CN111799104A - Preparation method of modified carbon electrode combining biodegradation and microwave treatment - Google Patents
Preparation method of modified carbon electrode combining biodegradation and microwave treatment Download PDFInfo
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- CN111799104A CN111799104A CN202010701076.2A CN202010701076A CN111799104A CN 111799104 A CN111799104 A CN 111799104A CN 202010701076 A CN202010701076 A CN 202010701076A CN 111799104 A CN111799104 A CN 111799104A
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- 150000001721 carbon Chemical class 0.000 title claims description 23
- 238000002360 preparation method Methods 0.000 title claims description 7
- 238000006065 biodegradation reaction Methods 0.000 title claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 200
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 145
- 239000000243 solution Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 19
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 14
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 14
- 230000004048 modification Effects 0.000 claims abstract description 11
- 238000012986 modification Methods 0.000 claims abstract description 11
- 229910001507 metal halide Inorganic materials 0.000 claims abstract description 7
- 150000005309 metal halides Chemical class 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 244000005700 microbiome Species 0.000 claims abstract description 6
- 239000012670 alkaline solution Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 32
- 239000002068 microbial inoculum Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 21
- 239000000853 adhesive Substances 0.000 claims description 18
- 230000001070 adhesive effect Effects 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 14
- 239000002033 PVDF binder Substances 0.000 claims description 14
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000002028 Biomass Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 241000894006 Bacteria Species 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 10
- 229920002472 Starch Polymers 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 9
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- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 239000008107 starch Substances 0.000 claims description 9
- 235000019698 starch Nutrition 0.000 claims description 9
- 239000006230 acetylene black Substances 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000006258 conductive agent Substances 0.000 claims description 6
- 238000000855 fermentation Methods 0.000 claims description 6
- 230000004151 fermentation Effects 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 4
- 239000002361 compost Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
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- 238000007598 dipping method Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 238000009395 breeding Methods 0.000 claims description 2
- 230000001488 breeding effect Effects 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229940102001 zinc bromide Drugs 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 7
- 239000012467 final product Substances 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000002715 modification method Methods 0.000 abstract description 3
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 3
- 239000011574 phosphorus Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000006181 electrochemical material Substances 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 abstract description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 239000007921 spray Substances 0.000 abstract 1
- 235000018102 proteins Nutrition 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 108010073771 Soybean Proteins Proteins 0.000 description 9
- 238000001816 cooling Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 230000000593 degrading effect Effects 0.000 description 5
- 238000007865 diluting Methods 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 235000019710 soybean protein Nutrition 0.000 description 5
- 150000001720 carbohydrates Chemical class 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 229920001592 potato starch Polymers 0.000 description 4
- 229940001941 soy protein Drugs 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000001580 bacterial effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 235000010980 cellulose Nutrition 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 241000589151 Azotobacter Species 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000003855 acyl compounds Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
-
- 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
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the field of electrochemical materials for preparing and modifying carbon electrodes, in particular to a modification method for modifying an activated carbon electrode. The invention adds biodegradable substance in the process of manufacturing the carbon electrode, firstly biodegrades the carbon electrode after the carbon electrode is manufactured, then sprays acid solution, alkaline solution or metal halide solution, and then carries out microwave treatment and modification to obtain the final product. Through the action of microorganisms, the space occupied by the original protein and the like becomes a gap after the degradation is finished, the specific surface area of the carbon electrode is increased, and the pore structure of the carbon electrode is enriched; the degraded product also contains abundant metal elements such as phosphorus, magnesium, calcium, manganese, iron and the like, so that a large number of functional groups can be generated in and on the surface of the carbon electrode, and a large number of metal elements are doped to generate free and combined states, so that the carbon electrode has a gain effect on charge adsorption and pseudo-electric reaction, and the effect of obviously improving the capacitance of the whole carbon electrode is achieved.
Description
Technical Field
The invention relates to the field of electrochemical materials for preparing and modifying carbon electrodes, in particular to a modification method for modifying an activated carbon electrode.
Technical Field
The activated carbon electrode is mainly applied to electrochemical energy storage equipment such as a super capacitor or a battery, and the size of specific capacitance and the multiplying power of the activated carbon electrode are main indexes for judging the performance of the carbon electrode. However, the existing technical method basically comprises the steps of firstly preparing activated carbon, modifying the activated carbon, mixing the modified activated carbon with a binder and a conductive agent in a certain proportion, tabletting and then preparing a formed carbon electrode, and the technical method for further modifying the formed carbon electrode to improve the electrochemical performance is lacked. The formed carbon electrode is added with a binder and a conductive agent in the preparation process, so that the space collapse and partial pore closure of the activated carbon can be caused in the mixing and pressing processes, the effective specific surface area is reduced, the specific capacitance is not high, and the electrochemical performance is not ideal. At present, only Chinese invention patent with patent number ZL201710658575.6 is found, the carbon electrode is processed at high temperature in a tubular furnace atmosphere after being formed, and the modified carbon electrode is obtained by a liquid nitrogen cooling method quickly. Therefore, the development of a simpler and easier carbon electrode modification technical method has certain practical significance.
At present, the microbial treatment technology is mainly used for degrading wastes and manufacturing fermentation products. Protein, starch and cellulose are biomass which widely exists in the nature and is easy to degrade, and effective bacterial strains and complex microbial inoculum for degrading are easy to obtain. Under the action of microbes, protein is mainly hydrolyzed into amino acid, deaminated and decarboxylated into fatty acid, and then converted into fatty acid. In the process, long-chain protein disappears, ammonia gas is released by decarboxylation of amino acid, free ammonium salt, amide, nitrogen oxide and oxygen-containing functional groups are generated, and the final products can generate beneficial influence on the capacitance of the material; the starch degradation process is to generate saccharides through hydrolysis, and then to degrade, in the process, besides generating alcohol and carbon dioxide, a large amount of amine phosphate compounds can be generated, a large amount of polyvalent phosphorus elements can be provided, and the influence on capacitance can be generated; the decomposition of cellulose can lead to the breaking of long chains of high molecules to form saccharides, and the continuous degradation effect of the saccharides is the same as that of the saccharides. The degradable biomass is creatively added in the preparation of the carbon electrode, and the structure of the carbon electrode and the group structure on the adsorption surface of the carbon electrode are changed by a biodegradation method, so that the aim of improving the capacitance of the carbon electrode is fulfilled.
At present, the microwave technology has become a widely applied technology in industry and is also applied in the preparation process of a plurality of new materials. The basic principle of a microwave oven or a microwave reactor is to vibrate reactant molecules by electromagnetic waves and frictionally generate heat, and thus microwave technology is used as a heating technology in many applications. The microwave technology has the advantages of high effect taking speed, high efficiency and no thermal inertia, and can quickly stop microwave treatment in production. The invention relates to a technical mode of carrying out modification, spraying or soaking and microwave modification on a formed carbon electrode after microorganism modification so as to achieve the aim of sterilizing and stabilizing the structure of the carbon electrode, and simultaneously, the carbon electrode with obviously improved specific capacitance of the modified carbon electrode can be obtained.
The invention content is as follows:
the invention aims to provide a carbon electrode modification method which is simple and high in processing speed and combines biodegradation and microwave technology processing.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a modified carbon electrode combining biodegradation and microwave treatment comprises the following steps:
(1) sieving the activated carbon with a 300-mesh sieve, and drying for later use; sieving the dried degradable biomass with a 300-mesh sieve for later use;
(2) mixing 80-85 parts of dried active carbon, 5-10 parts of degradable biomass, 5-10 parts of conductive agent and 5-10 parts of binder according to weight percentage, grinding and mixing by using a ball mill, and simultaneously weighing 1-10 parts of absolute ethyl alcohol for later use;
(3) adding a proper amount of N-methyl pyrrolidone or absolute ethyl alcohol into the mixture prepared in the step (2) as a solvent, heating to 40-60 ℃, and continuously stirring until a large amount of the solvent is volatilized to obtain a viscous mixture A;
(4) dripping a small amount of weighed absolute ethyl alcohol on the mixture A to obtain a mixture B;
(5) pressing the mixture B into a carbon electrode by using a tablet press under the pressure of 10-20MPa, and performing vacuum drying for 4-8 hours at the temperature of 25-40 ℃ to obtain a carbon electrode A for later use;
(6) preparing a complex microbial inoculum solution with a certain concentration;
(7) completely dipping the carbon electrode A into the composite microbial inoculum solution prepared in the step (6), controlling the temperature at 25-35 ℃ and the dipping time to be more than 2 hours, so as to obtain a carbon electrode B;
(8) placing the soaked carbon electrode B on a culture dish, placing the culture dish into a biological incubator, controlling the temperature at 70 ℃, maintaining the pH value at 7-8 and the humidity at more than 50%, and supplying oxygen in a proper amount (if the adopted degradable biomass is starch, oxygen is not required to be supplied, and the temperature is controlled at 40-50 ℃), wherein the maintaining time is 12-36 hours;
(9) preparing an acidic solution, an alkaline solution or a metal halide solution with a certain concentration for later use;
(10) taking out the carbon electrode B treated by the microorganisms in the step (8) together with the culture dish, fully spraying any one of the solutions prepared in the step (9) or pure water on the culture dish and the carbon electrode B, and then putting the culture dish containing the carbon electrode B into a microwave reactor;
(11) starting a microwave reactor to operate under certain power, and closing the microwave reactor after microwave modification for a period of time to obtain a carbon electrode C;
(12) washing the carbon electrode C with a large amount of pure water, and fully drying to obtain a carbon electrode D;
(13) and adhering the carbon electrode D to a flat current collecting plate coated with conductive adhesive, and fully drying to obtain a finished product modified carbon electrode E.
The degradable biomass in the steps (1) and (2) is protein powder or starch.
The conductive agent in the step (2) is any one of acetylene black, graphite powder, carbon nano tubes or graphene, the binder is polytetrafluoroethylene or polyvinylidene fluoride, and the binder needs to be processed into fine powder with the particle size of 100 meshes.
The complex microbial inoculum in the step (6) can be a special commercial complex microbial inoculum suitable for composting fermentation and breeding industry, needs to be provided with azotobacter, phosphate-solubilizing bacteria, potassium-releasing bacteria and the like, can decompose protein and starch and has a certain cellulose degradation function, and dilutes a commercial microbial inoculum with pure water to prepare a solution. The liquid microbial inoculum is diluted by 50-100 times according to the volume ratio, and the solid microbial inoculum is diluted by 1000-3000 times according to the mass ratio.
The acidic solution in the step (9) is any one of inorganic acid and organic acid solutions such as nitric acid, phosphoric acid, sulfuric acid, hydrochloric acid, hydrogen peroxide solution, acetic acid, oxalic acid and the like, and the mass concentration range is 5-80%; the alkaline solution refers to NaOH, KOH and FeSO4、MnSO4、AgNO3And any one of Co + and other solutions with the mass concentration of 5-60%; the metal halide solution refers to any one of solutions of zinc chloride, magnesium chloride, zinc bromide and the like, and the mass concentration of the metal halide solution is 5-60%.
In the step (11), the modification time of the microwave reactor is 0.5 to 60 minutes, and the power used is 100 to 3000W.
The conductive adhesive in the step (13) is any one of carbon conductive adhesive, silver conductive adhesive, gold conductive adhesive or copper conductive adhesive, and the collector plate is a metal collector plate or a carbon collector plate.
In the invention, biodegradable substances such as protein, starch and the like are added in the manufacturing process of the carbon electrode, and simultaneously, the biomass may not be completely carbonized in the carbonization process of the activated carbon and a part of cellulose is remained. After the carbon electrode is manufactured, the carbon electrode is firstly biodegraded, and the activated carbon, the carbon black and the binder of the carbon electrode cannot be influenced within a certain time. The selected composite microbial inoculum comprises fungi and bacteria (optional commercial composite microbial inoculum) capable of degrading protein, starch and cellulose, and space occupied by original protein and the like is changed into a gap through the action of microorganisms after degradation is finished, so that the specific surface area of the carbon electrode is increased, and the pore structure of the carbon electrode is enriched; the degraded product, such as soybean protein, not only has the basic structure of protein, but also contains abundant phosphorus, magnesium, calcium, manganese, iron, molybdenum, zinc, copper, cobalt, strontium, nickel and the like, so that a large amount of acyl compounds, nitrogen-containing groups, oxygen-containing groups and the like can be generated in and on the surface of the carbon electrode, and simultaneously a large amount of metal elements are doped, so that free and combined states can be generated, and the product plays a role in gaining the absorption of charges and pseudo-electric reaction, thereby playing a role in obviously improving the capacitance of the whole carbon electrode.
After the carbon electrode is degraded and modified by microorganisms, the carbon electrode can play a role in stabilizing carbon electrode groups, doped metal elements and the like by using solutions such as phosphoric acid and the like; microwave is adopted to make the inner part and the outer part of the carbon electrode move uniformly, so as to adjust and stabilize the structure of the carbon electrode and achieve the sterilization effect; and finally washing away soluble residual degradation products by using clear water to obtain the modified carbon electrode.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Grinding the dried active carbon, sieving with a 300-mesh sieve, and drying for later use. The soy protein powder is also dried and sieved through a 300 mesh sieve for later use. Mixing activated carbon, soybean protein powder, acetylene black and polyvinylidene fluoride (PVDF) according to a mass ratio of 75: 10: 10: 5 mixing, grinding for 3 hours by a ball mill, adding N-methyl pyrrolidone with the same mass as the mixture as a solvent, heating to 50 ℃, and stirring until the solvent is volatilized to form a viscous mixture A. Adding anhydrous ethanol with a mass of 2% of the solvent N-methyl pyrrolidone dropwise to obtain a mixture B, pressing the mixture B into a carbon electrode by a tablet press under 15MPa, and drying the carbon electrode in vacuum at 30 ℃ for 6 hours to obtain a carbon electrode A. And (3) taking compost fermentation compound bacteria liquid (mainly protein degrading bacteria), diluting by 100 times according to the volume ratio, and completely immersing the carbon electrode A into the microbial inoculum solution for 4 hours to obtain the carbon electrode B. And (2) placing the carbon electrode B into a culture dish, placing the culture dish into a biological incubator, controlling the temperature to be 70 ℃, properly adjusting the pH value to be about 7.5, controlling the humidity to be 80 percent and the oxygen flow to be 10L/h, taking out the carbon electrode B and the culture dish together after 24 hours, and spraying 20 percent wt phosphoric acid solution (which is sprayed on the electrode comprehensively) into the carbon electrode and the culture dish. And then placing the culture dish provided with the carbon electrode B into a rotating disc type microwave reactor, setting the power to 400W, and closing the culture dish after running for 120 seconds to obtain a modified carbon electrode C. The carbon electrode C was rinsed with a large amount of pure water and vacuum-dried at 50 ℃ for 6 hours to obtain a carbon electrode D. And (3) bonding the carbon electrode D to the smooth foam nickel coated with the graphite conductive adhesive, drying for 12 hours in vacuum at 50 ℃, and taking out after cooling to obtain the final product, namely the carbon electrode E.
The indexes of the product carbon electrode are as follows: the specific capacitance is 220.3F/g, and the capacitance retention rate is 97.3 percent after 3000 times of charge and discharge.
Example 2
Grinding the dried active carbon, sieving with a 300-mesh sieve, and drying for later use. The soy protein powder is also dried and sieved through a 300 mesh sieve for later use. Mixing activated carbon, soybean protein powder, acetylene black and polyvinylidene fluoride (PVDF) according to a mass ratio of 75: 10: 10: 5 mixing, grinding for 3 hours by a ball mill, adding N-methyl pyrrolidone with the same mass as the mixture as a solvent, heating to 50 ℃, and stirring until the solvent is volatilized to form a viscous mixture A. Adding anhydrous ethanol with a mass of 2% of the solvent N-methyl pyrrolidone dropwise to obtain a mixture B, pressing the mixture B into a carbon electrode by a tablet press under 15MPa, and drying the carbon electrode in vacuum at 30 ℃ for 6 hours to obtain a carbon electrode A. And (3) taking compost fermentation compound bacteria liquid (mainly protein degrading bacteria), diluting by 50 times according to the volume ratio, and completely immersing the carbon electrode A into the microbial inoculum solution for 4 hours to obtain the carbon electrode B. And (2) placing the carbon electrode B into a culture dish, placing the culture dish into a biological incubator, controlling the temperature to be 70 ℃, properly adjusting the pH value to be about 7.5, controlling the humidity to be 80 percent and the oxygen flow to be 10L/h, taking out the carbon electrode B and the culture dish together after 24 hours, and spraying 30 percent by weight phosphoric acid solution (which is sprayed on the electrode comprehensively) into the carbon electrode and the culture dish. And then placing the culture dish provided with the carbon electrode B into a rotating disc type microwave reactor, setting the power to 400W, and closing the culture dish after running for 120 seconds to obtain a modified carbon electrode C. The carbon electrode C was rinsed with a large amount of pure water and vacuum-dried at 50 ℃ for 6 hours to obtain a carbon electrode D. And (3) bonding the carbon electrode D to the smooth foam nickel coated with the graphite conductive adhesive, drying for 12 hours in vacuum at 50 ℃, and taking out after cooling to obtain the final product, namely the carbon electrode E.
The indexes of the product carbon electrode are as follows: the specific capacitance of 210F/g is 97 percent after 3000 times of charge and discharge.
Example 3
Grinding the dried active carbon, sieving with a 300-mesh sieve, and drying for later use. The potato starch was also dried and sieved through a 300 mesh sieve for use. Mixing activated carbon, potato starch, acetylene black and polyvinylidene fluoride (PVDF) according to a mass ratio of 75: 10: 10: 5 mixing, grinding for 3 hours by a ball mill, adding N-methyl pyrrolidone with the same mass as the mixture as a solvent, heating to 50 ℃, and stirring until the solvent is volatilized to form a viscous mixture A. Adding anhydrous ethanol with a mass of 2% of the solvent N-methyl pyrrolidone dropwise to obtain a mixture B, pressing the mixture B into a carbon electrode by a tablet press under 15MPa, and drying the carbon electrode in vacuum at 30 ℃ for 6 hours to obtain a carbon electrode A. Taking the special composite microbial inoculum (solid) for the planting industry, diluting each gram of microbial inoculum with 1000 milliliters of water to prepare a bacterial liquid or a suspension, and completely immersing the carbon electrode A into the microbial inoculum solution for 4 hours to obtain the carbon electrode B. And (3) placing the carbon electrode B into a culture dish, placing the culture dish into a biological incubator, controlling the temperature to be 50 ℃, controlling the humidity to be 80%, controlling the nitrogen flow to be 2L/h (the anaerobic environment effect is better), taking out the culture dish together with the carbon electrode B after 48 hours, fully spraying 20% wt phosphoric acid solution into the carbon electrode and the culture dish, placing the culture dish with the carbon electrode B into a rotary disc type microwave reactor, setting the power to be 600W, and closing the culture dish after running for 180 seconds to obtain the modified carbon electrode C. The carbon electrode C was rinsed with a large amount of pure water and vacuum-dried at 50 ℃ for 6 hours to obtain a carbon electrode D. And (3) bonding the carbon electrode D to the smooth foam nickel coated with the graphite conductive adhesive, drying for 12 hours in vacuum at 50 ℃, and taking out after cooling to obtain the final product, namely the carbon electrode E.
The indexes of the product carbon electrode are as follows: the specific capacitance is 170F/g, and the capacitance retention rate is 96 percent after 3000 times of charge and discharge.
Example 4
Grinding the dried active carbon, sieving with a 300-mesh sieve, and drying for later use. The potato starch was also dried and sieved through a 300 mesh sieve for use. Mixing activated carbon, potato starch, acetylene black and polyvinylidene fluoride (PVDF) according to a mass ratio of 75: 10: 10: 5 mixing, grinding for 3 hours by a ball mill, adding N-methyl pyrrolidone with the same mass as the mixture as a solvent, heating to 50 ℃, and stirring until the solvent is volatilized to form a viscous mixture A. Adding anhydrous ethanol with a mass of 2% of the solvent N-methyl pyrrolidone dropwise to obtain a mixture B, pressing the mixture B into a carbon electrode by a tablet press under 15MPa, and drying the carbon electrode in vacuum at 30 ℃ for 6 hours to obtain a carbon electrode A. Taking the special composite microbial inoculum (solid) for the planting industry, diluting each gram of microbial inoculum with 3000 ml of water to prepare a bacterial liquid or a suspension, and completely immersing the carbon electrode A into the microbial inoculum solution for 4 hours to obtain the carbon electrode B. And (3) placing the carbon electrode B into a culture dish, placing the culture dish into a biological incubator, controlling the temperature to be 50 ℃, controlling the humidity to be 80%, controlling the nitrogen flow to be 2L/h (the anaerobic environment effect is better), taking out the culture dish together with the carbon electrode B after 48 hours, fully spraying 20% wt phosphoric acid solution into the carbon electrode and the culture dish, placing the culture dish with the carbon electrode B into a rotary disc type microwave reactor, setting the power to be 600W, and closing the culture dish after running for 180 seconds to obtain the modified carbon electrode C. The carbon electrode C was rinsed with a large amount of pure water and vacuum-dried at 50 ℃ for 6 hours to obtain a carbon electrode D. And (3) bonding the carbon electrode D to the smooth foam nickel coated with the graphite conductive adhesive, drying for 12 hours in vacuum at 50 ℃, and taking out after cooling to obtain the final product, namely the carbon electrode E.
The indexes of the product carbon electrode are as follows: the specific capacitance of 165F/g, the capacitance retention rate after 3000 times of charge and discharge is 96%.
Example 5
Grinding the dried active carbon, sieving with a 300-mesh sieve, and drying for later use. The soy protein powder is also dried and sieved through a 300 mesh sieve for later use. Mixing activated carbon with soybean protein powder, corn starch, acetylene black and polyvinylidene fluoride (PVDF) according to a mass ratio of 75: 5: 5: 10: 5 mixing, grinding for 3 hours by a ball mill, adding N-methyl pyrrolidone with the same mass as the mixture as a solvent, heating to 50 ℃, and stirring until the solvent is volatilized to form a viscous mixture A. Adding anhydrous ethanol with a mass of 2% of the solvent N-methyl pyrrolidone dropwise to obtain a mixture B, pressing the mixture B into a carbon electrode by a tablet press under 15MPa, and drying the carbon electrode in vacuum at 30 ℃ for 6 hours to obtain a carbon electrode A. And (3) taking compost fermentation compound bacteria liquid, diluting by 100 times according to the volume ratio, and completely immersing the carbon electrode A into the microbial inoculum solution for 4 hours to obtain the carbon electrode B. And (3) placing the carbon electrode B into a culture dish, placing the culture dish into a biological incubator, controlling the temperature to be 60 ℃, properly adjusting the pH value to be about 7, controlling the humidity to be 60%, and controlling the air flow to be 3L/h, taking out the carbon electrode B and the culture dish together after 24 hours, and spraying 30% wt phosphoric acid solution (which is sprayed on the electrode comprehensively) into the carbon electrode B and the culture dish. And then placing the culture dish provided with the carbon electrode B into a rotating disc type microwave reactor, setting the power to 600W, and closing after running for 5 minutes to obtain a modified carbon electrode C. The carbon electrode C was rinsed with a large amount of pure water and vacuum-dried at 50 ℃ for 6 hours to obtain a carbon electrode D. And (3) bonding the carbon electrode D to a flat copper foil coated with a copper conductive adhesive, drying in vacuum at 50 ℃ for 12 hours, and taking out after cooling to obtain the final product, namely the carbon electrode E.
The indexes of the product carbon electrode are as follows: the specific capacitance is 193.3F/g, and the capacitance retention rate is 96.9 percent after 3000 times of charge and discharge.
Comparative example
Grinding the dried active carbon, sieving with a 300-mesh sieve, and drying for later use. The soy protein powder is also dried and sieved through a 300 mesh sieve for later use. Mixing activated carbon, soybean protein powder, acetylene black and polyvinylidene fluoride (PVDF) according to a mass ratio of 75: 10: 10: 5, adding N-methyl pyrrolidone with the same mass as the mixture as a solvent, heating to 50 ℃, and stirring until the solvent is volatilized to form a viscous mixture A. And (3) dropwise adding absolute ethyl alcohol accounting for 2% of the mass of the solvent N-methyl pyrrolidone, pressing into a carbon electrode by a tablet press under 15MPa, drying in vacuum at 50 ℃ for 12 hours, cooling, and taking out to obtain the carbon electrode A. And (3) bonding the carbon electrode A to a flat graphite sheet coated with a graphite conductive adhesive, carrying out vacuum drying at 60 ℃ for 12 hours, and taking out after cooling to obtain a carbon electrode D.
The indexes of the product carbon electrode are as follows: the specific capacitance is 87.6F/g, and the capacitance retention rate is 83.9 percent after 10000 times of charge and discharge.
The above description is only an embodiment and a proportion of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present disclosure, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A preparation method of a modified carbon electrode combining biodegradation and microwave treatment is characterized by comprising the following steps:
(1) sieving the activated carbon with a 300-mesh sieve, and drying for later use; sieving the dried degradable biomass with a 300-mesh sieve for later use;
(2) weighing 80-85 parts of dried active carbon, 5-10 parts of degradable biomass, 5-10 parts of conductive agent and 5-10 parts of binder according to weight fraction, mixing, and grinding and mixing by using a ball mill;
(3) adding a proper amount of N-methyl pyrrolidone or absolute ethyl alcohol into the mixture prepared in the step (2), heating to 40-60 ℃, and stirring until a large amount of solvent is volatilized to obtain a viscous mixture A;
(4) dripping a small amount of absolute ethyl alcohol on the mixture A to obtain a mixture B;
(5) pressing the mixture B into a carbon electrode by using a tablet press under 15MPa, and performing vacuum drying for 4-8 hours at the temperature of 25-40 ℃ to obtain a carbon electrode A for later use;
(6) preparing a complex microbial inoculum solution with a certain concentration;
(7) completely dipping the carbon electrode A into the solution prepared in the step (6), controlling the temperature to be 25-35 ℃, and dipping for more than 2 hours to obtain a carbon electrode B;
(8) placing the carbon electrode B on a culture dish, placing the culture dish into a biological incubator, and simultaneously controlling the temperature, the humidity and the pH value in the incubator to be in proper ranges and maintaining the temperature, the humidity and the pH value for 12 to 36 hours;
(9) preparing an acidic solution, an alkaline solution or a metal halide solution with a certain concentration for later use;
(10) spraying any one of the solutions prepared in the step (9) or pure water on the carbon electrode B treated by the microorganisms in the step (8), then loading the carbon electrode B on a culture dish, and putting the culture dish into a microwave reactor;
(11) starting a microwave reactor to operate under certain power, and closing the microwave reactor after microwave modification for a period of time to obtain a carbon electrode C;
(12) washing the carbon electrode C with a large amount of pure water, and fully drying to obtain a carbon electrode D;
(13) and adhering the carbon electrode D to a flat current collecting plate coated with conductive adhesive, and fully drying to obtain a finished product modified carbon electrode E.
2. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 1, wherein: the degradable biomass in the steps (1) and (2) is protein powder or starch.
3. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 1, wherein: the conductive agent in the step (2) is any one of acetylene black, graphite powder, carbon nano tubes or graphene, and the binder is polytetrafluoroethylene or polyvinylidene fluoride.
4. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 4, wherein: the binder is fine powder with the particle size of 100 meshes.
5. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 1, wherein: the composite microbial inoculum in the step (6) can be a special composite microbial inoculum which is commercially available and is suitable for compost fermentation and breeding industry, nitrogen-fixing bacteria, phosphate-solubilizing bacteria, potassium-releasing bacteria and the like are required, the liquid composite microbial inoculum is diluted by 50-100 times according to the volume ratio, and the solid composite microbial inoculum is diluted by 1000-3000 times according to the mass ratio.
6. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 2, wherein: when the degradable biomass is protein powder, the temperature in the biological incubator in the step (8) is controlled at 70 ℃, the pH value is 7-8, the humidity is more than 50 percent, and a proper amount of oxygen is supplied.
7. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 2, wherein: when the degradable biomass is starch, the temperature in the biological incubator in the step (8) is controlled to be 40-50 ℃, the pH value is 7-8, the humidity is more than 50 percent, and oxygen supply is not needed.
8. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 1, wherein: the acidic solution in the step (9) is any one of inorganic acid and organic acid solutions such as nitric acid, phosphoric acid, sulfuric acid, hydrochloric acid, hydrogen peroxide solution, acetic acid, oxalic acid and the like, and the mass concentration range is 5-80%; the alkaline solution is any one of NaOH, KOH, FeSO4, MnSO4, AgNO3, Co + and the like, and the mass concentration is 5-60%; the metal halide solution refers to any one of solutions of zinc chloride, magnesium chloride, zinc bromide and the like, and the mass concentration of the metal halide solution is 5-60%.
9. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 1, wherein: the microwave reactor in the step (11) has the modification time of 0.5-60 minutes and the power of 100-3000W.
10. The method for preparing a biodegradable and microwave treatment combined modified carbon electrode as claimed in claim 1, wherein: the conductive adhesive in the step (13) is any one of carbon conductive adhesive, silver conductive adhesive, gold conductive adhesive or copper conductive adhesive, and the collector plate is a metal collector plate or a carbon collector plate.
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