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Shell-based nitrogen-doped activated carbon catalyst prepared by one-step method, product and application

A nutshell-based nitrogen and catalyst technology, which is applied in catalyst activation/preparation, physical/chemical process catalyst, hydrogen halide addition preparation, etc., can solve the problems of complex process, high cost, unsuitable for industrial production, etc. Simplification, manufacturing cost reduction, cost saving effect

Pending Publication Date: 2020-07-03
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 flour-based sulfur-nitrogen co-doped carbon material. Mix and stir corn flour, templating agent and water evenly, extrude, dry, and carbonize in a tube furnace under the protection of an inert atmosphere. Rigid carbon skeleton, remove template, wash, dry for later use; but the preparation method of the catalyst needs to introduce and remove the template process, and use 10% hydrofluoric acid solution to remove the template, the process is complicated, the cost is high, and it is not suitable Industrial production

Method used

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  • Shell-based nitrogen-doped activated carbon catalyst prepared by one-step method, product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Blank test: Weigh 30g of husks and place them in an atmosphere furnace, heat up to 500°C at 5°C / min in a nitrogen atmosphere, keep the temperature for 4 hours, and then cool the furnace to obtain activated carbon.

[0027] Catalytic activity evaluation: reaction temperature 180℃, n (C2H2) :n (HCl) =1:1.1, acetylene space velocity 45h -1 , Acetylene conversion rate is 20.84%, and vinyl chloride selectivity is 98.35%.

Embodiment 2

[0029] The step of preparing the nutshell-based nitrogen-doped activated carbon catalyst is as follows:

[0030] 1) Pretreatment of the husk: crush the husk (walnut shell), sieving, and take particles with a particle size of 8-20 mesh, wash and dry for later use; dry at 80°C for 4 hours and then at 150°C;

[0031] 2) Weigh 40mL of deionized water, heat the water bath to 75°C, add 1.2g of melamine, 1.0g of dicyandiamide, and 0.2g of tetraethylammonium chloride, and stir for 1h to obtain a clear impregnating solution; (in other embodiments, the The nitrogen source can also be one or a mixture of two or more of urea, thiourea, cyanamide, hexamethylene diamine, triethanolamine, guanidine hydrochloride, imidazole, pyridine, pyrrole, and amino acids);

[0032] Weigh 40g of walnut shells, add the dipping solution to the walnut shells, stir well, immerse at 75°C for 12h, pour off excess water, keep at 80°C for 4h to dry the surface water stains, and then heat to 105°C to dry to obtain the ca...

Embodiment 3

[0038] The step of preparing the nutshell-based nitrogen-doped activated carbon catalyst is as follows:

[0039] 1) Pretreatment of the husk: crush the husk (walnut shell), sieving, and take particles with a particle size of 8-20 mesh, wash and dry for later use; dry at 80°C for 4 hours and then at 150°C;

[0040] 2) Dilute 1.8 mL of formaldehyde solution (commercially available, with a mass fraction of 37-40%, the same below) to 40 mL with deionized water, adjust the pH to 9.0 with triethylamine, add 0.8 g dicyandiamide and 0.2 g urea, 10 Stir at ℃ for 4h to obtain a clear impregnating solution;

[0041] Weigh 40g of walnut shells, add the dipping solution to the walnut shells, stir well, keep at 10°C for 12h, pour off the excess water, keep at 80°C for 4h to dry the surface water stains, and then heat to 105°C to dry to obtain the catalyst precursor; The loading amount of the amino compound is 2.5% of the mass of the husk;

[0042] 3) The catalyst precursor is placed in an atmosphe...

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Abstract

The invention discloses a shell-based nitrogen-doped activated carbon catalyst prepared by a one-step method. The method comprises the following steps: 1) preprocessing shells; 2) dipping shells in adipping solution containing a nitrogen source to obtain a catalyst precursor; and 3) carbonizing the catalyst precursor under the protection of inert gas to obtain the nitrogen-doped activated carboncatalyst. Compared with a preparation method taking activated carbon as a carrier, the preparation method takes shells (activated carbon precursor) as the carrier, the preparation process is more simplified, the production cost is greatly reduced, and the method is more energy-saving and environment-friendly. Compared with an organic micromolecular nitrogen-containing compound, amino resin has higher thermal stability, a catalyst with equivalent activity can be obtained under the condition of lower loading capacity, and the cost of raw materials is effectively saved.

Description

Technical field [0001] The invention belongs to the technical field of catalyst preparation and application, and specifically relates to a one-step method for preparing a nutshell-based nitrogen-doped activated carbon catalyst, products and applications. Background technique [0002] Vinyl chloride is an important organic chemical raw material, and its homopolymer polyvinyl chloride (PVC) is one of the world's five major engineering plastics and plays a decisive role in the plastics industry. The production method of vinyl chloride in industry mainly relies on two chemical routes: ethylene oxychlorination and acetylene hydrochlorination. The energy structure of my country's "rich coal and lean oil" determines that the acetylene hydrochlorination process using coal as raw material is An important position in the production of vinyl chloride. At present, acetylene hydrochlorination reaction mainly uses activated carbon loaded low-mercury catalyst (mercury chloride loading is 4 to 6...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/02B01J37/08C07C17/08C07C21/06
CPCB01J27/24B01J37/0203B01J37/082B01J37/084C07C17/08C07C21/06Y02P20/10
Inventor 曹少魁周晓飞刘应良王景涛
Owner ZHENGZHOU UNIV
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