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Method for preparing 2-chloro-3,3,3-trifluoropropylene catalyst by gas phase fluorination

A gas-phase fluorination and trifluoropropene technology, applied in the field of chemistry, can solve the problems of low yield, low catalyst service life, complicated reaction process, etc., and achieves simple preparation process, good service life, regeneration performance, repeatability, etc. Good results

Active Publication Date: 2015-06-17
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the preparation method of HCFC-1233xf in the above-mentioned comparative documents 1-3, the service life of the catalyst is improved by two-stage reaction of high and low temperature in the gas phase, addition of polymerization inhibitor, and two-stage reaction in the liquid phase and gas phase respectively. The reaction process is complicated and the yield is low. high
Although comparative literature 4-5 has a higher yield of 2-chloro-3,3,3-trifluoropropene, the service life of the catalyst is not high

Method used

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  • Method for preparing 2-chloro-3,3,3-trifluoropropylene catalyst by gas phase fluorination
  • Method for preparing 2-chloro-3,3,3-trifluoropropylene catalyst by gas phase fluorination
  • Method for preparing 2-chloro-3,3,3-trifluoropropylene catalyst by gas phase fluorination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Catalyst preparation:

[0027] 83.5g of Fe(NO 3 ) 3 9H 2 O and 317.9g of Mg(NO 3 ) 2 ·6H 2 O is formulated into a mixed solution according to the molar ratio of Fe and Mg elements of 1:6, heated to 40°C, adding 124g of urea and a certain amount of ammonia water to it, adjusting the pH value to 9.5, aging for 1h, and raising the temperature to 90°C. Continue to age for 8 hours, filter, wash the resulting colloidal precipitate to neutrality, and dry at 120°C. The obtained solid is calcined at 500°C for 6 hours to obtain Fe-Mg composite oxide.

[0028] Take 100g of Fe-Mg composite oxide and 25g of magnesium carbonate, mix according to the mass ratio of Fe-Mg composite oxide and magnesium carbonate of 4:1, fully grind with a ball mill, and then make a catalyst precursor by tableting. The catalyst precursor was calcined in a muffle furnace at 400°C for 8 hours, then 100ml of the catalyst precursor was loaded into a tubular reactor, the temperature was lowered to 200°C,...

Embodiment 2

[0032] Catalyst preparation:

[0033] 55.9g of FeCl 3 ·6H 2 O and 252.3 g of MgCl 2 ·6H 2 O is formulated into a mixed solution according to the molar ratio of Fe and Mg elements of 1:6, heated to 40°C, adding 124g of urea and a certain amount of NaOH to it, adjusting the pH value to 8.5, aging for 2h, and raising the temperature to 90°C. Continue to age for 12 hours, filter, wash the obtained colloidal precipitated product to neutrality, dry at 120°C, and roast the obtained solid at 450°C for 6 hours to obtain Fe-Mg composite oxide.

[0034] Evaluation of the catalyst was carried out in the same manner as in Example 1. After the reaction product was washed with water and alkali to remove HCl and HF, the conversion rate of 1,1,2,3-tetrachloropropene was 100% and the selectivity of HCFC-1233xf was 98.3% according to gas chromatography.

Embodiment 3

[0036] The preparation and evaluation of the catalyst of this embodiment are carried out according to the same method as in Example 1, except that 83.5g of Fe(NO 3 ) 3 9H 2 O and 317.9g of Mg(NO 3 ) 2 ·6H 2 O changed to 41.3g of Fe 2 (SO 4 ) 3 and 150g of MgSO 4 , 124g of urea was changed to 163.3g of ammonium bicarbonate, and the rest of the conditions remained unchanged. After the reaction product was washed with water and alkali to remove HCl and HF, the conversion rate of 1,1,2,3-tetrachloropropene was 100% and the selectivity of HCFC-1233xf was 99.3% according to gas chromatography.

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Abstract

The invention discloses a method for preparing a 2-chloro-3,3,3-trifluoropropylene catalyst by gas phase fluorination. The method comprises the following steps of preparing a mixed solution from a ferric soluble salt and a magnesium soluble salt according to a certain mole ratio of Fe / Mg, adding a precipitating agent into the mixed solution, carrying out aging, drying and roasting for a certain time to obtain a Fe-Mg composite oxide, blending the Fe-Mg composite oxide and magnesium carbonate according to a certain mass ratio, carrying out grinding and pressing molding to obtain a catalyst precursor, carrying out roasting and carrying out HF gas fluorination to obtain the fluorination catalyst. The 2-chloro-3,3,3-trifluoropropylene catalyst prepared by gas phase fluorination has a service life more than 1200h, has strong stability, can be regenerated after catalyst performance reduction so that catalyst performances are recovered and can be recycled.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for preparing a catalyst for gas-phase fluorination to prepare 2-chloro-3,3,3-trifluoropropene. Background technique [0002] 2-Chloro-3,3,3-trifluoropropene (HCFC-1233xf) is the starting material for the synthesis of 2,3,3,3-tetrafluoropropene (HFO-1234yf). HFO-1234yf, with zero ozone depletion potential and 4 greenhouse effect potential, has excellent environmental performance and is considered an ideal substitute for HFC-134a. [0003] Comparative Document 1. U.S. Patent US20070197842 discloses a preparation method of 2-chloro-3,3,3-trifluoropropene, which uses 2,3,3,3-tetrachloropropene or 1,1,2,3 -Tetrachloropropene is used as raw material, and FeCl is filled in the upper and middle parts of the reactor 3 / C catalyst, the lower part is filled with Cr 2 o 3 Catalyst, the reaction temperature of the upper and middle parts of the reactor is 120-220°C, the reaction temperat...

Claims

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Application Information

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IPC IPC(8): B01J23/745B01J35/10C07C21/18C07C17/20C07C17/10
CPCY02P20/584
Inventor 秦越吕剑王博毛伟马辉魏阿宝郝志军曾纪珺杨志强韩升张振华
Owner XIAN MODERN CHEM RES INST
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