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Preparation of porous hetero-element modified two-dimensional carbon material and application of porous hetero-element modified two-dimensional carbon material in chloroethylene synthesis reaction

A technology of two-dimensional carbon materials and heteroelements, which is applied in the direction of hydrogen halide addition preparation, catalyst activation/preparation, chemical instruments and methods, etc., to achieve the effects of low production cost, high specific surface area, and rich pore structure

Active Publication Date: 2020-07-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no research on porous two-dimensional carbon material catalysts for acetylene hydrochlorination.

Method used

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  • Preparation of porous hetero-element modified two-dimensional carbon material and application of porous hetero-element modified two-dimensional carbon material in chloroethylene synthesis reaction
  • Preparation of porous hetero-element modified two-dimensional carbon material and application of porous hetero-element modified two-dimensional carbon material in chloroethylene synthesis reaction
  • Preparation of porous hetero-element modified two-dimensional carbon material and application of porous hetero-element modified two-dimensional carbon material in chloroethylene synthesis reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1) Add 24.6g of 1-butyl-3-methylimidazolium tetraphenyl borate to 20g of graphene, microwave digestion frequency 300MHz, processing time 1h, so that heterogeneous elements are evenly distributed on the surface of graphene;

[0049] 2) Pass the above mixture into diborane for gas pre-adsorption for 2 hours at a temperature of 200°C;

[0050] 3) Put the above mixture in a plasma furnace with a nitrogen atmosphere, apply an electric field of 100V / m, and use the ions generated by the ionization of the working gas to further etch the defect and modify the material for 1 hour.

[0051] 4) washing the above-mentioned material with deionized water, and drying at 80° C. for 4 hours to obtain the porous heteroelement-doped porous two-dimensional graphene material;

[0052] 5) Evaluation of acetylene hydrochlorination reaction on a fixed bed reactor device: the effects of temperature and space velocity on the catalytic performance of the catalyst were investigated respectively, an...

Embodiment 2

[0054] 1) Add 17.5g of N-ethylpyridine dinitrile amine salt to 16g of graphene, microwave digestion frequency 800MHz, processing time 2h, so that heterogeneous elements are evenly distributed on the surface of graphene;

[0055] 2) Pass the above mixture into ammonia gas for gas pre-adsorption for 3 hours at a temperature of 300°C;

[0056] 3) Put the above mixture in a plasma furnace with a nitrogen atmosphere, apply an electric field of 500V / m, and use the ions produced by the ionization of the working gas to further etch the defect and modify the material for 1.5 hours.

[0057] 4) washing the above material with deionized water, and drying at 90° C. for 8 hours to obtain the porous heteroelement-doped porous two-dimensional graphene material;

[0058] 5) Evaluation of acetylene hydrochlorination reaction on a fixed bed reactor device: acetylene hydrochlorination reaction at 180°C, acetylene space velocity 40h -1 , under the condition of hydrogen chloride: acetylene = 1:1,...

Embodiment 3

[0060] 1) Add 15.2g N-picoline thiocyanate to 12g graphene alkyne, microwave digestion frequency 1200MHz, processing time 3h, make heterogeneous element evenly distribute on the graphene surface;

[0061] 2) Pass the above mixture into hydrogen sulfide for gas pre-adsorption for 4 hours at a temperature of 500°C;

[0062] 3) Put the above mixture in a plasma furnace with a nitrogen atmosphere, apply an electric field of 700V / m, and use the ions generated by the ionization of the working gas to further etch the defect and modify the material for 2 hours.

[0063] 4) washing the above material with deionized water, and drying at 120° C. for 12 hours to obtain the porous heteroelement-doped porous two-dimensional graphene material;

[0064] 5) Evaluation of acetylene hydrochlorination reaction on a fixed bed reactor device: acetylene hydrochlorination reaction at 180°C, acetylene space velocity 40h -1 , hydrogen chloride: acetylene = 1:1.1 conditions. The reaction conversion ra...

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Abstract

The invention discloses preparation of a porous miscellaneous element modified two-dimensional carbon material and application of the porous miscellaneous element modified two-dimensional carbon material in chloroethylene synthesis reaction. The preparation method comprises the following steps: (1) adding an ionic liquid containing hetero-elements into graphene or graphdiyne, and carrying out microwave digestion pretreatment, wherein the ionic liquid containing hetero-elements is at least one of boron-containing, nitrogen-containing, phosphorus-containing and sulfur-containing ionic liquids; (2) placing the obtained mixture in a boron-containing, nitrogen-containing, phosphorus-containing and / or sulfur-containing atmosphere, and carrying out pre-adsorption at 200-500 DEG C; (3) treating the pre-adsorbed material by using a plasma; and (4) washing the material obtained in the step (3) with water, and drying the material to obtain the porous miscellaneous element modified two-dimensionalcarbon material. The porous hetero-element modified two-dimensional carbon material disclosed by the invention has a relatively high specific surface area, rich pore channel structures, dispersed defect sites and high thermal stability, and has relatively good catalytic activity and stability in acetylene hydrochlorination reaction.

Description

[0001] (1) Technical field [0002] The invention relates to a preparation method of a porous heteroelement-modified two-dimensional carbon material and its application in the reaction of synthesizing vinyl chloride. [0003] (2) Background technology [0004] Polyvinyl chloride (PVC) is the third largest general-purpose plastic, and is generally obtained by polymerization of its monomer vinyl chloride. Due to the energy occurrence characteristics of rich coal, poor oil and little gas in my country, the preparation of vinyl chloride by coal-based calcium carbide method (acetylene hydrochlorination method) is the mainstream process of polyvinyl chloride production in my country. The existing catalysts used in the synthesis of vinyl chloride are mercuric chloride and mercury-free chlorides with metal chlorides as active components. Since mercuric chloride will cause serious pollution to the environment, and the polyvinyl chloride synthesized by it contains a small amount of merc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18B01J27/02B01J27/14B01J27/24B01J35/10B01J37/34C07C17/08C07C21/06
CPCB01J37/346B01J37/349B01J21/18B01J27/24B01J27/14B01J27/02C07C17/08B01J35/618B01J35/60B01J35/638B01J35/635B01J35/633C07C21/06
Inventor 赵佳岳玉学丰枫李小年金春晓方正倪珺王柏林陈志朱文锐
Owner ZHEJIANG UNIV OF TECH
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