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Nitrogen-doped palladium-carbon catalyst, preparation method thereof and application of nitrogen-doped palladium-carbon catalyst in CFC-113 hydrodechlorination

A palladium-carbon catalyst and nitrogen-doped technology, which is applied in the direction of catalyst activation/preparation, dehalogenation preparation, chemical instruments and methods, etc., can solve the problems of loss of catalytic activity and weak interaction, and achieve clear thinking, simple operation, and improved The effect of fixation and stability

Active Publication Date: 2021-01-12
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Supported Pd catalysts are often used in hydrodechlorination processes due to their high activity, however, during the reaction process, Pd tends to accumulate on the surface of carbon supports, thus losing catalytic activity, which may be due to the relative comparison between carbon and metal active components. Due to the weak interaction, the present invention attempts to modify the carbon-containing support to improve the dispersion, stability and catalytic activity of noble metals

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 10g of activated carbon, the particle size of activated carbon is 800 mesh, and the specific surface area is 1300m 2 / g, the average pore size is 3nm, and the mass ratio of dicyandiamide to activated carbon is 0.25. Dissolve it and 2.5g dicyandiamide in 100mL water and keep stirring for 3h until the mixture is uniform. The temperature was raised to 600° C., and calcined at high temperature for 4 hours to obtain a nitrogen-doped carrier material. Then, the above-mentioned nitrogen-doped mesoporous carbon was prepared into a slurry at 70°C in 100ml of deionized water, and 10ml of H 2 PdCl 4 Solution (Pd content is 0.1g / L), stir 2h, adjust the pH value of solution to 9 with 10wt% NaOH solution, filter after solution is cooled to room temperature, filter cake is washed to neutrality with deionized water; The cake was configured into a slurry at 70°C, 15ml of sodium formate solution (35wt%) was added dropwise, stirred magnetically for 2 hours, and then filtered. The ...

Embodiment 2

[0030] Weigh 10g of activated carbon, the particle size of activated carbon is 600 mesh, and the specific surface area is 1000m 2 / g, the average pore diameter is 2nm, and the doping mass ratio of dicyandiamide to activated carbon is 0.4. Dissolve it and 4g dicyandiamide in 100mL water and keep stirring for 3.5h to make it evenly mixed. The temperature was raised to 800° C. at a heating rate of min, and the nitrogen-doped carrier material was obtained by calcination at a high temperature for 5 hours. Then, the above-mentioned nitrogen-doped mesoporous carbon was prepared into a slurry at 80°C in 100ml of deionized water, and 8ml of H 2 PdCl 4 Solution (Pd content is 0.1g / L), stir 2.5h, adjust the pH value of solution to 8.5 with the NaOH solution of 10wt%, filter after solution is cooled to room temperature, filter cake is washed to neutrality with deionized water; The filter cake was configured into a slurry at 80°C, 10ml of hydrazine hydrate solution (60wt%) was added drop...

Embodiment 3

[0032] Weigh 10g of activated carbon, the particle size of activated carbon is 400 mesh, and the specific surface area is 900m 2 / g, the average pore size is 4nm, and the mass ratio of dicyandiamide to activated carbon is 0.6. Dissolve it and 6g dicyandiamide in 100mL water and keep stirring for 5h to mix evenly. The temperature was raised to 900°C, and then calcined at high temperature for 3 hours to obtain nitrogen-doped activated carbon. Then, the above-mentioned nitrogen-doped mesoporous carbon was prepared into a slurry at 60°C in 100ml of deionized water, and 10ml of H 2 PdCl 4 Solution (Pd content is 0.2g / L), stirred for 2.5h, the pH value of the solution was adjusted to 9.5 with KOH solution, the solution was cooled to room temperature and then filtered, and the filter cake was washed with deionized water until neutral; then the filter cake was placed in Prepare a slurry at 60°C, add 10ml of methanol solution (20wt%) dropwise, and filter after magnetic stirring for 3 ...

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Abstract

The invention provides a nitrogen-doped palladium-carbon catalyst and a preparation method thereof, and an application of the nitrogen-doped palladium-carbon catalyst in a reaction for synthesizing chlorotrifluoroethylene by taking 1, 1, 2-trifluorotrichloroethane as a raw material. In the catalyst carrier nitrogen-doped activated carbon, nitrogen is mainly graphite nitrogen, and nitrogen doping can increase the binding energy of metal and carbon so that the dispersion of metal is facilitated, the fixation and stability of metal in the reaction process are improved, the operation is simple, and the obtained catalyst is easy to recycle.

Description

technical field [0001] The invention relates to a nitrogen-doped palladium-carbon catalyst and a preparation method thereof, as well as an application in preparing chlorotrifluoroethylene from 1,1,2-trifluorotrichloroethane (commonly known as CFC-113) as a raw material. 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. These fluorine-containing materials have excellent chemical inertness and weather resistance, and are widely used in cutting-edge technology, military aerospace, and electronics industries. In addition, CTFE is also an important fluorine-containing intermediate, which can be used to prepare downstream products such as trifluoroethylene, bromotrifluoroethylene, hexafluorobutadiene, trifluorostyrene, and fluorobromooil. Therefore, the research on the process development of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08B01J37/03B01J37/16C07C17/23C07C21/18
CPCB01J27/24B01J37/08B01J37/038B01J37/16C07C17/23B01J35/23C07C21/18Y02P20/584
Inventor 张群峰文晓宇周媛卢春山丰枫李小年
Owner ZHEJIANG UNIV OF TECH
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