Method for purifying butadiene hexafluoride

A technology of hexafluorobutadiene and graphene, applied in the field of purification, can solve the problems of HFBD purity and yield decline, and achieve the effect of high adsorption and increase of adsorption capacity

Active Publication Date: 2017-01-25
ZHEJIANG BRITECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Most of the adsorbents in the prior art use activated carbon, molecular sieves, boron oxides, etc., and the disproportionation and decomposition reactions that occur when unsaturated fluorocarbons contact with molecular sieves may still cause a decrease in the purity and yield of HFBD. Sorbent for optimization

Method used

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  • Method for purifying butadiene hexafluoride
  • Method for purifying butadiene hexafluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation of efficient adsorbent

[0020] Add 100Kg of adsorption resin to a 2000L reactor with a specific surface area of ​​800m 2 / g, 8Kg graphene oxide aqueous solution (mass percentage concentration 15), 0.3Kg potassium borohydride, 800Kg pure water mixed, stirred at 80°C for 50h, filtered, dried, passed into nitrogen, roasted at 300°C for 2h, 700°C It was calcined at ℃ for 3h, at 1100℃ for 2h, and cooled to room temperature to obtain a high-efficiency adsorbent.

[0021] (2) Purification of hexafluorobutadiene

[0022] Crude hexafluorobutadiene undergoes the well-known impurity removal and refining technology in the industry, including extraction technology to separate the solvent, absorbs moisture through molecular sieves, and then enters the adsorption tower equipped with this high-efficiency adsorbent. At 20 ° C, the pressure is 0.5 MPa, and the flow rate is 3 BV Adsorbed under the condition of / h, the adsorbed hexafluorobutadiene is then subjected to th...

Embodiment 2

[0024] (1) Preparation of efficient adsorbent

[0025] Add 100Kg of adsorption resin to a 2000L reactor with a specific surface area of ​​500m 2 / g, 2Kg graphene oxide aqueous solution (mass percentage concentration 5), 0.05Kg potassium borohydride, 300Kg pure water mixed, stirred at 50°C for 30h, filtered, dried, passed into nitrogen, roasted at 200°C for 1h, 500°C It was calcined at ℃ for 1 h, and at 900 °C for 1 h, and cooled to room temperature to obtain a highly efficient adsorbent.

[0026] (2) Purification of hexafluorobutadiene

[0027] Crude hexafluorobutadiene undergoes the well-known impurity removal and refining technology in the industry, including extraction technology to separate the solvent, absorbs moisture through molecular sieves, and then enters the adsorption tower equipped with this high-efficiency adsorbent. At 0 ° C, the pressure is 0.1 MPa, and the flow rate is 1 BV Adsorbed under the condition of / h, the adsorbed hexafluorobutadiene is then subjecte...

Embodiment 3

[0029] (1) Preparation of efficient adsorbent

[0030] Add 100Kg of adsorption resin to a 2000L reactor with a specific surface area of ​​1000m 2 / g, 10Kg graphene oxide aqueous solution (mass percentage concentration 5), 0.5Kg potassium borohydride, 1000Kg deionized water were mixed, stirred at 100°C for 80h, filtered, dried, passed into nitrogen, and roasted at 400°C for 3h, Calcined at 800°C for 5 hours, 1200°C for 5 hours, and cooled to room temperature to obtain a high-efficiency adsorbent.

[0031] (2) Purification of hexafluorobutadiene

[0032] Crude hexafluorobutadiene undergoes well-known impurity removal and refining technologies in the industry, including extraction technology to separate solvents, and then absorbs moisture through molecular sieves, and then enters the adsorption tower equipped with this high-efficiency adsorbent. At 30°C, pressure 1MPa, flow rate 5BV / Adsorbed under the condition of h, the adsorbed hexafluorobutadiene undergoes impurity removal ...

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Abstract

The invention provides a method for purifying butadiene hexafluoride. The method comprises the following steps: pumping pure water, adsorption resin, a graphene oxide aqueous solution and potassium borohydride into a reaction kettle, heating to reaction temperature and stirring, performing filtering, drying and heating roasting at the end of the reaction, and cooling to room temperature to obtain an efficient adsorbent; performing an impurity removal rectification technology which is publically known in the industry, including performing an extraction technology, on a coarse butadiene hexafluoride product to separate out a solvent, then adsorbing by a molecular sieve to remove water, putting into an adsorption tower with the efficient adsorbent, adjusting to proper reaction temperature, pressure and flowing rate for adsorption, performing the impurity removal rectification technology which is publically known in the industry again, including decompression rectification, on adsorbed fluorine-containing organic gas, and removing impurities to obtain a high-purity butadiene hexafluoride product.

Description

technical field [0001] The invention relates to a purification method, especially a method for purifying hexafluorobutadiene. Background technique [0002] Hexafluoro-1,3-butadiene (Hexafluoro-1,3-butadiene, HFBD) has many applications in industry, not only as a monomer for the preparation of various fluorine-containing polymer elastic materials polyhexafluorobutadiene , or a very low greenhouse effect, green and efficient dry etching gas. It has a higher etch selectivity than conventional plasma etch gases. Compared with traditional fluorine-containing etching gases, HFBD has two advantages: superior etching performance and excellent environmental performance. Especially in the etching of insulator materials, HFBD has gradually replaced the most widely used c-C 4 f 8 the trend of. Commonly used methods for purifying gases are: cryogenic rectification, physical absorption, chemical conversion, selective adsorption, condensation, freezing and membrane separation. The di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/38C07C17/389C07C21/20B01J20/26
CPCB01J20/04B01J20/20B01J20/26B01J2220/46C07C17/38C07C17/389C07C21/20
Inventor 陈刚张晓东周井森李军张广第王宁陈立峰钱红东花永紧郑九丽
Owner ZHEJIANG BRITECH CO LTD
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