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Metal carbide catalyst for catalyzing a CFC-113a hydrogenation coupling reaction and preparation method and application thereof

A metal carbide, cfc-113a technology, applied in the field of metal carbide catalyst and its preparation, can solve the problems of low conversion rate and selectivity, high yield, and achieve the effect of high catalytic stability

Active Publication Date: 2019-05-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, the target product yield from CFC-1316 hydrogenation to HFO-1336 reaction is high, and side reactions are few, but the conversion rate and selectivity of CFC-1316 obtained from CFC-113a hydrogenation coupling are not high

Method used

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  • Metal carbide catalyst for catalyzing a CFC-113a hydrogenation coupling reaction and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Grind ferric nitrate nonahydrate and oxalic acid aqueous solution with a molar ratio of 1:3 into a yellow viscous liquid in an agate mortar (the concentration of oxalic acid aqueous solution is 30wt%, and the molar ratio of ferric nitrate nonahydrate and oxalic acid is 1:3) , to obtain ferric oxalate solution. After the ferric oxalate solution is dried at 100°C to remove moisture, it is calcined in a tube furnace under a CO atmosphere. The calcining temperature is 500°C, and the CO volume flow rate is 80mL / min. Promptly obtain the metal carbide catalyst (the metal carbide catalyst prepared in this embodiment is iron carbide), the XRD pattern of the metal carbide catalyst is as follows figure 1 shown, from figure 1 It can be seen that the structure of the catalyst presents the crystalline structure of iron carbide.

[0023] Take 2mL of the above-prepared iron carbide catalyst in the constant temperature zone of a reaction tube with an inner diameter of 8mm, raise the t...

Embodiment 2

[0025] Ruthenium trichloride and formic acid aqueous solution with a molar ratio of 1:3 were ground into a viscous liquid in an agate mortar (the concentration of formic acid aqueous solution was 40wt%, and the molar ratio of ruthenium trichloride and formic acid was 1:3), to obtain Solution A. After solution A was dried at 120°C to remove moisture, it was fired in a tube furnace at 350°C for 7 hours in a carbon-containing atmosphere, and the gas in the carbon-containing atmosphere was CH 4Mixed gas with diluent, CH 4 The volume flow rate is 20mL / min, the diluent gas is nitrogen and the volume flow rate is 40 mL / min. After the calcination is completed, the tablet is formed, and the metal carbide catalyst is obtained by sieving under 60-100 mesh (the metal carbide catalyst prepared in this embodiment for ruthenium carbide).

[0026] The process of using the metal carbide catalyst prepared in this example to catalyze the hydrocoupling reaction of CFC-113a was repeated in Examp...

Embodiment 3

[0028] Grind cobalt carbonate and citric acid aqueous solution with a molar ratio of 1:3 into a viscous liquid in an agate mortar (the concentration of citric acid aqueous solution is 40wt%, and the molar ratio of cobalt carbonate and citric acid is 1:3), and then Add 2wt% potassium nitrate and re-grind into a viscous liquid (based on the total amount of cobalt carbonate, citric acid and potassium nitrate as raw materials, the amount of potassium nitrate added is 2wt%) to obtain solution B. After solution B was dried at 120°C to remove moisture, it was fired in a tube furnace at 450°C for 1 hour in a carbon-containing atmosphere. The gas in the carbon-containing atmosphere was a mixture of carbon-containing gas and diluent gas. The carbon-containing gas was CO and CO 2 Mixed gas, CO and CO 2 The volume flow rate is 20mL / min, the diluent gas is nitrogen and the flow rate is 70 mL / min, after the calcination is completed, it is pressed into tablets, and sieved under 60-100 mesh ...

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Abstract

The invention discloses a metal carbide catalyst for catalyzing a CFC-113a hydrogenation coupling reaction and a preparation method and application thereof. The metal carbide catalyst is mainly composed of at least one of iron carbide, nickel carbide, ruthenium carbide, palladium carbide and cobalt carbide. When the metal carbide catalyst is used for catalyzing the CFC-113a hydrogenation couplingreaction, the reaction is performed on a fixed bed reaction device, the feeding volume ratio of CFC-113a to H2 is 1:3-5, the reaction temperature is 200-400 DEG C, the gas air speed is 100-1,000 h<-1>, the reaction pressure is normal pressure, the CFC-113a reaction raw materials are easy to obtain, the conversion rate is high (the conversion rate can reach 90% or above), the target product CFC-1316 is high in selectivity (the selectivity can reach 90% or above), and the metal carbide catalyst has the high catalytic stability in a gas phase catalysis hydrogenation coupling dechlorination reaction.

Description

technical field [0001] The invention relates to a metal carbide catalyst for catalyzing CFC-113a hydrogenation coupling reaction, its preparation method and application. Background technique [0002] Fluorodichloroethane (HCFC-141b) is widely used as a blowing agent, but the ODP of HCFC-141b is not zero, and it will still cause damage to the atmospheric ozone layer, so the Montreal Protocol includes it in the phase-out plan. Now international substitutes mainly include 1,1,1,3,3-pentafluorobutane (HFC-365mfc), 1,1,1,3,3-pentafluoropropane (HFC-245fa), etc. The ozone layer is not destructive, but they still significantly contribute to global warming (larger GWP), so they should only be used as a transitional replacement for polyurethane foams. Therefore, the research and development of compounds with zero ozone depletion and low global warming potential is an urgent demand in the current market, and 1,1,1,4,4,4-hexafluoro-2-butene ( HFO-1336mzz) just meets the current requi...

Claims

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Application Information

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IPC IPC(8): B01J27/22C07C17/269C07C21/18
Inventor 唐浩东徐玉萍邹超煜韩文锋李瑛刘宗健
Owner ZHEJIANG UNIV OF TECH
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