CN115043401A - Nitrogen-doped hierarchical pore biochar prepared by wet biomass pyrolysis and application thereof - Google Patents
Nitrogen-doped hierarchical pore biochar prepared by wet biomass pyrolysis and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of porous carbon materials, and particularly relates to nitrogen-doped hierarchical porous biochar as well as a preparation method and application thereof. Aiming at the problems of shortage of fossil energy, huge yield of waste biomass, complex utilization steps, low utilization rate and the like at present, and the defects that a large amount of tar which is easy to cause secondary pollution is difficult to remove and the like generated in the process of preparing biochar by pyrolysis, the invention provides a method for preparing nitrogen-doped hierarchical pore biochar by pyrolyzing waste wet biomass and nitrogen-containing substances in one step by using the water contained in the waste biomass, wherein the method takes the nitrogen-containing substances as nitrogen-doping activating agents and comprises the following steps: and uniformly mixing the waste wet biomass with a nitrogen doping agent, and pyrolyzing at high temperature in an inert atmosphere to obtain the nitrogen-doped hierarchical pore biochar. The invention has wide raw materials and low cost; the method does not use a strong corrosive activating agent and does not produce tar, and is easy to realize industrial application; and the prepared biochar has a developed hierarchical pore structure and rich alkaline oxygen-containing and nitrogen-containing functional groups.
Description
Technical Field
The invention belongs to the technical field of porous carbon materials, and particularly relates to nitrogen-doped hierarchical porous biochar as well as a preparation method and application thereof.
Background
Compared with the continuously reduced and non-renewable fossil energy sources, the biomass resources on the earth are rich and highly renewable. With the increase of the population number of the world and the development of urbanization, the production amount of waste biomass in human production and life is huge, and the annual yield of crop straws can reach 7 hundred million tons only in China. The waste biomass is praised as 'resource in wrong place', and the harmless treatment and the resource utilization are important measures for accelerating the ecological civilization construction and realizing the carbon neutralization target. The biochar with a developed pore structure and rich surface functional groups is prepared by pyrolyzing the waste biomass, is widely applied to the fields of environmental protection, energy, agricultural production and the like, and is a very representative technology for realizing the recycling of the waste biomass.
According to investigation, the waste biomass is stored by adopting a natural wind dry method, the waste biomass has a certain water content, the water content is greatly influenced by weather, for example, the water content can reach 5-50% in rainy days with low air resistance or high humidity, and the water content of industrial waste biomass such as vinasse and the like can reach 50-80%. In the existing method, the water-containing biomass is usually dried and then used as a carbon precursor for pyrolysis, wherein evaporation of water needs to consume a large amount of heat and energy, the generated water vapor cannot be reasonably and effectively utilized, and tar generated in the pyrolysis process is difficult to remove, so that secondary pollution is caused and the recycling efficiency is reduced.
In the removal of the pollutants, the pore structure of the biochar determines the diffusion, mass transfer, adsorption, product transport and storage and the like of the pollutants. The biochar obtained by directly pyrolyzing the dried biomass has a less developed pore structure, and the specific surface area and the pore volume are usually less than 200m 2 G and 0.2cm 3 Per g, a certain activating agent is usually added for pore-forming treatment. CN110467180A adopts soybean as a biomass charcoal source, adopts KOH as an activating agent, and obtains a porous biomass derived charcoal material after high-temperature calcination, and the specific surface area can reach 300-1100m 2 (ii) in terms of/g. However, the activating agent is usually strong acid, strong base, metal salt and other reagents, which easily corrode equipment and may cause injury to personnel, and meanwhile, a large amount of water is needed for cleaning after the pore is formed by the activation method, a large amount of waste water is generated, and secondary pollution to the environment is easily caused.
Therefore, developing and searching a method for preparing porous biochar with simple and convenient preparation process, cleanness, environmental protection and low price becomes a development trend of high-value utilization of waste wet biomass.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing nitrogen-doped hierarchical pore biochar by utilizing the moisture of biomass and simultaneously inhibiting tar generation. In the pyrolysis process, under the low-flow-rate nitrogen atmosphere, the steam atmosphere formed by water contained in the waste wet biomass is utilized, biomass pyrolysis and tar catalytic reforming are promoted at high temperature, tar generation is inhibited, and finally, the biochar with rich surface functional groups and developed pore structures is formed.
The invention firstly provides a preparation method of nitrogen-doped hierarchical pore biochar, which comprises the following steps: and uniformly mixing the waste wet biomass with a nitrogen doping agent, and pyrolyzing at high temperature in an inert atmosphere to obtain the nitrogen-doped hierarchical pore biochar.
The waste wet biomass raw material is waste biomass rich in lignocellulose and comprises at least one of wood chips, vinasse, bamboo powder, rice hulls, coconut shells, walnut shells, straws or bagasse.
Wherein the particle size range of the waste wet biomass is controlled to be 50-200 mu m.
Wherein the mass water content of the waste wet biomass is 0-80%.
Preferably, the water content of the waste wet biomass is 5-80%.
More preferably, the water content of the waste wet biomass is 25-50%.
Wherein the nitrogen doping agent is at least one of urea, melamine, dicyandiamide, melamine cyanurate salt or carbon nitride.
Preferably, the nitrogen doping agent is melamine cyanurate salt and/or carbon nitride.
Wherein the mass ratio of the waste wet biomass to the nitrogen-doped agent is 1: 0.1 to 10.
Preferably, the mass ratio of the waste wet biomass to the nitrogen doping agent is 1: 0.5 to 5.
The inert atmosphere is preferably nitrogen, and the gas flow is 10-150 mL/min.
Preferably, the gas flow is 20-40 mL/min.
Wherein the nitrogen purity is 99.9%.
Wherein the pyrolysis temperature is 600-1000 ℃.
Wherein the pyrolysis time is 30-120 min.
Preferably, the pyrolysis temperature is 900 ℃.
The invention also provides the nitrogen-doped hierarchical pore biochar prepared by the method.
Wherein the specific surface area of the nitrogen-doped hierarchical porous biochar reaches 1000cm 3 The nitrogen content is 3.0 wt% or more, the basic nitrogen-containing functional group is 67% by weight, and the oxygen content is 13.0 wt% or more.
Preferably, the specific surface area is 1000-2000 m 2 And the nitrogen content of the nitrogen-doped hierarchical pore biochar is 3-20 wt%.
The invention also provides application of the nitrogen-doped hierarchical pore biochar prepared by the method in acid gas removal.
Has the advantages that:
(1) the invention selects the waste wet biomass with wide source and low price, can reduce the production cost of the activated carbon, and is an ideal material of the activated carbon precursor.
(2) In the method, under the low nitrogen flow rate, in the lignocellulose biomass, the lignin and the moisture in the gaps of the cellulose structure swell molecules in the pyrolysis process, so that larger pores are created; meanwhile, the water vapor environment formed by water evaporation can further perform etching reaction with the carbon matrix to form numerous micropores. In the environment, rich oxygen-containing functional groups are formed on the surface of the carbon material along with the steam etching reaction, and the oxygen-containing functional groups can perform the Maillard reaction with ammonia gas generated by pyrolysis to promote nitrogen doping, so that the nitrogen loss in the conventional pyrolysis process is inhibited. Finally, the specific surface area is developed (1000 m) 2 More than g), high nitrogen content (more than 3wt percent) and rich oxygen-containing functional groups (more than 13wt percent).
(3) In the preparation method, the moisture of the lignocellulose biomass is utilized, strong corrosive activating agents such as KOH and the like are avoided in the whole process, the corrosion to equipment is greatly reduced, the obtained product does not need to be washed to be neutral, the waste of water resources is reduced, and the production cost is reduced.
(4) The nitrogen-doped hierarchical pore biochar prepared by the invention has developed porous structures such as micropores, mesopores and the like (the pore volume of the micropores can reach 0.65 cm) 3 The pore volume of the mesopore can reach 0.55cm 3 The surface of the material is rich in nitrogen-containing and oxygen-containing functional groups, the nitrogen content of the material is 3-20 wt%, the main nitrogen-containing groups are pyrrole nitrogen (PyN) and pyridine nitrogen (PdN), the occupation ratio is up to 65%, the nitrogen-containing groups are basic functional groups, and the H pair ratio can be greatly improved 2 The ability to remove acid gases such as S.
Drawings
FIG. 1 is a nitrogen adsorption/desorption curve of biochar prepared in example 1 of the present invention and comparative example 1;
FIG. 2 is an electron micrograph of samples prepared according to example 1 and comparative example 1 of the present invention;
FIG. 3 is a graph showing the binding energy of nitrogen-containing functional groups of biochar prepared in example 1 of the present invention and comparative example 1.
Detailed Description
According to the invention, under the atmosphere of low-flow-rate nitrogen, water vapor formed by water contained in the waste wet biomass forms oxygen radicals in a high-temperature environment to attack a carbon matrix, so that the pyrolysis of the biomass is promoted, the generation of tar is inhibited, and finally the nitrogen-doped hierarchical-pore biochar with rich oxygen-containing functional groups and nitrogen-containing functional groups and developed pores is formed. The method has the advantages of simple operation, low cost, environmental protection and the like, and the prepared nitrogen-doped hierarchical pore biochar has developed pores, rich oxygen-containing and nitrogen-containing functional groups and good environmental and economic effects.
The invention firstly provides a preparation method of nitrogen-doped hierarchical pore biochar, which comprises the following steps: and uniformly mixing the waste wet biomass with a nitrogen doping agent, and pyrolyzing at high temperature in an inert atmosphere to obtain the nitrogen-doped hierarchical pore biochar.
Wherein the waste wet biomass raw material is at least one of wood chips, vinasse, bamboo powder, rice hulls, coconut shells, walnut shells, straws or bagasse. The invention selects common agricultural and forestry wastes and industrial wastes, and the wastes are waste biomasses mainly comprising lignocellulose, because the lignocellulose contains a large amount of hydroxyl groups, the more the hydroxyl groups are, the stronger the water absorption of the plant fiber is, and the plant fiber has stronger water absorption and water retention.
Wherein the particle size range of the waste wet biomass is controlled to be 50-200 mu m. The invention aims to control the particle size range of waste wet biomass: the method is convenient for the moisture in the gaps between the lignin and the cellulose structure in the pyrolysis process to fully swell the molecules, creates proper pores and can obtain biochar with more uniform properties.
Wherein the mass water content of the waste wet biomass is 0-80%.
Preferably, the water content of the waste wet biomass is 5-80%.
More preferably, the water content of the waste wet biomass is 25-50%.
Wherein the nitrogen doping agent is at least one of urea, melamine, dicyandiamide, melamine cyanurate salt or carbon nitride.
Preferably, the nitrogen doping agent is a nitrogen source with better thermal stability, such as melamine cyanurate salt and carbon nitride.
The nitrogen doping agent is selected from the following components: the substances are mainly organic nitrogen and only generate ammonia gas and CO by thermal decomposition 2 And other substances needing to be treated are not easily generated after the nitrogen is doped in the gas, so that the operation process is simplified, and the cost is reduced. And the melamine cyanurate salt and the carbon nitride are nitrogen precursors with stronger thermal stability, and the nitrogen doping performance is better at high temperature.
Wherein the mass ratio of the waste wet biomass to the nitrogen-doped agent is 1: 0.1 to 10. Preferably, the mass ratio of the waste wet biomass to the nitrogen doping agent is 1: 0.5 to 5.
The inert atmosphere is preferably nitrogen, and the gas flow is 10-150 mL/min.
Preferably, the gas flow is 20-40 mL/min.
Wherein the nitrogen purity is 99.9%.
Wherein the pyrolysis temperature is 600-1000 ℃.
Wherein the pyrolysis time is 30-120 min.
Preferably, the pyrolysis temperature is 900 ℃.
The purpose of controlling the pyrolysis temperature in the range is to fully react and realize pore-forming.
The invention also provides the nitrogen-doped hierarchical pore biochar prepared by the method.
Wherein the specific surface area of the nitrogen-doped hierarchical porous biochar reaches 1000cm 3 The nitrogen content is 3.0 wt% or more, the ratio of basic nitrogen-containing functional groups (pyridine nitrogen and pyrrole nitrogen) is 67%, and the oxygen content is 13.0 wt% or more.
The invention also provides application of the nitrogen-doped hierarchical pore biochar prepared by the method in acid gas removal.
The operation flow for preparing the biochar in the prior art is complex, a series of flows including pre-carbonization, oxidation treatment, nitrogen-doped impregnation, high-temperature calcination and the like are needed, and the biochar with a developed pore structure can be obtained by pyrolyzing a wet biomass sample by a one-step method.
In the prior art, for example, CN110935280A nitrogen flow rate control has two stages, namely a pre-carbonization stage and a nitrogen-doping calcination stage, wherein the nitrogen flow rate is 50-200 mL/min, so that the purpose of providing an inert gas atmosphere is mainly to prevent the burning loss phenomenon of the biochar in the preparation process.
The main purposes of the present application for regulating the nitrogen flow rate are: in the pyrolysis process, the swelling rate of water in gaps between lignin and cellulose structures is controlled, steam atmospheres with different concentrations are formed, the steam and the carbon matrix are subjected to reforming reaction to etch the carbon matrix to generate a pore structure, and simultaneously, a large amount of CO and H are formed by the reforming reaction 2 The carbon nitride can be subjected to polycondensation reaction with nitrogen doping agents such as urea and the like to form carbon nitride with good stability, so that the carbon nitride can be slowly decomposed to release ammonia gas in a thermal decomposition stage, and the nitrogen doping level can be improved.
Now, the technical scheme of the present invention will be further described in detail by taking a specific preparation method for preparing nitrogen-doped hierarchical porous biochar by pyrolyzing wet biomass at a low nitrogen flow rate as an example. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
Selecting cedar chip powder with the particle size of 50-150 mu m and the water content of 50% as a biomass raw material for preparing the nitrogen-doped hierarchical pore biochar, adding urea according to the mass ratio of the wet biomass to the nitrogen doping agent of 1:1, and uniformly mixing. Placing the mixture in a tube furnace, introducing nitrogen for half an hour to completely exhaust the air in the furnaceAnd (4) qi. The nitrogen flow is 40mL/min, the heating rate is 5 ℃/min, the activation target temperature is 900 ℃, and the activation time is 2 h. Naturally cooling to obtain the nitrogen-doped hierarchical pore biochar, wherein the specific surface area of the doped hierarchical pore biochar is 1718m 2 The nitrogen content was 3.03 wt%, the oxygen content was 19.68 wt%, and the breakthrough sulfur content was 630 mg/g.
Example 2
Selecting wet distiller's grain powder with the grain diameter of 100-150 mu m and the water content of 50% as a biomass raw material for preparing the nitrogen-doped hierarchical pore biochar, adding urea according to the mass ratio of the wet biomass to the nitrogen-doping agent of 1:3, and uniformly mixing. The mixture was placed in a tube furnace and nitrogen was introduced for half an hour to purge the air from the furnace. The nitrogen flow is 20mL/min, the heating rate is 5 ℃/min, the temperature is increased to 900 ℃, and the temperature is maintained for 1 h. Naturally cooling to obtain nitrogen-doped hierarchical porous biochar, wherein the specific surface area of the doped porous carbon is 1434m 2 The nitrogen content was 6.34 wt%, the oxygen content was 15.03 wt%, and the breakthrough sulfur capacity was 471 mg/g.
Example 3
Selecting cypress chips with the grain size of 50-150 mu m and the water content of 25% as a biomass raw material for preparing the nitrogen-doped hierarchical pore biochar, adding melamine according to the mass ratio of the wet biomass to the nitrogen doping agent of 1:2, and uniformly mixing. The mixture was placed in a tube furnace and nitrogen was introduced for half an hour to purge the air from the furnace. The nitrogen flow is 60mL/min, the heating rate is 5 ℃/min, the activation target temperature is 900 ℃, and the activation time is 2 h. Naturally cooling to obtain the nitrogen-doped hierarchical porous biochar, wherein the specific surface area of the doped porous carbon is 1427m 2 The nitrogen content was 5.39 wt%, the oxygen content was 13.04 wt%, and the breakthrough sulfur capacity was 579 mg/g.
Example 4
Selecting cypress chips with the particle size of 50-80 mu m and the water content of 50% as a biomass raw material for preparing the nitrogen-doped hierarchical pore biochar, adding carbon nitride according to the mass ratio of the wet biomass to the nitrogen doping agent of 1:3, and uniformly mixing. The mixture was placed in a tube furnace and nitrogen was introduced for half an hour to purge the air from the furnace. The nitrogen flow is 40mL/min, the heating rate is 5 ℃/min, the activation target temperature is 900 ℃, and the activation time is 0.5 h. Nature of natureCooling to obtain nitrogen-doped hierarchical pore biochar, wherein the specific surface area of the doped hierarchical pore biochar is 1069m 2 The nitrogen content was 6.47 wt%, the oxygen content was 16.73 wt%, and the breakthrough sulfur content was 338 mg/g.
Comparative example 1
Selecting dry cedar chip powder with the particle size of 50-150 mu m and the water content of 0 as a biomass raw material for preparing the nitrogen-doped hierarchical pore biochar, adding urea according to the mass ratio of the dry biomass to the nitrogen-doping agent of 1:1, and uniformly mixing. The mixture was placed in a tube furnace and nitrogen was introduced for half an hour to purge the air from the furnace. The nitrogen flow is 40mL/min, the heating rate is 5 ℃/min, the activation target temperature is 900 ℃, and the activation time is 1 h. Naturally cooling to obtain the nitrogen-doped hierarchical pore biochar, wherein the specific surface area of the doped porous carbon is 660m 2 The nitrogen content was 2.38 wt%, the oxygen content was 10.06 wt%, and the breakthrough sulfur content was 41 mg/g.
Claims (10)
1. The preparation method of the nitrogen-doped hierarchical pore biochar is characterized by comprising the following steps: the method comprises the following steps: and uniformly mixing the waste wet biomass with a nitrogen doping agent, and pyrolyzing at high temperature in an inert atmosphere to obtain the nitrogen-doped hierarchical pore biochar.
2. The method for preparing nitrogen-doped hierarchical pore biochar according to claim 1, wherein the method comprises the following steps: the waste wet biomass raw material is waste biomass rich in lignocellulose and comprises at least one of wood chips, vinasse, bamboo powder, rice hulls, coconut shells, walnut shells, straws or bagasse.
3. The method for preparing nitrogen-doped hierarchical pore biochar according to claim 1 or 2, wherein the method comprises the following steps: the particle size range of the waste wet biomass is controlled to be 50-200 mu m.
4. The method for preparing nitrogen-doped hierarchical pore biochar according to any one of claims 1 to 3, wherein the method comprises the following steps: the mass water content of the waste wet biomass is 0-80%; preferably, the water content of the waste wet biomass is 5-80%; more preferably, the water content of the waste wet biomass is 25-50%.
5. The method for preparing nitrogen-doped hierarchical pore biochar according to any one of claims 1 to 4, wherein the method comprises the following steps: the nitrogen doping agent is at least one of urea, melamine, dicyandiamide, melamine cyanurate salt or carbon nitride; preferably, the nitrogen doping agent is melamine cyanurate salt and/or carbon nitride.
6. The method for preparing nitrogen-doped hierarchical pore biochar according to any one of claims 1 to 5, wherein the method comprises the following steps: the mass ratio of the waste wet biomass to the nitrogen-doped agent is 1: 0.1 to 10; preferably, the mass ratio of the waste wet biomass to the nitrogen doping agent is 1: 0.5 to 5.
7. The method for preparing nitrogen-doped hierarchical pore biochar according to any one of claims 1 to 6, wherein the method comprises the following steps: the inert atmosphere is preferably nitrogen, and the gas flow is 10-150 mL/min; preferably, the gas flow is 20-40 mL/min.
8. The method for preparing nitrogen-doped hierarchical pore biochar according to any one of claims 1 to 7, wherein the method comprises the following steps: the pyrolysis temperature is 600-1000 ℃; the pyrolysis time is 30-120 min; preferably, the pyrolysis temperature is 900 ℃.
9. The nitrogen-doped hierarchical pore biochar prepared by the preparation method of the nitrogen-doped hierarchical pore biochar according to any one of claims 1 to 8; preferably, the specific surface area is up to 1000cm 3 The nitrogen content is 3.0 wt% or more, the basic nitrogen-containing functional group is 67% by weight, and the oxygen content is 13.0 wt% or more.
10. Use of the nitrogen-doped hierarchical pore biochar of claim 9 in acid gas removal.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116393155A (en) * | 2023-04-20 | 2023-07-07 | 江苏大学 | Carbocyclic doped g-C 3 N 4 Preparation method of heterojunction in basal plane and application of heterojunction in photo-reforming cellulose |
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