CN114804069A - Method for preparing nitrogen-doped porous carbon material by gas-phase stripping of lignin and application - Google Patents
Method for preparing nitrogen-doped porous carbon material by gas-phase stripping of lignin and application Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 67
- 229920005610 lignin Polymers 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 4
- 239000007773 negative electrode material Substances 0.000 claims description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 4
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- -1 nitrogen-containing compound Chemical class 0.000 claims description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000000197 pyrolysis Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000005530 etching Methods 0.000 abstract description 2
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 238000005906 dihydroxylation reaction Methods 0.000 abstract 1
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 11
- 239000002244 precipitate Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000010411 electrocatalyst Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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Abstract
The invention provides a method for preparing a nitrogen-doped porous carbon material by stripping lignin in a gas phase and application, wherein the preparation method comprises the following steps: the method comprises the steps of taking alkali lignin and a gas-phase stripping auxiliary agent as raw materials, performing blending ball milling, performing pyrolysis in an inert gas atmosphere, and performing thermal decomposition on the gas-phase stripping auxiliary agent, etching the lignin and performing dehydroxylation to obtain the nitrogen-doped porous carbon material. The raw materials for preparing the material have wide sources and low cost, and the cost can be reduced to a greater extent. Meanwhile, the technical route is simple, the nitrogen-doped porous carbon material is obtained through one-step reaction, and the preparation process is convenient. The nitrogen-doped porous carbon material can be obtained only by simple washing and drying treatment after the reaction is finished, and the material is applied to the field of electrocatalysis and has higher catalytic activity.
Description
Technical Field
The invention relates to the field of electrochemistry, and particularly relates to a method for preparing a nitrogen-doped porous carbon material by gas-phase stripping of lignin and application of the nitrogen-doped porous carbon material.
Background
In the current situation of large energy consumption at present, the non-regenerability and high pollution of the traditional fossil fuel do not meet the requirements of sustainable development of human society. Therefore, a series of new energy utilization devices, such as: fuel cells, metal-air cells and water splitting systems, which are green, clean, high capacity and renewable, are considered to be promising alternatives to traditional fossil fuels. Among them, Oxygen Reduction Reaction (ORR) and Oxygen Evolution Reaction (OER) play a crucial role in this kind of advanced energy storage and conversion device. However, the precious metal materials (Pt, Ru, Ir) have proven to be excellent electrocatalysts, but due to their high price and scarce current storage, poor durability and poor resistance to methanol cross-effects, the large-scale application of these catalysts is limited, which also affects the development of new energy devices.
In recent years, researchers have been devoted to research on non-noble metal platinum catalysts and have proposed a number of alternative materials, such as carbides, transition metal oxides, metal sulfides, and the like. The porous carbon material has the advantages of high specific surface area, strong conductive capability, good thermal stability and chemical stability and the like, and is considered to be a good material for replacing the traditional noble metal electrocatalyst. The mesoporous graphitized carbon material has high specific surface area and porous structure, and the carbon material doped with heteroatoms (N, P, S or B) has the characteristics of low cost, high activity, high stability and the like. Therefore, how to design a convenient technical synthesis route and prepare a high-performance electrocatalyst becomes a hotspot of extensive research of researchers.
Therefore, the invention provides a method for preparing a nitrogen-doped porous carbon material based on a gas phase stripping method, which comprises the following steps: the nitrogen-doped porous carbon material is obtained by taking lignin as a carbon source and blending and pyrolyzing the lignin and a gas phase stripping aid. The method has the advantages of wide raw material source, low cost and capability of reducing the cost to a greater extent. Meanwhile, the technical route is simple, and the preparation method is convenient. The obtained nitrogen-doped porous carbon material can be applied to the field of electrocatalysis, can be used as a negative electrode material for preparing a zinc-air battery, and has the performance equivalent to that of a noble metal catalyst.
Disclosure of Invention
The invention aims to provide a method for preparing a nitrogen-doped porous carbon material by gas-phase stripping of lignin and application thereof, which have the advantages of wide raw material source, low cost and capability of reducing the cost to a greater extent. Meanwhile, the technical route is simple, the nitrogen-doped porous carbon material is obtained through one-step reaction, and the preparation process is convenient. The nitrogen-doped porous carbon material can be obtained only by simple washing and drying treatment after the reaction is finished, and the material is applied to the field of electrocatalysis and has higher catalytic activity and considerable application prospect.
The technical scheme of the invention is as follows: a method for preparing a nitrogen-doped porous carbon material by stripping lignin in a gas phase comprises the following steps:
mixing lignin and a gas phase stripping auxiliary agent, putting the mixture into a ball milling tank, carrying out ball milling for 24 hours at the rotating speed of 300r/min, transferring the mixture into a tubular furnace, and heating and carbonizing the mixture by stages; and after carbonization is finished, adding hydrochloric acid into the obtained porous carbon material, stirring and washing, washing with deionized water, performing centrifugal precipitation, and drying to obtain the nitrogen-doped porous carbon material.
Further, the lignin is alkali lignin washed with deionized water.
Further, the gas phase stripping aid comprises Zn 2+ Salts and nitrogen-containing compounds.
Further, the nitrogen-containing compound is NH 4 Cl, melamine or carbon nitride; said Zn 2+ The salt being ZnCl 2 、ZnC 2 O 4 Or ZnCO 3 。
Further, lignin, nitrogen-containing compound, Zn are used 2+ The mass ratio of the salt is 1:4-6: 1.
The rotation speed of the ball milling is 300r/min, and the reaction time of the ball milling is 24 h.
Further, during carbonization, inert gas is used as nitrogen or argon, the temperature is raised to 350 ℃ at the speed of 1 ℃/min in stages, and the temperature is kept for 3 hours; then the temperature is raised to 800 ℃ at the speed of 1 ℃/min, and the temperature is kept for 3 h.
Further, the hydrochloric acid concentration for washing the porous carbon material is 2mol/L, the stirring time is 12h, and then the porous carbon material is washed by deionized water and then centrifugally dried to obtain the nitrogen-doped porous carbon material.
Further, the nitrogen-doped porous carbon material is applied to the field of electrocatalysis and used as a negative electrode material for preparing a zinc-air battery.
Compared with the prior art, the technical scheme provided by the invention has the following advantages:
1. the method disclosed by the invention has the advantages that the alkali lignin is used as the raw material, the source is wide, the cost is low, and the cost can be reduced to a greater extent. Meanwhile, the technical route is simple, the nitrogen-doped porous carbon material is obtained only through blending pyrolysis reaction, and the preparation process is convenient.
2. According to the invention, the lignin is stripped in a gas phase by adopting the nitrogen-containing auxiliary agent, N element can be doped in the carbon chain structure of the lignin in the pyrolysis process, and the original lignin microspheres are converted into a wrinkled and fluffy porous structure through gas phase etching. The hetero atoms provide more active sites for the carbon material to enhance the electro-catalytic activity, and the porous structure also provides more channels for electron transmission in the electrochemical reaction process.
3. The nitrogen-doped porous carbon material prepared by the method disclosed by the invention can be applied to the field of electrocatalysis, can be used as a negative electrode material for preparing a zinc-air battery, and has better performance.
Description of the drawings:
FIG. 1 is a sorption-desorption isotherm diagram of a nitrogen-doped porous carbon material obtained by vapor phase exfoliation and a carbon material obtained by direct pyrolysis of lignin in example 1.
FIG. 2 is a graph showing the pore size distribution of the nitrogen-doped porous carbon material obtained by vapor phase exfoliation and the carbon material obtained by direct pyrolysis of lignin in example 1.
Fig. 3 is an XPS spectrum of the nitrogen-doped porous carbon material prepared in embodiment 1.
Fig. 4 is an SEM photograph of the nitrogen-doped porous carbon material produced in embodiment 1.
Fig. 5 shows the peak power density of the nitrogen-doped porous carbon material assembled zinc-air battery prepared in embodiment 1.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
1g of alkali lignin and 4g of NH 4 Cl、1g ZnCl 2 Blending, ball-milling for 24h by using a planetary ball mill under the condition of 300r/min until the mixture is ground into grey powder, putting the grey powder into a corundum boat, pyrolyzing the grey powder in a tube furnace, heating up by stages, heating up to 350 ℃ at the speed of 1 ℃/min in the first stage, and preserving heat for 3 h; then the temperature is raised to 800 ℃ at the speed of 1 ℃/min, and the temperature is kept for 3 h. By reaction of NH 4 Cl and ZnCl 2 Complete decomposition (NH) 4 Cl decomposition temperature is 337.8 ℃, ZnCl 2 Boiling point 732 deg.c) to produce a complete reaction of gas and lignin.
And pouring the pyrolyzed porous carbon material into 50ml of 2mol/L hydrochloric acid, stirring for 12 hours, performing centrifugal separation on the precipitate, washing the precipitate for 3 times by using deionized water, drying the precipitate in an oven at 60 ℃, and drying the dried precipitate to obtain the nitrogen-doped porous carbon material.
FIG. 1 is a diagram showing adsorption and desorption isotherms of a carbon material obtained by directly pyrolyzing lignin and the nitrogen-doped porous carbon material obtained by gas phase stripping, and the specific surface area is calculated to show that the specific surface area of the carbon material obtained by directly pyrolyzing lignin is only 148.3m 2 G, and the specific surface area of the nitrogen-doped porous carbon material is 1011.4m 2 /g。
Fig. 2 is a calculated pore size distribution diagram of a BJH model, in contrast to the pore size structure of the nitrogen-doped porous carbon material, in which a large number of micropores appear.
As can be seen from the XPS spectrum of fig. 3, the nitrogen-doped porous carbon material is composed of C, O, N elements.
As can be seen from the SEM image of fig. 4, the nitrogen-doped porous carbon material is a porous structure with surface wrinkles, fluffiness and many pores, and the abundant pore structure and the high specific surface area thereof provide more channels for transporting intermediates in the electrochemical reaction, which is beneficial to improving the electrocatalytic activity of the material.
As can be seen from FIG. 5, when the nitrogen-doped porous carbon material was used as a negative electrode to assemble a zinc-air battery, the peak power density was 62.4mW/cm 2 Slightly larger than Pt/C-RuO 2 Peak power density of(54.1mW/cm 2 ). These results fully demonstrate that the nitrogen-doped porous carbon material can be used as a metal-air battery dual-functional cathode material with great application potential.
Example 2
1g of alkali lignin, 5g of melamine and 1g of ZnC 2 O 4 Blending, ball-milling for 24h by using a planetary ball mill under the condition of 300r/min until the mixture is ground into grey powder, putting the grey powder into a corundum boat, pyrolyzing the grey powder in a tube furnace, heating up by stages, heating up to 350 ℃ at the speed of 1 ℃/min in the first stage, and preserving heat for 3 h; then the temperature is raised to 800 ℃ at the speed of 1 ℃/min, and the temperature is kept for 3 h. And pouring the pyrolyzed porous carbon material into 80ml of 2mol/L hydrochloric acid, stirring for 12h, performing centrifugal separation on the precipitate, washing the precipitate for 3 times by using deionized water, drying the precipitate in an oven at 60 ℃, and drying to obtain the nitrogen-doped porous carbon material.
The specific surface area of the obtained nitrogen-doped porous carbon material is 923.1m 2 The nitrogen-doped porous carbon material is used as a negative electrode to assemble a zinc-air battery, and the peak power density is 59.3mW/cm 2 。
Example 3
1g of alkali lignin, 6g of carbon nitride and 1g of ZnCO 3 Blending, ball milling for 24h at 300r/min by using a planetary ball mill until the mixture is ground into grey powder, putting the grey powder into a corundum boat, pyrolyzing the grey powder in a tube furnace, heating the mixture in stages, heating the mixture to 350 ℃ at the speed of 1 ℃/min in the first stage, and keeping the temperature for 3 h; then the temperature is raised to 800 ℃ at the speed of 1 ℃/min, and the temperature is kept for 3 h. And pouring the pyrolyzed porous carbon material into 150ml of 2mol/L hydrochloric acid, stirring for 12h, performing centrifugal separation on the precipitate, washing the precipitate for 3 times by using deionized water, drying the precipitate in an oven at 60 ℃, and drying to obtain the nitrogen-doped porous carbon material.
The specific surface area of the obtained nitrogen-doped porous carbon material is 805.5m 2 The nitrogen-doped porous carbon material is used as a negative electrode to assemble a zinc-air battery, and the peak power density is 52.1mW/cm 2 。
Claims (9)
1. A method for preparing a nitrogen-doped porous carbon material by stripping lignin in a gas phase comprises the following steps:
mixing lignin and a gas phase stripping auxiliary agent, putting the mixture into a ball milling tank, carrying out ball milling for 24 hours at the rotating speed of 300r/min, transferring the mixture into a tubular furnace, and heating and carbonizing the mixture by stages; and after carbonization is finished, adding hydrochloric acid into the obtained porous carbon material, stirring and washing, washing with deionized water, performing centrifugal precipitation, and drying to obtain the nitrogen-doped porous carbon material.
2. The method for preparing the nitrogen-doped porous carbon material by gas-phase stripping of lignin according to claim 1, wherein: the lignin is alkali lignin washed by deionized water.
3. The method for preparing the nitrogen-doped porous carbon material by gas-phase stripping of lignin according to claim 1, wherein: the gas phase stripping auxiliary agent comprises Zn 2+ Salts and nitrogen-containing compounds.
4. The method for preparing the nitrogen-doped porous carbon material by gas-phase stripping of lignin according to claim 3, wherein: the nitrogen-containing compound is NH 4 Cl, melamine or carbon nitride; said Zn 2+ The salt being ZnCl 2 、ZnC 2 O 4 Or ZnCO 3 。
5. The method for preparing the nitrogen-doped porous carbon material by gas-phase stripping of lignin according to claim 3, wherein: lignin, nitrogenous compounds, Zn used 2+ The mass ratio of the salt is 1:4-6: 1.
6. The method for preparing the nitrogen-doped porous carbon material by gas-phase stripping of lignin according to claim 1, wherein: the rotation speed of the ball milling is 300r/min, and the reaction time of the ball milling is 24 h.
7. The method for preparing the nitrogen-doped porous carbon material by gas-phase stripping of lignin according to claim 1, wherein: during carbonization, inert gas is used as nitrogen or argon, the temperature is raised to 350 ℃ at the speed of 1 ℃/min in stages, and the temperature is kept for 3 h; then the temperature is raised to 800 ℃ at the speed of 1 ℃/min, and the temperature is kept for 3 h.
8. The method for preparing the nitrogen-doped porous carbon material by gas-phase stripping of lignin according to claim 1, wherein: the hydrochloric acid concentration for washing the porous carbon material is 2mol/L, the stirring time is 12h, and then the porous carbon material is washed by deionized water and then centrifugally dried to obtain the nitrogen-doped porous carbon material.
9. Use of a nitrogen doped porous material prepared by the method according to any one of claims 1 to 8, characterized in that: the nitrogen-doped porous carbon material is applied to the field of electrocatalysis and used as a negative electrode material for preparing a zinc-air battery.
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