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Method for synthesizing hexafluoro-1,3-butadiene through gas-phase catalytic isomerization

A technology of isomerization of hexafluorobutadiene, applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., to achieve the effects of safe synthesis process, high yield, and simple technical route

Pending Publication Date: 2020-05-01
CHINA UNIV OF MINING & TECH (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few reports on the synthesis of hexafluoro-1,3-butadiene by gas phase isomerization

Method used

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  • Method for synthesizing hexafluoro-1,3-butadiene through gas-phase catalytic isomerization
  • Method for synthesizing hexafluoro-1,3-butadiene through gas-phase catalytic isomerization

Examples

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Effect test

Embodiment 1

[0021] The preparation of catalyst: adopt loading method, the steps are as follows: 5.0gNiCl 3 Dissolve in 100ml of deionized aqueous solution, and quickly pour the above solution into the dried alumina. After impregnating for 5 hours, the water was slowly drained using a rotary evaporator to obtain Ni / Al 2 o 3 catalyst.

[0022] Ni / Al 2 o 3 Catalyst drying process: 40mlNi / Al 2 o 3 The catalyst is loaded into the fixed bed reactor, and then the fixed bed reactor is heated with an open tube heating furnace. make Ni / Al 2 o 3 Under the protection of 50ml / min nitrogen, the catalyst is first raised to 400°C at a rate of 10°C / min and dried for 10 hours, and then the temperature is lowered to 200°C, thereby completing the Ni / Al 2 o 3 Catalyst drying process.

[0023] Ni / Al 2 o 3 Catalyst activation process: heat the fixed bed reactor to 200°C, first use 100ml / min nitrogen and 20ml / min hydrogen fluoride to activate and catalyze for 4 hours; then use 100ml / min nitrogen and...

Embodiment 2

[0026] The preparation of catalyst: adopt loading method, step is as follows: 4.75gMgCl 2 Dissolve in 100ml of deionized water solution, and quickly pour the above solution into 100g of dried alumina. After impregnating for 5 hours, the water was slowly drained using a rotary evaporator to obtain the Mg / Al 2 o 3 catalyst.

[0027] Mg / Al 2 o 3 Catalyst drying process: 40mlMg / Al 2 o 3 The catalyst is loaded into the fixed bed reactor, and then the fixed bed reactor is heated with an open tube heating furnace. Make Mg / Al 2 o 3 Under the protection of 50ml / min nitrogen, the catalyst is first raised to 400°C at a rate of 10°C / min and dried for 10 hours, then the temperature is lowered to 200°C, thus completing the Mg / Al 2 o 3 Catalyst drying process.

[0028] Mg / Al 2 o 3 Catalyst activation process: heat the fixed bed reactor to 200°C, first use 100ml / min nitrogen and 20ml / min difluorodichloromethane to activate and catalyze for 4 hours; then use 100ml / min nitrogen and...

Embodiment 3

[0031] The preparation of catalyst: adopt loading method, the steps are as follows: 6.30gNiCl 3 and 2.22g CaCl 2 Dissolve in 100ml of deionized aqueous solution, and quickly pour the above solution into 100g of molecular sieves that have been dried. After impregnating for 5 hours, the water was slowly drained using a rotary evaporator to obtain a Ni-Ca / MS catalyst.

[0032] The drying process of Ni-Ca / MS catalyst: 40ml of Ni-Ca / MS catalyst was loaded into the fixed-bed reactor, and then the fixed-bed reactor was heated with an open tube heating furnace. Under the protection of 50ml / min nitrogen, the Ni-Ca / MS catalyst is first raised to 400°C at a rate of 10°C / min and dried for 10 hours, and then the temperature is lowered to 200°C, thus completing the Ni-Ca / MS catalyst drying process.

[0033]Activation process of Ni-Ca / MS catalyst: Heat the fixed-bed reactor to 200°C, first use 100ml / min nitrogen and 20ml / min difluorochloromethane to activate and catalyze for 4 hours; then...

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Abstract

The invention relates to a method for synthesizing hexafluoro-1,3-butadiene through gas-phase catalytic isomerization, and belongs to the field of organic chemical synthesis. The method is characterized in that octafluorocyclobutene is heated under the action of an isomerization catalyst to generate hexafluoro-1,3-butadiene. The catalyst is good in stability and long in service life; the product separation and purification are simple; and the method is easy for industrial production.

Description

technical field [0001] The invention is a method for synthesizing hexafluoro-1,3-butadiene by gas-phase catalytic isomerization, and relates to a method for synthesizing hexafluoro-1,3-butadiene by isomerization with an easy industrial method. Background technique [0002] Hexafluoro-1,3-butadiene is a new type of electronic etching gas. It can not only be used as a monomer to prepare many fluoropolymer materials, but also can be used in dry etching of ultra-large-scale integrated circuits. The main Used in the field of semiconductor etching. Because of its good selectivity and aspect ratio, it has attracted strong attention from experts and scholars at home and abroad. There is a huge market for high-purity hexafluoro-1,3-butadiene. With the rapid development of electronic products, in the field of high-end dry etching, the market demand for high-purity hexafluoro-1,3-butadiene is increasing. [0003] There are few related studies on the preparation method of hexafluoro-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/358C07C21/18B01J23/755B01J21/10B01J29/072
CPCC07C17/358B01J23/755B01J21/10B01J29/072B01J2229/18C07C21/18
Inventor 周彪柯巍孙绪坤
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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