A kind of preparation method and device of 2,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and tetrafluoropropane, which is applied in the field of preparation of 2,3,3,3-tetrafluoropropene, can solve the problems of low reaction selectivity, difficult product separation, low conversion rate, etc., and achieve the total conversion rate High, overcome difficult to separate, low cost effect

Active Publication Date: 2021-06-08
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI +1
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  • Description
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Problems solved by technology

[0029] Aiming at the defects of low reaction selectivity, difficult product separation and low conversion rate in the preparation of HFO-1234yf by using HFC-244cc as raw material in the prior art, the present invention provides a kind of 2,3,3,3-tetrafluoropropene The preparation method and device, through the improvement of the device and reaction engineering process, realize the high selectivity and high yield of the reaction

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  • A kind of preparation method and device of 2,3,3,3-tetrafluoropropene
  • A kind of preparation method and device of 2,3,3,3-tetrafluoropropene
  • A kind of preparation method and device of 2,3,3,3-tetrafluoropropene

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Embodiment 1

[0085] (1) Preparation of raw material 1,1,1,3-tetrachloro-2,2,3,3-tetrafluoropropane (CFC-214cb) by addition of tetrafluoroethylene and carbon tetrachloride:

[0086] CCl 4 +TFE→CFC-214cb

[0087] In a 10L stainless steel autoclave, carbon tetrachloride (10.0kg, 65.0mol) was added, and anhydrous aluminum chloride (0.5kg, 3.7mol) was used to replace three times with tetrafluoroethylene under stirring conditions. Heat the internal temperature to 60-70°C, then feed tetrafluoroethylene (TFE) into the autoclave, maintain the pressure at 3-5 atm, until the reaction system does not absorb tetrafluoroethylene, stir the reaction for about 12 hours, and put the high-pressure After the kettle was cooled to room temperature, the material was discharged, and the obtained material was added to 1.5 L of 2.0 mol / L hydrochloric acid under stirring conditions, stirred, and static liquid separation. The organic phase was separated and purified by rectification using a 1.0-meter-long rectificat...

Embodiment 2

[0095] (1) Preparation of raw material 1,1,3-trichloro-2,2,3,3-tetrafluoropropane (CFC-214cb) by addition of tetrafluoroethylene and chloroform:

[0096] CHCl 3 +TFE→HFC-224ca

[0097] In a 10L stainless steel autoclave, add chloroform (10.0kg, 83.8mol), use anhydrous aluminum chloride (1.12kg, 8.4mol), and under stirring conditions, use tetrafluoroethylene to replace three times, and heat the inner temperature of the reactor to 70-80°C, then feed tetrafluoroethylene (TFE) into the autoclave, maintain the pressure at 5-8 atm, until the reaction system does not absorb tetrafluoroethylene, stir the reaction for about 24 hours, and cool the autoclave to After discharging at room temperature, add the obtained material into 3.4L of 2.0mol / L hydrochloric acid under stirring conditions, stir, and separate liquids at rest. The organic phase is separated and purified by rectification using a 1-meter-long rectification column. Collect 90 ~ Fraction between 93°C, the product 1,1,3-tric...

Embodiment 3

[0105] Alumina-supported catalyst preparation.

[0106] Preparation of Catalyst-1:

[0107] (1) Take 500 g of a spherical alumina carrier with a diameter between 1 and 2 mm, bake it at 450° C. for 4 hours, and store it under dry conditions for later use. Characterization results of physical and chemical properties of the carrier: the specific surface area is 320m 2 / g, the average pore diameter is 9.1nm, the pore volume is 0.73mL / g, the acidity of infrared pyridine adsorption Lewis acid is 0.083mmol pyridine / g (160°C), 0.052mmol pyridine / g (450°C).

[0108] (2) Weigh 150g titanium tetrachloride (TiCl 4 ) was dissolved in 100mL dilute hydrochloric acid (0.1mol / L), and set aside;

[0109] (3) Take 100 g of the above-mentioned calcined alumina carrier in a rotating container (drum), spray 80 mL of dilute hydrochloric acid solution of titanium tetrachloride, and rotate for 20 minutes after the spraying;

[0110] (4) The impregnated catalyst was dried at 120° C. for 4 hours, an...

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Abstract

The invention provides a preparation method and device for 2,3,3,3-tetrafluoropropene. The device for preparing 2,3,3,3-tetrafluoropropene includes a loop reactor, a first rectification tower, a first cooling tower, a second rectification tower and a second cooling tower. The method of the present invention adopts continuous loop reactor technology, realizes the technology of separating hydrogen chloride by-product in real time under reaction conditions, the selectivity of the reaction is greatly improved, and the total conversion rate of the reaction is very high because the continuous circulation operation of raw materials is realized. . The 2,3,3,3-tetrafluoropropene obtained by the present invention has the advantages of low cost, less by-products and wastes of the production technology, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method and device of 2,3,3,3-tetrafluoropropene. Background technique [0002] The research and development of fluorine refrigerant substitutes has always been a hot topic in the world. As an ideal refrigerant, ODP value (ozone depletion potential value) is required to be 0, GWP value (greenhouse gas effect potential value) is low, and the atmospheric life is short. As the third generation refrigerant, HFC-134a is widely used in the field of automobile refrigerants. Although the ODP value of HFC-134a is 0, the GWP value is as high as 1300. Leakage or waste will easily cause the greenhouse effect and cause global warming. The lifespan in the atmosphere is as long as 44 years, and the United States and the European Union have successively begun to restrict its use. [0003] It is imminent to find new environmentally friendly refrigerants with low GWP value and short atmospheric residence time. At present, 2,3,3,3-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/25C07C17/358C07C21/18
CPCC07C17/25C07C17/358C07C21/18C07C19/10
Inventor 肖吉昌林锦鸿沈伯清
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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