the improved Siemens method. Background technique [0002] Polycrystalline silicon is the basic material of the semiconductor and solar energy industries, the main raw material for the manufacture of silicon polished wafers, solar cells and high-purity silicon products, and an important cornerstone for the development of the information industry and new energy industry, which makes the production of raw material polycrystalline silicon a hot industry. In recent years, my country's polysilicon industry has developed rapidly, and its production capacity has leapt to the first place in the world. However, due to various factors such as technological blockade, China still cannot achieve the goal of stabilizing the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B3/56
Inventor 张鹏田洪先刘强吴学林
Owner YICHANG CSG POLYSILICON CO LTD
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