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A method for synthesizing 2,3,3,3-tetrafluoropropene by multi-step continuous reaction of hexafluoropropene

A technology of hexafluoropropene and tetrafluoropropene, which is applied in the preparation of dehydrohalogenation, organic chemistry, etc., can solve the problems of cumbersome process control, complex process steps, large equipment investment, etc., to simplify the process flow, simplify the synthesis process, reduce the The effect of equipment investment

Active Publication Date: 2015-12-23
JUHUA GROUP TECH CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the methods provided by these patents, the product of each step of the reaction must be separated before entering the next step of the reaction, which requires a lot of separation equipment. There are complex process steps, large equipment investment, high separation cost, high energy consumption, and more waste discharge. Disadvantages: In addition, when HFO-1225ye is hydrogenated to generate 1,1,1,2,3-pentafluoropropane (HFC-245eb), hydrogen or hydrogen / nitrogen mixed gas needs to be added again, and the process control is cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A method for synthesizing 2,3,3,3-tetrafluoropropene by the multi-step continuous reaction of hexafluoropropene, comprising the following steps:

[0043] (1) Fill a 14mm 316L tube with 10ml1%Pd / Al2O3 (the mass percentage of Pd is 1%) catalyst, place the 316L tube in an oil bath, heat up to 100°C, and pass in hexafluoropropylene and hydrogen for reaction, control h 2 The molar ratio to HFP is 10, and the space velocity is 1000h -1 , the reaction pressure is normal pressure, and the gas phase product containing 1,1,1,2,3,3-hexafluoropropane is obtained;

[0044] (2) The gas-phase product obtained in step (1) is directly passed into a saponification reactor for dehydrofluorination reaction. In the saponification reactor, 1000 g of KOH aqueous solution with a mass percentage concentration of 50% and 50 g of dimethyl sulfoxide are added, and the reaction temperature is 90°C, the reaction pressure is normal pressure, and the gas phase product containing 1,1,1,2,3-pentafluor...

Embodiment 2

[0048] A method for synthesizing 2,3,3,3-tetrafluoropropene by the multi-step continuous reaction of hexafluoropropene, comprising the following steps:

[0049] (1) Fill 10ml Pd / Al in a 14mm 316L tube 2 o 3 (The mass percentage of Pd is 1%) catalyst, 316L tube is placed in an oil bath, the temperature is raised to 30°C, and hexafluoropropylene and hydrogen are introduced to react, and the H 2 The molar ratio to HFP is 20, and the space velocity is 500h -1 , the reaction pressure is normal pressure, and the gas phase product containing 1,1,1,2,3,3-hexafluoropropane is obtained;

[0050] (2) The above-mentioned gas phase product containing 1,1,1,2,3,3-hexafluoropropane is directly passed into a saponification reactor for dehydrofluorination reaction, and 1000 g of 60% by mass concentration of hexafluoropropane is added to the saponification reactor KOH aqueous solution and 20 g of dimethyl sulfoxide, the reaction temperature is 80 ° C, the reaction pressure is normal pressure...

Embodiment 3

[0054] A method for synthesizing 2,3,3,3-tetrafluoropropene by the multi-step continuous reaction of hexafluoropropene, comprising the following steps:

[0055] (1) Fill a 14mm 316L tube with 10ml of Pd / C (the mass percentage of Pd is 0.1%) catalyst, place the 316L tube in an oil bath, raise the temperature to 150°C, and pass in hexafluoropropylene and hydrogen to react, and control the H 2 The molar ratio to HFP is 3, and the space velocity is 500h -1 , the reaction pressure is normal pressure, and the gas phase product containing 1,1,1,2,3,3-hexafluoropropane is obtained;

[0056] (2) The above-mentioned gas phase product containing 1,1,1,2,3,3-hexafluoropropane is directly passed into the saponification reactor for dehydrofluorination reaction, and 1000g of 10% by mass concentration is added to the saponification reactor KOH aqueous solution and 50g of dimethylformamide, the reaction temperature is 50°C, and the reaction pressure is normal pressure to obtain a gas phase pr...

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Abstract

The invention discloses a method for synthesizing 2,3,3,3-tetrafluoropropene through multi-step successive reaction of hexafluoropropylene, which comprises the following steps: (1) performing hydrogenation reaction on hexafluoropropylene and hydrogen gas to generate a product containing 1,1,1,2,3,3-hexafluoropropane; (2) directly introducing the product containing the 1,1,1,2,3,3-hexafluoropropane into a mixture of an alkaline solution and organic solvent, and performing dehydrofluorination to generate a product containing 1,1,1,2,3-pentafluoropropene; (3) dehydrating the product containing the 1,1,1,2,3-pentafluoropropene, and performing hydrogenation reaction to generate a product containing 1,1,1,2,3-pentafluoropropane; and (4) directly introducing the product containing the 1,1,1,2,3-pentafluoropropane into a mixture of an alkaline solution and organic solvent, and performing dehydrofluorination to generate the 2,3,3,3-tetrafluoropropene. The method has the advantages of simple process, less equipment investment, low energy consumption and less discharge of three wastes.

Description

technical field [0001] The invention relates to a synthesis method of 2,3,3,3-tetrafluoropropene, in particular to a method for synthesizing 2,3,3,3-tetrafluoropropene by multi-step continuous reaction of hexafluoropropene. Background technique [0002] HFO-1234yf is 2,3,3,3-tetrafluoropropene, its ODP is zero, its GWP value is 4, its atmospheric life is only 11 days, it has excellent physical and chemical properties, its molecular weight is similar to that of HFC-134a, and its Its boiling point and high saturated vapor pressure at room temperature, and its density and critical point are similar to HFC-134a, so it is considered as a "direct substitute" for HFC-134a and a potential low-carbon refrigerant. [0003] According to the literature and patents, the current synthesis routes of HFO-1234yf mainly include: tetrafluoroethylene method, trifluoropropyne method, trifluoropropylene method, tetrafluoropropanol method, hexafluoropropylene method (HFP), four Chloropropene meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/25
Inventor 杨仲苗周强周黎旸王树华雷俊吴奕
Owner JUHUA GROUP TECH CENT
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