CN106952746A - Active carbon electrode material preparation method and manganese oxide/activated carbon composite electrode material preparation method - Google Patents
Active carbon electrode material preparation method and manganese oxide/activated carbon composite electrode material preparation method Download PDFInfo
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- manganese oxide
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 38
- 239000007772 electrode material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 24
- 240000008042 Zea mays Species 0.000 claims abstract description 22
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 22
- 239000010902 straw Substances 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims abstract description 15
- 235000009973 maize Nutrition 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 235000005822 corn Nutrition 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract 3
- 239000002245 particle Substances 0.000 claims description 35
- 239000011259 mixed solution Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002250 absorbent Substances 0.000 claims description 10
- 230000002745 absorbent Effects 0.000 claims description 10
- 229940058641 actidose Drugs 0.000 claims description 10
- 239000003610 charcoal Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000006258 conductive agent Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000005539 carbonized material Substances 0.000 claims description 2
- 229910052571 earthenware Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000003513 alkali Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract 1
- 238000005984 hydrogenation reaction Methods 0.000 abstract 1
- 238000005554 pickling Methods 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- 238000003763 carbonization Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000004913 activation Effects 0.000 description 4
- 239000012286 potassium permanganate Substances 0.000 description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- -1 timber Substances 0.000 description 2
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000011874 heated mixture Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
Classifications
-
- 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
-
- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
-
- 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
-
- 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
-
- 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
- H01G11/46—Metal oxides
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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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Manufacturing & Machinery (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Active carbon electrode material preparation method is made the invention discloses a kind of maize straw, and it is a kind of with maize straw making manganese oxide/activated carbon composite electrode material preparation method, can be by adding alkali and mixing corn straw smashing, heating, then the processing step such as heating, pickling, distillation produces active carbon electrode material, by the activated carbon produced and the mixture of liquor potassic permanganate and ethanol solution, manganese oxide/activated carbon composite electrode material is produced through overpickling, washing, drying process after hydrogenation sodium hydroxide solution reaction.Pass through combination electrode material made from this method, effectively improve the cycle performance of transition metal oxide, improve the cyclical stability of material, enhance the high rate performance of electrode material, and solve stalk waste gas and burn the wasting of resources brought and problem of environmental pollution, improve the comprehensive development and utilization and its utilization rate of agricultural crop straw.
Description
Technical field
The present invention relates to electrode material preparing technical field, specifically, it is related to a kind of active carbon electrode material preparation side
Method and manganese oxide/activated carbon composite electrode material preparation method.
Background technology
At present, the electrode material of ultracapacitor mainly uses manganese oxide/activated carbon composite electrode material, and combination electrode
The raw material of activated carbon in material has coal, timber, shell, walnut shell and stalk etc., and these carbonaceous materials are placed in activation furnace,
Activated carbon is converted into by pyrolysis under high temperature and certain pressure.Compared with active carbon from coal, stalk production activated carbon
There is intensity and activation grade is relatively low, conductance is poor, while the yield of stalk production activated carbon is relatively low, most of stalk
The achievement in research of active carbon electrode material also rests on laboratory stage at present.And agricultural crop straw is widely present, crop straw burning
Atmospheric environment is had a strong impact on, therefore, it is necessary to solve how to improve the comprehensive utilization of agricultural crop straw and its asking for utilization rate
Topic.
The content of the invention
First technical problem to be solved by this invention be：One kind is provided using stalk as raw material, and specific surface area height,
The high active carbon electrode material preparation method of mesoporous.
Second technical problem to be solved by this invention be：The oxygen that a kind of cyclical stability is high, high rate performance is strong is provided
Change manganese/active carbon electrode material preparation method.
To solve above-mentioned first technical problem, the technical scheme is that：
Active carbon electrode material preparation method, comprises the following steps：
A, corn stalk powder are broken to 0.35~0.42mm of particle diameter stalk particle, stalk particle are crossed into 40 mesh sieves, and dry
Moisture to stalk particle is less than 10%；
B, by dried stalk particle load crucible, under the protection atmosphere of inert gas, according to 5~10 DEG C/min's
The rate of heat addition is heated to 500~600 DEG C in kiln, constant temperature is then kept in kiln 3~5 hours, obtains maize straw carbon
Compound material；
C, the maize straw is carbonized material and activator according to mass ratio 1：1~5：Add after 1 ratio is well mixed
Enter crucible, under the protection atmosphere of inert gas, heated the mixture to according to 5~10 DEG C/min rate of heat addition in kiln
700~1000 DEG C, insulation is cooled to normal temperature after 2 hours；
D, the mixture that will be cooled to normal temperature are washed with acid solution, are then 6~7 with pure water to pH value, are dried
The particle of 15~20 μm of particle diameter is crushed to after processing, absorbent charcoal material is made.
It is preferred that, the inert gas is argon gas, nitrogen or argon gas nitrogen mixed gas.
It is preferred that, the activator is KOH, CaCl2Or NaOH.
To solve above-mentioned second technical problem, the technical scheme is that：
Manganese oxide/activated carbon composite electrode material preparation method, it is characterised in that：First pass through above-mentioned absorbent charcoal material electricity
Absorbent charcoal material is made in pole material preparation method, then further comprising the steps of：
E, the liquor potassic permanganate for being 0.5~2.0mol/L by concentration, 200ml ethanol solutions and concentration is 1.0~
3.0mol/L Actidose is well mixed, and is stirred 1~2 hour at normal temperatures, is obtained mixed solution, wherein, the Gao Meng
Sour potassium solution is 2 with the mass ratio of the Actidose：1~10：1；
F, to the mixed solution and dripping concentration be 1.0~1.5mol/L NaOH solution, while stir mixed solution,
Then mixed solution is heated to 80~100 DEG C, isothermal reaction is cooled to normal temperature after 3~5 hours；
G, mixed solution washed with hydrochloric acid solution, then filtered with pure water, conductive agent is added after drying process and is mixed
Close uniform, under inert gas shielding, be heated to 400-700 DEG C, be cooled to normal temperature, manganese oxide/active carbon combined electrode is made
Material.
It is preferred that, the conductive agent is conductive black or graphite agent.
Employ after above-mentioned technical proposal, the beneficial effects of the invention are as follows：
Active carbon electrode material preparation method is made with maize straw method proposes one kind, and uses maize straw system
Make manganese oxide/activated carbon composite electrode material preparation method, by combination electrode material made from this method, effectively improve
The cycle performance of transition metal oxide, the distinctive loose structure of activated carbon that this method is made can effectively alleviate transition gold
Belong to Volume Changes of the oxide in charge and discharge process, improve the cyclical stability of material, meanwhile, the activated carbon that this method is made
The loose structure having, can increase the contact area of electrolyte and electrode material, and more reactions are provided for electrochemical reaction
Point, is conducive to the quick progress of electrochemical reaction, so as to strengthen the high rate performance of electrode material.
Manganese oxide/activated carbon composite electrode material, adds conductive agent made from this method, efficiently solves stalk life
The low intensity of the activated carbon presence of production, the shortcoming that activation grade is low and conductance is poor, improve obtained absorbent charcoal material
Intensity, activation grade and conductance.
This method is raw material using crops maize straw, produces active carbon electrode material, it is proposed that crops corn stalk
The new processing method of stalk, solves stalk waste gas and burns the wasting of resources brought and problem of environmental pollution, improve farming
The comprehensive development and utilization and its utilization rate of thing stalk.
Embodiment
The present invention is expanded on further with reference to specific embodiment.
Embodiment one
Corn stalk powder is broken to 0.35~0.42mm of particle diameter stalk particle, stalk particle is crossed into 40 mesh sieves, and dry extremely
The moisture of stalk particle is less than 10%；Dried stalk particle is loaded into crucible, under the protection atmosphere of inert gas,
500~600 DEG C are heated in kiln according to 5~10 DEG C/min rate of heat addition, constant temperature is then kept in kiln 4 hours,
Obtain maize straw carbonization material；By maize straw carbonization material and KOH according to mass ratio 1：1~5：1 ratio is well mixed
After add crucible, under the protection atmosphere of argon gas, heated the mixture to according to 5~10 DEG C/min rate of heat addition in kiln
700~1000 DEG C, insulation is cooled to normal temperature after 2 hours；The mixture that will be cooled to normal temperature is washed with acid solution, then with pure
Water washing to pH value is 6~7, and the particle of 15~20 μm of particle diameter is crushed to after drying process, and absorbent charcoal material is made.
Then the liquor potassic permanganate for being 1.0mol/L by concentration, 200ml ethanol solutions and concentration are 2.0mol/L's
Actidose is well mixed, and ethanol is by potassium permanganate oxidation, generation acetic acid and manganese oxide, chemical formula：5C2H5OH+4MnO4 -
+12H+=5CH3COOH+4Mn2 ++11H2O), then stir 1 hour at normal temperatures, obtain mixed solution, wherein, potassium permanganate is molten
The mass ratio of liquid and Actidose is 2：1~10：1,；To the NaOH solution that mixed solution and dripping concentration is 1.2mol/L,
Generation acid-base neutralization reaction, chemical formula is：
NaOH+CH3COOH=CH3COONa+H2O
(OH-)+(CH3COOH)=(CH3COO-)+H2O)
Mixed solution is stirred simultaneously, mixed solution is then heated to 80~100 DEG C, isothermal reaction is cooled to after 3 hours
Normal temperature；Mixed solution is washed with hydrochloric acid solution, then filtered with pure water, conductive black mixing is added after drying process equal
It is even, under inert gas shielding, 400-700 DEG C is heated to, normal temperature is cooled to, manganese oxide/activated carbon composite electrode material is made.
Embodiment two
Corn stalk powder is broken to 0.35~0.42mm of particle diameter stalk particle, stalk particle is crossed into 40 mesh sieves, and dry extremely
The moisture of stalk particle is less than 10%；Dried stalk particle is loaded into crucible, under the protection atmosphere of inert gas,
500~600 DEG C are heated in kiln according to 5~10 DEG C/min rate of heat addition, constant temperature is then kept in kiln 3 hours,
Obtain maize straw carbonization material；By maize straw carbonization material and NaOH according to mass ratio 1：1~5：1 ratio is well mixed
After add crucible, under the protection atmosphere of argon gas, heated the mixture to according to 5~10 DEG C/min rate of heat addition in kiln
700~1000 DEG C, insulation is cooled to normal temperature after 2 hours；The mixture that will be cooled to normal temperature is washed with acid solution, then with pure
Water washing to pH value is 6~7, and the particle of 15~20 μm of particle diameter is crushed to after drying process, and absorbent charcoal material is made.
Then the liquor potassic permanganate for being 1.0mol/L by concentration, 200ml ethanol solutions and concentration are 2.0mol/L's
Actidose is well mixed, and ethanol is by potassium permanganate oxidation, generation acetic acid and manganese oxide, chemical formula：5C2H5OH+4MnO4 -
+12H+=5CH3COOH+4Mn2 ++11H2O), at normal temperatures stir 2 hours, obtain mixed solution, wherein, liquor potassic permanganate with
The mass ratio of Actidose is 2：1~10：1；To the NaOH solution that mixed solution and dripping concentration is 1.2mol/L, occurs acid
Alkali neutralization reaction, chemical formula is：
NaOH+CH3COOH=CH3COONa+H2O
(OH-)+(CH3COOH)=(CH3COO-)+H2O)
Mixed solution is stirred simultaneously, mixed solution is then heated to 80~100 DEG C, isothermal reaction is cooled to after 4 hours
Normal temperature；Mixed solution is washed with hydrochloric acid solution, then filtered with pure water, graphite agent mixing is added after drying process
Uniformly, under inert gas shielding, 400-700 DEG C is heated to, normal temperature is cooled to, manganese oxide/active carbon combined electrode material is made
Material.
Embodiment three
Corn stalk powder is broken to 0.35~0.42mm of particle diameter stalk particle, stalk particle is crossed into 40 mesh sieves, and dry extremely
The moisture of stalk particle is less than 10%；Dried stalk particle is loaded into crucible, under the protection atmosphere of inert gas,
500~600 DEG C are heated in kiln according to 5~10 DEG C/min rate of heat addition, constant temperature is then kept in kiln 5 hours,
Obtain maize straw carbonization material；By maize straw carbonization material and CaCl2According to mass ratio 1：1~5：1 ratio mixing is equal
Crucible is added after even, under the protection atmosphere of argon gas, is heated mixture in kiln according to 5~10 DEG C/min rate of heat addition
To 700~1000 DEG C, insulation is cooled to normal temperature after 2 hours；The mixture that will be cooled to normal temperature is washed with acid solution, Ran Houyong
Pure water to pH value is 6~7, and the particle of 15~20 μm of particle diameter is crushed to after drying process, and absorbent charcoal material is made.
Then the liquor potassic permanganate for being 1.0mol/L by concentration, 200ml ethanol solutions and concentration are 2.0mol/L's
Actidose is well mixed, and ethanol is by potassium permanganate oxidation, generation acetic acid and manganese oxide, chemical formula：5C2H5OH+4MnO4 -
+12H+=5CH3COOH+4Mn2 ++11H2O), at normal temperatures stir 1 hour, obtain mixed solution, wherein, liquor potassic permanganate with
The mass ratio of Actidose is 2：1~10：1；To the NaOH solution that mixed solution and dripping concentration is 1.2mol/L, occurs acid
Alkali neutralization reaction, chemical formula is：
NaOH+CH3COOH=CH3COONa+H2O
(OH-)+(CH3COOH)=(CH3COO-)+H2O)
Mixed solution is stirred simultaneously, mixed solution is then heated to 80~100 DEG C, isothermal reaction is cooled to after 5 hours
Normal temperature；Mixed solution is washed with hydrochloric acid solution, then filtered with pure water, conductive black mixing is added after drying process equal
It is even, under inert gas shielding, 400-700 DEG C is heated to, normal temperature is cooled to, manganese oxide/activated carbon composite electrode material is made.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, without departing from the spirit and scope of the present invention, this hair
Bright also to have various changes and modifications, these changes and improvements all fall within the protetion scope of the claimed invention.Application claims
Protection domain is by appending claims and its equivalent thereof.
Claims (5)
1. active carbon electrode material preparation method, it is characterised in that comprise the following steps：
A, corn stalk powder are broken to 0.35~0.42mm of particle diameter stalk particle, stalk particle are crossed into 40 mesh sieves, and dry to straw
The moisture of stalk particle is less than 10%；
B, by dried stalk particle load crucible, under the protection atmosphere of inert gas, according to 5~10 DEG C/min heating
Speed is heated to 500~600 DEG C in kiln, constant temperature is then kept in kiln 3~5 hours, obtains maize straw carbide
Material；
C, the maize straw is carbonized material and activator according to mass ratio 1：1~5：Earthenware is added after 1 ratio is well mixed
Crucible, under the protection atmosphere of inert gas, 700 are heated the mixture to according to 5~10 DEG C/min rate of heat addition in kiln
~1000 DEG C, insulation is cooled to normal temperature after 2 hours；
D, the mixture that will be cooled to normal temperature are washed with acid solution, are then 6~7, drying process with pure water to pH value
The particle of 15~20 μm of particle diameter is crushed to afterwards, and absorbent charcoal material is made.
2. active carbon electrode material preparation method as claimed in claim 1, it is characterised in that：The inert gas be argon gas,
Nitrogen or argon gas nitrogen mixed gas.
3. active carbon electrode material preparation method as claimed in claim 1 or 2, it is characterised in that：The activator be KOH,
CaCl2Or NaOH.
4. manganese oxide/activated carbon composite electrode material preparation method, it is characterised in that：First pass through any one of claims 1 to 3 institute
Absorbent charcoal material is made in the absorbent charcoal material electrode material preparation method stated, then further comprising the steps of：
E, the liquor potassic permanganate for being 0.5~2.0mol/L by concentration, 200ml ethanol solutions and concentration are 1.0~3.0mol/
L Actidose is well mixed, and is stirred 1~2 hour at normal temperatures, is obtained mixed solution, wherein, the liquor potassic permanganate
Mass ratio with the Actidose is 2：1~10：1；
F, to the mixed solution and dripping concentration be 1.0~1.5mol/L NaOH solution, while stir mixed solution, then
Mixed solution is heated to 80~100 DEG C, isothermal reaction is cooled to normal temperature after 3~5 hours；
G, mixed solution washed with hydrochloric acid solution, then filtered with pure water, conductive agent mixing is added after drying process equal
It is even, under inert gas shielding, 400-700 DEG C is heated to, normal temperature is cooled to, manganese oxide/activated carbon composite electrode material is made.
5. manganese oxide as claimed in claim 4/activated carbon composite electrode material preparation method, it is characterised in that：The conduction
Agent is conductive black or graphite agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710179015.2A CN106952746B (en) | 2017-03-23 | 2017-03-23 | Active carbon electrode material preparation method and manganese oxide/activated carbon composite electrode material preparation method |
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| CN108584956A (en) * | 2018-04-20 | 2018-09-28 | 句容市盛达环保净化材料有限公司 | A kind of production equipment producing high grade activated carbon |
| CN110518262A (en) * | 2019-08-13 | 2019-11-29 | 武汉长海电力推进和化学电源有限公司 | A kind of anode of microbial fuel cell material and preparation method thereof |
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