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Catalyst for preparing chlorotrifluoroethylene by selective hydrodechlorination

A technology of selective hydrogenation of chlorotrifluoroethylene, applied in dehalogenation preparation, physical/chemical process catalyst, organic chemistry, etc., can solve the problems of high price, increased production cost, low conversion rate of raw materials, etc., and achieve low raw material cost , Good anti-sintering ability at high temperature

Active Publication Date: 2021-12-21
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalysts for hydrodechlorination disclosed in Chinese patents CN1065261.A and CN1351903 all use noble metals as the main catalyst, and add other metals as auxiliary agents at the same time, because noble metal catalysts are expensive, which leads to increased production costs
[0005] At present, the process of preparing chlorotrifluoroethylene by selective hydrodechlorination has problems such as expensive catalyst or low conversion rate of raw materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: preparation mass fraction 30%Ni 2 P / SiO 2 catalyst

[0022] 9.48g nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) and 3.45g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 20 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear green solution. An equal volume of the above solution was impregnated onto 10g of silica, then aged at room temperature for 12h, dried at 120°C for 12h to dry the moisture, and calcined at 500°C for 3h to obtain Ni 2 P / SiO 2 precursors. The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and kept at 120°C for 1h to remove the water adsorbed by the catalyst; (2) from 120°C to 120°C at a rate of 5°C / min 400°C, then increase...

Embodiment 2

[0023] Embodiment 2: preparation mass fraction 30%MoP / C catalyst

[0024] 3.52g ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 4H 2 O) and 2.63g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 10 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear solution. An equal volume of the above solution was impregnated onto 10 g of activated carbon, then aged at room temperature for 12 h, dried at 120 °C for 12 h to dry the water, and baked at 500 °C for 3 h in a nitrogen atmosphere to obtain the oxide precursor of MoP / C. The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and kept at 120°C for 1h to drive off the water adsorbed by the catalyst; (2) from 120°C to 120°...

Embodiment 3

[0025] Embodiment 3: preparation mass fraction 30%WP / MgF 2 catalyst

[0026] At room temperature, 3.73g ammonium metatungstate ((NH 4 ) 6 ·W 12 h 2 o 40 ·nH 2 O) and 1.87g diammonium hydrogen phosphate ((NH 4 ) 2 HPO 4 ) was added to 20 mL of deionized aqueous solution, and then the pH of the solution was adjusted to 2-3 with concentrated nitric acid to obtain a clear solution. Immerse an equal volume of the above solution into 10 g of MgF 2 After aging at room temperature for 12h, drying at 120°C for 12h to dry moisture, and firing at 500°C for 6h, WP / MgF 2 oxide precursors. The phosphide catalyst was prepared by in-situ temperature-programmed reduction method. The temperature programming step mainly includes two steps: (1) in H 2 Under the atmosphere (flow rate 150mL / min), the temperature was raised from room temperature to 120°C at 5°C / min, and kept at 120°C for 1h to drive off the water adsorbed by the catalyst; (2) from 120°C to 120°C at a rate of 5°C / min 40...

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Abstract

The invention discloses a catalyst for preparing chlorotrifluoroethylene by gas-phase selective hydrodechlorination of 1,1,2-trifluoro-2,2,1-trichloroethane. It is to solve the problems of high cost and easy deactivation of traditional HCFC hydrodechlorination catalysts. The catalyst disclosed in the present invention is that the catalyst is composed of an active component and a carrier, wherein the active component is M x P y ,M x P y for Ni 2 P, MoP, WP, Co 2 A combination of one or more of P, CoP, and FeP. The catalyst in the invention has excellent performance, high activity, good stability, low reaction temperature, effectively reduces reaction energy consumption, and has industrial application value.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing chlorotrifluoroethylene. It belongs to multiple catalytic technical fields. Background technique [0002] Chlorotrifluoroethylene (CTFE) is an important fluorine-containing polymer monomer, which can be used to prepare a series of fluorine coatings, fluorine resins, fluorine rubber and fluorine-chlorine lubricants. At the same time, chlorotrifluoroethylene is also an important fluorine-containing intermediate, which can be used to prepare downstream products such as trifluoroethylene, bromotrifluoroethylene, hexafluorobutadiene, trifluorostyrene, and fluorinated bromine oil. [0003] The traditional synthesis of chlorotrifluoroethylene adopts the reduction process of 1,1,2-trifluoro-2,2,1-trichloroethane (CFC-113) zinc powder method. This process is batch production, with huge production equipment and high efficiency. Low, the production rate of chlorotrifluoroethylene is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/185B01J27/188B01J27/19C07C17/23C07C21/18
CPCB01J27/1853B01J27/19B01J27/188C07C17/23C07C21/18
Inventor 吕剑田松王博毛伟马辉李晨白彦波贾兆华秦越
Owner XIAN MODERN CHEM RES INST
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