CN112466671A - Nitrogen-self-doped tobacco stem-based activated carbon electrode material and preparation method and application thereof - Google Patents
Nitrogen-self-doped tobacco stem-based activated carbon electrode material and preparation method and application thereof Download PDFInfo
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 193
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 193
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 239000007772 electrode material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 212
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 106
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000010902 straw Substances 0.000 claims abstract description 46
- 239000002243 precursor Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000004898 kneading Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000003990 capacitor Substances 0.000 claims abstract description 6
- 239000003337 fertilizer Substances 0.000 claims description 62
- 244000183278 Nephelium litchi Species 0.000 claims description 43
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 41
- 239000011591 potassium Substances 0.000 claims description 41
- 229910052700 potassium Inorganic materials 0.000 claims description 41
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 35
- 239000000284 extract Substances 0.000 claims description 35
- 229910052698 phosphorus Inorganic materials 0.000 claims description 35
- 239000011574 phosphorus Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 32
- 239000000618 nitrogen fertilizer Substances 0.000 claims description 21
- 230000004720 fertilization Effects 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 6
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 67
- 239000002686 phosphate fertilizer Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 241000723346 Cinnamomum camphora Species 0.000 description 8
- 229940072033 potash Drugs 0.000 description 7
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 7
- 235000015320 potassium carbonate Nutrition 0.000 description 7
- NGLMYMJASOJOJY-UHFFFAOYSA-O azanium;calcium;nitrate Chemical compound [NH4+].[Ca].[O-][N+]([O-])=O NGLMYMJASOJOJY-UHFFFAOYSA-O 0.000 description 6
- KMQAPZBMEMMKSS-UHFFFAOYSA-K calcium;magnesium;phosphate Chemical compound [Mg+2].[Ca+2].[O-]P([O-])([O-])=O KMQAPZBMEMMKSS-UHFFFAOYSA-K 0.000 description 6
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 6
- 229910052939 potassium sulfate Inorganic materials 0.000 description 6
- 235000011151 potassium sulphates Nutrition 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000006286 aqueous extract Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Microelectronics & Electronic Packaging (AREA)
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- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention relates to the technical field of electrode material preparation, and particularly discloses a tobacco stem-based activated carbon electrode material self-doped with nitrogen element, and a preparation method and application thereof. The preparation method of the tobacco rod-based activated carbon electrode material self-doped with nitrogen comprises the following steps: (1) planting flue-cured tobacco; (2) taking tobacco straws, crushing the tobacco straws to obtain tobacco straw powder, and then drying the tobacco straw powder; (3) carrying out pyrolysis treatment on the dried tobacco stalk powder in the atmosphere of nitrogen to obtain a tobacco stalk carbon powder precursor; (4) mixing the tobacco stem carbon powder precursor with KOH, adding water for further grinding and kneading, and drying to obtain a tobacco stem carbon powder/KOH mixture; (5) and then carrying out pyrolysis treatment on the tobacco stalk carbon powder/KOH mixture to obtain the tobacco stalk-based active carbon electrode material self-doped with nitrogen. The tobacco stem-based activated carbon electrode material is used for preparing the super capacitor, so that the specific capacitance of the super capacitor can be improved, and the energy density can be increased.
Description
Technical Field
The invention relates to the technical field of electrode material preparation, in particular to a tobacco stem-based activated carbon electrode material self-doped with nitrogen element and a preparation method and application thereof.
Background
The tobacco stems are tobacco stems, and a large amount of tobacco stems are generated after tobacco leaves are picked every year; for tobacco straw, incineration and disposal are mainly adopted at present. However, the burning and discarding of the tobacco straw can cause certain pollution to the atmosphere and the environment; therefore, it is necessary to develop a method for recycling tobacco straw.
In order to reduce the pollution to the environment, improve the utilization rate of the tobacco straws and improve the economic value of tobacco planting, the preparation of the activated carbon electrode material by taking the tobacco straws as the raw material is one of the utilization modes of the tobacco straws. The active carbon electrode material is used for preparing an electrode material of a super capacitor, and in order to improve the specific capacitance of the super capacitor and increase the energy density, the active carbon is modified by a common method, nitrogen is introduced, and a nitrogen-doped carbon material is prepared.
The self-doping nitrogen element means that the nitrogen element is absorbed by the plant in the growth process, and then the nitrogen element is left in the plant body to become a component of the plant; then, the plants containing nitrogen elements are used as raw materials to be pyrolyzed to obtain the tobacco stem-based active carbon electrode material self-doped with nitrogen elements.
The nitrogen element is an essential element for the growth of tobacco leaves, however, the inventor finds that in the tobacco planting process, the content of the nitrogen element precipitated in the tobacco straws is low, and the activated carbon electrode material prepared by taking the tobacco straws as a raw material cannot obtain the activated carbon electrode material doped with the high nitrogen element, and the performance of the supercapacitor can be influenced by taking the activated carbon electrode material as the electrode material of the supercapacitor. However, how to increase the content of nitrogen element in the activated carbon electrode material by adopting the self-doping method to prepare the activated carbon electrode material is a technical difficulty in the field.
Disclosure of Invention
In order to overcome at least one technical problem mentioned in the background technology, the invention provides a preparation method of a tobacco stem-based activated carbon electrode material self-doped with nitrogen.
The technical problem to be solved by the invention is realized by the following technical scheme:
a preparation method of a tobacco stem-based activated carbon electrode material self-doped with nitrogen comprises the following steps:
(1) planting flue-cured tobacco;
(2) taking tobacco straws, crushing the tobacco straws to obtain tobacco straw powder, and then drying the tobacco straw powder;
(3) drying the tobacco stalk powder at 3-6 ℃ per min under the atmosphere of nitrogen-1Raising the speed to 500-600 ℃, and keeping the temperature for 1-3 h to obtain a tobacco stem carbon powder precursor;
(4) mixing the tobacco stem carbon powder precursor with KOH, adding water for further grinding and kneading, and drying to obtain a tobacco stem carbon powder/KOH mixture;
(5) then, the tobacco stalk carbon powder/KOH mixture is put under the atmosphere of nitrogen at the temperature of 3-6 ℃ per minute-1The temperature is increased to 800-900 ℃ and is kept for 1-3 h; cooling to room temperature and taking out to obtain the tobacco stem-based activated carbon electrode material self-doped with nitrogen.
Preferably, in the flue-cured tobacco planting process in the step (1), nitrogen, phosphorus and potassium fertilizers are applied to the tobacco.
Preferably, in the flue-cured tobacco planting process in the step (1), when nitrogen, phosphorus and potassium fertilizers are applied to the tobacco, the nitrogen, phosphorus and potassium fertilizers and the litchi branch and leaf water extract are applied together.
The inventor researches and discovers that during the tobacco planting process, the content of nitrogen elements enriched in tobacco stems is low, and the content of nitrogen elements precipitated in corresponding tobacco straws is also low; therefore, the activated carbon electrode material prepared by taking tobacco straws as a raw material in a self-doping manner cannot be obtained, and the activated carbon electrode material doped with higher nitrogen elements is obtained. In order to improve the content of nitrogen element in the active carbon electrode material prepared in a self-doping mode. The inventor finds in research that when applying nitrogen, phosphorus and potassium fertilizers to tobacco, the nitrogen, phosphorus and potassium fertilizers and the aqueous extract of the branches and leaves of the litchi are applied together; the litchi branch and leaf water extract can promote the enrichment of nitrogen elements in tobacco stems, and relatively more nitrogen element content is precipitated in the corresponding tobacco straws; thereby effectively improving the nitrogen content in the tobacco rod-based active carbon electrode material self-doped with nitrogen.
Preferably, in the flue-cured tobacco planting process in the step (1), when nitrogen, phosphorus and potassium fertilizers are applied to the tobacco, the nitrogen, phosphorus and potassium fertilizers are dissolved in the litchi branch and leaf water extract for fertilization.
Specifically, the nitrogen fertilizer is applied with calcium ammonium nitrate, the phosphate fertilizer is applied with calcium magnesium phosphate fertilizer, and the potassium fertilizer is applied with potassium sulfate;
preferably, the fertilizing amount of the nitrogen fertilizer is 100-130 kg/hm2(ii) a The fertilizing amount of the phosphate fertilizer and the potash fertilizer is 200-250 kg/hm2。
The fertilization dosage of the nitrogen fertilizer is 112.5kg/hm2(ii) a The fertilizing amount of the phosphate fertilizer and the potash fertilizer is 225kg/hm2。
Further preferably, the litchi branch and leaf water extract is prepared by the following method:
and (3) putting the litchi branches and leaves into water, and soaking for 15-45 days to obtain the litchi branch and leaf water extract.
Further preferably, the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the litchi branch and leaf water extract is 1: 3-10.
Most preferably, the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the litchi branch and leaf water extract is 1: 5.
Further preferably, the weight ratio of the litchi branches and leaves to the water is 1: 10-30.
Most preferably, the weight ratio of the litchi branches and leaves to the water is 1: 20.
Further preferably, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 3-8;
most preferably, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 5.
The invention also provides the tobacco stem-based activated carbon electrode material self-doped with nitrogen prepared by the preparation method.
The invention also provides an application of the tobacco stem-based activated carbon electrode material self-doped with nitrogen in preparing a capacitor.
Has the advantages that: the invention provides a brand-new preparation method of a tobacco stem-based activated carbon electrode material self-doped with nitrogen; the tobacco stem-based activated carbon electrode material prepared by the method is self-doped with active nitrogen elements with higher content, and the specific capacitance of the supercapacitor can be improved and the energy density can be increased by adopting the tobacco stem-based activated carbon electrode material to prepare the supercapacitor. In addition, the method is a brand-new method for recycling the tobacco straws; the method reduces the harm of burning and discarding the tobacco straws to the atmosphere and the environment, and improves the additional economic value of tobacco planting.
Detailed Description
The present invention is further explained below with reference to specific examples, which are not intended to limit the present invention in any way.
Example 1
(1) Planting flue-cured tobacco;
(2) taking tobacco straws, crushing the tobacco straws into 200 meshes to obtain tobacco straw powder, and then putting the tobacco straw powder into an oven to be dried for 24 hours at the temperature of 70 ℃;
(3) putting the dried tobacco stalk powder into a tube furnace under the atmosphere of nitrogen (the flow rate is 3 mL/min)-1) At 5 ℃ in min-1The temperature is increased to 550 ℃ and kept for 2 hours for pyrolysis treatment; cooling to room temperature along with the furnace after heat treatment, and taking out to obtain a tobacco stem carbon powder precursor;
(4) mixing the tobacco stalk carbon powder precursor with KOH, adding water for further grinding and kneading, then putting the mixture into a vacuum drying oven for drying at 70 ℃ for 12 hours, and drying to obtain a tobacco stalk carbon powder/KOH mixture;
(5) then putting the tobacco stalk carbon powder/KOH mixture into a tube furnace under the atmosphere of nitrogen (the flow rate is 3mL & min)-1) At 5 ℃ in min-1The temperature is increased to 850 ℃ and kept for 2h, and then pyrolysis treatment is carried out; cooling to room temperature, taking out, and fully washing the obtained sample by using 1M hydrochloric acid solution; obtaining the tobacco stem-based activated carbon electrode material self-doped with nitrogen;
specifically, in the flue-cured tobacco planting process in the step (1), when nitrogen, phosphorus and potassium fertilizers are applied to tobacco, the nitrogen, phosphorus and potassium fertilizers are dissolved in the litchi branch and leaf water extract for fertilization; wherein the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the litchi branch and leaf water extract is 1: 5; the litchi branch and leaf water extract is prepared by the following method: putting the dried branches and leaves of the litchi into water, and soaking for 30 days to obtain the litchi branch and leaf water extract; the weight ratio of the branches and leaves of the litchi tree to the water is 1: 20.
Specifically, the nitrogen fertilizer is applied with calcium ammonium nitrate, the phosphate fertilizer is applied with calcium magnesium phosphate fertilizer, and the potassium fertilizer is applied with potassium sulfate; the fertilization dosage of the nitrogen fertilizer is 112.5kg/hm2(ii) a The fertilizing amount of the phosphate fertilizer and the potash fertilizer is 225kg/hm2。
Specifically, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 5; the ratio of the added weight of the water to the total weight of the tobacco stalk carbon powder precursor and the KOH in the step (4) is 1: 1.
Example 2
(1) Planting flue-cured tobacco;
(2) taking tobacco straws, crushing the tobacco straws into 100 meshes to obtain tobacco straw powder, and then putting the tobacco straw powder into an oven to be dried for 24 hours at the temperature of 70 ℃;
(3) putting the dried tobacco stalk powder into a tube furnace under the atmosphere of nitrogen (the flow rate is 3 mL/min)-1) At 3 ℃ min-1The temperature is increased to 500 ℃ and is preserved for 3 hours for pyrolysis treatment; cooling to room temperature along with the furnace after heat treatment, and taking out to obtain a tobacco stem carbon powder precursor;
(4) mixing the tobacco stalk carbon powder precursor with KOH, adding water for further grinding and kneading, then putting the mixture into a vacuum drying oven for drying at 70 ℃ for 12 hours, and drying to obtain a tobacco stalk carbon powder/KOH mixture;
(5) then putting the tobacco stalk carbon powder/KOH mixture into a tube furnace under the atmosphere of nitrogen (the flow rate is 3mL & min)-1) At 3 ℃ min-1The temperature is increased to 800 ℃ and is preserved for 3 hours for pyrolysis treatment; cooling to room temperature, taking out, and fully washing the obtained sample by using 1M hydrochloric acid solution; obtaining the tobacco stem-based activated carbon electrode material self-doped with nitrogen;
specifically, in the flue-cured tobacco planting process in the step (1), when nitrogen, phosphorus and potassium fertilizers are applied to tobacco, the nitrogen, phosphorus and potassium fertilizers are dissolved in the litchi branch and leaf water extract for fertilization; wherein the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the litchi branch and leaf water extract is 1: 3; the litchi branch and leaf water extract is prepared by the following method: putting the dried branches and leaves of the litchi into water, and soaking for 45 days to obtain the litchi branch and leaf water extract; the weight ratio of the branches and leaves of the litchi tree to the water is 1: 10.
Specifically, the nitrogen fertilizer is applied with calcium ammonium nitrate, the phosphate fertilizer is applied with calcium magnesium phosphate fertilizer, and the potassium fertilizer is applied with potassium sulfate; the fertilization dosage of the nitrogen fertilizer is 100kg/hm2(ii) a The fertilizing amount of the phosphate fertilizer and the potash fertilizer is 200kg/hm2。
Specifically, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 3; the ratio of the added weight of the water to the total weight of the tobacco stalk carbon powder precursor and the KOH in the step (4) is 1: 1.
Example 3
(1) Planting flue-cured tobacco;
(2) taking tobacco straws, crushing the tobacco straws into 50 meshes to obtain tobacco straw powder, and then putting the tobacco straw powder into an oven to be dried for 24 hours at the temperature of 70 ℃;
(3) putting the dried tobacco stalk powder into a tube furnace under the atmosphere of nitrogen (the flow rate is 3 mL/min)-1) At 6 ℃ min-1The temperature is increased to 600 ℃ and is kept for 1.5h for pyrolysis treatment; cooling to room temperature along with the furnace after heat treatment, and taking out to obtain a tobacco stem carbon powder precursor;
(4) mixing the tobacco stalk carbon powder precursor with KOH, adding water for further grinding and kneading, then putting the mixture into a vacuum drying oven for drying at 70 ℃ for 12 hours, and drying to obtain a tobacco stalk carbon powder/KOH mixture;
(5) then putting the tobacco stalk carbon powder/KOH mixture into a tube furnace under the atmosphere of nitrogen (the flow rate is 3mL & min)-1) At 6 ℃ min-1The temperature is increased to 900 ℃ and is kept for 1.5h for pyrolysis treatment; cooling to room temperature, taking out, and fully washing the obtained sample by using 1M hydrochloric acid solution; obtaining the tobacco stem-based activated carbon electrode material self-doped with nitrogen;
specifically, in the flue-cured tobacco planting process in the step (1), when nitrogen, phosphorus and potassium fertilizers are applied to tobacco, the nitrogen, phosphorus and potassium fertilizers are dissolved in the litchi branch and leaf water extract for fertilization; wherein the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the litchi branch and leaf water extract is 1: 10; the litchi branch and leaf water extract is prepared by the following method: putting the dried branches and leaves of the litchi into water, and soaking for 20 days to obtain the litchi branch and leaf water extract; the weight ratio of the branches and leaves of the litchi tree to the water is 1: 30.
Specifically, the nitrogen fertilizer is applied with calcium ammonium nitrate, the phosphate fertilizer is applied with calcium magnesium phosphate fertilizer, and the potassium fertilizer is applied with potassium sulfate; the fertilizing amount of the nitrogen fertilizer is 130kg/hm2(ii) a The fertilizing amount of the phosphate fertilizer and the potash fertilizer is 250kg/hm2。
Specifically, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 8; the ratio of the added weight of the water to the total weight of the tobacco stalk carbon powder precursor and the KOH in the step (4) is 1: 1.
Comparative example 1
(1) Planting flue-cured tobacco;
(2) taking tobacco straws, crushing the tobacco straws into 200 meshes to obtain tobacco straw powder, and then putting the tobacco straw powder into an oven to be dried for 24 hours at the temperature of 70 ℃;
(3) putting the dried tobacco stalk powder into a tube furnace under the atmosphere of nitrogen (the flow rate is 3 mL/min)-1) At 5 ℃ in min-1The temperature is increased to 550 ℃ and kept for 2 hours for pyrolysis treatment; cooling to room temperature along with the furnace after heat treatment, and taking out to obtain a tobacco stem carbon powder precursor;
(4) mixing the tobacco stalk carbon powder precursor with KOH, adding water for further grinding and kneading, then putting the mixture into a vacuum drying oven for drying at 70 ℃ for 12 hours, and drying to obtain a tobacco stalk carbon powder/KOH mixture;
(5) then putting the tobacco stalk carbon powder/KOH mixture into a tube furnace under the atmosphere of nitrogen (the flow rate is 3mL & min)-1) At 5 ℃ in min-1The temperature is increased to 850 ℃ and kept for 2h, and then pyrolysis treatment is carried out; cooling to room temperature, taking out, and fully washing the obtained sample by using 1M hydrochloric acid solution; obtaining the tobacco stem-based activated carbon electrode material self-doped with nitrogen;
specifically, in the flue-cured tobacco planting process in the step (1), when nitrogen, phosphorus and potassium fertilizers are applied to tobacco, the nitrogen, phosphorus and potassium fertilizers are dissolved in water for fertilization; wherein the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the water is 1: 5.
Specifically, the nitrogen fertilizer is applied with calcium ammonium nitrate, the phosphate fertilizer is applied with calcium magnesium phosphate fertilizer, and the potassium fertilizer is applied with potassium sulfate; the fertilization dosage of the nitrogen fertilizer is 112.5kg/hm2(ii) a The fertilizing amount of the phosphate fertilizer and the potash fertilizer is 225kg/hm2。
Specifically, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 5; the ratio of the added weight of the water to the total weight of the tobacco stalk carbon powder precursor and the KOH in the step (4) is 1: 1.
The difference between the comparative example 1 and the example 1 is that the litchi branch and leaf water extract is not applied in the fertilizing process in the comparative example 1.
Comparative example 2
(1) Planting flue-cured tobacco;
(2) taking tobacco straws, crushing the tobacco straws into 200 meshes to obtain tobacco straw powder, and then putting the tobacco straw powder into an oven to be dried for 24 hours at the temperature of 70 ℃;
(3) putting the dried tobacco stalk powder into a tube furnace under the atmosphere of nitrogen (the flow rate is 3 mL/min)-1) At 5 ℃ in min-1The temperature is increased to 550 ℃ and kept for 2 hours for pyrolysis treatment; cooling to room temperature along with the furnace after heat treatment, and taking out to obtain a tobacco stem carbon powder precursor;
(4) mixing the tobacco stalk carbon powder precursor with KOH, adding water for further grinding and kneading, then putting the mixture into a vacuum drying oven for drying at 70 ℃ for 12 hours, and drying to obtain a tobacco stalk carbon powder/KOH mixture;
(5) then putting the tobacco stalk carbon powder/KOH mixture into a tube furnace under the atmosphere of nitrogen (the flow rate is 3mL & min)-1) At 5 ℃ in min-1The temperature is increased to 850 ℃ and kept for 2h, and then pyrolysis treatment is carried out; cooling to room temperature, taking out, and fully washing the obtained sample by using 1M hydrochloric acid solution; obtaining the tobacco stem-based activated carbon electrode material self-doped with nitrogen;
specifically, in the flue-cured tobacco planting process in the step (1), when nitrogen, phosphorus and potassium fertilizers are applied to tobacco, the nitrogen, phosphorus and potassium fertilizers are dissolved in the camphor tree branch and leaf water extract for fertilization; wherein the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the water extract of the camphor tree branches and leaves is 1: 5; the camphor tree branch and leaf water extract is prepared by the following method: putting dried branches and leaves of the cinnamomum camphora into water, and soaking for 30 days to obtain the cinnamomum camphora branch and leaf water extract; the weight ratio of the branches and leaves of the litchi tree to the water is 1: 20.
Specifically, the nitrogen fertilizer is applied with calcium ammonium nitrate, the phosphate fertilizer is applied with calcium magnesium phosphate fertilizer, and the potassium fertilizer is applied with potassium sulfate; the fertilization dosage of the nitrogen fertilizer is 112.5kg/hm2(ii) a The fertilizing amount of the phosphate fertilizer and the potash fertilizer is 225kg/hm2。
Specifically, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 5; the ratio of the added weight of the water to the total weight of the tobacco stalk carbon powder precursor and the KOH in the step (4) is 1: 1.
Comparative example 2 differs from example 1 in that comparative example 2 applies an aqueous extract of the branches and leaves of cinnamomum camphora at the same time during the fertilization process.
The content of nitrogen in the self-doped nitrogen tobacco rod-based activated carbon electrode materials prepared in examples 1 to 3 and comparative examples 1 and 2 was measured by using an elemental analysis tester, and the test results are shown in table 1.
TABLE 1 determination of nitrogen content in self-doped nitrogen tobacco rod-based activated carbon electrode material
| Content of nitrogen element | |
| EXAMPLE 1 tobacco-based activated carbon electrode Material self-doped with Nitrogen | 0.78％ |
| EXAMPLE 2 tobacco-based activated carbon electrode Material self-doped with Nitrogen | 0.66％ |
| EXAMPLE 3 tobacco-based activated carbon electrode Material self-doped with Nitrogen | 0.71％ |
| Comparative example 1 tobacco rod-based activated carbon electrode material self-doped with nitrogen element | 0.11％ |
| Comparative example 2 tobacco rod based active carbon electrode material self-doped with nitrogen element | 0.15％ |
As can be seen from the test data in Table 1, the nitrogen content in the self-doping nitrogen-element tobacco rod-based activated carbon electrode material prepared in the examples 1-3 is greatly improved compared with that in the comparative example 1; this shows that when applying nitrogen, phosphorus and potassium fertilizers to tobacco, the nitrogen, phosphorus and potassium fertilizers and the litchi branch and leaf water extract are applied together; the litchi branch and leaf water extract can promote the enrichment of nitrogen elements in tobacco stems, and more nitrogen elements are precipitated in corresponding tobacco straws; thereby improving the nitrogen content in the tobacco rod-based active carbon electrode material self-doped with nitrogen.
As can be seen from the test data in table 1, the nitrogen content in the tobacco stem-based activated carbon electrode material self-doped with nitrogen prepared in comparative example 2 is not significantly increased compared to that in comparative example 1, compared to examples 1 to 3, which indicates that when applying nitrogen, phosphorus and potassium fertilizers to tobacco, the nitrogen, phosphorus and potassium fertilizers are applied together with the cinnamomum camphora branch and leaf water extract; the camphor tree branch and leaf water extract cannot promote the enrichment of nitrogen elements in tobacco stems, and cannot effectively improve the nitrogen element content of the tobacco stem-based active carbon electrode material self-doped with nitrogen elements. This also indicates that not any aqueous extract promotes the enrichment of nitrogen in the tobacco stalks; only the litchi branch and leaf water extract can promote the enrichment of nitrogen in tobacco stems, and further the nitrogen content of the tobacco stem-based active carbon electrode material self-doped with nitrogen can be improved.
Claims (10)
1. A preparation method of a tobacco stem-based activated carbon electrode material self-doped with nitrogen is characterized by comprising the following steps:
(1) planting flue-cured tobacco;
(2) taking tobacco straws, crushing the tobacco straws to obtain tobacco straw powder, and then drying the tobacco straw powder;
(3) drying the tobacco stalk powder at 3-6 ℃ per min under the atmosphere of nitrogen-1Raising the speed to 500-600 ℃, and keeping the temperature for 1-3 h to obtain a tobacco stem carbon powder precursor;
(4) mixing the tobacco stem carbon powder precursor with KOH, adding water for further grinding and kneading, and drying to obtain a tobacco stem carbon powder/KOH mixture;
(5) then, the tobacco stalk carbon powder/KOH mixture is put under the atmosphere of nitrogen at the temperature of 3-6 ℃ per minute-1The temperature is increased to 800-900 ℃ and is kept for 1-3 h; cooling to room temperature and taking out to obtain the tobacco stem-based activated carbon electrode material self-doped with nitrogen.
2. The method for preparing the tobacco rod-based activated carbon electrode material self-doped with nitrogen element as claimed in claim 1, wherein in the flue-cured tobacco planting process in the step (1), nitrogen, phosphorus and potassium fertilizers are applied to tobacco.
3. The method for preparing a nitrogen-self-doped tobacco stem-based activated carbon electrode material as claimed in claim 2, wherein in the flue-cured tobacco planting process in step (1), when applying nitrogen, phosphorus and potassium fertilizers to tobacco, the nitrogen, phosphorus and potassium fertilizers are applied together with the litchi branch and leaf water extract.
4. The method for preparing a nitrogen-self-doped tobacco stem-based activated carbon electrode material as claimed in claim 2, wherein in the flue-cured tobacco planting process in step (1), when applying nitrogen, phosphorus and potassium fertilizers to tobacco, the nitrogen, phosphorus and potassium fertilizers are dissolved in litchi branch and leaf water extract for fertilization.
5. The preparation method of the tobacco stem-based activated carbon electrode material self-doped with nitrogen element as claimed in claim 3 or 4, wherein the litchi branch and leaf water extract is prepared by the following method:
and (3) putting the litchi branches and leaves into water, and soaking for 15-45 days to obtain the litchi branch and leaf water extract.
6. The preparation method of the nitrogen self-doped tobacco rod-based activated carbon electrode material as claimed in claim 3 or 4, wherein the weight ratio of the total weight of nitrogen, phosphorus and potassium fertilizers to the litchi branch and leaf water extract is 1: 3-10;
most preferably, the weight ratio of the total weight of the nitrogen fertilizer, the phosphorus fertilizer and the potassium fertilizer to the litchi branch and leaf water extract is 1: 5.
7. The preparation method of the tobacco stem-based activated carbon electrode material self-doped with nitrogen element as claimed in claim 5, wherein the weight ratio of the litchi branches and leaves to water is 1: 10-30;
most preferably, the weight ratio of the litchi branches and leaves to the water is 1: 20.
8. The preparation method of the tobacco stem-based activated carbon electrode material self-doped with nitrogen element as claimed in claim 1, wherein the weight ratio of the tobacco stem carbon powder precursor to KOH in the step (4) is 1: 3-8;
most preferably, the weight ratio of the tobacco stalk carbon powder precursor to KOH in the step (4) is 1: 5.
9. A self-doped nitrogen-element tobacco rod-based activated carbon electrode material prepared by the preparation method of any one of claims 1 to 8.
10. Use of the self-doping nitrogen element tobacco rod based activated carbon electrode material of claim 9 in the preparation of capacitors.
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