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Amino resin modified nitrogen-doped activated carbon catalyst as well as preparation method and application thereof

Amino resin modification, amino resin technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, hydrogen halide addition preparation, etc., can solve the problems of complicated procedures, unsuitable for industrial production, and high cost, and achieve environmental friendliness, Conducive to industrial promotion and application, the effect of high decomposition temperature

Active Publication Date: 2020-06-30
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN108187721A uses silkworm cocoon shells with high natural nitrogen content as a precursor, and directly obtains nitrogen-doped carbon catalysts through carbonization and activation without complicated introduction of nitrogen elements. The obtained catalyst is in the form of powder, which is not suitable for the needs of industrial production equipment for acetylene hydrochlorination
Patent CN108097229A has invented a preparation method of corn powder-based sulfur-nitrogen co-doped carbon material. Mix and stir corn powder, templating agent and water evenly, extrude, dry, and carbonize in a tube furnace under the protection of an inert atmosphere. Rigid carbon skeleton, template agent removed, washed, dried for later use; patent CN109622016A uses commercial melamine formaldehyde resin and phenolic resin as precursors, and obtains nitrogen-doped carbon catalyst by curing and roasting in an inert atmosphere; but these two catalysts The preparation method needs to introduce and remove the template process, use 10% hydrofluoric acid solution to remove the template, the process is complicated, the cost is high, and it is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A nitrogen-doped activated carbon catalyst modified by amino resin is prepared by loading amino resin on activated carbon, drying and carbonizing. Its preparation method is:

[0027] 1) Preparation of amino resin impregnation solution: Dilute 0.9mL formaldehyde solution (commercially available, 37-40% mass fraction, the same below) to 10mL, adjust the pH to 9.6 with triethanolamine, add 0.5g melamine, heat to 65°C in a water bath, and react 1h to obtain amino resin impregnation solution; the molar ratio of the aldehyde compound to the amino compound is 3:1.

[0028] 2) Equal-volume impregnation: Add the amino resin impregnating solution in step 1) to 10 g of coconut shell activated carbon and mix, stir evenly, heat at 60°C for 12 hours, and dry at 125°C to obtain a catalyst precursor.

[0029] 3) Carbonization: the catalyst precursor is heated to 550°C at a heating rate of 2-5°C / min under the protection of nitrogen in an atmosphere furnace, and kept for 4 hours.

[00...

Embodiment 2

[0032] An amino resin-modified nitrogen-doped activated carbon catalyst is prepared by loading amino resin on activated carbon, drying and carbonizing. Its preparation method is:

[0033] 1) Preparation of amino resin impregnation solution: dilute 1.8mL formaldehyde solution to 10mL, adjust pH to 9.6 with triethanolamine, add 0.5g melamine, heat to 65°C in water bath and stir to dissolve to obtain amino resin impregnation solution; the aldehyde compound and amino compound The molar ratio is 6:1.

[0034] 2) Equal-volume impregnation: Add the impregnating solution in step 1) dropwise to 10 g of coconut shell activated carbon, stir evenly, heat at 60° C. for 12 hours, and dry at 125° C. to obtain a catalyst precursor.

[0035] 3) Carbonization: the catalyst precursor is heated to 550°C at a heating rate of 2-5°C / min under the protection of nitrogen in an atmosphere furnace, and kept for 4 hours.

[0036]The amino resin modified nitrogen-doped activated carbon catalyst is used ...

Embodiment 3

[0038] An amino resin-modified nitrogen-doped activated carbon catalyst is prepared by loading amino resin on activated carbon, drying and carbonizing. Its preparation method is:

[0039] 1) Preparation of amino resin impregnation solution: dilute 1.8mL formaldehyde solution to 10mL, adjust pH to 9.5 with triethanolamine, add 1g of melamine, heat in water bath to 65-70°C and stir to dissolve to obtain impregnation solution; the mole ratio of the aldehyde compound and amino compound The ratio is 3:1.

[0040] 2) Equal-volume impregnation: Add the impregnating solution in step 1) dropwise to 10 g of coconut shell activated carbon, stir evenly, keep warm at 60° C. for 16 hours, and dry at 125° C. to obtain a catalyst precursor.

[0041] 3) Carbonization: the catalyst precursor is heated to 550°C at a heating rate of 2-5°C / min under the protection of nitrogen in an atmosphere furnace, and kept for 4 hours.

[0042] The amino resin modified nitrogen-doped activated carbon catalys...

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PUM

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Abstract

The invention discloses an amino resin modified nitrogen-doped activated carbon catalyst and a preparation method thereof. The preparation method comprises the following steps: 1) preparing an amino resin impregnation liquid: carrying out a reaction on an amino compound with an aldehyde compound at the temperature of 10-75 DEG C and pH of 9.0-10.0 for 1-4 h to obtain the amino resin impregnation liquid; 2) impregnation: mixing activated carbon with the amino resin impregnation liquid obtained in the step 1), carrying out heat preservation at the temperature of 10-60 DEG C for 6-12 h, and drying to obtain a catalyst precursor; and (3) carbonizing: carbonizing the catalyst precursor obtained in the step (2) under the protection of inert gas, and thus obtaining the nitrogen-doped activated carbon catalyst. The invention also discloses an application of the nitrogen-doped activated carbon catalyst in a reaction for synthesizing vinyl chloride by hydrochlorination of acetylene. The nitrogen-doped activated carbon catalyst is an economical and practical green catalyst, the preparation method is simple and feasible, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation and application, and in particular relates to an amino resin-modified nitrogen-doped activated carbon catalyst and a preparation method and application thereof. Background technique [0002] Vinyl chloride monomer is an important raw material for organic chemical synthesis. The main purpose is to produce polyvinyl chloride and vinyl chloride copolymer. Polyvinyl chloride (PVC) is one of the world's top five engineering plastics and plays a pivotal role in the plastics industry. At present, there are two main production methods of vinyl chloride monomer in the world: calcium carbide method acetylene hydrochlorination method and ethylene method ethylene oxychlorination method, and my country's "coal-rich, oil-poor" energy structure determines the production of vinyl chloride The process mainly adopts the coal-based calcium carbide method. In the industrial production of vinyl chloride, ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/02B01J37/08C07C17/08C07C21/06
CPCB01J27/24B01J37/0203B01J37/0213B01J37/082B01J37/084C07C17/08C07C21/06Y02P20/584
Inventor 曹少魁周晓飞刘应良王景涛
Owner ZHENGZHOU UNIV