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Preparation method and use method of nitrogen doped carbon catalyst for preparing vinyl chloride by acetylene hydrochlorination of fixed bed

A technology of acetylene hydrochlorination and nitrogen-doped carbon, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, hydrogen halide addition preparation, etc. It can solve the problems of polluting the environment, demanding conditions, and unfavorable mass production. Achieve the effects of simplifying the preparation process, reducing pollution, and avoiding doping steps

Active Publication Date: 2018-06-22
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst has the following disadvantages: in the reaction process, the mercury-containing components in the catalyst are easily volatilized and lost, which seriously pollutes the environment and threatens human health
The g-C prepared by Professor Dai Bin et al. 3 N 4 / AC catalyst, which shows good catalytic activity in the acetylene hydrochlorination reaction; the SiC@C-N and h-BN catalysts prepared by Bao Xinhe of Dalian Institute of Chemistry and Physics and others showed excellent catalytic activity in the reaction Catalytic performance, but the preparation steps of the catalyst are more, and the condition requirements are relatively harsh, which is not conducive to mass production

Method used

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  • Preparation method and use method of nitrogen doped carbon catalyst for preparing vinyl chloride by acetylene hydrochlorination of fixed bed
  • Preparation method and use method of nitrogen doped carbon catalyst for preparing vinyl chloride by acetylene hydrochlorination of fixed bed
  • Preparation method and use method of nitrogen doped carbon catalyst for preparing vinyl chloride by acetylene hydrochlorination of fixed bed

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1) Shred about 10g of silkworm cocoon shells, soak them in deionized water at 50°C for more than 6 hours to remove impurities and soluble inorganic salts in the silkworm cocoons, then filter and separate the samples, and wash them with deionized water for more than 5 times , and then dried at 100 °C to obtain sample A;

[0044] 2) Place sample A in a tube furnace, heat up to 250 °C in a flowing air atmosphere at a rate of 5 °C / min for pre-carbonization, and keep the temperature at 250 °C for 40 min to obtain sample B, in which air The volumetric space velocity is 180 h -1 , the constant temperature at a lower temperature of 250 ℃ is to avoid excessive oxidation of the surface groups of the material;

[0045] 3) Grind sample B into powder and place it in 5% dilute hydrochloric acid solution, stir at room temperature for 12 hours, then filter and separate the powder, wash with deionized water until neutral, and dry the obtained filter cake at 120 °C , that is, the nitro...

Embodiment 2

[0047] 1) Shred about 10g of silkworm cocoon shells, soak them in deionized water at 50°C for more than 6 hours to remove impurities and soluble inorganic salts in the silkworm cocoons, then filter and separate the samples, and wash them with deionized water for more than 5 times , and then dried at 100 °C to obtain sample A;

[0048] 2) Place sample A in a tube furnace, heat up to 350 °C in a flowing air atmosphere at a rate of 5 °C / min for pre-carbonization, and keep the temperature at 350 °C for 40 min to obtain sample B, in which air The volumetric space velocity is 180 h -1 , the constant temperature at a lower temperature of 350 ℃ is to avoid excessive oxidation of the surface groups of the material;

[0049] 3) Grind sample B into powder and place it in 5% dilute hydrochloric acid solution, stir at room temperature for 12 hours, then filter and separate the powder, wash with deionized water until neutral, and dry the obtained filter cake at 120 °C dry, the nitrogen-do...

Embodiment 3

[0051] 1) Shred about 10g of silkworm cocoon shells, soak them in deionized water at 50°C for 6 hours to remove impurities and soluble inorganic salts in the silkworm cocoons, then filter and separate the samples, and wash them with deionized water for more than 5 times. Then dry at 100°C to obtain sample A;

[0052] 2) Place sample A in a tube furnace, heat up to 350 °C in a flowing air atmosphere at a rate of 5 °C / min for pre-carbonization, and keep the temperature at 350 °C for 40 min to obtain sample B, in which air The volumetric space velocity is 180 h -1 ;

[0053] 3) Grind sample B into powder and place it in dilute hydrochloric acid solution, stir at room temperature for 12 hours, then filter and separate the powder with suction, wash with deionized water until neutral, and dry the obtained filter cake at 120 °C to obtain sample C ;

[0054] 4) Mix 3g of sample C with 3g of KOH powder, transfer the mixture to a tube furnace after fully grinding, in flowing N 2 Und...

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Abstract

The invention discloses a preparation method and a use method of a nitrogen doped carbon catalyst for preparing vinyl chloride by acetylene hydrochlorination of a fixed bed, and belongs to the technical field of material synthesis. The method comprises the following steps: adopting a natural silkworm cocoon shell with high nitrogen content as a precursor, and performing carbonization and activation to obtain a nitrogen doped carbon non-metal catalyst. The preparation method disclosed by the invention has the characteristics that the a natural biomass with high nitrogen content is adopted as the precursor of the catalyst, so that a complicated nitrogen element introducing step is not needed; the operation is simple, and the cost is reduced; and by virtue of carbonization and activation of preparation processes, the nitrogen element can be uniformly distributed in the catalyst. The invention develops a novel non-metal catalyst and provides a preparation technology, and the catalyst has certain catalytic activity and selectively when being applied to reaction for preparing vinyl chloride by acetylene hydrochlorination of the fixed bed.

Description

technical field [0001] The invention proposes a method for preparing a nitrogen-doped carbon catalyst used in fixed-bed hydrochlorination of acetylene to produce vinyl chloride and a method for using it, belonging to the technical field of material synthesis. The method adopts the natural silkworm cocoon shell with high nitrogen content as a precursor, and obtains a nitrogen-doped carbon catalyst through carbonization and activation in an inert gas. The catalyst is applied in the reaction of preparing vinyl chloride by hydrochlorination of acetylene in a fixed bed, and has certain catalytic activity and selectivity. Background technique [0002] Polyvinyl chloride is the first general-purpose resin material in China and the second largest in the world, with a wide range of applications. Vinyl chloride is the main monomer for the synthesis of polyvinyl chloride. In China, the production of vinyl chloride mainly uses acetylene as a raw material, and the reaction mainly uses m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08C07C17/08C07C21/06
CPCB01J27/24B01J37/082B01J37/084C07C17/08C07C21/06
Inventor 李伟乔贤亮关庆鑫
Owner NANKAI UNIV
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