CN112591746B - Tobacco stem-based activated carbon electrode material self-doped with sulfur element and preparation method and application thereof - Google Patents
Tobacco stem-based activated carbon electrode material self-doped with sulfur element and preparation method and application thereof Download PDFInfo
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- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 183
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 140
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000011593 sulfur Substances 0.000 title claims abstract description 67
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 67
- 239000007772 electrode material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 244000061176 Nicotiana tabacum Species 0.000 title 1
- 241000208125 Nicotiana Species 0.000 claims abstract description 182
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000010902 straw Substances 0.000 claims abstract description 47
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000197 pyrolysis Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 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 66
- 150000001875 compounds Chemical class 0.000 claims description 52
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- 239000000284 extract Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 30
- 241000218657 Picea Species 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 241000017433 Schefflera heptaphylla Species 0.000 claims description 16
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 14
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 14
- 239000005696 Diammonium phosphate Substances 0.000 claims description 7
- 244000184734 Pyrus japonica Species 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000001506 calcium phosphate Substances 0.000 claims description 7
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 7
- 235000011010 calcium phosphates Nutrition 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 7
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 7
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 7
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 7
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 7
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 7
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 7
- 239000004323 potassium nitrate Substances 0.000 claims description 7
- 235000010333 potassium nitrate Nutrition 0.000 claims description 7
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 7
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 7
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 7
- 235000011151 potassium sulphates Nutrition 0.000 claims description 7
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 6
- 235000013877 carbamide Nutrition 0.000 claims description 2
- 102000020897 Formins Human genes 0.000 claims 2
- 108091022623 Formins Proteins 0.000 claims 2
- 230000000052 comparative effect Effects 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 241000723346 Cinnamomum camphora Species 0.000 description 9
- 230000004720 fertilization Effects 0.000 description 7
- 239000006286 aqueous extract Substances 0.000 description 6
- 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 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 230000002015 leaf growth Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01C—PLANTING; SOWING; FERTILISING
- A01C21/00—Methods of fertilising, sowing or planting
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Soil Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
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 sulfur element, and a preparation method and application thereof. The preparation method of the tobacco rod-based activated carbon electrode material self-doped with the sulfur element 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 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) then carrying out heat treatment on the tobacco stalk carbon powder/KOH mixture; and obtaining the tobacco stem-based active carbon electrode material self-doped with the sulfur element. 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 sulfur 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 activated carbon electrode material is an electrode material for preparing a supercapacitor, and in order to improve the performance of the supercapacitor, a person skilled in the art generally dopes sulfur element in a carbon material. The sulfur element is doped in the activated carbon, the electron density of the surface of a sample can be improved through the synergistic activation of the conjugated C and the electron-rich element S, meanwhile, the existence of the S element can provide reversible reaction sites and provide pseudocapacitance, and the possible reaction formula is as follows:
the self-doping sulfur element means that the sulfur element is absorbed by the plant in the growth process, and then the sulfur element is left in the plant body to become a component of the plant; then, the plants containing the sulfur elements are used as raw materials to be pyrolyzed to obtain the tobacco stem-based active carbon electrode material doped with the sulfur elements.
The sulfur element is one of essential elements for tobacco leaf growth, however, the inventor finds that in the tobacco planting process, the content of the sulfur element precipitated in the tobacco straw is low, and the activated carbon electrode material prepared by taking the tobacco straw as a raw material cannot obtain the activated carbon electrode material doped with the high sulfur element, and the performance of the supercapacitor can be affected by taking the activated carbon electrode material as the electrode material of the supercapacitor. However, how to increase the sulfur content in the activated carbon electrode material by using 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 sulfur element.
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 sulfur elements 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 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) then carrying out heat treatment on the tobacco stalk carbon powder/KOH mixture; obtaining the tobacco stem-based active carbon electrode material self-doped with sulfur element;
wherein, in the flue-cured tobacco planting process in the step (1), compound fertilizer is applied to the tobacco; when the compound fertilizer is applied to the tobacco, the compound fertilizer and the picea japonica branch and leaf water extract are applied together.
The inventor researches and discovers that during the tobacco planting process, the content of sulfur elements enriched in tobacco stems is lower, and the content of sulfur elements precipitated in corresponding tobacco straws is also lower; 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 sulfur elements is obtained. In order to improve the content of sulfur element in the active carbon electrode material prepared in a self-doping mode. The inventor finds in research that when the compound fertilizer is applied to the tobacco, the compound fertilizer and the picea japonica branch and leaf water extract are applied together; the aqueous extract of the branches and leaves of the schefflera octophylla can promote the enrichment of sulfur elements in tobacco stems, and relatively more sulfur element content is precipitated in the corresponding tobacco straws; thereby effectively improving the sulfur content in the tobacco rod-based active carbon electrode material self-doped with sulfur.
Preferably, the compound fertilizer consists of monopotassium phosphate fertilizer, diammonium phosphate, urea, potassium nitrate fertilizer, calcium phosphate, potassium sulfate and magnesium sulfate.
Preferably, the total nitrogen application amount of the compound fertilizer is 90-100 kg/hm2。
Preferably, the N: P in the compound fertilizer2O5:K2O＝1:2～3:3～4。
Preferably, the picea javanica branch and leaf water extract is prepared by the following method: and (3) putting the schefflera octophylla branches and leaves into water, and soaking for 10-30 days to obtain the schefflera octophylla branch and leaf water extract.
Preferably, the weight ratio of the compound fertilizer to the picea javanica branch and leaf water extract is 1: 3-10.
Most preferably, the weight ratio of the compound fertilizer to the picea javanica branch and leaf water extract is 1: 5.
Preferably, the weight ratio of the picea javanica branches and leaves to water is 1: 8-25.
Most preferably, the weight ratio of the picea schlegeli branches and leaves to the water is 1: 15.
Preferably, the heat treatment conditions in step (3) are: under the atmosphere of nitrogen at 3-6 ℃ per minute-1The temperature is increased to 500-600 ℃ and is kept for 1-3 h;
the heat treatment conditions in the step (5) are as follows: under the atmosphere of nitrogen at 3-6 ℃ per minute-1The temperature is increased to 800-900 ℃ and kept for 1-3 h.
The invention also provides the tobacco stem-based activated carbon electrode material self-doped with the sulfur element, which is prepared by the preparation method.
The invention also provides an application of the tobacco stem-based activated carbon electrode material self-doped with the sulfur element 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 sulfur element; the tobacco stem-based active carbon electrode material prepared by the method is self-doped with active sulfur element with higher content, and the specific capacitance of the super capacitor can be improved and the energy density can be increased by adopting the tobacco stem-based active carbon electrode material to prepare the super capacitor. 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 active carbon electrode material self-doped with sulfur element;
specifically, in the flue-cured tobacco planting process in the step (1), when compound fertilizer is applied to tobacco, the compound fertilizer is dissolved in the picea japonica branch and leaf water extract for fertilization; wherein the weight ratio of the compound fertilizer to the picea javanica branch and leaf water extract is 1: 5; the picea javanica branch and leaf water extract is prepared by the following method: putting the dried schefflera octophylla branches and leaves into water, and soaking for 20 days to obtain the schefflera octophylla branch and leaf water extract; the weight ratio of the picea javanica branches and leaves to water is 1: 15.
Specifically, the compound fertilizer consists of a monopotassium phosphate fertilizer, diammonium phosphate, urea, a potassium nitrate fertilizer, calcium phosphate, potassium sulfate and magnesium sulfate; the total nitrogen application amount of the compound fertilizer is 97.5kg/hm2(ii) a P in the compound fertilizer2O5:K2O＝1:2:3.5。
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 active carbon electrode material self-doped with sulfur element;
specifically, in the flue-cured tobacco planting process in the step (1), when compound fertilizer is applied to tobacco, the compound fertilizer is dissolved in the picea japonica branch and leaf water extract for fertilization; wherein the weight ratio of the compound fertilizer to the picea javanica branch and leaf water extract is 1: 3; the picea javanica branch and leaf water extract is prepared by the following method: putting the dried schefflera octophylla branches and leaves into water, and soaking for 10 days to obtain the schefflera octophylla branch and leaf water extract; the weight ratio of the schefflera octophylla branches and leaves to the water is 1: 8.
Specifically, the compound fertilizer consists of a monopotassium phosphate fertilizer, diammonium phosphate, urea, a potassium nitrate fertilizer, calcium phosphate, potassium sulfate and magnesium sulfate; the total nitrogen application amount of the compound fertilizer is 90kg/hm2(ii) a P in the compound fertilizer2O5:K2O＝1:2:4。
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 300 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 kept for 1h 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 kept for 1h 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 active carbon electrode material self-doped with sulfur element;
specifically, in the flue-cured tobacco planting process in the step (1), when compound fertilizer is applied to tobacco, the compound fertilizer is dissolved in the picea japonica branch and leaf water extract for fertilization; wherein the weight ratio of the compound fertilizer to the picea javanica branch and leaf water extract is 1: 8; the picea javanica branch and leaf water extract is prepared by the following method: putting the dried schefflera octophylla branches and leaves into water, and soaking for 30 days to obtain the schefflera octophylla branch and leaf water extract; the weight ratio of the picea javanica branches and leaves to water is 1: 25.
Specifically, the compound fertilizer consists of a monopotassium phosphate fertilizer, diammonium phosphate, urea, a potassium nitrate fertilizer, calcium phosphate, potassium sulfate and magnesium sulfate; the total nitrogen application amount of the compound fertilizer is 100kg/hm2(ii) a P in the compound fertilizer2O5:K2O＝1:3:3。
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 active carbon electrode material self-doped with sulfur element;
specifically, in the flue-cured tobacco planting process in the step (1), when compound fertilizer is applied to tobacco, the compound fertilizer is dissolved in water for fertilization; wherein the weight ratio of the compound fertilizer to the water is 1: 5.
Specifically, the compound fertilizer consists of a monopotassium phosphate fertilizer, diammonium phosphate, urea, a potassium nitrate fertilizer, calcium phosphate, potassium sulfate and magnesium sulfate; the total nitrogen application amount of the compound fertilizer is 97.5kg/hm2(ii) a P in the compound fertilizer2O5:K2O＝1:2:3.5。
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 1 is different from example 1 in that comparative example 1 does not apply the aqueous extract of the twig and leaf of schefflera octophylla simultaneously during the fertilization process.
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 active carbon electrode material self-doped with sulfur element;
specifically, in the flue-cured tobacco planting process in the step (1), when compound fertilizer is applied to tobacco, the compound fertilizer is dissolved in the camphor tree branch and leaf water extract for fertilization; wherein the weight ratio of the compound fertilizer to the camphor tree branch and leaf water extract 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 20 days to obtain the cinnamomum camphora branch and leaf water extract; the weight ratio of the branches and leaves of the camphor trees to the water is 1: 15.
Specifically, the compound fertilizer consists of a monopotassium phosphate fertilizer, diammonium phosphate, urea, a potassium nitrate fertilizer, calcium phosphate, potassium sulfate and magnesium sulfate; the total nitrogen application amount of the compound fertilizer is 97.5kg/hm2(ii) a P in the compound fertilizer2O5:K2O＝1:2:3.5。
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 sulfur content in the tobacco rod-based activated carbon electrode material self-doped with sulfur 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 sulfur content in sulfur-doped tobacco rod-based activated carbon electrode materials
| Elemental sulfur content | |
| EXAMPLE 1 tobacco-based activated carbon electrode Material self-doped with elemental Sulfur | 4.38％ |
| EXAMPLE 2 tobacco-rod-based activated carbon electrode Material self-doped with elemental Sulfur | 3.91％ |
| EXAMPLE 3 tobacco-straw-based activated carbon electrode Material self-doped with elemental Sulfur | 3.74％ |
| Comparative example 1 tobacco rod-based active carbon electrode material self-doped with sulfur element | 0.62％ |
| Comparative example 2 tobacco rod based active carbon electrode material self-doped with sulfur element | 0.77％ |
As can be seen from the test data in Table 1, the sulfur content in the tobacco rod-based activated carbon electrode material self-doped with sulfur prepared in examples 1-3 is greatly improved compared with that in comparative example 1; the method is characterized in that when the compound fertilizer is applied to the tobacco, the compound fertilizer and the picea japonica branch and leaf water extract are applied together; the aqueous extract of the branches and leaves of the schefflera octophylla can promote the enrichment of sulfur elements in tobacco stems, and more sulfur elements are precipitated in corresponding tobacco straws; further improving the sulfur content in the tobacco rod-based active carbon electrode material self-doped with sulfur.
As can be seen from the test data in table 1, the sulfur content in the tobacco stem-based activated carbon electrode material self-doped with sulfur prepared in comparative example 2 is not significantly increased compared to that in comparative example 1 in examples 1 to 3, which indicates that when applying a compound fertilizer to tobacco, the compound fertilizer and the water extract of the branches and leaves of cinnamomum camphora are applied together; the cinnamomum camphora branch and leaf water extract cannot promote the enrichment of sulfur elements in tobacco stems and cannot effectively improve the sulfur element content of the tobacco stem-based active carbon electrode material doped with sulfur elements. This also suggests that not any aqueous extract will promote sulfur enrichment in the tobacco stems; only the aqueous extract of the branches and leaves of the schefflera octophylla can promote the enrichment of sulfur elements in tobacco stems, and further the sulfur element content of the tobacco stem-based active carbon electrode material self-doped with sulfur elements can be improved.
Claims (12)
1. A preparation method of a tobacco stem-based activated carbon electrode material self-doped with sulfur elements 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) carrying out pyrolysis treatment on the dried tobacco stalk powder 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) then carrying out heat treatment on the tobacco stalk carbon powder/KOH mixture; obtaining the tobacco stem-based active carbon electrode material self-doped with sulfur element;
wherein, in the flue-cured tobacco planting process in the step (1), compound fertilizer is applied to the tobacco; when the compound fertilizer is applied to the tobacco, the compound fertilizer and the picea japonica branch and leaf water extract are applied together.
2. The method for preparing a tobacco rod-based activated carbon electrode material self-doped with sulfur element as claimed in claim 1, wherein said compound fertilizer is composed of monopotassium phosphate fertilizer, diammonium phosphate, urea, potassium nitrate fertilizer, calcium phosphate, potassium sulfate and magnesium sulfate.
3. The method for preparing a sulfur-doped tobacco rod-based activated carbon electrode material as claimed in claim 1, wherein the total nitrogen application amount of the compound fertilizer is 90-100 kg/hm2。
4. The method for preparing tobacco rod-based activated carbon electrode material self-doped with sulfur element as claimed in claim 1, wherein P is N in the compound fertilizer2O5:K2O=1:2~3:3~4。
5. The preparation method of the tobacco stem-based activated carbon electrode material self-doped with the sulfur element as claimed in claim 1, wherein the picea javanica branch and leaf water extract is prepared by the following method: and (3) putting the schefflera octophylla branches and leaves into water, and soaking for 10-30 days to obtain the schefflera octophylla branch and leaf water extract.
6. The preparation method of the sulfur-element-auto-doped tobacco rod-based activated carbon electrode material as claimed in claim 1, wherein the weight ratio of the compound fertilizer to the picea javanica branch and leaf water extract is 1: 3-10.
7. The method for preparing tobacco stem-based activated carbon electrode material doped with sulfur element as claimed in claim 6, wherein the weight ratio of the compound fertilizer to the water extract of the twig and leaf of schefflera octophylla is 1: 5.
8. The preparation method of the tobacco rod-based activated carbon electrode material doped with sulfur elements as claimed in claim 5, wherein the weight ratio of the picea javanica branches and leaves to water is 1: 8-25.
9. The method for preparing a tobacco rod-based activated carbon electrode material self-doped with elemental sulfur as claimed in claim 8, wherein the weight ratio of the picea javanica branches and leaves to water is 1: 15.
10. The preparation method of the tobacco rod-based activated carbon electrode material self-doped with sulfur element as claimed in claim 1,
the heat treatment conditions in the step (3) are as follows: at 3-6 ℃ for min in nitrogen atmosphere-1The temperature is increased to 500-600 ℃ and is kept for 1-3 h;
the heat treatment conditions in the step (5) are as follows: at 3-6 ℃ for min in nitrogen atmosphere-1The temperature is increased to 800-900 ℃ and kept for 1-3 h.
11. A tobacco rod-based activated carbon electrode material which is self-doped with sulfur and is prepared by the preparation method of any one of claims 1 to 10.
12. Use of the self-sulfur doped tobacco rod based activated carbon electrode material of claim 11 in the preparation of a capacitor.
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