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Catalyst for preparing chlorotrifluoroethene from trichlorotrifluoroethane through catalytic hydrodechlorination and preparation method of catalyst

A technology of trifluorotrichloroethane and chlorotrifluoroethylene, which is applied in the field of catalysts, can solve the problems of low reaction selectivity, many side reactions, easy deactivation and stability, and achieve good reaction selectivity, mild reaction conditions, Operation stable and good effect

Active Publication Date: 2016-09-21
CHANGSHU 3F FLUOROCHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reduction dechlorination method of trifluorotrichloroethane zinc powder is a traditional technique for producing chlorotrifluoroethylene, which is relatively mature in industrial development, but still has many disadvantages: 1. the production equipment is huge, and the initial investment is more; 2. .Reaction selectivity is low, and side reactions are many; 3. The amount of zinc powder used is much larger than the theoretical amount, and the generated zinc chloride is difficult to handle, and the recovery of solvent methanol and ethanol is difficult, which will cause relatively large pollution to the environment
[0006] The catalysts reported above all have defects such as low activity, easy deactivation and poor stability. It is particularly important to develop a new catalyst with high activity and strong stability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Using cobalt (first catalyst) and chromium (second catalyst) supported on SiO 2 In addition, the auxiliary agent is potassium alkali metal.

[0023] SiO at 400°C 2 The particles are roasted, and then a certain amount of CoCl is configured 2 ·6H 2 O, CrCl 3 ·6H 2 O, Ni(H 2 PO 2 )·6H 2 O and KCl 6H 2 O mixed solution, the mass fractions were 3.1%, 5.2%, 15.6% and 4.5%, and then the SiO 2 The particles were impregnated with equal volume and dried at 60 °C for 12 h. The dried material was put into a tube furnace, nitrogen was introduced, the temperature was raised to 240 °C at a rate of 6 °C / min, the reaction time was 4 h, and then naturally cooled to room temperature, and finally O 2 2% N 2 The passivation treatment was carried out for 4 hours. In the catalyst thus prepared, the mass content of Co was 2.0%, Cr was 2.6%, and K was 2.5%. The catalyst is used to carry out hydrodechlorination reaction of trifluorotrichloroethane, the conversion rate is 97.5%, and t...

Embodiment 2

[0025] Cobalt (first catalyst) and manganese (second catalyst) supported on pretreated SiO 2 Above, the auxiliary agent is selected from the rare earth metal rhenium.

[0026] SiO at 400°C 2 The particles are roasted, and then a certain amount of CoCl is configured 2 ·6H 2 O, MnCl 2 4H 2 O, Ni(H 2 PO 2 )·6H 2 The mixed solution of O and perrhenic acid, the mass fractions are 2.2%, 4.3%, 9.8% and 2.7%, and then the SiO 2 The particles were impregnated with equal volume and dried at 80°C for 16h. The dried material was put into a tube furnace, nitrogen was introduced, the temperature was raised to 300 °C at a rate of 8 °C / min, the reaction time was 6 h, and then naturally cooled to room temperature, and finally O 2 2% N 2 The passivation treatment was carried out for 4 hours. In the catalyst thus prepared, the mass content of Co was 2.5%, Cr was 2.8%, and Re was 3.0%. The catalyst is used to carry out hydrodechlorination reaction of trifluorotrichloroethane, the conve...

Embodiment 3

[0028] Cobalt (first catalyst) and manganese (second catalyst) supported on pretreated SiO 2 Above, the auxiliary agent is selected from the rare earth metal rhenium.

[0029] SiO at 400°C 2 The particles are roasted, and then a certain amount of CoCl is configured 2 ·6H 2 O, MnCl 2 4H 2 O, Ni(H 2 PO 2 )·6H 2 The mixed solution of O and perrhenic acid, the mass fractions are 5.3%, 6.2%, 12.8% and 2.1%, and then the SiO 2 The particles were impregnated with equal volume and dried at 80°C for 16h. The dried material was put into a tube furnace, nitrogen was introduced, the temperature was raised to 300 °C at a rate of 8 °C / min, the reaction time was 6 h, and then naturally cooled to room temperature, and finally O 2 2% N 2The passivation treatment was carried out, and the treatment time was 4 hours. In the catalyst thus prepared, the mass content of Co was 3.3%, that of Cr was 3.0%, and that of Re was 3.8%. The catalyst is used to carry out hydrodechlorination reactio...

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Abstract

The invention discloses a catalyst for preparing chlorotrifluoroethene from trichlorotrifluoroethane through catalytic hydrodechlorination and a preparation method of the catalyst. The method comprises steps as follows: SiO2 particles are roasted at a temperature of 400 DEG C; a mixed solution containing CoC12.6H2O or RhCl3.3H2O, CrCl3.6H2O or MnCl2.4H2O, KCl.6H2O or perrhenic acid and Ni (H2PO2).6H2O is prepared; the SiO2 particles are subjected to isometric impregnation and dried at a temperature of 60-80 DEG C for 12-16 h; dried substances are put into a tube furnace, nitrogen is introduced, the temperature is raised to 240-300 DEG C at the speed of 6-8 DEG C / min, the reaction pressure is 0-2 MPa, and the reaction time is 4 h; products are naturally cooled to the room temperature, and O2 containing 2% of N2 is introduced for passivating treatment for 4 h. The prepared catalyst contains 0.1%-15% of Co or Rh, 0.5%-22% of Cr or Mn and 0.1%-5% of alkali metal K or rare-earth metal Re. The catalyst has the advantages of high activity, good stability, good reaction selectivity, mild reaction condition and the like.

Description

technical field [0001] The invention relates to a catalyst for preparing trifluorochloroethane by catalytic hydrodechlorination of trifluorotrichloroethane. Background technique [0002] Chlorotrifluoroethylene (CTFE), also known as chlorotrifluoroethylene, is one of the important monomers for the synthesis of fluorine-containing materials. It can produce fluorine resins, fluorine coatings, fluorine rubber and chlorofluorolubricants through homopolymerization and copolymerization. These materials have Very good chemical inertness and high temperature resistance, widely used in cutting-edge technology, military navigation and electronics industry. The reduction dechlorination method of trifluorotrichloroethane zinc powder is a traditional technique for producing chlorotrifluoroethylene, which is relatively mature in industrial development, but still has many disadvantages: 1. the production equipment is huge, and the initial investment is more; 2. .Reaction selectivity is lo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/86B01J23/889C07C17/23C07C21/18
CPCB01J23/864B01J23/8896B01J37/0207B01J37/08C07C17/23C07C21/18
Inventor 李佳琦司林旭李程燕
Owner CHANGSHU 3F FLUOROCHEM IND CO LTD
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