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Purification method of hexafluoro-1,3-butadiene

A kind of technology of hexafluorobutadiene and purification method, applied in the field of purification of hexafluorobutadiene

Active Publication Date: 2017-08-11
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method enables the N 2 , O 2 、H 2 The mass fraction of O is reduced to below 1ppm, but the purity of hexafluorobutadiene can only reach 99.98%

Method used

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  • Purification method of hexafluoro-1,3-butadiene
  • Purification method of hexafluoro-1,3-butadiene
  • Purification method of hexafluoro-1,3-butadiene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Weigh a certain amount of Y molecular sieve raw powder, mix with 0.1mol / L concentration Cu(NO 3 ) 2 The solution was mixed at a solid-to-liquid ratio of 1:3, and stirred at 80°C for 4h. Filter molecular sieves and wash with distilled water until Cu-free 2+ . Dry at 110°C for 8 hours. After a certain amount of sample is taken and molded, it is placed in a gas-solid phase adsorption device, and at 350 ° C, N 2 Activate in situ in the atmosphere for 2 hours, pass the raw material gas hexafluorobutadiene after cooling down, and carry out adsorption and removal of impurities at normal temperature (25°C) and normal pressure; Vent for 10 minutes at 40°C, 0.3MPa, and vent flow rate of 5L / min. Finally, a hexafluorobutadiene product with a purity of more than 99.99% is obtained, and the volume concentration of impurities included in the hexafluorobutadiene product is total organic impurities≤20.0ppm, inorganic impurities≤40.0ppm, H 2 O≤2.5ppm, acidity≤0.1ppm.

Embodiment 2

[0049] Weigh a certain amount of 13X molecular sieve powder, and mix it with 0.1mol / L Cu(NO 3 ) 2 The solution was mixed at a solid-to-liquid ratio of 1:3, and stirred at 80°C for 4h. Filter molecular sieves and wash with distilled water until Cu-free 2+ . Dry at 110°C for 8 hours. After a certain amount of sample is taken and molded, it is placed in a gas-solid phase adsorption device, and at 350 ° C, N 2 Activate in situ in the atmosphere for 2 hours, pass the raw material gas hexafluorobutadiene after cooling down, and carry out adsorption and removal of impurities at normal temperature (25°C) and normal pressure; 50°C, 0.4MPa, and vent flow rate of 5L / min for 20 minutes. Finally, a hexafluorobutadiene product with a purity of more than 99.995% is obtained, and the volume concentration of impurities included in the hexafluorobutadiene product is total organic impurities≤5.0ppm, inorganic impurities≤30.0ppm, H 2 O≤2.0ppm, acidity≤0.1ppm.

Embodiment 3

[0051] Weigh a certain amount of 13X molecular sieve raw powder and mix it with 0.1mol / L LiNO 3 The solution was mixed at a solid-to-liquid ratio of 1:3, and stirred at 80°C for 4h. Filter molecular sieves and wash with distilled water until Cu-free 2+ . Dry at 110°C for 8 hours. After a certain amount of sample is taken and molded, it is placed in a gas-solid phase adsorption device, and at 350 ° C, N 2 Activate in situ in the atmosphere for 2 hours, pass the raw material gas hexafluorobutadiene after cooling down, and carry out adsorption and removal of impurities at normal temperature (25°C) and normal pressure; Vent for 30 minutes at 60°C, 0.5MPa, and a vent flow rate of 5L / min. Finally, a hexafluorobutadiene product with a purity of more than 99.995% is obtained. The volume concentration of impurities included in the hexafluorobutadiene product is total organic impurities≤30.0ppm, inorganic impurities≤5.0ppm, H 2 O≤2.0ppm, acidity≤0.1ppm.

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Abstract

The invention discloses a purification method of hexafluoro-1,3-butadiene. The purification method comprises steps of adsorption and distillation, wherein an adsorbent is modified with at least one of an ion exchange method, a ball-milling method and an impregnation method in the adsorption step. According to the purification method, organic impurities and inorganic impurities can be removed simultaneously, and purity of hexafluoro-1,3-butadiene can be increased to 99.99% or higher and even 99.999% or higher.

Description

technical field [0001] The invention relates to a method for purifying hexafluorobutadiene. Background technique [0002] Hexafluorobutadiene molecular formula CF 2 =CF-CF=CF 2 , boiling point 6°C, density 1.4g / ml (15°C), GWP value 290, is an environment-friendly compound. High-purity hexafluorobutadiene is a dry etching gas with excellent performance. It has high accuracy and selectivity when performing dry etching on a width smaller than 100nm or even narrower. It can replace perfluorosaturated fluorocarbons for ultra-large-scale integration. Line etching. [0003] Regarding the preparation method of hexafluoro-1,3-butadiene, 1,2,3,4-tetrachloro-1,1,2,3,4,4-6 Fluorobutane, followed by dechlorination of zinc powder in the presence of alcohol solvent to obtain hexafluoro1,3-butadiene. In the later period, the preparation method of hexafluoro-1,3-butadiene was improved. First, the intermediate trifluorovinyl zinc bromide was prepared, and then hexafluoro-1,3-butadiene wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/38
CPCC07C17/38C07C21/18
Inventor 张金柯白占旗徐娇何双材胡欣
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH