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

A technology of tetrafluoropropene and tetrachloropropene, which is applied in 1 field, can solve the problems of complex process, poor economy, difficulty in obtaining HCFC-1233zd and HFC-245fa, etc., and achieve the effect of simple process route and easy price

Active Publication Date: 2012-07-18
海宁市袁花镇工业投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the above-mentioned preparation method of HFO-1234ze, the raw materials HCFC-1233zd and HFC-245fa are not easy to obtain, and the raw materials HCFC-1233zd and HFC-245fa need to be prepared
And the price is high, the economy is poor, and the dehydrohalogenation step under the action of strong alkali is required, the process is complicated, and it is not conducive to industrial production

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Catalyst A preparation. First, weigh Al according to the molar ratio of Cr to Al of 9:1 2 o 3 ·H 2 O and Cr(NO 3 ) 3 9H 2 O, mix evenly with an appropriate amount of water, add a certain amount of ammonium carbonate until the precipitation is complete, then separate and wash until the filtrate is neutral, and then dry the precipitate at 120°C. Shape the dried precipitate at 500°C, N 2 Calcined in the atmosphere for 10 hours to obtain a catalyst precursor; the catalyst precursor was treated with HF at 350° C. for 5 hours to obtain catalyst A.

[0034] Catalyst B, according to AlF 3 Loading capacity 1% (activated carbon mass fraction), weigh Al(NO 3 ) 3 9H 2 O and activated carbon, mixed with appropriate amount of water, dried at 400°C N 2 Roasting in the atmosphere for 5 hours; then according to the Pd loading 0.2% (activated carbon mass fraction), measure H 2 PdCl 4 The solution was mixed with the above-mentioned calcined product, impregnated overnight, and...

Embodiment 2

[0038] Catalyst A preparation. First, weigh Al according to the molar ratio of Cr to Al of 8:2 2 o 3 ·H 2 O and Cr(NO 3 ) 3 9H 2 O, mix evenly with an appropriate amount of water, add a certain amount of ammonium carbonate until the precipitation is complete, then separate and wash until the filtrate is neutral, and then dry the precipitate at 120°C. The dried precipitate was shaped and calcined at 500°C in N2 atmosphere for 10 hours to obtain a catalyst precursor; the catalyst precursor was treated with HF at 350°C for 5 hours to obtain catalyst A.

[0039] Catalyst B, according to AlF 3 Loading capacity 1% (activated carbon mass fraction), weigh Al(NO 3 ) 3 9H 2 O and activated carbon, mixed with appropriate amount of water, dried at 400°C N 2 Roasting in the atmosphere for 5 hours; then according to the Pd loading 0.2% (activated carbon mass fraction), measure H 2 PdCl 4 The solution was mixed with the above-mentioned calcined product, impregnated overnight, and...

Embodiment 3

[0043] Catalyst A preparation. First, weigh Al according to the molar ratio of Cr to Al of 7:3 2 o 3 ·H 2 O and Cr(NO 3 ) 3 9H 2 O, mix evenly with an appropriate amount of water, add a certain amount of ammonium carbonate until the precipitation is complete, then separate and wash until the filtrate is neutral, and then dry the precipitate at 120°C. Shape the dried precipitate at 500°C, N 2 Calcined in the atmosphere for 10 hours to obtain a catalyst precursor; the catalyst precursor was treated with HF at 350° C. for 5 hours to obtain catalyst A.

[0044] Catalyst B, according to AlF 3 Loading capacity 1% (activated carbon mass fraction), weigh Al(NO 3 ) 3 9H 2 O and activated carbon, mixed with appropriate amount of water, dried at 400°C N 2 Roasting in the atmosphere for 5 hours; then according to the Pd loading 0.5% (activated carbon mass fraction), measure the H 2 PdCl 4 The solution was mixed with the above-mentioned calcined product, impregnated overnight,...

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Abstract

The invention discloses a preparation method of 1,1,1,3-tetrafluoropropene. The method comprises the following steps of: filling a fluorination catalyst into the front end of a reactor I and filling a Pd / AlF3 / C catalyst into the back end of the reactor I, wherein the volume ratio of the fluorination catalyst to the Pd / AlF3 / C catalyst is (3-1):(1-2); filling a Pd / AlF3 / C catalyst into a reactor II; reacting 1,1,2,3-tetrafluoropropene with fluorine hydride gas in the reactor I in the molar ratio of 1:(10-50) at the temperature of 250-400 and the air speed of 600-1,000 h<-1> under the normal pressure, and feeding produced fluorine hydride, HCFC-1233xf, chlorine hydride and HFO-1234ze into a separating tower 2; feeding separated HCl and HFO-1234ze into a rectifying tower; feeding HF and HCFC-1233xf into a separating tower 3, feeding the separated HCFC-1233xf and a part of HF into the reactor II in the molar ratio of 1:(5-45), reacting at the temperature of 250-400 DEG C and the air speed of 600-1,000 h<-1> and under the normal pressure, and circulating tail gas to the separating tower 2; and separating gas entering the rectifying tower through the rectifying tower, separating a fraction HCl and other side products out, washing HFO-1234ze with alkali, drying and packaging. The method has a simple process flow, and the selectivity of 1,1,1,3-tetrafluoropropene is high.

Description

Technical field: [0001] The present invention relates to a process for the synthesis of hydrofluoroolefins. In particular, it relates to a preparation method of 1,1,1,3-tetrafluoropropene. Background technique [0002] 1,1,1,3-Tetrafluoropropene (HFO-1234ze), which has low greenhouse effect potential (GWP) and zero ozone depletion potential (ODP), is considered to be the most potential alternative to 1,1,1 , one of the new generation ODS substitutes of 2-tetrafluoroethane HFC-134a, widely used as refrigerant, blowing agent, aerosol propellant, solvent, etc. In addition, HFO-1234ze is the basic material for the synthesis of thermoplastic materials with high thermal stability and high elasticity, and is widely used in fire protection, aerospace, aviation and other fields. [0003] Among the known HFO-1234ze preparation methods, U.S. Patents US6124510, US5986151, Japanese Patents JP10007605, JP11140002 and other patents disclose a method of removing 1,1,1,3,3-pentafluoropropa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/20
Inventor 罗孟飞谢遵运程永香谢冠群鲁继青彭小波蔚辰刚
Owner 海宁市袁花镇工业投资有限公司
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