Starch-based nitrogen doped mesoporous molding carbon as well as preparation method and application thereof

A technology of nitrogen doping and pore forming, which is applied in hydrogen halide addition preparation, chemical instruments and methods, catalyst activation/preparation, etc. It can solve the problems of unsuitability for large-scale production, high requirements for reaction conditions, and high cost of templates. Achieve excellent catalytic performance, simple and easy-to-control preparation process, and stable batch performance

Active Publication Date: 2017-09-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the cost of the template used in this method is high, and the reaction conditions of the self-assembly process are demanding, which is not suitable for large-scale production
At present, there are no reports and related technologies on the preparation of nitrogen-doped mesoporous carbon directly using natural starch as a carbon source and its use as a mercury-free catalyst and catalyst carrier for acetylene hydrochlorination.

Method used

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  • Starch-based nitrogen doped mesoporous molding carbon as well as preparation method and application thereof
  • Starch-based nitrogen doped mesoporous molding carbon as well as preparation method and application thereof
  • Starch-based nitrogen doped mesoporous molding carbon as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Grind 50g of wheat starch and 5g of silica balls with a particle size of 15nm fully, add 25mL of water, stir evenly and extrude into strips with a particle size of 3.5mm and a length of 5cm. Place it at room temperature for 4 hours, and then put it in an oven at 110°C Drying for 12 hours yielded a carbon precursor. The dried samples were placed in a tube furnace, and treated at 850 °C for 3 h under a nitrogen atmosphere, with a heating rate of 3 °C / min. The heat-treated sample was put into a plastic beaker, and the template was removed with 10% HF solution, then washed with deionized water, and dried at 110°C to obtain starch-based nitrogen-doped mesoporous carbon. The particle size of the obtained carbon material is Ф3.5×5cm, and the content of N is 1.5%. The specific surface area is 800cc / g, the pore size is 10.2nm, and the pore volume is 0.86cc / g.

[0045] Take 2mL of catalyst for acetylene hydrochlorination. The pressure of acetylene and hydrogen chloride is: 0.1...

Embodiment 2

[0049] 40g of wheat starch and 10g of corn starch and 12.5g of silicon dioxide balls with a particle size of 30nm are fully ground, add 25mL of water, stir evenly and form a tablet to obtain a sheet-shaped carbon precursor with a diameter of 2cm and a thickness of 1cm, and then Place at room temperature for 4h. Then put it into an oven and dry it at 110 degrees for 8 hours to obtain a catalyst precursor. The dried samples were placed in a tube furnace, and treated at 700 °C for 3 h under a nitrogen atmosphere, with a heating rate of 2 °C / min. The heat-treated sample was put into a plastic beaker, the template was removed with 10% HF solution, then washed with deionized water, and dried at 110oC to obtain starch-based nitrogen-doped mesoporous carbon. The particle size of the obtained shaped mesoporous carbon material is Ф2×1 cm, and the content of N is 1.8%. The specific surface area is 670m 2 / g, the pore size is 18.2nm, and the pore volume is 0.76cc / g.

[0050] Take 2mL ...

Embodiment 3

[0053] 50g of wheat starch and 10g of nano-magnesium oxide with a particle size of 20nm were fully ground, added 25mL of water, stirred evenly and pressed into tablets to obtain a sheet-shaped carbon precursor with a diameter of 2cm and a thickness of 1cm, and then placed at room temperature for 4h. Then put it into an oven and dry it at 110 degrees for 8 hours to obtain a catalyst precursor. The dried samples were placed in a tube furnace, and treated at 700 °C for 3 h under a nitrogen atmosphere, with a heating rate of 2 °C / min. The heat-treated sample was put into a plastic beaker, and the template was removed with 5% HCl solution, then washed with deionized water, and dried at 110°C to obtain starch-based nitrogen-doped mesoporous carbon. The particle size of the obtained shaped mesoporous carbon material is Ф3.5×5 cm, and the content of N is 1.2%. The specific surface area is 960m 2 / g, the pore size is 17.1nm, and the pore volume is 0.86cc / g.

[0054] Take 2mL of cata...

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Abstract

The invention provides starch-based nitrogen doped mesoporous molding carbon. A preparation method of the carbon comprises the following steps: mixing natural starch with a template agent, adding water of a water absorption volume capacity equal to that of the mixture, uniformly stirring, performing extrusion modeling, leaving to stand for a time, and drying in an oven so as to obtain a mesoporous carbon precursor; putting the obtained mesoporous carbon precursor into a tubular furnace; in the presence of an inert gas, heating to 400-1000 DEG C, and roasting for 1-5 hours at a constant temperature so as to obtain a carbonized material; removing the template agent from the obtained carbonized material, washing till being neutral with deionized water, and drying, so as to obtain a finished product. The starch-based nitrogen doped mesoporous molding carbon provided by the invention is simple in preparation process, low in ash range and impurity content, free of extract nitrogen source, rich in pore, high in mesoporous structure ratio, adjustable in aperture and excellent in catalysis property in reaction for preparing vinyl chloride monomers by using a calcium carbide method, and can be used as a mercury-free catalyst or a catalyst carrier.

Description

[0001] (1) Technical field [0002] The invention relates to a starch-based nitrogen-doped mesoporous formed carbon and its preparation method and application. The starch-based nitrogen-doped mesoporous formed carbon can be directly used as a mercury-free catalyst for vinyl chloride in the calcium carbide method or as a mercury-free catalyst. carrier. [0003] (2) Background technology [0004] Various carbon materials such as activated carbon, carbon nanotubes, and mesoporous carbon materials have the advantages of strong adsorption, good chemical stability, and adjustable surface chemical groups. They are often used as carriers for loading noble metal catalysts and chloride catalysts. Recently, these Carbon materials can be directly used as catalysts for some dehydrogenation reactions, chlorination reactions, and acetylene hydrochlorination reactions, but they need to be pretreated and introduced into active centers, such as introducing acidic oxygen-containing groups through...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J32/00B01J37/02B01J37/08B01J35/10C07C17/08C07C21/06
CPCB01J27/24B01J35/1023B01J35/1042B01J35/1061B01J37/0018B01J37/0201C07C17/08C07C21/06
Inventor 李瑛蓝国钧王言唐浩东王小龙韩文锋刘化章
Owner ZHEJIANG UNIV OF TECH
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