Preparation method of Z-1-halogen-3, 3, 3-trifluoropropene
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A technology of trifluoropropene and Z-1-, which is used in the preparation of halogenated hydrocarbons, halogen substitution preparation, organic chemical methods, etc.
Active Publication Date: 2021-04-30
泉州宇极新材料科技有限公司
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Up to now, there is no literature report on a catalyst that satisfies both high conversion
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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-halogen-3, 3, 3-trifluoropropene. The preparation method comprises the following steps: in the presence of a block catalyst, E-1-halogen-3, 3, 3-trifluoropropene is subjected to a gas phase isomerization reaction in a tubular reactor to obtain Z-1-halogen-3, 3, 3-trifluoropropene, and halogen is fluorine or chlorine. According to the preparation method, 1, 1, 1, 3, 3-pentachloropropane is used as an initial raw material, Z-1-chloro-3, 3, 3-trifluoropropene or Z-1, 3, 3, 3-tetrafluoropropene secondary product is prepared through a gas-phase fluorination reaction and an isomerization reaction, the materials which are not completely reacted are independently circulated through a 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 a process system, and thus liquid waste and waste gas are not generated, and green production is realized.
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...
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