Method for synthesizing perfluorobut-2-ene by gas phase catalysis

A technology of butene and catalyst, which is applied in the field of organic synthesis, can solve the problems of easy decomposition, high price, and ignition temperature of only 180°C, and achieve the effects of convenient transportation and storage, reduced production cost, and increased possibility

Active Publication Date: 2017-11-10
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the conversion efficiency of this synthesis reaction is relatively high, which can be close to 83%, there are many unfavorable factors in this synthesis method: firstly, tetrafluoroethylene is an unstable compound that is easy to polymerize, and it needs to be stabilized during storage and transportation. Explosive mixture, ignition temperature is only 180°C
Pentafluoroiodoethane is also an unstable compound, easy to decompose when exposed to light, and expensive, which increases the production cost of octafluoro-2-butene

Method used

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  • Method for synthesizing perfluorobut-2-ene by gas phase catalysis
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  • Method for synthesizing perfluorobut-2-ene by gas phase catalysis

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Effect test

Embodiment 1

[0032] ① Catalyst preparation

[0033] Weigh 50 g of pretreated columnar coconut shell activated carbon, and then soak it in KF solution containing 10% of its mass fraction. After ultrasonicating the impregnating solution for 30 minutes, naturally impregnate for 8 hours, and then use a rotary evaporator to distill the impregnating solution under reduced pressure. After the impregnating solution is distilled, the catalyst is prepared.

[0034] ②Catalyst activation and pretreatment before reaction

[0035] Feed 150ml / min of N into the reactor equipped with 30ml catalyst 2 , and then the reactor was heated to 150° C. at a heating rate of 300° C. / h and kept for 4 hours to dry the catalyst. After drying for 4 hours, continue to heat the reactor to 500° C. at a heating rate of 300° C. / h and keep it for 4 hours to activate the catalyst. After the activation is completed, continue to heat the reactor to 550°C at a heating rate of 300°C / h and maintain a constant temperature. Adjust...

Embodiment 2

[0039] ① Catalyst preparation

[0040] Take the pretreated columnar coconut shell activated carbon 50g, then impregnate it in KNO containing 10% of its mass fraction 3in solution. After ultrasonicating the impregnating solution for 30 minutes, naturally impregnate for 8 hours, and then use a rotary evaporator to distill the impregnating solution under reduced pressure. After the impregnating solution is distilled, the catalyst is prepared.

[0041] ②Catalyst activation and pretreatment before reaction

[0042] Feed 150ml / min of N into the reactor equipped with 30ml catalyst 2 , and then the reactor was heated to 150° C. at a heating rate of 300° C. / h and kept for 4 hours to dry the catalyst. After drying for 4 hours, continue to heat the reactor to 500° C. at a heating rate of 300° C. / h and keep it for 4 hours to activate the catalyst. After the activation is completed, continue to heat the reactor to 550°C at a heating rate of 300°C / h and maintain a constant temperature. ...

Embodiment 3

[0046] ① Catalyst preparation

[0047] Weigh 50 g of pretreated columnar coconut shell activated carbon, and then impregnate it in Ce(NO 3 ) 3 ﹒ 6H 2 O and Ca(NO 3 ) 2 Mixed solution (mass ratio 1:1). After ultrasonicating the impregnating solution for 30 minutes, naturally impregnate for 8 hours, and then use a rotary evaporator to distill the impregnating solution under reduced pressure. After the impregnating solution is distilled, the catalyst is prepared.

[0048] ②Catalyst activation and pretreatment before reaction

[0049] Feed 150ml / min of N into the reactor equipped with 30ml catalyst 2 , and then the reactor was heated to 150° C. at a heating rate of 300° C. / h and kept for 4 hours to dry the catalyst. After drying for 4 hours, continue to heat the reactor to 500° C. at a heating rate of 300° C. / h and keep it for 4 hours to activate the catalyst. After the activation is completed, continue to heat the reactor to 600°C at a heating rate of 300°C / h and keep th...

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Abstract

The invention relates to a method for synthesizing perfluorobut-2-ene by gas phase catalysis, and belongs to the field of organic chemical synthesis. According to the method, one or more of alkali metal, alkaline earth metal or transition metal is or are used as active components of a catalyst, porous activated carbon is used as a carrier, and pentafluoroethane and elemental iodine are selected as raw materials to react under a high-temperature gas phase, and perfluorobut-2-ene is synthesized. The method has the advantages that raw materials are conveniently sourced and available, and are easy to transport and store; unreacted raw materials in reaction products can be recycled, and the production cost is greatly reduced; meanwhile, the conversion rate and selectivity are high, so that the possibility of continuous industrialized production is greatly increased.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and is a method for preparing perfluoro-2-butene in a gas phase by using pentafluoroethane and iodine simple substance under the action of a catalyst under high temperature conditions. Background technique [0002] In the semiconductor industry, the dry etching gas that has been widely used in dielectric etching mainly contains CF 4 、C 2 f 6 、C 3 f 8 and c-C 4 f 8 And other PFCs substances. Since such substances have high GWP values, it is urgent to find their substitutes. At present, several different types of PFCs replacement candidates have emerged, including hydrofluorocarbons, iodofluorocarbons, unsaturated fluorocarbons (UFCs), etc., among which UFCs are considered to be good substitutes, firstly because of their own double bonds It can easily react with hydroxyl radicals and decompose in the atmosphere. Secondly, it has good etching properties and can be well used in the semiconduc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/278
CPCC07C17/278C07C21/18
Inventor 庆飞要陈朝晖郭占英权恒道
Owner 泉州宇极新材料科技有限公司
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