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

A technology of tetrafluoropropene and 1.E-1, which is applied in the field of preparation of E-1,3,3,3-tetrafluoropropene, can solve the problems of low single-pass yield, high reaction energy consumption, and low reaction temperature

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

AI Technical Summary

Problems solved by technology

[0016] Among the above-mentioned numerous synthetic routes, there are the following problems: (1) The single-pass yield of E-1,3,3,3-tetrafluoropropene is low, and the product 1,3,3,3-tetrafluoropropene synthesized by the reaction It is a mixture of E-1,3,3,3-tetrafluoropropene and Z-1,3,3,3-tetrafluoropropene, the molar ratio n(E-1,3,3,3-tetrafluoropropene Propylene) / n(Z-1,3,3,3-tetrafluoropropene) is mostly close to 6 / 1, therefore, the per-pass yield of E-1,3,3,3-tetrafluoropropene is generally less than 90%; ( 2) The reaction of olefins and halogenated alkanes to telomerize raw materials is mostly a liquid phase reaction. Using a large amount of solvents and initiators will generate a large amount of liquid waste and solid waste, which will seriously pollute the environment; (3) Some reaction temperatures are too low (such as -30 degrees to -60 degrees bromine fluorination reaction), some reaction temperatures are too high (such as 525 degrees dehydrobromination reaction), these reactions consume too much energy

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0042] The preparation of embodiment 1 trifluoropropadiene

[0043] 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 20%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 oxygen to 1,2,3,3,4,4,5-heptafluorocyclopentene is 1:1, the contact time is 0.25s, and the reaction pressure is 0.1MPa. The reaction product was collected by a polytetrafluoroethylene sampling bag. After 10 hours, a sample was taken from the samp...

Embodiment 2

[0045] Example 2 Preparation of 3,3,3-trifluoropropyne

[0046] Preparation of isomerization catalyst: Put molybdenum trioxide in the reactor, at a temperature of 400°C, pass a mixed gas composed of chlorodifluoromethane and nitrogen with a substance ratio of 1:4, activate for 12 hours, stop the flow into the mixed gas to obtain the catalyst.

[0047] 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 trifluoropropadiene 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 results are: the conversion rate of trifluoropropadiene is 100%, and the selectivity of 3,3,3-trifluoropropyne is 99.8%.

Embodiment 3

[0050] Preparation of fluorination catalyst: According to the percentage composition of tungsten and cobalt elements of 90% and 10%, tungsten trichloride and cobalt nitrate are dissolved in water, concentrated ammonia water is added dropwise for precipitation, the pH value is adjusted to 7.5, and then aged 24 hours, washed with water, filtered, dried in an oven at 120°C for 15 hours, crushed the obtained solid, and pressed into tablets to obtain a catalyst precursor. Put 10 mL of the catalyst precursor into a Monel with an inner diameter of 1 / 2 inch and a length of 30 cm Tubular reactor made of material, filled with nitrogen and baked at 350°C for 12 hours, nitrogen space velocity is 200h -1 , and then lower the temperature to 300°C, and at the same time pass a mixed gas composed of hydrogen fluoride and nitrogen with a mass ratio of 1:2, and the total space velocity of the gas is 220h -1 , activate for 12 hours, stop the above mixed gas, and prepare the tungsten-based catalys...

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Abstract

The invention discloses a preparation method of E-1, 3, 3, 3-tetrafluoropropene, which comprises the following steps: by taking 3, 3, 3-trifluoropropyne or / and an isomer 1, 3, 3-trifluoropropadiene thereof as a raw material, carrying out gas-phase selective fluorination reaction in the presence of a fluorination catalyst to obtain E-1, 3, 3, 3-tetrafluoropropene. The method provided by the invention is mainly used for producing E-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 E-1,3,3,3-tetrafluoropropene with high conversion rate and high selectivity, in particular to a method for preparing E-1,3,3-tetrafluoropropene with 3,3,3-trifluoropropyne or / and its isomerization The method for preparing E-1,3,3,3-tetrafluoropropene with high conversion rate and high selectivity through gas-phase hydrogen fluoride addition reaction as raw material, and raw material 3, Synthesis of 3,3-trifluoropropyne and its isomer 1,3,3-trifluoropropadiene. Background technique [0002] Up to now, the synthesis routes of 1,3,3,3-tetrafluoropropene mainly include the following types: [0003] (1) Using vinyl fluoride as raw material [0004] US2005245773A1 reported that the steps of synthesizing 1,3,3,3-tetrafluoropropene with vinyl fluoride as the starting material are as follows: first, in an autoclave, vinyl fluoride and trifluoroiodomethane were reacted at 200 degrees for 48 hours to obtain an int...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/087C07C21/18C07C17/358C07C21/22C07C17/361C07C21/19C07C51/58C07C53/50B01J27/132B01J27/138B01J37/03B01J37/08B01J37/26
CPCB01J27/132B01J27/138B01J37/031B01J37/082B01J37/26C07C17/087C07C17/358C07C17/361C07C51/58C07C53/50C07C21/19C07C21/22C07C21/18
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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