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Method and device for preparing high-purity fluorine gas or high-purity fluorine-containing mixed gas

A mixed gas and high-purity technology, which is applied in the direction of combined devices, separation methods, fluorine/hydrogen fluoride, etc., can solve the problems that cannot meet the requirements of fine chemical industry and high-end electronics industry, low purity of fluorine gas, and great difference between high-purity fluorine gas and other problems , to achieve good economic value, improve the purity, and expand the effect of the application market

Active Publication Date: 2017-05-24
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the purity of fluorine gas produced by the medium-temperature electrolysis industrial method of fluorine gas is relatively low, among which HF, CF 4 The content of impurities such as high content is far from being able to meet the application in the fine chemical industry and high-end electronics industry.
The existing method of producing fluorine gas by electrolysis only uses activated spherical sodium fluoride for adsorption and purification, and the purity after adsorption can reach about 92% to 98%, which is still far from the requirement of high-purity fluorine gas

Method used

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  • Method and device for preparing high-purity fluorine gas or high-purity fluorine-containing mixed gas

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The device for preparing high-purity fluorine gas or high-purity fluorine-containing mixed gas in this embodiment, such as figure 1As shown, it includes an electrolysis device and a primary filter 5 connected in series, a primary condenser 6 with a condensation temperature of -60 to -100°C, and a secondary condenser 7 with a condensation temperature of -120 to -180°C; In the flow direction, the upstream of the primary filter 5 is connected with a gas booster device 4, which is used to mix the fluorine gas prepared by electrolysis or the fluorine gas prepared by electrolysis in the upstream. Gas pressurization; the refrigerant used in the primary condenser 6 and secondary condenser 7 is liquid nitrogen; the bottom of the primary condenser 6 is connected with a liquid collection device 13 for collecting condensed liquid HF;

[0042] After the gas pressurization device 4 (before the primary filter 5), a gas flow meter is installed to adjust the gas flow;

[0043] The elec...

Embodiment 2

[0049] The method for preparing high-purity fluorine gas in this embodiment adopts the device described in Embodiment 1, specifically:

[0050] Pressurize 1500g of purified fluorine gas produced by medium-temperature electrolysis KF·2HF to a pressure of 0.15MPa, and adjust the flow rate to 0.2m 3 / min, after being filtered through a primary filter with a pore size of 5 μm, the primary condensation and secondary condensation are performed in sequence; the temperature of the primary condensation is controlled at -75°C, and the temperature of the secondary condensation is controlled at -140°C ;

[0051] After the secondary condensed gas is purified, it is filtered through a secondary filter with a pore size of 0.2 μm, and then enters the finished product storage tank, which is high-purity fluorine gas.

[0052] 300 g of gas samples in the storage tank of the finished product are tested by a gas chromatograph, and the purity of the obtained high-purity fluorine gas is 99.9%.

Embodiment 3

[0054] The method for preparing high-purity fluorine-containing mixed gas (fluorine-nitrogen mixed gas) in this embodiment adopts the device described in Example 1, specifically:

[0055] Prepare 2000g of fluorine-nitrogen mixed gas (in the fluorine-nitrogen mixed gas, the mass percentage of fluorine gas is 20%) from the purified fluorine gas produced by medium-temperature electrolysis KF·2HF, pressurize to a pressure of 0.20MPa, and adjust the flow rate to 0.4m 3 / min, after being filtered through a primary filter with a pore size of 10 μm, the primary condensation and secondary condensation are performed in sequence; the temperature of the primary condensation is controlled at -80°C, and the temperature of the secondary condensation is controlled at -130°C ;

[0056] After the secondary condensed gas is purified, it is filtered through a secondary filter with a pore size of 1.0 μm, and then enters the finished product storage tank, which is a high-purity fluorine-nitrogen m...

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Abstract

The invention relates to a method and device for preparing high-purity fluorine gas or high-purity fluorine-containing mixed gas and belongs to the technical field of fluorine chemicals. The method comprises the following steps: pressurizing fluorine gas made by electrolysis or fluorine-containing mixed gas blended by the fluorine gas made by electrolysis to positive pressure, filtering, and sequentially performing primary condensation and secondary condensation, wherein the temperature of the primary condensation is 60-100 DEG C below zero, and the temperature of the secondary condensation is 120-180 DEG C below zero. The purity of the fluorine gas product obtained by the method is 99.9% or higher, and the fluorine gas requirements for production in the existing electron industry and fine chemical engineering are met; the purity of the obtained fluorine-containing mixed gas is 99.9% or higher, and the production requirements of fluorine-containing special gases are met; and the quality of the fluorine gas product is wholly improved, the application market is expanded, the reject ratio of downstream finished products caused by low purity of the fluorine gas or fluorine-containing mixed gas in the production process is reduced, and the method has high economic values and wide application prospects.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemical industry, and specifically relates to a method for preparing high-purity fluorine gas or high-purity fluorine-containing mixed gas, and also relates to a device for preparing high-purity fluorine gas or high-purity fluorine-containing mixed gas. Background technique [0002] High-purity fluorine gas (F 2 ) is a very active gas with strong oxidizing properties. It can react with most inorganic or organic substances at room temperature or below room temperature, releasing a lot of heat, which often leads to combustion and explosion. High-purity fluorine gas is an important raw material in the field of fine chemicals, widely used in electronics, laser technology, medical plastics and other fields; due to its strong oxidizing properties, it can be used for glass etching, surface passivation treatment of metal materials, and pipelines. It is used in national defense to prepare rocket propell...

Claims

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Application Information

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IPC IPC(8): C01B7/20C25B1/24B01D50/00B01D53/00
CPCB01D50/00B01D53/002B01D2257/204B01D2257/2047C01B7/20C25B1/245
Inventor 王矿宾闫春生许胜霞晁金伟冯晓港李磊张枝芝张凯王晓峰徐州程申王选
Owner DO FLUORIDE CHEM CO LTD
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