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Preparation method of 2,3,3,3-tetrafluoropropene

A technology of tetrafluoropropene and propylene, applied in the field of chemical synthesis, can solve the problems of low tetrafluoropropene yield, difficult catalyst preparation, etc., and achieve the effects of high economic value, large-scale industrial application prospects, and fewer by-products

Active Publication Date: 2019-04-12
ZHEJIANG SANMEI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this preparation method is that it consumes the toxic substance CF 3 CF 2 CH 3 , the disadvantage is the low yield of 2,3,3,3-tetrafluoropropene
The preparation method has a high conversion rate, but the catalyst CrO x f y more difficult to prepare

Method used

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  • Preparation method of 2,3,3,3-tetrafluoropropene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of 1,1,1,3,3-pentachloropropane

[0032] 1320gCCl 4 Join in 5L stainless steel autoclave I, add iron powder 30g and tributyl phosphate 142.7g to the reactor, seal the reactor; Control by gas mass flowmeter, slowly add CH to the reactor 2 CHCl520g, the pressure of the reactor passed through N 2 and CH 2 CHCl is adjusted by itself; the temperature of the reaction kettle is raised to 80°C, and the pressure is controlled at 2 bar. Under this condition, the reaction is stirred for 3 hours, and 1,527.1 g of 1,1,1,3,3-pentachloropropane is obtained after the reaction is completed.

[0033] (2) Preparation of 1,1,3,3-tetrachloro-1-propene

[0034] Add 700g 80% KOH solution and 1527.1g 1,1,1,3,3-pentachloropropane into 5L Hastelloy material autoclave II, pass N 2 The pressure of the reaction kettle was controlled; the pressure of the reaction kettle was controlled to be 3 bar and the temperature was 80° C. The reaction was stirred for 2 h under these conditio...

Embodiment 2

[0045] (1) Preparation of 1,1,1,3,3-pentachloropropane

[0046] 1320gCCl 4 Join in 5L stainless steel autoclave I, add iron powder 37.2g and tributyl phosphate 176.9g to the reactor, seal the reactor; Control by gas mass flowmeter, slowly add CH to the reactor 2 CHCl520g, the pressure of the reactor passed through N 2 and CH 2 CHCl self-adjusted; the temperature of the reaction kettle was raised to 120°C, and the pressure was controlled at 4 bar. Under this condition, the reaction was stirred for 5 hours, and 1619.8 g of 1,1,1,3,3-pentachloropropane was obtained after the reaction was completed.

[0047] (2) Preparation of 1,1,3,3-tetrachloro-1-propene

[0048] Add 694.2g of 80% KOH solution and 1619.8g of 1,1,1,3,3-pentachloropropane into 5L Hastelloy material autoclave II, pass N 2 The pressure of the reaction kettle was controlled; the pressure of the reaction kettle was controlled to be 4 bar, and the temperature was 140° C. Under these conditions, the reaction was sti...

Embodiment 3

[0059] (1) Preparation of 1,1,1,3,3-pentachloropropane

[0060] 1320gCCl 4 Join in 5L stainless steel autoclave I, add iron powder 40g and tributyl phosphate 190.2g to the reactor, seal the reactor; Control by gas mass flowmeter, slowly add CH to the reactor 2 CHCl520g, the pressure of the reactor passed through N 2 and CH 2 CHCl self-adjustment; the temperature of the reaction kettle was raised to 100°C, and the pressure was controlled at 3 bar, under this condition, the reaction was stirred for 4 hours, and 1632.2 g of 1,1,1,3,3-pentachloropropane was obtained after the reaction was completed.

[0061] (2) Preparation of 1,1,3,3-tetrachloro-1-propene

[0062] Add 650g 80% NaOH solution and 1632.2g 1,1,1,3,3-pentachloropropane into 5L Hastelloy material autoclave II, pass N 2 The pressure of the reaction kettle was controlled; the pressure of the reaction kettle was controlled to be 5 bar and the temperature was 130° C. Under these conditions, the reaction was stirred for...

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Abstract

The invention discloses a preparation method of 2,3,3,3-tetrafluoropropene. The preparation method comprises the steps: performing telomerization on chloroethylene and CCl4 so as to produce 1,1,1,3,3-pentachloropropane, then performing dehydrochlorination so as to generate 1,1,3,3-tetrachloro-1-propylene, performing exchange of fluorine and chlorine and dehydrochlorination so as to prepare 3,3,3-trifluoro-1-chloropropene, then performing an isomerization reaction so as to obtain 3,3,3-trifluoro-2-chloropropene, performing a liquid phase fluorination reaction so as to synthesize 1,1,1,2-tetrafluoro-2-chloropropane, and finally performing dehydrochlorination so as to obtain 2,3,3,3-tetrafluoropropene. The raw materials have low price, and are easy to obtain, so that the raw material cost inthe production process of 2,3,3,3-tetrafluoropropene is reduced; an industrial chain is formed in the reaction process, and highly-economic values are provided through purification of the intermediateproducts; the reaction conditions are mild, the equipment has simple operation, the raw material conversion rate and product selectivity are high at the reaction stages, and by-products are few, so that a large industrial application prospect is achieved.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a preparation method of 2,3,3,3-tetrafluoropropene. Background technique [0002] 2,3,3,3-Tetrafluoropropene is a new generation refrigerant with good refrigeration effect, small greenhouse effect, short atmospheric life, low flammability and low toxicity, and can be widely used in refrigeration appliances such as automobiles, air conditioners, refrigerators, etc. It can also be used in fire extinguishing agents, foaming agents, foaming agents, grinding and polishing machines and other fields. But compared to similar substitutes, 2,3,3,3-tetrafluoropropene is expensive to manufacture and expensive. [0003] U.S. Patent US7560602B2 discloses the use of CF 3 CF 2 CF 2 CHCl 2 As raw material, first hydrodechlorination generates CF 3 CF 2 CH 3 , and then remove HF to obtain 2,3,3,3-tetrafluoropropene. The advantage of this preparation method is that the toxic substance CF i...

Claims

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Application Information

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IPC IPC(8): C07C17/25C07C21/18
CPCC07C17/087C07C17/25C07C17/269C07C21/18C07C19/10C07C19/01C07C21/02
Inventor 徐庆瑞王晓东吴业铧陈成凯吴陈兴徐煜胡胜伟李飞占林喜
Owner ZHEJIANG SANMEI CHEM IND
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