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Preparation method and application of a nitrogen-containing carbon material

A technology for nitrogen-carbon materials and raw materials, which is applied in the field of preparation of nitrogen-containing carbon materials, can solve problems such as equipment corrosion, and achieve the effects of avoiding corrosion, achieving significant effects and reducing significantly.

Active Publication Date: 2019-01-15
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN1669918A and Publication No. CN101648707A Because the use of alkali or acid is under high temperature conditions, the problem of corrosion to equipment is serious

Method used

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  • Preparation method and application of a nitrogen-containing carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put the tobacco rod raw material in an oven at 60°C and dry until the moisture content is below 5%, crush it to 20-40 mesh, weigh 10 g of the sample, and mix it with methanol aqueous solution (methanol concentration 5%wt) according to the solid-liquid volume ratio of 1:15 Mix and transfer to a ball mill jar, add 1.0 g of HY molecular sieve (10% of the weight of the tobacco rod) and mix at room temperature for 5 h at a ball mill speed of 300 rpm to obtain a feed solution. The feed liquid and the agate beads were separated and transferred to a high-pressure reactor, and reacted at 100 °C and 5 MPa for 24 h under a nitrogen atmosphere. The reaction solution was filtered while it was hot, washed three times with deionized water, and the filter residue was dried and then placed in a tube furnace for carbonization at 600°C for 5 hours under a nitrogen atmosphere to obtain a primary carbonized material. Soak the primary carbonized material in 200 ml of 1 M HNO 3 -0.5 M H 2 o...

Embodiment 2

[0028] Put the raw material of the tobacco stem in an oven at 80°C and dry until the moisture content is below 5%, crush it to 40-60 mesh, weigh 10 g of the sample, and mix it with propanol aqueous solution (propanol concentration 10%wt) according to the solid-liquid volume ratio of 1:5 Mix and transfer to a ball mill jar, add SO 3 0.5 g of H-MCM-41 mesoporous material (5% of the weight of the tobacco rod) was mixed at room temperature for 2 h at a ball milling speed of 200 rpm. The feed liquid and the agate beads were separated and transferred to a high-pressure reactor, and reacted at 200 °C and 5 MPa for 1 h under a nitrogen atmosphere. The reaction solution was filtered while it was hot, washed three times with deionized water, and the filter residue was dried and placed in a tube furnace for carbonization at 800 °C for 1 h in a nitrogen atmosphere to obtain a primary carbonized material. The obtained primary carbonized material was soaked in 200 ml of 4 MHNO 3 -2 M H 2...

Embodiment 3

[0030] Put the tobacco rod raw material in an oven at 100°C and dry until the moisture content is below 5%, crush it to 60-90 mesh, weigh 10 g of the sample, and mix it with ethanol aqueous solution (ethanol concentration 8%wt) according to the solid-liquid volume ratio of 1:10. Mix and transfer to a ball mill jar, add 2.0 g of HZSM-5 molecular sieve (20% of the weight of the tobacco rod) and mix at room temperature for 4 h at a ball mill speed of 400 rpm. The feed liquid and the agate beads were separated and transferred to a high-pressure reactor, and reacted at 150 °C and 12 MPa for 14 h under a nitrogen atmosphere. The reaction solution was filtered while it was hot, washed three times with deionized water, and the filter residue was dried and placed in a tube furnace for carbonization at 700 °C for 2 h under a nitrogen atmosphere to obtain a primary carbonized material. The resulting primary carbon material was soaked in 200 ml of 8 MHNO 3 -8 M H 2 o 2 Stir in the mixe...

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Abstract

The invention a preparation method of a nitrogen-containing carbon material. The method is characterized by comprising the following steps: catalytically hydrolyzing tobacco stems serving as a raw material with solid acid, oxidizing, ammoniating and carbonizing to prepare a high-porosity nitrogen-containing gradient porous carbon material; and preparing an N-containing carbon material by sequentially adding nitric acid-hydrogen peroxide or pypocholoride-hydrogen peroxide and organic amine in subsequent step. The nitrogen-containing gradient porous carbon material has certain distribution in the range of micropores, mesopores and macropores, and is more applicable to adsorption of cigarette tar with wider grain size distribution; and the prepared nitrogen-containing gradient porous added into cigarette filter tips has a remarkable effect for reducing main stream smoke Cd and tar. The preparation method has the advantages that organic acid generated in a solid acid catalyzing cellulose hydrolysis process reacts with alcohol to generate ester, and the problem of corrosion of a reactor by organic acid can be avoided; content increase of the element N is favorable to complex adsorption of N on Cd in the smoke, and has a remarkable effect for reducing Cd in cigarette smoke.

Description

technical field [0001] The invention relates to a method for preparing a nitrogen-containing carbon material, in particular to a method for preparing a high-porosity nitrogen-containing step-pore carbon material by catalyzing and hydrolyzing tobacco rods after being pulverized, followed by oxidation, ammonification and carbonization. The material can be added to cigarette filters, and has a significant effect on reducing smoke Cd and tar. Background technique [0002] my country is a big tobacco country in the world, and its planting area, total output, cigarette output and sales volume all rank first in the world. A large amount of waste will inevitably be generated in the tobacco leaf and processing process. According to statistics, the tobacco stem produced in 2015 alone reached 1.163×10 6 Ton. Due to the relatively poor availability of tobacco stalks, most of them are disposed of by landfill or incineration, and the comprehensive utilization rate is extremely low, whic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05A24D3/06
CPCA24D3/06C01P2002/54C01P2006/12C01P2006/14C01P2006/16
Inventor 王金棒程多福高运谦邱纪青高健汪志波邓楠孟庆华刘亚丽洪群业郑路张仕华冯伟华郑新章
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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