Preparation method of nitrogen trifluoride and nitrogen trifluoride mixed gas

A nitrogen trifluoride and mixed gas technology, which is applied in the field of chemical engineering, can solve the problems of insufficient preparation efficiency, many by-products, and unfavorable use of fluorine elements, so as to overcome the low fluorine content, increase the content of F elements, and react The effect of high conversion efficiency

Pending Publication Date: 2022-06-03
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, the fluorine content in conventional fluorine-nitrogen mixed gas is currently low, which is not conducive to meeting the demand for fluorine in special industries. 2 / N 2 Mixture as an example, F 2 The content is 0-20%, the F / N atomic ratio is only 0-0.18, and the adjustable range of F / N element content is also very limited
At the same time, the currently reported methods for preparing nitrogen trifluoride and its mixed gas have problems such as low product selectivity, many by-products, and insufficient preparation efficiency.

Method used

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  • Preparation method of nitrogen trifluoride and nitrogen trifluoride mixed gas
  • Preparation method of nitrogen trifluoride and nitrogen trifluoride mixed gas

Examples

Experimental program
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Effect test

Embodiment 1

[0034] The fluorination reactor used in this embodiment is a circular pipeline fluorination reactor, and the reaction tube is 4.8m long and has an inner diameter of 65mm;

[0035] Before the reaction, the pressure in the reaction tube was pumped to 180Pa by a vacuum pump, the temperature was normal temperature, and then the reaction gas was slowly added to react, and the molar ratio of ammonia to fluorine was controlled to be 1:7.2, and the mass content of ammonia in the fluorine-containing mixed gas is 5.0%; in the specific reaction process, the ammonia gas enters the above-mentioned fluorination reactor after adjusting the flow rate to 2.0g / h, and the fluorine-containing mixed gas (the mass percentage of fluorine gas is 85%, and the rest is nitrogen) adjusts the flow rate to 38.0 g / h, enter the fluorination reactor for reaction;

[0036] The mixed gas prepared by the fluorination reactor is pressurized to a pressure of 0.15 MPa, followed by the first-stage condensation separ...

Embodiment 2

[0040] The difference between this example and Example 1 is that the molar ratio of ammonia gas to fluorine gas is 1:6.6, and the mass content of ammonia gas in the fluorine-containing mixed gas is 5.0%; during the reaction, the flow rate of ammonia gas is adjusted to 2.0 g / g Enter the above-mentioned fluorination reactor after h, and the fluorine-containing mixed gas (the mass percentage of fluorine gas is 78%, and the rest is nitrogen) adjusts the flow rate to 38.0g / h, and enters the fluorination reactor for reaction;

[0041] The mixed gas prepared by the reaction is pressurized to a pressure of 0.25 MPa, and the first stage and the second stage condensation separation are carried out in turn, wherein the first stage condensation temperature is controlled at -25 ° C, and the condensation temperature of the second stage separation device is Controlled at -145℃;

[0042]The liquid after secondary condensation is nitrogen trifluoride liquid; the nitrogen trifluoride sample is ...

Embodiment 3

[0045] The difference between this example and Example 2 is that the molar ratio of ammonia gas to fluorine gas is controlled to be 1:11.0, and the mass content of ammonia gas in the fluorine-containing mixed gas is 2.9%; in the specific reaction process, the flow rate of ammonia gas is adjusted to After 1.2g / h, enter the above-mentioned fluorination reactor, and the fluorine-containing mixed gas (the mass percentage of fluorine gas is 75%, and the rest are nitrogen), adjust the flow rate to 39.5g / h, and enter the fluorination reactor to react;

[0046] The purity of the obtained nitrogen trifluoride was 99.999% as detected by gas chromatography.

[0047] Mix and modulate fluorine gas and nitrogen trifluoride, and control the temperature of the mixed gas conditioning device to -20°C to ensure that nitrogen trifluoride is completely vaporized and mixed with fluorine gas. A mixed gas of nitrogen fluoride / 35% fluorine gas, the F / N atomic ratio of the mixed gas is 5.

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Abstract

The invention discloses a preparation method of nitrogen trifluoride and nitrogen trifluoride mixed gas. The method disclosed by the invention comprises the following steps: carrying out reaction on ammonia gas and fluorine-containing mixed gas in a fluorination reactor to generate a mixture containing hydrogen fluoride, nitrogen trifluoride and inert gas; the fluorine-containing mixed gas is mixed gas of fluorine gas and inert gas, the inert gas is one or a mixture of more than two of nitrogen gas, helium gas and neon gas, and the mass percentage of the ammonia gas in the mixed gas of the ammonia gas and the fluorine-containing mixed gas is 0-5.2% or 50.2-100%; and condensing and separating the mixture to obtain nitrogen trifluoride. And further mixing the prepared nitrogen trifluoride with fluorine gas to prepare nitrogen trifluoride mixed gas. According to the method, the F element content of the mixed gas can be greatly increased, the F / N atomic ratio of the mixed gas can be flexibly regulated and controlled to be 3.2-5.0, the reaction conversion efficiency is high, complete conversion of ammonia gas can be achieved, meanwhile, few by-products are generated, the generated by-product HF can be returned to the procedure of preparing fluorine through electrolysis, and ordered circulation of materials is achieved.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and particularly relates to a preparation method of nitrogen trifluoride and nitrogen trifluoride mixed gas. Background technique [0002] Nitrogen trifluoride is mainly used in the microelectronics industry, and it is an excellent plasma etchant and cleaning agent, especially for semiconductor materials such as silicon and silicon nitride, which has excellent etching speed and selectivity; As a gas cleaner, nitrogen trifluoride cleans efficiently and leaves no traces. In addition, nitrogen trifluoride can be used in high-energy lasers, acting as a fluorine source in HF / DF high-energy chemical lasers; nitrogen trifluoride can also be used as an electrochemical fluorinating agent for the production of perfluorinated organic and inorganic compounds, such as for the preparation of tetrafluoroethylene Fluorine hydrazine and reagents for producing fluorozirconate glass, etc.; in the nucl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/083C01B7/19B01F23/10
CPCC01B21/0832C01B7/191
Inventor 石坚杨建明吕剑惠丰袁俊李佳霖肖川余秦伟梅苏宁张前王为强
Owner XIAN MODERN CHEM RES INST
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