CN108682566A - A kind of super capacitance cell special compound additive slurry and preparation method thereof - Google Patents
A kind of super capacitance cell special compound additive slurry and preparation method thereof Download PDFInfo
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- CN108682566A CN108682566A CN201810661796.3A CN201810661796A CN108682566A CN 108682566 A CN108682566 A CN 108682566A CN 201810661796 A CN201810661796 A CN 201810661796A CN 108682566 A CN108682566 A CN 108682566A
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- compound additive
- filter cake
- capacitance cell
- super capacitance
- special compound
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- 239000000654 additive Substances 0.000 title claims abstract description 62
- 230000000996 additive effect Effects 0.000 title claims abstract description 62
- 150000001875 compounds Chemical class 0.000 title claims abstract description 59
- 239000002002 slurry Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims description 9
- 238000007613 slurry method Methods 0.000 title description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 181
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 48
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 34
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 150000003839 salts Chemical class 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000003990 capacitor Substances 0.000 claims abstract description 11
- 239000012065 filter cake Substances 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 22
- 229910021645 metal ion Inorganic materials 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 17
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- -1 graphite alkene Chemical class 0.000 claims description 7
- 230000002687 intercalation Effects 0.000 claims description 7
- 238000009830 intercalation Methods 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 150000001621 bismuth Chemical class 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000004448 titration Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 2
- 239000002071 nanotube Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 238000004146 energy storage Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 239000011149 active material Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 14
- 238000012876 topography Methods 0.000 description 8
- 239000003610 charcoal Substances 0.000 description 6
- 210000003298 dental enamel Anatomy 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 229940068984 polyvinyl alcohol Drugs 0.000 description 5
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 150000001409 amidines Chemical group 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical class CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical class [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 1
- KKKAMDZVMJEEHQ-UHFFFAOYSA-N [Sn].[N+](=O)(O)[O-] Chemical compound [Sn].[N+](=O)(O)[O-] KKKAMDZVMJEEHQ-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007803 itching Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005486 organic electrolyte Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009736 wetting Methods 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
- H01G11/22—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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of super capacitance cell special compound additive slurries, belong to capacitor batteries field of material technology, consist of the following compositions：Carbon nanotube, metal salt, activated carbon, graphene oxide, reducing agent, surfactant and deionized water, the invention has the active material utilization for improving energy storage device, be conducive to accumulator play high-energy-density, specific power and long circulation life, stabilization performance the advantages of, realize the combination of battery and capacitive property.
Description
Technical field
The invention belongs to capacitor batteries field of material technology, and in particular to a kind of super capacitance cell special compound additive
Slurry and preparation method thereof.
Background technology
Super capacitance cell be it is a kind of gathered ultracapacitor, traditional storage battery (lead-acid battery, Ni-MH battery, lithium from
Sub- battery) performance in one new type of energy storage device, be mainly characterized by：1) power density is less than ultracapacitor, is more than
Conventional batteries；2) energy density is less than conventional batteries, is more than ultracapacitor；3) service life is less than ultracapacitor, is more than
Conventional batteries；4) internal resistance, leakage current are small, and low-temperature characteristics is excellent, environmentally protective etc..Super capacitance cell core is in battery
Positive and negative plate adds additive or compound additive with capacitive property, and for super capacitance cell, conventional additive is such as
Graphite, acetylene black, Ketjen black etc. and novel graphene, carbon nanotube, conductive black etc. make super capacitance cell power
The disadvantages such as density is low, electric conductivity is poor, dispersion performance is poor, specific capacitance is low, to cause super capacitance cell reduced service life.
Invention content
It is an object of the invention to be received using conventional additive, novel graphene, carbon for above-mentioned super capacitance cell
Mitron, conductive black cause the problem of super capacitance cell lost of life, and it is special multiple that the present invention provides a kind of super capacitance cell
Close additive slurry.
The technical solution of use is as follows：
A kind of super capacitance cell special compound additive slurry, consists of the following compositions：Carbon nanotube, metal salt, work
Property charcoal, graphene oxide, reducing agent, surfactant and deionized water.
Operation principle/advantageous effect of the present invention：Metal ion in metal salt is carried on the surface of activated carbon, enhancing
The hydrophilicity and proportion of activated carbon are easily combined with reducing agent under aqueous systems, and carbon nanotube is easily dispersed in the table of activated carbon
Carbon nanotube is wrapped in outside activated carbon by face, graphene oxide, is formed a large amount of middle micropore, is moved in middle micropore convenient for ion
It moves, more electrolyte can be adsorbed, enhance the immersional wetting of electrolyte and electrode material, reduce the concentration caused by exoelectrical reaction
Difference polarization；Specific capacity is big in organic electrolyte, is easily mixed with other electrode materials, the excellent in compatibility of electrode is formed, in electricity
Chi Zhongneng forms electric double layer, pseudo capacitance (fake capacitance) energy storage mechnism, improves the active material utilization of energy storage device, has
Conducive to accumulator play high-energy-density, specific power and long circulation life, stabilization performance the advantages of, realize battery and capacitive property
Combination.
Preferably, by following mass parts at being grouped as：By following mass parts at being grouped as：5-8 parts of carbon nanotubes,
84-86 parts of activated carbons, 4-6 parts of metal salts, 1-3 parts of graphene oxides, 1-3 parts of reducing agents, 1-3 parts of surfactants and 100-
120 parts of deionized waters.
Operation principle/advantageous effect of the present invention：The slurry that each component of above-mentioned mass parts is formed makes the ratio of activated carbon
Increase again, easily sink, easily mix to form mixture with other materials so that the aperture of slurry and Kong Rong reach maximum, are conducive to
The migration of ion, when reducing electric discharge, the ion concentration of electrolyte each section is poor, so that the performance of super capacitance cell is more
Stablize, life.
Preferably, it is 30-45nm, the carbon nanotube that length is 5-20 μm that the carbon nanotube, which selects wall thickness,.
Operation principle/advantageous effect of the present invention：The surface of activated carbon is easily dispersed in using the carbon nanotube of above-mentioned specification,
Can be formed after being coated by graphene oxide it is more in micropores, and middle micropore is the important channel of Ion transfer, so for from
The migration of son provides more channels, and is smoothly migrated convenient for ion, and concentration difference when electric discharge is avoided to polarize.
Preferably, the metal salt is any one of zinc salt, bismuth salt, lead salt and pink salt.
Operation principle/advantageous effect of the present invention：Metal ion in above-mentioned several metal salts is easily attached to activated carbon table
On face, the electric conductivity of activated carbon surface is helped to improve, reduces hydrogen-evolution overpotential, and makes the hydrophilicity enhancing of activated carbon,
It is dissolved in deionized water convenient for activated carbon.
Preferably, the color of the graphene oxide is brown color, and the graphene oxide uses " low-temperature oxidation intercalation "
It is prepared in conjunction with " stripping of machinery mill " method.
Operation principle/advantageous effect of the present invention：The graphene oxide prepared using the above method is at low cost, brown color
Graphene oxide quickly and can be coated securely by carbon nanotube to be formed in micropore.
Preferably, the reducing agent is any one of urea, thiocarbamide and hydrazine hydrate.
Operation principle/advantageous effect of the present invention：Contain in above-mentioned reducing agent there are two amidine functional group, one of them
Amidine functional group is combined with graphene oxide, another amidine functional group is combined with the metal ion of activated carbon surface so that oxygen
Graphite alkene is firmly adhered to the surface of activated carbon and is coated on carbon nanotube on activated carbon surface securely, forming quantity
The middle micropore that more and aperture is stablized.
Preferably, the surfactant is polyvinylpyrrolidone, dodecyl sodium sulfate, polyvinyl alcohol and 16
Any one of alkyl trimethyl ammonium bromide.
Operation principle/advantageous effect of the present invention：Above-mentioned several surfactants can effectively disperse activated carbon, carbon
Nanotube, graphene oxide, and residuals do not interfere with the electric conductivity of composite mortar after high temperature.
The present invention also provides a kind of preparation method of super capacitance cell special compound additive slurry, the technical sides of use
Case is as follows：
A kind of preparation method of super capacitance cell special compound additive slurry, includes the following steps：
A) carbon nanotube is cleaned with inorganic strong protonic acid, cabonic acid filter wash cake A is obtained by filtration；
B) activated carbon is added in ionized water and is dissolved, and reactant is cleaned to filtering repeatedly through overpickling and alkali cleaning successively
To Ph=7, filter cake B0 is obtained；
C) deionized water, filter cake B0 and weak oxidant are mixed, heating and stirring, heating rate are 5 DEG C/min~8
DEG C/min, temperature control is between 90 DEG C~100 DEG C, and stirring 4h~6h, cleans repeatedly to neutrality, filter cake is obtained by filtration after constant temperature
B1；
D) filter cake B1 is added in metal ion salt solution, is warming up to 45-55 DEG C, add appropriate potassium hydroxide, ammonium hydroxide,
And any one of ammonium bicarbonate carries out drop reaction, as PH=8.2-8.8, stops titration and stirring 2.5h~3.5h, centrifugation
Water is gone to obtain filter cake B2；
E) in oxygen-free environment, filter cake B2 is heated, heating rate is 15 DEG C/min, and thermostat temperature is 300 DEG C, constant temperature oxygen
The change reaction time is 4h, obtains filter cake B3；
F) filter cake B3 carries out the secondary load of metal ion：Filter cake B3 is added in metal ion salt solution, after stirring 1h,
Sodium sulphate is added, stirs 2.5h, water is removed in centrifugation and cleaning filter cake to filtrate is in neutrality；Filter cake is dried, drying temperature is
85 DEG C~90 DEG C, drying time is for 24 hours~26h, obtains modified high reference area activated carbon B；
G) graphene oxide is fully dispersed at graphene oxide slurry in disperse systems；
H) oxidation stone is added in cabonic acid filter wash cake A, modified high reference area activated carbon B and deionized water
Black alkene slurry agitation uniformly obtains mixture, is 80 according to mass ratio:1 mixture and reducing agent, is obtained by filtration filter after milling
Cake C；
I) in inert gas environment, filter cake C is freezed in the case where temperature is less than 5%, vacuum condition less than -45 DEG C, humidity
Dry 36-48h, obtains compound additive presoma；
J) in inert gas environment, by compound additive presoma light microwave deoxidation treatment 8-15min, super electricity is obtained
Hold battery special compound additive powder；
K) in inert gas environment, super capacitance cell special compound additive powder is added in ionized water, and is added
Enter surfactant, mills and super capacitance cell special compound additive slurry is obtained by filtration in 300 mesh screens.
Operation principle/advantageous effect of the present invention：Carbon nanotube is cleaned with inorganic strong protonic acid, for reducing carbon nanotube
The content of the foreign metal on surface, such as iron ion, copper ion；Pickling and alkali cleaning activated carbon are the portions for removing activated carbon surface
Divide metal impurities, is conducive to the surface that later stage metal ion is attached to activated carbon；It will filter by the way of weak oxidant and heating
Lower valency metal ion in cake B0 is oxidized to the metal ion of high-valence state and so that metal ion is dissolved in deionized water, into one
Step removes part metals impurity and is titrated with alkali by filter cake B1 in metal ion salt solution so that metal ion is attached to
The surface of activated carbon, obtains modified high reference area activated carbon B, modified high reference area activity made from which
Charcoal B performances are stablized, and are scattered in modified high reference area activated carbon B's convenient for the attachment of graphene oxide and carbon nanotube
On surface；The processing that processing graphene oxide is carried out in inert gas environment, avoids graphene oxide by the oxygen in air
Oxidation influence slurry electric conductivity, light microwave deoxidation treatment have shock effect and be capable of providing enough energy make it is compound
Disengaging of itching in additive presoma, to obtain super capacitance cell special compound additive powder；Ionized water or N- methyl
Pyrrolidones and surfactant can come powder is fully dispersed, form the good slurry of electric conductivity.
Preferably, inorganic strong protonic acid described in step a) is any one of nitric acid, phosphoric acid and sulfuric acid, a concentration of
Weak oxidant in 0.1mol/L~0.5mol/L, step c) is one kind in sulphur or iodine.
Operation principle/advantageous effect of the present invention：Nitric acid, phosphoric acid and sulfuric acid are strong acid and can ionize completely, energy
It is enough to remove the metal impurities adhered in carbon nanotube as much as possible.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1. by the quantity of micropore in increase, to increase the channel of Ion transfer, caused by when reducing battery discharge
Concentration of electrolyte is poor, to extend the service life of capacitor batteries, is conducive to accumulator and plays high-energy-density, specific power and length
The advantages of cycle life, performance of stabilization, realizes the combination of battery and capacitive property.
2. in inert gas to graphene oxide and the material containing graphene oxide processing, avoid graphite oxide
Alkene is caused to attach to the reduced performance on activated carbon by the dioxygen oxidation in air, to the few middle micropore of forming quantity, shadow
Ring the conductivity of super capacitance cell.
3. smooth microwave deoxidation treatment enables to the oxygen in compound additive presoma can be completely out, slurry is avoided to exist
During use, by oxidation and in making, the quantity of micropore is reduced graphene oxide therein, influences super capacitance cell
Electric conductivity.
Description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein：
Fig. 1 is the surface topography map of reaction product in step (2) in embodiment five；
Fig. 2 is the surface topography map of step (5) high temperature treated substance in embodiment five；
Fig. 3 is the surface topography map in step (6) after secondary load in embodiment five；
Fig. 4 is the surface topography map of compound additive presoma in embodiment five；
Fig. 5 is the surface topography map of super capacitance cell special compound additive powder in embodiment five；
Fig. 6 is high reference area activated carbon in embodiment five, compound additive and modified high-specific surface area activity
The time of charcoal and voltage pattern；
Fig. 7 is high reference area activated carbon in embodiment five, compound additive and modified high-specific surface area activity
The recycling number of charcoal and specific volume spirogram；
Fig. 8 is high reference area activated carbon in embodiment five, compound additive and modified high-specific surface area activity
The volt-ampere Tequ line chart of charcoal；
Fig. 9 is impedance real part and imaginary impedance figure；
Figure 10 is the enlarged drawing in the regions K in Fig. 9.
Specific implementation mode
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
The technical scheme is that：A kind of super capacitance cell special compound additive slurry, consists of the following compositions：
Carbon nanotube, metal salt, activated carbon, graphene oxide, reducing agent, surfactant and deionized water.
Preferably, by following mass parts at being grouped as：By following mass parts at being grouped as：5-8 parts of carbon nanotubes,
84-86 parts of activated carbons, 4-6 parts of metal salts, 1-3 parts of graphene oxides, 1-3 parts of reducing agents, 1-3 parts of surfactants and 100-
120 parts of deionized waters.
Preferably, it is 30-45nm, the carbon nanotube that length is 5-20 μm that the carbon nanotube, which selects wall thickness,.
Preferably, the metal salt is any one of zinc salt, bismuth salt, lead salt and pink salt.
Preferably, the color of the graphene oxide is brown color, and the graphene oxide uses " low-temperature oxidation intercalation "
It is prepared in conjunction with " stripping of machinery mill " method.
Preferably, the reducing agent is any one of urea, thiocarbamide and hydrazine hydrate.
Preferably, the surfactant is polyvinylpyrrolidone, dodecyl sodium sulfate, polyvinyl alcohol and 16
Any one of alkyl trimethyl ammonium bromide.
It is described in detail with reference to specific embodiment.
Embodiment one
A kind of super capacitance cell special compound additive slurry, consists of the following compositions：Wall thickness is 30-45nm, length
For 5-20 μm of carbon nanotube；Metal salt selects the lead salt of tetravalence, and it is 2150m that activated carbon, which selects specific surface,2/ g~2250m2/ g,
Proportion is 0.35g/cm2~0.5g/cm2, Kong Rongwei 0.3cm3/ g~5cm3/ g, aperture are 3nm~5nm, and grain size (D50) is 15 μ
The high reference area activated carbon of m~25 μm, graphene oxide are prepared using " low-temperature oxidation intercalation " combination " stripping of machinery mill " method
The graphene oxide of the brown color no more than 6 hours gone out, reducing agent select thiocarbamide, surfactant to select polyvinyl alcohol, go
Ionized water.
Embodiment two
A kind of super capacitance cell special compound additive slurry, by following mass parts at being grouped as：8 parts of carbon nanometers
Pipe, 86 parts of activated carbons, 6 parts of metal salts, 3 parts of graphene oxides, 3 parts of reducing agents, 3 parts of surfactants and 120 parts of deionizations
Water, the carbon nanotube select wall thickness for 30-45nm, and the carbon nanotube that length is 5-20 μm, metal salt selects the bismuth salt of tetravalence,
The brown color for being no more than 6 hours that the graphene oxide is prepared using " low-temperature oxidation intercalation " combination " stripping of machinery mill " method
Graphene oxide, reducing agent select urea, surfactant select dodecyl sodium sulfate.
Embodiment three
A kind of super capacitance cell special compound additive slurry, by following mass parts at being grouped as：5 parts of carbon nanometers
Pipe, 84 parts of activated carbons, 4 parts of metal salts, 1 part of graphene oxide, 1 part of reducing agent, 1 part of surfactant and 100 parts of deionizations
Water；Selection wall thickness is 30-45nm, the carbon nanotube that length is 5-20 μm；Metal salt selects the pink salt of tetravalence, graphene oxide to adopt
With the graphene oxide for the brown color no more than 6 hours that " low-temperature oxidation intercalation " combination " stripping of machinery mill " method is prepared, go back
Former agent selects hydrazine hydrate, surfactant to select cetyl trimethylammonium bromide.
Example IV
A kind of super capacitance cell special compound additive slurry, by following mass parts at being grouped as：7 parts of carbon nanometers
Pipe, 85 parts of activated carbons, 5 parts of metal salts, 2 parts of graphene oxides, 2 parts of reducing agents, 2 parts of surfactants and 110 parts of deionizations
Water；Selection wall thickness is 30-45nm, the carbon nanotube that length is 5-20 μm；Metal salt select the zinc salt of tetravalence, bismuth salt, lead salt with
And the mixture of pink salt composition, graphene oxide are not surpassed using what " low-temperature oxidation intercalation " combination " stripping of machinery mill " method was prepared
The graphene oxide of 6 hours brown colors is crossed, reducing agent selects hydrazine hydrate, surfactant to select polyvinylpyrrolidone.
The technical scheme is that：A kind of preparation method of super capacitance cell special compound additive slurry, including
Following steps：
A) carbon nanotube is cleaned with inorganic strong protonic acid, cabonic acid filter wash cake A is obtained by filtration；
B) activated carbon is added in ionized water and is dissolved, and reactant is cleaned to filtering repeatedly through overpickling and alkali cleaning successively
To Ph=7, filter cake B0 is obtained；
C) deionized water, filter cake B0 and weak oxidant are mixed, heating and stirring, heating rate are 5 DEG C/min~8
DEG C/min, temperature control is between 90 DEG C~100 DEG C, and stirring 4h~6h, cleans repeatedly to neutrality, filter cake is obtained by filtration after constant temperature
B1；
D) filter cake B1 is added in metal ion salt solution, is warming up to 45-55 DEG C, add appropriate potassium hydroxide, ammonium hydroxide,
And any one of ammonium bicarbonate carries out drop reaction, as PH=8.2-8.8, stops titration and stirring 2.5h~3.5h, centrifugation
Water is gone to obtain filter cake B2；
E) in oxygen-free environment, filter cake B2 is heated, heating rate is 15 DEG C/min, and thermostat temperature is 300 DEG C, constant temperature oxygen
The change reaction time is 4h, obtains filter cake B3；
F) filter cake B3 carries out the secondary load of metal ion：Filter cake B3 is added in metal ion salt solution, after stirring 1h,
Sodium sulphate is added, stirs 2.5h, water is removed in centrifugation and cleaning filter cake to filtrate is in neutrality；Filter cake is dried, drying temperature is
85 DEG C~90 DEG C, drying time is for 24 hours~26h, obtains modified high reference area activated carbon B；
G) graphene oxide is fully dispersed at graphene oxide slurry in disperse systems；
H) graphene oxide slurry is added in cabonic acid filter wash cake A and modified high reference area activated carbon B to stir
It mixes and uniformly obtains mixture, be 80 according to mass ratio:1 mixture and reducing agent, is obtained by filtration filter cake C after milling；
I) in inert gas environment, filter cake C is freezed in the case where temperature is less than 5%, vacuum condition less than -45 DEG C, humidity
Dry 36-48h, obtains compound additive presoma；
J) in inert gas environment, by compound additive presoma light microwave deoxidation treatment 8-15min, super electricity is obtained
Hold battery special compound additive powder；
K) in inert gas environment, super capacitance cell special compound additive powder is added in ionized water, and is added
Enter surfactant, mills and super capacitance cell special compound additive slurry is obtained by filtration in 300 mesh screens.
It is described in detail with reference to specific embodiment and attached drawing.
Embodiment five
(1) 9.62kg carbon nanotubes, 0.38kg nitric acid, 200kg deionized water machineries are weighed in 500L glass reaction kettles
1h is stirred, mixture is transferred in 500L ultrasonic stirrers, ultrasonic disperse 2h, ultrasonic power 1.0kw, rotating speed 200r/ are set
Carbon nanotube filter cake is obtained by filtration in min.
(2) pickling and alkali cleaning：It weighs 100kg active carbon with high specific surface area and is added to 1.5m3In enamel reaction still, it is added
0.9t deionized waters stir 30min, are slowly added to a concentration of 0.1mol/L~3mol/L nitric acid of 45kg~50kg, solid-liquid quality
Than being 1:5~20,2h~3h is stirred, reactant is cleaned to filtrate repeatedly in plate and frame filter press and is in neutrality；Add in filter cake
Enter the potassium hydroxide of 100Kg, solid-liquid mass ratio 1:5~20,2h~3h is stirred, reactant is repeatedly clear in plate and frame filter press
Filtrate is washed till to be in neutrality.
(3) it is surface-treated：Product in (2) is added in the enamel reaction still with heating device, be added 0.8t go from
Sub- water, then be added 100Kg iodine, heating, heating rate be 5 DEG C/min~8 DEG C/min, temperature control 90 DEG C~100 DEG C it
Between, 4h~6h is stirred after constant temperature, and above-mentioned reactant is cleaned to filtrate repeatedly in plate and frame filter press and is in neutrality；Reaction product
Surface topography map is as shown in Figure 1, charcoal material surface hole after treatment is clear.
(4) load of oxygen metal compound：In 1.5m30.9t deionized waters are added in enamel reaction still, 2.5Kg is added
Bismuth nitrate stirs to being completely dissolved, reactant in (3) is added in above-mentioned enamel reaction still, stirs 0.5h~1.5h；It measures
The concentrated ammonia liquor that 7.5Kg mass fractions are 25% is slowly added in above-mentioned enamel reaction still, after addition, is stirred 3h, is then used
Centrifuge goes to remove water, and product is dried to moisture under the conditions of 90 DEG C and is less than 5% by obtained filter cake；Load percentage control 0.5%
Between~15%, the pH value of reaction system controls between 8.3~8.5, and solid-liquid mass ratio is controlled 1:Between 5~20；
(5) high-temperature oxydation, by (4) load desciccate be put into the resistance furnace of nitrogen protection, heating rate be 15 DEG C/
Min, thermostat temperature are 300 DEG C, and the constant temperature oxidation reaction time is 4h；Surface topography map after high temperature oxidation process as shown in Fig. 2,
It can be seen that the square metal oxide after high temperature sintering is scattered on activated carbon surface by the figure；
(6) 0.9t deionized waters are added in the secondary load of oxygen metal compound in enamel reaction still, and bismuth nitrate is added
36Kg, nitric acid tin 42Kg, 5% polyethylene glycol-400 solution 20Kg, stirring is to being completely dissolved；Step (5) is added, and treated
Product after stirring 1h, weighs sodium sulphate 56.5Kg, stirs 2.5h, remove moisture removal with plate and frame filter press and clean filter cake to filtrate
It is in neutrality；Filter cake is dried, drying temperature is 85 DEG C~90 DEG C, and drying time is for 24 hours~26h, obtains modified height
Reference area activated carbon；The specific surface area of this modified high reference area activated carbon is 1500m2/ g~1800m2/ g, proportion are
0.75g/cm2~0.9g/cm2, Kong Rongwei 0.3cm3/ g~1cm3/ g, aperture are 3nm~8nm, and grain size is 32 μm~68 μm, gold
It is 3%~15% to belong to compounds content；The surface topography map of modified high reference area activated carbon is as shown in figure 3, can by figure
To find out that metallic compound in the form of sheets, is uniformly supported on active carbon material surface；
(7) in helium environment, 33.2kg graphene oxides and 20kg deionized waters no more than 6 hours will be prepared
It is mixed and stirred for being formed uniformly graphene oxide slurry.
(8) prepared by compound additive presoma：In helium environment, by carbon nanotube filter cake 15.60kg, modified height
Reference area activated carbon 182.7kg, graphene oxide slurry 53.2kg, deionized water 250kg and 50kg urea are put into and carry
In the mechanical agitator tank of Vltrasonic device, first mechanical agitation 1h is then turned on ultrasound, and ultrasonic power is set as 1.0kw, ultrasonic agitation
4h；Obtained reactant is directly transferred in cold dry equipment, cryogenic vacuum is freeze-dried 48h, before obtaining puffy composite material
Drive body；As shown in figure 4, the surface of compound additive presoma is fluffy as seen from the figure, it is similar to aeroge.
(9) composite material precursor that step (8) obtains is put into duct type continuous tunnel furnace and uses light microwave irradiation, helium
Under protective condition, irradiation time 2h obtains super capacitance cell special compound additive powder, as shown in figure 5, can be with by figure
Find out that the surface of the super capacitance cell special compound additive powder is fluffy.
(10) preparation of slurry：69.5Kg deionized waters are weighed in being stirred under vacuum tank, are slowly added to 800g polyvinyl alcohol,
4h is stirred under vacuum, is configured to the poly-vinyl alcohol solution that mass fraction is 0.5%, the super capacitor that will be obtained in (9)
Battery special compound additive powder is added high speed mixer high speed and mixes 2h~3h；It is then added to be stirred under vacuum in tank and stir
2h~3h is transferred in ball mill ball milling 2h~3h and that super capacitance cell is obtained by filtration by 300 mesh flame filter presses is special multiple
Close additive slurry.
It is respectively adopted in the capacitor batteries of the active carbon with high specific surface area for not making any processing in step (2), step (6)
The super capacitance cell of compound additive in the capacitor batteries and step (9) of the modified active carbon with high specific surface area arrived
Performance is as shown in Fig. 6 to Figure 10, it will be appreciated from fig. 6 that the super capacitor of the capacitor batteries of active carbon with high specific surface area, compound additive
Battery, modified active carbon with high specific surface area capacitor batteries first charge-discharge capacity be respectively 114,140.67,91.33F/
g；As shown in Figure 7, with the increase for recycling number, using the decline of the specific capacity of the super capacitance cell of compound additive
The slow and initial specific capacity of speed is all higher than the specific capacity of the capacitor batteries using active carbon with high specific surface area；As shown in Figure 8,
The CV curves of compound additive are rectangular, and in the case of same current, specific capacity is apparently higher than the capacitance of active carbon with high specific surface area
The electrochemistry capacitance of battery and modified active carbon with high specific surface area illustrates that the performance of its charge and discharge process is stablized；By Fig. 9
It is found that the intrinsic resistance using the super capacitance cell after compound additive does not greatly improve.In conclusion adding from compound
From the point of view of the super capacitance cell cyclic voltammetric and electrochemical impedance that add agent, compound additive shows excellent capacitive property.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (9)
1. a kind of super capacitance cell special compound additive slurry, which is characterized in that consist of the following compositions：Carbon nanotube,
Metal salt, activated carbon, graphene oxide, reducing agent, surfactant and deionized water.
2. a kind of super capacitance cell special compound additive slurry according to claim 1, which is characterized in that by following
Mass parts at being grouped as：5-8 parts of carbon nanotubes, 84-86 parts of activated carbons, 4-6 parts of metal salts, 1-3 parts of graphene oxides, 1-3
Part reducing agent, 1-3 parts of surfactants and 100-120 parts of deionized waters.
3. a kind of super capacitance cell special compound additive slurry according to claim 1, which is characterized in that the carbon
It is 30-45nm, the carbon nanotube that length is 5-20 μm that nanotube, which selects wall thickness,.
4. a kind of super capacitance cell special compound additive slurry according to claim 1, which is characterized in that the gold
Category salt is any one of zinc salt, bismuth salt, lead salt and pink salt.
5. a kind of super capacitance cell special compound additive slurry according to claim 1, which is characterized in that the oxygen
The color of graphite alkene is brown color, and the graphene oxide is using " low-temperature oxidation intercalation " combination " stripping of machinery mill " method system
It is standby.
6. a kind of super capacitance cell special compound additive slurry according to claim 1, which is characterized in that described to go back
Former agent is any one of urea, thiocarbamide and hydrazine hydrate.
7. a kind of super capacitance cell special compound additive slurry according to claim 1, which is characterized in that the table
Face activating agent is in polyvinylpyrrolidone, dodecyl sodium sulfate, polyvinyl alcohol and cetyl trimethylammonium bromide
It is any.
8. a kind of preparation method of super capacitance cell special compound additive slurry, which is characterized in that include the following steps：
A) carbon nanotube is cleaned with inorganic strong protonic acid, cabonic acid filter wash cake A is obtained by filtration；
B) activated carbon is added in ionized water and is dissolved, and successively through overpickling and alkali cleaning, reactant is cleaned to filtering repeatedly to Ph
=7, obtain filter cake B0；
C) by deionized water, filter cake B0 and weak oxidant mix, heating and stir, heating rate be 5 DEG C/min~8 DEG C/
Min, temperature control between 90 DEG C~100 DEG C, and 4h~6h is stirred after constant temperature, is cleaned repeatedly to neutrality, filter cake B1 is obtained by filtration；
D) filter cake B1 is added in metal ion salt solution, is warming up to 45-55 DEG C, add appropriate potassium hydroxide, ammonium hydroxide and
Any one of ammonium bicarbonate carries out drop reaction, as PH=8.2-8.8, stops titration and water is removed in stirring 2.5h~3.5h, centrifugation
Obtain filter cake B2；
E) in oxygen-free environment, filter cake B2 is heated, heating rate is 15 DEG C/min, and thermostat temperature is 300 DEG C, and constant temperature oxidation is anti-
It is 4h between seasonable, obtains filter cake B3；
F) filter cake B3 carries out the secondary load of metal ion：Filter cake B3 is added in metal ion salt solution, after stirring 1h, is added
Sodium sulphate stirs 2.5h, and water is removed in centrifugation and cleaning filter cake to filtrate is in neutrality；Filter cake is dried, drying temperature is 85 DEG C
~90 DEG C, drying time is for 24 hours~26h, obtains modified high reference area activated carbon B；
G) graphene oxide is fully dispersed at graphene oxide slurry in disperse systems；
H) graphene oxide is added in cabonic acid filter wash cake A, modified high reference area activated carbon B and deionized water
Slurry agitation uniformly obtains mixture, is 80 according to mass ratio:1 mixture and reducing agent, is obtained by filtration filter cake C after milling；
I) in inert gas environment, filter cake C is freeze-dried in the case where temperature is less than 5%, vacuum condition less than -45 DEG C, humidity
36-48h obtains compound additive presoma；
J) in inert gas environment, by compound additive presoma light microwave deoxidation treatment 8-15min, super capacitor electricity is obtained
Pond special compound additive powder；
K) in inert gas environment, super capacitance cell special compound additive powder is added in ionized water, and table is added
Face activating agent, mills and super capacitance cell special compound additive slurry is obtained by filtration in 300 mesh screens.
9. a kind of preparation method of super capacitance cell special compound additive slurry according to claim 1, feature
It is, inorganic strong protonic acid described in step a) is any one of nitric acid, phosphoric acid and sulfuric acid, a concentration of 0.1mol/L~
Weak oxidant in 0.5mol/L, step c) is one kind in sulphur or iodine.
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