A kind of preparation method of rhenium hexafluoride

A technology of rhenium hexafluoride and nitrogen trifluoride, which is applied in the field of preparation of rhenium hexafluoride, can solve the problems of increased processing costs, difficult removal of impurities, and influence on the purification of rhenium hexafluoride, so as to achieve safe operation process Economical, high industrial application value, and high synthetic conversion rate

Active Publication Date: 2022-03-25
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the synthesis of rhenium hexafluoride, it is often accompanied by the generation of a large amount of by-products such as rhenium trifluoride, rhenium tetrafluoride, rhenium pentafluoride and rhenium heptafluoride, which leads to an increase in subsequent processing costs and affects the further purification of rhenium hexafluoride , impurities are not easy to remove

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Spread 5g of rhenium powder in the reactor Ⅰ, and the air velocity is 20h -1 ~30h -1 Nitrogen trifluoride gas, the fluorination reaction is carried out at a reaction temperature of 400°C to 430°C and a reaction pressure of 0.15MPa to 0.2MPa, and the product is collected by condenser I, and the nitrogen and nitrogen trifluoride in the product are evacuated The valve is removed, and the rhenium hexafluoride and rhenium heptafluoride in the product are liquefied into mixed solids;

[0025] (2) First heat and sublimate the mixed solid collected in condenser I into a mixed gas, and then -1 ~10h -1 The space velocity is passed into the reactor II equipped with 10g rhenium powder, and the reduction reaction is carried out at a reaction temperature of 100 ° C ~ 120 ° C and a reaction pressure of 0.1 MPa ~ 0.3 MPa, and the product is collected by condenser II. The rhenium hexafluoride gas has a purity of 91.2 wt%.

Embodiment 2

[0027] (1) Spread 5g of rhenium powder in the reactor Ⅰ, and the air velocity is 30h -1 ~50h -1 Nitrogen trifluoride gas, the fluorination reaction is carried out at a reaction temperature of 470°C to 500°C and a reaction pressure of 0.1MPa to 0.12MPa, and the product is collected by condenser I, and the nitrogen and nitrogen trifluoride in the product are evacuated The valve is removed, and the rhenium hexafluoride and rhenium heptafluoride in the product are liquefied into mixed solids;

[0028] (2) First heat and sublimate the mixed solid collected in condenser I into a mixed gas, and then -1 ~10h -1 The space velocity is passed into the reactor II equipped with 10g rhenium powder, and the reduction reaction is carried out at a reaction temperature of 130 ° C ~ 150 ° C and a reaction pressure of 0.3 MPa ~ 0.5 MPa, and the product is collected by condenser II. The rhenium hexafluoride gas has a purity of 95.4 wt%.

Embodiment 3

[0030] (1) Spread 5g of rhenium powder in the reactor Ⅰ, and the air velocity is 30h -1 ~50h -1 Nitrogen trifluoride gas, the fluorination reaction is carried out at a reaction temperature of 440°C to 460°C and a reaction pressure of 0.13MPa to 0.15MPa, and the product is collected by condenser I, and the nitrogen and nitrogen trifluoride in the product are evacuated The valve is removed, and the rhenium hexafluoride and rhenium heptafluoride in the product are liquefied into mixed solids;

[0031] (2) First heat and sublimate the mixed solid collected in condenser I into a mixed gas, and then -1 ~10h -1 The space velocity is passed into the reactor II equipped with 10g rhenium powder, and the reduction reaction is carried out at a reaction temperature of 120°C to 140°C and a reaction pressure of 0.2MPa to 0.4MPa, and the product is collected by condenser II. The rhenium hexafluoride gas has a purity of 92.3 wt%.

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Abstract

The invention relates to a preparation method of rhenium hexafluoride, which belongs to the technical field of fluorine chemical industry. In this method, the rhenium powder and nitrogen trifluoride mainly generate a mixture of rhenium hexafluoride and rhenium heptafluoride by adjusting the fluorination reaction conditions, and the disproportionation reaction of other valence rhenium fluorides can be basically avoided; The reaction conditions are such that rhenium heptafluoride reacts with rhenium powder to form rhenium hexafluoride, preventing rhenium heptafluoride and rhenium hexafluoride from being reduced to rhenium fluoride in a lower valence state. The method of the invention has the advantages of simple operation, safety and economy, high synthesis conversion rate, and the prepared rhenium hexafluoride has a purity higher than 90 wt%.

Description

technical field [0001] The invention relates to a preparation method of rhenium hexafluoride, which belongs to the technical field of fluorine chemical industry. Background technique [0002] Rhenium is a silver-white metal with an atomic weight of 186. Its melting point (3186°C) is the third highest after tungsten and carbon, its boiling point (5596°C) ranks first, and its density ranks fourth. It is very hard, wear-resistant, and corrosion-resistant. The use of rhenium metal is mainly to use the "rhenium effect" to make alloys with tungsten, molybdenum, etc., which greatly improves the strength and plasticity of the alloy, and the dosage is 4% to 50%. Among them, tungsten and rhenium alloys are widely used in aerospace, atomic energy, metallurgy, electronics, petrochemical and other industries. Using tungsten hexafluoride, rhenium hexafluoride and hydrogen as source gases, high-quality tungsten-rhenium coatings can also be prepared by chemical vapor deposition (CVD), whic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G47/00
CPCC01G47/00
Inventor 张琴张长金杨万吉王占卫孟祥军李翔宇彭立培胡帅李丹丹
Owner PERIC SPECIAL GASES CO LTD
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