Preparation method for 1,1,1,3-tetrafluoropropene

A technology of tetrafluoropropene and trifluoropropene, which is applied in halogen substitution preparation, dehydrohalogenation preparation and other directions, can solve the problems of difficult availability, low selectivity of HFO-1234ze, high price of raw material HCFC-1233zd, etc., and achieves improved selectivity. Effect

Inactive Publication Date: 2008-07-09
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the methods for preparing HFO-1234ze mostly use 1-chloro-3,3,3-trifluoropropene (HCFC-1233zd) as a raw material. Japanese patent JP10007604 discloses a one-step gas phase catalytic fluorination of HCFC-1233zd to synthesize HFO-1234ze The method uses Cr, Ti, Al, Mn, Ni, Co and other metal oxides loaded on activated carbon as catalysts, which has a high single-pass conversion rate, but this method is prone to further fluorination of the target product HFO-1234ze to generate HFC- The reaction of 245fa leads to low selectivity of the target product HFO-1234ze, and the raw material HCFC-1233zd is expensive and difficult to obtain

Method used

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  • Preparation method for 1,1,1,3-tetrafluoropropene

Examples

Experimental program
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Effect test

Embodiment 1

[0030] In a nickel tube reactor with an inner diameter of 38 mm, add 50 ml of chromium-based fluorination catalyst containing Al, Zn, Mg, and Ni metal powders. HCC-240fa and HF enter the reactor to react. The reaction conditions are: the molar ratio of HF to HCC-240fa is 20, the reaction temperature is 300°C, the contact time is 7s, and the reaction pressure is 0.25Mpa. After 20 hours, the reaction product was washed with water, washed with alkali, and dried with alkali to remove HCl and HF, and then analyzed by gas chromatography. The reaction results are listed in Table 1.

Embodiment 2

[0032] The same operation as in Example 1, the difference is that the organic phase HCC-240fa at the reactor inlet is changed into a mixture of 40% by volume of HCC-240fa and 50% of HCFC-1233zd and 10% of HFC-245fa , and the results are listed in Table 1.

[0033] Table 1

[0034] Example

[0035] Other products include CF 3 CH 2 CHFCl (HCFC-244fa), CF 3 CH 2 CHCl 2 (HCFC-243fa), and traces of heavy substances C 6 h 4 f 7 Cl, C 6 h 4 f 6 Cl 2 、C 6 h 2 f 6 Cl 2 、C 6 h 3 f 6 Cl 3 Wait

Embodiment 3

[0037] In a nickel tube reactor with an inner diameter of 38 mm, add 50 ml of chromium-based fluorination catalyst containing Al, Zn, Mg, and Ni metal powders. The organic phase is composed of a mixture of 40% HCC-240fa and 55% HCFC-1233zd and 5% HFC-245fa by volume, and HF enters the reactor for reaction. The reaction conditions are: reaction temperature 280°C, total amount of HF and organic phase The molar ratio is 20, the contact time is 5s, and the reaction pressure is 0.02 Mpa. After 20h, the reaction product was washed with water, washed with alkali, and dried with alkali to remove HCl and HF, and then analyzed by gas chromatography. The reaction results are listed in Table 3.

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Abstract

The invention discloses a process for preparing 1, 1, 1, 3-HFO-1234ze, which resolves the problem of low selectivity of HFO-1234ze. The invention takes 1, 1, 1, 3, 3-HCC-240fa as raw material, including the following steps that a, placing hydrogen fluoride (HF) and HCC-240fa into a reactor to react with fluorination catalyst, b, distilling and detaching the produced fluid in step a which flows into a distillation tower, the tower bottom components of 1, 1, 1, 3, 3-HCC-240fa, 1-chlorine-3, 3, 3-HCFC-1233zd and hydrogen fluoride recycle to the reactor, the tower top components of hydrogen fluoride and HFO-1234ze enter after-treatment system and obtaining object product HFO-1234ze after processes of deoxidation, dehydration and distillation and the like. The invention is mainly used to prepare HFO-1234ze.

Description

technical field [0001] The invention relates to a preparation method of 1,1,1,3-tetrafluoropropene (referred to as HFO-1234ze), in particular to a gas-phase catalytic fluorination of 1,1,1,3,3-pentafluoropropene with hydrogen fluoride (referred to as HF). Chloropropane (referred to as HCC-240fa) for the preparation of 1,1,1,3-tetrafluoropropene. Background technique [0002] In recent years, the problem of global warming has become increasingly serious, and reducing greenhouse gas emissions has become one of the focuses of global environmental protection. 1,1,1,3-Tetrafluoropropene, due to its zero ozone depletion potential (ODP) and low greenhouse effect potential (GWP), is considered to have the most potential to replace the greenhouse gas 1,1,1,2- The third-generation ODS substitute of tetrafluoroethane (HFC-134a), widely used as refrigerant, blowing agent, aerosol propellant, solvent, etc. In addition, HFO-1234ze can also be used as a fluorinated monomer, which is the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/25C07C17/20
Inventor 吕剑王博张伟寇联岗马洋博郝志军
Owner XIAN MODERN CHEM RES INST
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