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Preparation method of E-1-halogen-3, 3, 3-trifluoropropene

A technology of trifluoropropene and Z-1-, which is applied in the preparation of halogenated hydrocarbons, dehalogenation, halogen substitution, etc., can solve the problems of difficult recycling, high reaction pressure, low selectivity, etc., and reach the service life Long, high yield per pass, high activity effect

Active Publication Date: 2021-04-30
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The above prior art has the following disadvantages: (1) Although the ionic liquid catalysis has the advantages of high selectivity and high yield of the target product E-1,3,3,3-tetrafluoropropene, the price of the ionic liquid is too expensive, It is difficult to recycle; the process is a high-pressure intermittent reaction, and there are great safety hazards; (2) SbCl 5 or SbF 5 The liquid-phase fluorination of the catalyst is an intermittent process in terms of technology, the reaction pressure is high, the catalyst is difficult to recycle and reuse, it is easy to generate a large amount of solid waste, and seriously pollutes the environment, and its main products are 1,1,1,3,3 - pentafluoropropane, while the yield of E-1-chloro-3,3,3-trifluoropropene is not disclosed, but according to the literature it can be inferred that its yield is less than 43%, there is E-1-chloro-3, The defect of low yield of 3,3-trifluoropropene; (3) The target product E-1-chloro-3,3,3-trifluoropropene or E-1,3,3, Defects of lower yield and lower selectivity of 3-tetrafluoropropene

Method used

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  • Preparation method of E-1-halogen-3, 3, 3-trifluoropropene

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Preparation of block catalyst: (1) Dissolve tungsten trichloride in water, then dropwise add 10% by mass ammonia water to completely precipitate metal ions, adjust the pH value to 7.0-9.0, and make it fully precipitate under stirring conditions , aged for 24 hours, filtered the formed slurry, then dried at 150°C for 18 hours, pulverized the solid, and pressed into shape to obtain a carrier precursor; the obtained carrier precursor was roasted at 400°C under a nitrogen atmosphere After 18 hours, it was activated at 300°C for 18 hours with a mixed gas consisting of hydrogen fluoride and nitrogen with a molar ratio of 1:2 to obtain a carrier, which was confirmed to be tungsten oxyfluoride by XPS detection; (2) in dry, high-purity In nitrogen or helium or argon atmosphere, according to 20% SbF in block catalyst 5 Composed of 80% tungsten oxyfluoride mass percentage content, the precursor of the active component SbCl 5 Coating on tungsten oxyfluoride to obtain a catalyst pr...

Embodiment 2

[0057] The same operation as in Example 1, the difference is that the block catalyst is made of 30%SbF 5 Composed with 70% tungsten oxyfluoride, and the reaction temperature was changed to 100°C, the reaction result was: the conversion rate of 1,1,1,3,3-pentachloropropane was 54.6%, E-1-chloro-3,3, The selectivity of 3-trifluoropropene was 99.1%, and the selectivity of Z-1-chloro-3,3,3-trifluoropropene was 0.9%.

Embodiment 3

[0059] The same operation as in Example 1, the difference is that the block catalyst is made of 20%SbF 5 Composed of 80% tungsten oxyfluoride, and the reaction temperature was changed to 150°C, the reaction result was: the conversion rate of 1,1,1,3,3-pentachloropropane was 71.6%, E-1-chloro-3,3, The selectivity of 3-trifluoropropene was 97.4%, and the selectivity of Z-1-chloro-3,3,3-trifluoropropene was 2.6%.

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Abstract

The invention discloses a preparation method of E-1-halogen-3, 3, 3-trifluoropropene. The preparation method comprises the following steps: in the presence of a block catalyst, carrying out gas-phase fluorination reaction on 1, 1, 1, 3, 3-pentachloropropane and hydrogen fluoride in a tubular reactor to obtain a main product E-1-chlorine-3, 3, 3-trifluoropropene and a small amount of product Z-1-chlorine-3, 3, 3-trifluoropropene; furthermore, in the presence of the block catalyst, E-1-chlorine-3, 3, 3-trifluoropropene or / and Z-1-chlorine-3, 3, 3-trifluoropropene and hydrogen fluoride are subjected to a gas-phase fluorination reaction in the tubular reactor, and a main product E-1, 3, 3, 3-tetrafluoropropene is obtained. The one-way yield of the method is high; especially for the second-step process, only HCl in the product flow in the first step needs to be removed, and the remaining substances can be directly used for fluorination reaction after new HF is added. The block catalyst has the characteristics of high activity and long service life.

Description

technical field [0001] The present invention relates to a method for preparing E-1-halo-3,3,3-trifluoropropene (halogen = fluorine or chlorine) by catalyzed fluorination with a block catalyst, especially relates to a method with 1,1,1,3 , 3-pentachloropropane as the starting material, the method of co-producing E-1-halo-3,3,3-trifluoropropene (halogen = fluorine, chlorine) through gas-phase fluorination reaction, wherein 1-halo-3, 3,3-Trifluoropropene includes E-1,3,3,3-tetrafluoropropene and E-1-chloro-3,3,3-trifluoropropene. Background technique [0002] Currently, 1,1,1,3,3-pentafluoropropane, E-1,3,3,3- Tetrafluoropropene or E-1-chloro-3,3,3-trifluoropropene methods mainly include the following three categories: [0003] (1) Ionic liquid [0004] CN105849072A reported that 300 grams of hydrogen fluoride, 250 grams of 1,1,1,3,3-pentachloropropane, 6 grams of EMIm (HF) 2.3 F (EMIm refers to 1-ethyl 3-methylimidazolium) ionic liquid is charged into the reactor at room t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/383C07C21/18C07C17/20B01J27/135
CPCB01J27/135C07C17/20C07C17/23C07C17/383C07C21/18
Inventor 贾晓卿张妮董利张呈平
Owner 泉州宇极新材料科技有限公司
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