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Preparation method of Z-1, 3, 3, 3-tetrafluoropropene

A technology of tetrafluoropropene and Z-1, which is applied in the field of highly selective preparation of Z-1,3,3,3-tetrafluoropropene, which can solve the problem of low yield of tetrafluoropropene in one pass

Active Publication Date: 2021-05-18
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

[0009] To sum up, the problem with the above technical scheme is that the yield per pass of Z-1,3,3,3-tetrafluoropropene is too low, the highest is only 31.1% (see CN101535228B)
Up to now, there is no literature report on a method for synthesizing Z-1,3,3,3-tetrafluoropropene that simultaneously satisfies high conversion rate and high selectivity

Method used

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  • Preparation method of Z-1, 3, 3, 3-tetrafluoropropene

Examples

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Embodiment 1

[0036] The preparation of embodiment 1 tetrafluoropropadiene

[0037] Step (1): Dissolve an appropriate amount of silver nitrate in an appropriate amount of water according to the mass percentage of silver oxide and carrier, add aluminum fluoride carrier, impregnate for 18 hours, then filter, dry in an oven at 80°C for 24 hours, and then place Under the protection of nitrogen, calcined at 400° C. for 10 hours to obtain the oxidation catalyst. Fill 10 milliliters of the oxidation catalyst 10%Ag prepared by the above-mentioned method in the tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30 cm 2 O / AlF 3 . The reaction conditions are as follows: the reaction temperature is 260°C, the molar ratio of the inert gas helium, oxygen and octafluorocyclopentene is 1:1:1, the contact time is 0.1s, and the reaction pressure is 0.1MPa. The reaction product was collected by a polytetrafluoroethylene sampling bag. After 10 hours, a sample was taken fr...

Embodiment 2

[0039] Example 2 Preparation of 1,3,3,3-tetrafluoropropyne

[0040] Preparation of isomerization catalyst: put alumina in the reactor, at a temperature of 400°C, feed a mixed gas composed of chlorodifluoromethane and nitrogen with a substance ratio of 1:4, activate for 12 hours, and stop feeding Mixed gas, prepared catalyst.

[0041] 10 mL of the above-prepared catalyst was filled in a tubular reactor made of Inconium alloy with an inner diameter of 1 / 2 inch and a length of 30 cm. The reaction conditions are as follows: the reaction temperature is 20° C., the contact time of tetrafluoropropadiene is 60 s, and the reaction pressure is 0.1 MPa. After running for 10 hours, the reaction product was collected and heated, and the gas phase organic phase was taken for GC analysis. The reaction result is: the conversion rate of tetrafluoropropadiene is 100%, and the selectivity of 1,3,3,3-tetrafluoropropyne is 99.5%.

Embodiment 3

[0043] Preparation of hydrogenation catalyst: according to Pd, Bi, AlF 3 The mass percentages of the three are respectively 2%: 0.2%: 97.8%. Palladium chloride and bismuth chloride are dissolved in water together, and the pH value of the solution is adjusted to 4 to 6 with dilute hydrochloric acid to obtain an impregnating solution; and room temperature conditions, the impregnating solution to the carrier AlF 3 Add dropwise, after the dropwise addition, maintain immersion for 4 hours, filter and dry to obtain the catalyst precursor; dry the catalyst precursor at 120°C for 8 hours under the protection of nitrogen, then heat up to 300°C for 8 hours, and then use nitrogen The mixed gas with a molar ratio of 4:1 to hydrogen was activated at 250°C for 14 hours to obtain a hydrogenation catalyst. It was confirmed by XRD that the existing forms of Pd and Bi in the hydrogenation catalyst were simple substances.

[0044] 10 mL of the above-prepared catalyst was filled in a tubular rea...

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Abstract

The invention discloses a preparation method of Z-1, 3, 3, 3-tetrafluoropropene, which comprises the following steps: by taking 1, 3, 3, 3-tetrafluoropropyne or / and an isomer 1, 1, 3, 3-tetrafluoropropadiene thereof as a raw material, carrying out gas-phase selective hydrogenation in the presence of a hydrogenation catalyst to obtain the Z-1, 3, 3, 3-tetrafluoropropene. The method provided by the invention is mainly used for producing Z-1, 3, 3, 3-tetrafluoropropene in a high-efficiency and gas-phase continuous circulation manner.

Description

technical field [0001] The invention relates to a method for preparing Z-1,3,3,3-tetrafluoropropene with high conversion rate and high selectivity, in particular to a method for preparing Z-1,3,3,3-tetrafluoropropyne or / and its isomerism Constituent 1,1,3,3-tetrafluoropropadiene is used as raw material, and Z-1,3,3,3-tetrafluoropropene is prepared with high conversion rate and high selectivity through gas phase hydrogenation reaction, and raw material 1-3 , Synthesis of 3,3-tetrafluoropropyne and its isomer 1,1,3,3-tetrafluoropropadiene. 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-tetrafluoropropen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/354
CPCC07C17/354C07C21/18
Inventor 贾晓卿张呈平庆飞要权恒道
Owner 泉州宇极新材料科技有限公司
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