Method for preparing 1,3,3,3-tetrafluoropropene by gas phase fluorination

A technology of tetrafluoropropene and gas-phase fluorination, which is applied in chemical instruments and methods, halogen substitution preparation, organic chemistry, etc., can solve the problem of low yield of HFO-1234ze and achieve high reaction yield

Active Publication Date: 2010-12-15
XIAN MODERN CHEM RES INST
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  • Abstract
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AI Technical Summary

Problems solved by technology

But the yield of this method HCFC-1233zd synthetic HFO-1234ze is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0014] Preparation of fluorination catalyst

[0015] Dissolve ferric chloride in water, react with precipitating agent ammonia water at 60°C, adjust the pH value of the reaction solution in the range of 7.0 to 7.5, and make it fully precipitate under stirring conditions. Hot filtration followed by overnight drying at 120°C for 12 hours yields Fe(OH) 3 .

[0016] CaF 2 , Fe(OH) 3 and CaCO 3 Mix uniformly according to the mass ratio of 60:30:10, and press into tablets to obtain the catalyst precursor. The catalyst precursor was calcined in a muffle furnace at 450°C for 8 hours, then loaded into a tubular reactor, heated to 300°C, fed with hydrogen fluoride gas for fluorination for 1 hour, then raised to 400°C at a heating rate of 1°C / min, and continued After fluorination for 8 hours, a calcium fluoride-based fluorination catalyst was obtained.

Embodiment 1

[0018] In a nickel tube fixed-bed tubular reactor with an internal diameter of 38mm, 60ml of the above-mentioned calcium fluoride-based fluorination catalyst is charged, and HF and HCFC-1233zd are introduced to react, and the molar ratio of HF and HCFC-1233zd is controlled to be 10:1, the contact time is 10 seconds, the reaction temperature is 380 ° C, after 20 hours of reaction, the reaction product is washed with water and alkali to remove HCl and HF, and the conversion rate of HCFC-1233zd is 90% according to gas chromatography analysis, HFO- The selectivity of 1234ze was 89%.

Embodiment 2

[0020] The operation is basically the same as in Example 1, except that the reaction temperature is changed to 300° C., and 60 ml of the calcium fluoride-based fluorination catalyst prepared above is loaded into a nickel tube fixed-bed tubular reactor with an inner diameter of 38 mm. , feed HF and HCFC-1233zd to react, control the molar ratio of HF and HCFC-1233zd to be 10:1, contact time is 10 seconds, reaction temperature is 300°C, after reaction for 20 hours, the reaction product is washed with water and alkali to remove HCl and HF, the conversion rate of HCFC-1233zd was 85% and the selectivity of HFO-1234ze was 90% according to gas chromatography.

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Abstract

The invention discloses a preparation method of 1,3,3,3-tetrafluoropropene. The method takes 1-Cl-3,3,3-trifluoropropene as a raw material and comprises the following steps of: performing the reaction of hydrogen fluoride (HF) and the 1-Cl-3,3,3-trifluoropropene under the catalytic action of a fluorinated catalyst, wherein the reaction conditions are as follow: the mol ratio of the HF and the 1-Cl-3,3,3-trifluoropropene is 5-15:1, the contact time is 2 to 20 seconds, the reaction temperature is 300 to 450 DEG C, precursors of the fluorinated catalyst comprise 60 percent by mass of calcium fluoride, 30 percent by mass of iron hydroxide and 10 percent by mass of calcium carbonate, and the fluorinated catalyst can be prepared by evenly mixing the precursors of the fluorinated catalyst, pressing and moulding, roasting at 450 DEG C and carrying out the fluorination by using hydrogen fluoride gas at 400 DEG C. The invention is mainly used for preparing the 1,3,3,3-tetrafluoropropene.

Description

technical field [0001] The invention relates to a method for preparing 1,3,3,3-tetrafluoropropene by gas-phase fluorination, in particular to a gas-phase fluorination of 1-chloro-3,3 in the next step under the catalysis of a calcium fluoride-based fluorination catalyst. , A method for preparing 1,3,3,3-tetrafluoropropene (HFO-1234ze) from 3-trifluoropropene (HCFC-1233zd). Background technique [0002] Chlorofluorocarbons (CFCs) are harmful to the Earth's ozone layer, and many hydrofluorocarbons (HFCs) used to replace CFCs contribute to global warming. HFOs will not destroy the ozone layer, nor will it cause global warming, and are being considered for use in refrigerants, cleaning agents, foaming agents, aerosol propellants, etc., of which 1,3,3,3-tetrafluoropropene (HFO -1234ze) is used in blowing agent to replace 1,1,1,2 tetrafluoroethane (HFC-134a). [0003] Currently, gas phase fluorination of halogenated hydrocarbons is often used to prepare hydrofluoroolefins in fluo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/20B01J27/138
Inventor 吕剑王博张伟寇联岗李凤仙石磊郝志军曾纪珺薛云娜
Owner XIAN MODERN CHEM RES INST
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