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Method for purifying high-concentration N2F2 in large-flow NF3 electrolysis gas

A purification method and electrolytic gas technology, which is applied in the field of NF3 purification, can solve the problems of low adsorption efficiency, high energy consumption, and small electrolytic gas treatment capacity, and achieve the effects of less power consumption, reduced safety risks, and prolonged residence time

Inactive Publication Date: 2021-07-27
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the patent US4933158, will contain N 2 f 2 NF of impurities 3 The gas passes through the zeolite packing layer at (-125~50) °C, and N can be effectively removed by adsorption. 2 f 2 , but the adsorption method requires repeated adsorption and desorption, which consumes a lot of energy, and N 2 Large dosage, low adsorption efficiency
In the patent ZL 200510085395.0, NF is made by heat treatment 3 N in gas 2 f 2 For impurity cracking, the diameter of the pyrolyzer used is (100-200) mm, the tower height is (1000-3000) mm, and the operating pressure is (0.2-0.7) MPa. Due to the relatively small size of the pyrolyzer, NF 3 The electrolytic gas treatment capacity is small, and the NF 3 N in electrolytic gas 2 f 2 The impurity concentration is (0.1~1)vol%, and it is impossible to achieve high-concentration N 2 f 2 Effective removal of impurities

Method used

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  • Method for purifying high-concentration N2F2 in large-flow NF3 electrolysis gas
  • Method for purifying high-concentration N2F2 in large-flow NF3 electrolysis gas
  • Method for purifying high-concentration N2F2 in large-flow NF3 electrolysis gas

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Experimental program
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Effect test

Embodiment 1

[0028] A pyrolysis tower with a diameter of 800mm and a height of 9000mm is selected for use; nickel Pall rings (nickel purity is 99.5wt%) are used as the internal packing of the pyrolysis tower with a specification or nominal size of 25mm, and the filling height of the packing is 7000mm, and the specific surface area of ​​the packing is 300m 2 / m 3 ; Choose 4 electromagnetic heating devices to heat the cracking tower, and the 4 electromagnetic heating devices are evenly distributed in the axial direction of the cracking tower.

[0029] The above cracking tower is directly connected with the electrolyzer, and the NF output from the electrolyzer is 3The content is 50vol% and N 2 f 2 5.5vol% NF 3 When the electrolytic gas is purified:

[0030] NF 3 The electrolytic gas enters the pyrolysis tower from the bottom of the tower at the inlet flow rate of 200kg / h, 300kg / h, 350kg / h, 400kg / h, 550kg / h and 650kg / h respectively. 3 During the process of electrolysis gas flowing from t...

Embodiment 2

[0035] A pyrolysis tower with a diameter of 1000mm and a height of 10000mm is selected; nickel Pall rings with a specification or nominal size of 25mm (the purity of nickel is 99.5wt%) are used as the internal packing of the pyrolysis tower, and the filling height of the packing is 8000mm, and the specific surface area of ​​the packing is 300m 2 / m 3 ; Choose 4 electromagnetic heating devices to heat the cracking tower, and the 4 electromagnetic heating devices are evenly distributed in the axial direction of the cracking tower.

[0036] The above cracking tower is directly connected with the electrolyzer, and the NF output from the electrolyzer is 3 The content is 50vol% and N 2 f 2 5.5vol% NF 3 When the electrolytic gas is purified:

[0037] NF 3 The electrolytic gas enters the pyrolysis tower from the bottom of the tower at the inlet flow rate of 200kg / h, 300kg / h, 350kg / h, 400kg / h, 550kg / h and 650kg / h respectively. 3 During the process of electrolysis gas flowing from...

Embodiment 3

[0042] A pyrolysis tower with a diameter of 1200mm and a height of 13000mm is used; nickel Pall rings (nickel purity of 99.5wt%) are used as the internal packing of the pyrolysis tower with a specification or nominal size of 25mm, and the filling height of the packing is 10000mm, and the specific surface area of ​​the packing is 300m 2 / m 3 ; Choose 4 electromagnetic heating devices to heat the cracking tower, and the 4 electromagnetic heating devices are evenly distributed in the axial direction of the cracking tower.

[0043] The above cracking tower is directly connected with the electrolyzer, and the NF output from the electrolyzer is 3 The content is 50vol% and N 2 f 2 5.5vol% NF 3 When the electrolytic gas is purified:

[0044] NF 3 The electrolytic gas enters the pyrolysis tower from the bottom of the tower at the inlet flow rate of 200kg / h, 300kg / h, 350kg / h, 400kg / h, 550kg / h and 650kg / h respectively. 3 During the process of electrolysis gas flowing from the botto...

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Abstract

The invention relates to a method for purifying high-concentration N2F2 in large-flow NF3 electrolysis gas, and belongs to the technical field of NF3 purification. NF3 electrolysis gas enters a cracking tower with a diameter of 500-1500 mm and a height of 5000-15000 mm from the tower bottom, N2F2 is completely decomposed and removed at a temperature of 150-350 DEG C in the process that the NF3 electrolysis gas flows to the tower top from the tower bottom, the NF3 electrolysis gas with the N2F2 removed is discharged from the tower top, and the residence time of the NF3 electrolysis gas in the cracking tower is not less than 0.5 min by selecting the reasonable size of the cracking tower and the reasonable gas inlet flow, so that the NF3 electrolysis gas with the gas inlet flow of (100-650) kg / h and the N2F2 content of 8 vol% or below can be effectively treated, and the application prospect is very wide.

Description

technical field [0001] The invention relates to a kind of purified large flow NF 3 High concentration of N in the electrolytic gas 2 f 2 method of NF 3 field of purification technology. Background technique [0002] NF 3 Gases are widely used in fields such as high-energy lasers, semiconductor technology, and chemical vapor deposition, and have good application prospects. current NF 3 There are two main methods of preparation: (1) direct chemical method: ① gas-gas reaction: use fluorine gas (F 2 ) and ammonia (NH 3 ) direct chemical reaction to generate NF 3 ; ② gas-liquid reaction: using F 2 With liquid ammonia (or liquid ammonium bifluoride (NH 4 HF 2 )) Reaction, F 2 with urea (NH 2 CONH 2 ) reaction to generate NF 3 ; ③ gas-solid reaction: F 2 React with solid aluminum ammonium fluoride to generate NF 3 ; (2) electrolysis method: electrolytic melting NH 4 HF 2 / HF, electrolytic NH 3 with HF. The synthesis process of the direct chemical method is not ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/083
CPCC01B21/0832
Inventor 冀延治宋富财武建鹏郝春辉陈宝健李海军郑秋艳申文超张旭罗文键
Owner PERIC SPECIAL GASES CO LTD
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