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Process and special equipment for producing trifluoro ethylene with catalytic hydrogenolysis of chlorotrifluoroethylene

A technology of chlorotrifluoroethylene and trifluoroethylene, which is applied in the field of catalytic hydrogenolysis of chlorotrifluoroethylene to prepare trifluoroethylene, can solve the problems of low output per unit reaction volume, low conversion rate and selectivity, and large equipment investment, and achieves Process method and equipment optimization, high conversion rate and selectivity, and obvious economic benefits

Inactive Publication Date: 2009-04-08
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the low conversion rate and selectivity of the reaction of preparing trifluoroethylene by catalytic hydrogenolysis of chlorotrifluoroethylene or long operating cycle, low yield per unit reaction volume and too much equipment investment. However, it provides a process and special equipment for preparing trifluoroethylene by catalytic hydrogenolysis of chlorotrifluoroethylene, which can obtain higher conversion rate and selectivity, and can realize continuous operation and provide higher production capacity.

Method used

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  • Process and special equipment for producing trifluoro ethylene with catalytic hydrogenolysis of chlorotrifluoroethylene
  • Process and special equipment for producing trifluoro ethylene with catalytic hydrogenolysis of chlorotrifluoroethylene

Examples

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Effect test

Embodiment 1

[0039] Example 1 The temperature is 110°C, and the pulse frequency is 1 / 30min -1

[0040] Through the automatic regulating valve 1, through the liquid flow meter 2, into the three stainless steel autoclaves 7 with a volume of 1 L in series, 1.25 mol of raw material chlorotrifluoroethylene, 0.625 mol of hydrogen, 25 g of HCl acceptor zinc powder and The aqueous solution 350ml of reaction solvent 25% ethanol, raw material is fully stirred and mixed by motor agitator 4 in reactor 7, is stirred and reacted at 110 ℃ by temperature controller 6 control temperature, the 5%Pd in ​​the shaft plate frame 8 of stirring paddle Hydrogenolysis reaction occurs under the action of a catalyst of 0.7g / C; observe the pressure gauge 3, according to the pulse frequency, pulse feeding and discharging once every 30min, the feeding amount of hydrogen and chlorotrifluoroethylene is 1 / 10 of the gas pressure in the kettle , the molar ratio of hydrogen to chlorotrifluoroethylene is 0.5; with the feedin...

Embodiment 2

[0041] Example 2 The temperature is 100°C, and the pulse frequency is 1 / 60min -1

[0042] The process flow is the same as that in Example 1, and sequentially add 0.6 g of 5% Pd / C catalyst, 0.09375 mol of ammonia, 200 ml of solvent DMF, 0.75 mol of chlorotrifluoroethylene raw material, and 0.375 mol of hydrogen into two stainless steel autoclaves connected in series with a volume of 1 L. , stirring and reacting at 100°C, pulse feeding and discharging once every 60min, the feeding amount of hydrogen and chlorotrifluoroethylene is 1 / 8 of the gas pressure in the kettle, and the molar ratio of hydrogen to chlorotrifluoroethylene is 0.6; Taking the feeding amount of chlorotrifluoroethylene as a reference, the feeding amount of the hydrogen chloride acceptor is 0.75 times of the molar weight of chlorotrifluoroethylene, and the feeding amount of the solvent is 200ml / 1mol chlorotrifluoroethylene. Continuous operation for 24h consumes The raw material is 13mol of chlorotrifluoroethylen...

Embodiment 3

[0043] Example 3 The temperature is 200°C, and the pulse frequency is 1 / 10min -1

[0044] The technological process is the same as in Example 1, and successively add 0.625 g of 5% Pt / C catalyst, 15 mol of pyridine, 500 ml of solvent cyclohexane, 1.5 mol of chlorotrifluoroethylene raw material, hydrogen 2.7mol, stirring reaction at 200°C, pulse feeding and discharging once every 10min, the feeding amount of hydrogen and chlorotrifluoroethylene is 1 / 7 of the gas pressure in the kettle, and the molar ratio of hydrogen to chlorotrifluoroethylene is 0.7; With reference to the feeding amount of chlorotrifluoroethylene, the feeding amount of hydrogen chloride acceptor is 0.8 times of the molar weight of chlorotrifluoroethylene, and the feeding amount of solvent is 300ml / 1mol chlorotrifluoroethylene, continuous operation 24h, A total of 13 mol of raw material chlorotrifluoroethylene was consumed. Gas chromatographic analysis shows that the selectivity of trifluoroethylene is 95%, an...

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Abstract

The invention discloses a process method for preparing trifluoroethene through the catalytic hydrogenolysis of chlorotrifluoroethylene. Trifluoroethene can be prepared through the hydrogenolysis of hydrogen and chlorotrifluoroethylene under the action of a catalyst in a solvent containing a hydrogen chloride acceptor, wherein the hydrogen chloride acceptor, the solvent, hydrogen and chlorotrifluoroethylene, after the initial feeding, pulse type continuous operation is adopted both for the feeding and discharging of the reaction. The hydrogenolysis is carried out in one or a plurality of reaction kettles connected in series. The invention also discloses a special device for the technical method. The technical method has the advantages that the technical method can realize continuous operation, has a higher conversion rate and selectivity,can be easily applied to the industrialized production; in addition, the dosage of the hydrogen chloride acceptor and the solvent needed by unit chlorotrifluoroethylene is reduced, thereby bringing about obvious economic benefits; and the pulse intermittent feeding and discharging of liquid generate no solid residue in the kettle, thereby facilitating the stability of the reaction kettle.

Description

technical field [0001] The invention relates to a process and special equipment for preparing trifluoroethylene by catalytic hydrogenolysis of chlorotrifluoroethylene. Background technique [0002] Trifluoroethylene is an important monomer raw material for preparing many fluorine-containing polymers (homopolymer or copolymer), and is an important polymer monomer. For example, trifluoroethylene is an important finishing agent raw material for high-grade pure cotton fabrics; the copolymer with trifluoroethylene as the main body and vinylidene fluoride has extraordinary piezoelectric (electrostrictive) properties, so it can be used in human organs and Electronics industry has a wide range of application value. At the same time, trifluoroethylene is also an important intermediate for the synthesis of many other compounds. Tetrafluoroethane obtained by adding trifluoroethylene to anhydrous hydrogen fluoride is an environmentally friendly refrigerant tetrafluoroethane (HFC-134a);...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/23
Inventor 曹贵平粟小理孟保川车延超张明华孙朝阳
Owner EAST CHINA UNIV OF SCI & TECH
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