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The preparation method of z-1-halo-3,3,3-trifluoropropene

A trifluoropropene, Z-1- technology, applied in the preparation of halogenated hydrocarbons, halogen substitution preparation, organic chemical methods, etc., to achieve the effects of high single-pass single rate, long service life and high activity

Active Publication Date: 2021-07-16
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Up to now, there is no literature report on a catalyst that satisfies both high conversion rate and high selectivity for the reaction of isomerization of E-1,3,3,3-tetrafluoropropene

Method used

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  • The preparation method of z-1-halo-3,3,3-trifluoropropene
  • The preparation method of z-1-halo-3,3,3-trifluoropropene

Examples

Experimental program
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Effect test

Embodiment 1

[0052] 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

[0055] 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

[0057] The same operation as in Example 1, the difference is that the block catalyst is made of 25%SbF 5 Composed with 75% 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 Z‑1‑halo‑3,3,3‑trifluoropropene. In the presence of a block catalyst, in a tubular reactor, E‑1‑halo‑3,3,3 -Trifluoropropene undergoes gas phase isomerization reaction to obtain Z-1-halo-3,3,3-trifluoropropene, wherein halogen=fluorine or chlorine, the present invention uses 1,1,1,3,3-pentachloro Propane is used as the starting material, and Z-1-chloro-3,3,3-trifluoropropene or Z-1,3,3,3-tetrafluoropropene are prepared by gas-phase fluorination reaction and isomerization reaction Products, the present invention independently circulates the incompletely reacted materials through the gas phase independent circulation process, so that the initial raw materials can be almost completely converted into the target product, and finally the target product is extracted from the process system, so that no liquid waste and waste gas are generated, and the realization of Green production.

Description

technical field [0001] The present invention relates to a preparation method of Z-1-halo-3,3,3-trifluoropropene, in particular to a method of using 1,1,1,3,3-pentachloropropane as a starting material through gas-phase fluorination reaction , Isomerization reaction to produce Z-1-halo-3,3,3-trifluoropropene (halogen = fluorine or chlorine). Background technique [0002] Since the compound energy of Z-1,3,3,3-tetrafluoropropene is higher than that of E-1,3,3,3-tetrafluoropropene, its stability is lower than that of E-1,3,3,3-tetrafluoropropene Propylene, so in the gas phase fluorination of E-1-chloro-3,3,3-trifluoropropene or Z-1-chloro-3,3,3-trifluoropropene, 1,1,1,3,3 - In the dehydrofluorination reaction of pentafluoropropane, the main product is E-1,3,3,3-tetrafluoropropene, while Z-1,3,3,3-tetrafluoropropene is a by-product, and its content is much smaller than that of E -1,3,3,3-tetrafluoropropene, so none of the above methods is an ideal route for synthesizing Z-1,3,3...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/358C07C17/20C07C21/18B01J27/132B01J23/30
CPCB01J23/30B01J27/132C07B2200/09C07C17/206C07C17/358C07C21/18
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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