Method for preparing hierarchical-pore phosphorus-doped carbon material from biomass

A biomass, multi-level pore technology, applied in chemical instruments and methods, carbon compounds, sustainable manufacturing/processing, etc., can solve the problems of inability to achieve simultaneous deashing, acid loading and pre-carbonization, uniform incorporation of phosphorus atoms, The problems of small specific surface area of ​​carbon materials, etc., to achieve the effect of simple and easy production process, low price and high doping amount

Inactive Publication Date: 2020-12-01
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process is simple, but the use of organic carbon precursors and phosphorus-containing ligands is usually costly
[0005] (2) Post-treatment doping method: This method usually refers to the introduction of functional groups containing phosphorus atoms on the activated carbon material through surface modification such as dry or wet methods. This method may cause the collapse of the activated carbon structure and cause its specific surface area decrease, due to the stable chemical properties of activated carbon materials, it is difficult to uniformly incorporate phosphorus atoms
[0010] c) CN201810591723.1 A phosphorus-doped microporous / mesoporous carbon material and its preparation method, the patent relates to a preparation method of phosphorus-doped microporous / mesoporous carbon material, said microporous / mesoporous carbon material The preparation method comprises the following steps: washing the okra with clear water, drying it, and freeze-drying it at -45°C to -80°C for 48 hours to 96 hours to obtain the freeze-dried okra; Heat treatment for 2 hours to 4 hours to obtain phosphorus-doped microporous / mesoporous carbon materials; the pretreatment method involved in this patent is low-temperature freeze-dried okra, which is different from the acid hydrothermal pretreatment method in this patent and cannot be realized Simultaneous deashing, acid loading and pre-carbonization cannot promote the carbonization process and reduce the processing time; the raw material used is usable okra, not biomass waste, and the cost is high; heat treatment at high temperature for 2 to 4 hours, It takes a long time, consumes a lot of energy, and the prepared carbon material has a small specific surface area

Method used

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  • Method for preparing hierarchical-pore phosphorus-doped carbon material from biomass
  • Method for preparing hierarchical-pore phosphorus-doped carbon material from biomass
  • Method for preparing hierarchical-pore phosphorus-doped carbon material from biomass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] In this example, six different types of biomass raw materials were selected and pulverized into 40-80 mesh particles, and 4g of the above biomass particles were weighed for use, and hierarchically porous phosphorus-doped carbons were prepared according to the following preparation methods Material;

[0060] A method for preparing a hierarchically porous phosphorus-doped carbon material from biomass, comprising the following steps:

[0061] Step 1, crushing the biomass into 40-80 mesh particles;

[0062] Step 2, weighing 4 g of the pulverized biomass particles and mixing them evenly with phosphoric acid solution at a ratio of phosphorus to carbon mass ratio of 3:1 to form a mixture;

[0063] Step 3. Put the mixture into a 50ml hydrothermal reaction kettle, and perform a hydrothermal reaction at a hydrothermal temperature of 200°C for 12 hours to generate hydrothermal carbon;

[0064] Step 4, open the reaction kettle after complete cooling, pour the hydrothermal carbon ...

Embodiment 2

[0070] In this example, the influence of different phosphorus sources and acid sources on the properties of the hierarchically porous phosphorus-doped carbon material was tested, only the types of phosphorus sources and acid sources were changed, and the materials were prepared according to the following preparation method;

[0071] A method for preparing a hierarchically porous phosphorus-doped carbon material from biomass, comprising the following steps:

[0072] Step 1, pulverizing the sawdust biomass into 40-80 mesh particles;

[0073] Step 2, weighing 4 g of the pulverized biomass particles and mixing them evenly with the phosphoric acid-containing solution at a phosphorus-to-carbon mass ratio of 3:1 to form a mixture;

[0074] Step 3. Put the mixture into a 50ml hydrothermal reaction kettle, and perform a hydrothermal reaction at a hydrothermal temperature of 200°C for 12 hours to generate hydrothermal carbon;

[0075] Step 4, open the reaction kettle after complete coo...

Embodiment 3

[0081] In this example, the influence of different hydrothermal temperatures on the properties of the hierarchically porous phosphorus-doped carbon material was tested, only the hydrothermal temperature was changed, and the material was prepared according to the following preparation method;

[0082] A method for preparing a hierarchically porous phosphorus-doped carbon material from biomass, comprising the following steps:

[0083] Step 1, pulverizing the sawdust biomass into 40-80 mesh particles;

[0084] Step 2, weighing 4 g of the pulverized biomass particles and mixing them evenly with phosphoric acid solution at a ratio of phosphorus to carbon mass ratio of 3:1 to form a mixture;

[0085] Step 3. Put the mixture into a 50ml hydrothermal reaction kettle, and perform a hydrothermal reaction at a hydrothermal temperature of 70°C, 150°C, 200°C, and 300°C for 12 hours to generate hydrothermal carbon;

[0086] Step 4, open the reaction kettle after complete cooling, pour the ...

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Abstract

The invention relates to a method for preparing a hierarchical-pore phosphorus-doped carbon material from biomass. The method comprises the following steps: firstly, crushing the biomass into tiny particles; then uniformly mixing the crushed biomass particles with a phosphoric acid-containing solution according to a certain ratio to form a mixture; putting the mixture into a hydrothermal reactionkettle, and carrying out a hydrothermal reaction at a certain temperature to generate hydrothermal carbon; dehydrating and drying the hydrothermal carbon obtained after the hydrothermal reaction; andputting the dried hydrothermal carbon into a pyrolyzing furnace, and carrying out rapid pyrolysis under the protection of an inert atmosphere to obtain a hierarchical-pore phosphorus-doped carbon material after rapid pyrolysis. According to the method disclosed by the invention, a rapid pyrolysis scheme is combined with phosphoric acid hydrothermal pre-carbonization, so a very ideal effect can beachieved only by performing rapid pyrolysis in a very short time, carbon preparation efficiency is greatly improved, and energy consumption is remarkably reduced; and meanwhile, due to the existence of phosphorus, a good carbon sequestration effect can be achieved, and carbon yield is increased.

Description

technical field [0001] The invention belongs to the field of preparation of phosphorus-doped carbon materials, in particular to the field of preparing hierarchical porous phosphorus-doped carbon materials from biomass. Background technique [0002] Biomass is the world's fourth largest energy after coal, oil and natural gas, accounting for about 14% of the world's primary energy consumption. China produces about 2.4 billion tons of waste biomass (crop rice straw, sawdust, weeds, etc.) every year. The energy contained in these waste biomass is equivalent to 1 billion tons of standard coal, which is a huge treasure house of resources. However, due to high labor costs, low economic benefits and increasingly stringent environmental regulations, the recycling of biomass has not been widely promoted at present, and most of the biomass is directly discarded; carbon materials are characterized by their good surface chemical properties, excellent It has the characteristics of mecha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/324C01B32/342
CPCC01B32/324C01B32/342Y02P20/10
Inventor 马培勇林凤飞张颖刘小好黄瑞毅祁风雷邢献军
Owner HEFEI UNIV OF TECH
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