CN104538632B - A kind of carbon composite electrode material and preparation method thereof - Google Patents
A kind of carbon composite electrode material and preparation method thereof Download PDFInfo
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- CN104538632B CN104538632B CN201510000462.8A CN201510000462A CN104538632B CN 104538632 B CN104538632 B CN 104538632B CN 201510000462 A CN201510000462 A CN 201510000462A CN 104538632 B CN104538632 B CN 104538632B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 49
- 239000007772 electrode material Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 43
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 27
- 244000046052 Phaseolus vulgaris Species 0.000 claims abstract description 21
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims abstract description 21
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 17
- 239000011230 binding agent Substances 0.000 claims abstract description 14
- 238000003763 carbonization Methods 0.000 claims abstract description 5
- 238000002604 ultrasonography Methods 0.000 claims abstract description 4
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 244000068988 Glycine max Species 0.000 claims description 19
- 235000010469 Glycine max Nutrition 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 12
- 239000000428 dust Substances 0.000 claims description 11
- 238000005516 engineering process Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 240000004713 Pisum sativum Species 0.000 claims description 4
- 235000010582 Pisum sativum Nutrition 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
- 240000004922 Vigna radiata Species 0.000 claims description 4
- 235000010721 Vigna radiata var radiata Nutrition 0.000 claims description 4
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 claims description 4
- 240000001417 Vigna umbellata Species 0.000 claims description 4
- 235000011453 Vigna umbellata Nutrition 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 229910003472 fullerene Inorganic materials 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 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
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical group OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 240000006677 Vicia faba Species 0.000 claims description 2
- 235000010749 Vicia faba Nutrition 0.000 claims description 2
- 235000002098 Vicia faba var. major Nutrition 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- PLMFYJJFUUUCRZ-UHFFFAOYSA-M decyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCC[N+](C)(C)C PLMFYJJFUUUCRZ-UHFFFAOYSA-M 0.000 claims 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 19
- 230000007613 environmental effect Effects 0.000 abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 239000002910 solid waste Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 239000002893 slag Substances 0.000 description 10
- 239000002028 Biomass Substances 0.000 description 7
- 230000001351 cycling effect Effects 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229940068984 polyvinyl alcohol Drugs 0.000 description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- LLYXJBROWQDVMI-UHFFFAOYSA-N 2-chloro-4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1Cl LLYXJBROWQDVMI-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/38—Carbon pastes or blends; Binders or additives therein
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention discloses a kind of carbon and its composite and its preparation method using bean dregs as carbon source, and carbon and its composite are used for into lithium ion battery and electrode material for super capacitor.Preparation method is as follows：Described carbon material solid waste common in life, is specifically to be used as carbon source using bean dregs.Bean dregs are immersed in dilute nitric acid solution; and tube furnace is put into after being cleaned through high frequency ultrasound; carbonization treatment is carried out under inert gas shielding, obtained bean dregs carbon last be sufficiently mixed with other carbon materials ball milling in the presence of binding agent of pulverizing obtains lithium ion battery and electrode material for super capacitor.The lithium ion battery and electrode material for super capacitor that the carbon and its composite of the present invention is made have more excellent performance than conventional carbon, and preparation method is simple and easy to apply, cost is low, environmental protection, has a good application prospect.
Description
Technical field
The present invention relates to electrode material manufacturing process technology field, lithium ion battery and super capacitor electrode are specifically related to
The preparation method of pole material.
Background technology
As greenhouse effects cause the lasting rising on sea level, attention rate more and more higher of the whole society to environment.It is same with this
When, expanding economy is increasing to the demand of the energy, and on the one hand the fossil energy such as traditional oil, coal, natural gas belongs to
In non-renewable resources, on the other hand, their use brings serious environmental problem, causes people urgently to need exploitation can
The renewable sources of energy, to meet economic, society and the sustainable development of environment.
Lithium ion battery is due to having the advantages that specific energy is big, operating voltage is high, safe, environmental pollution is small, each
The fields such as portable electric appts, electric automobile and new energy storage are planted to have a wide range of applications.In general, negative pole material
Expect the main body as lithium ion battery storage lithium, the insertion and abjection of lithium ion are realized in charge and discharge process, be to improve lithium ion
The key of the correlated performances such as the total specific capacity of battery, cyclicity, discharge and recharge.Current commercialized negative material mainly using graphite as
Main traditional carbon material, and the theoretical specific capacity of graphite only has 372 mAh/g, which greatly limits the total specific energy of lithium ion battery
Further raising.Therefore, Development of Novel has the negative material of height ratio capacity very urgent.
Ultracapacitor is a kind of new energy storage device, because its specific power is high, good cycle, can be used not only as calculating
The power power-supply of the back-up sources such as machine and various small electronic apparatus, can also be used as electric automobile with assembling lithium ion battery
Dynamic power system.Therefore ultracapacitor is also one of focus in mechanism of new electrochemical power sources research.At present, it is commercialized super
The carbon material of capacitor is mainly used as electrode material using activated carbon.Activated carbon has a high-specific surface area, higher conductance and
Good electrochemical stability.However, the Double-layer supercapacitors energy density by electrode material of activated carbon is relatively low, only
5Wh/kg or so.And electrode material determines the good and bad vital factor of performance of the supercapacitor, therefore we need to open
New electrode material is sent out and utilizes, so as to further improve the performance of ultracapacitor.
Biomass carbon source, including timber, shell, agricultural crop straw, bean dregs, oil cake etc., all it is solid common in living
Discarded object, is a kind of important regenerative resource, be readily obtained, cost it is low.Although these biomass resources enrich, due to protecting
That deposits and convert is backward in technique, causes biomass resource to waste serious, such as stalk agricultural wastes are burned in field, forestry production
Wood chip, sawdust that product processing is produced etc. is simply discarded, and shell, pericarp of food processing etc. are taken as garbage disposal, and this is not only
Environment is polluted, the huge waste of resource is also resulted in.At present, many countries all utilize biomass energy being actively researched and developed,
Because the charcoal prepared by raw material of biomass is pollution-free, high reserves, it is renewable the features such as, it has also become it is most potential
One of new material and new energy.If high property can be prepared using some cheap biomass as raw material, using the succinct technique of cleaning
The lithium ion battery of energy and the electrode material of ultracapacitor, are beneficial to the green production of battery industry, with important reality
With value and good application prospect, while the benign cycle that will promote human lives and the Nature, is conducive to ecological environment
Sustainable development.
The content of the invention
Good it is an object of the invention to provide a kind of chemical property, cost is low, and the bean dregs carbon of environmental protection both can be used for
Lithium ion battery negative material is also used as electrode material for super capacitor and preparation method thereof, so as to overcome in the prior art
The deficiency of presence.
In order to solve the above technical problems, technical scheme proposed by the present invention be a kind of carbon and composite electrode material and
Its preparation method, it is characterised in that：Bean dregs are immersed in dilute nitric acid solution, and cleaned through high frequency ultrasound, after then cleaning
Bean dregs be put into tube furnace, carbonization treatment is carried out under inert gas shielding, obtained bean dregs carbon pulverize it is last and other
Carbon material ball milling in the presence of binding agent, which is sufficiently mixed, obtains carbon composite.
In above-mentioned technical proposal, bean dregs are one kind in soya bean, green soya bean, mung bean, red bean, black soya bean, green soya bean, broad bean and pea
Or it is a variety of.
In above-mentioned technical proposal, electrode material is the electrode material of lithium ion battery negative material and ultracapacitor.
In above-mentioned technical proposal, bean dregs are impregnated with dust technology, and 0.5~20h of ultrasonic cleaning under 40~100KHz high frequencies.
In above-mentioned technical proposal, the bean dregs carbon dust after carbonization treatment is before other carbon material ball milling mixings first individually
1~20h of ball milling.
In above-mentioned technical proposal, other carbon materials are graphene, CNT, fullerene, carbon fiber, graphite, carbon black, second
One or more in acetylene black, its consumption is the 1~20% of bean dregs quality.
In above-mentioned technical proposal, other carbon materials of addition are first dissolved in 1~50ml mixed solutions of distilled water and alcohol,
The ratio of distilled water and alcohol is 1:1~1：20, and adding surfactant makes it be uniformly dispersed, then 0.5~24h of ultrasound.
In above-mentioned technical proposal, surfactant is lauryl sodium sulfate, cetyl trimethylammonium bromide, dodecane
One or more in base trimethylammonium bromide and the basic sodium sulfonate of dodecane.
In above-mentioned technical proposal, the binding agent of addition is in sucrose solution, glucose solution, polyethylene glycol, polyvinyl alcohol
One or more, its consumption is the 0.1~20% of bean dregs quality.
In above-mentioned technical proposal, ball milling mixing order is, first by the independent ball milling of bean dregs carbon, then to add other carbon materials
Ball milling, finally adds binding agent ball milling again.
Compared with prior art, the advantage of the invention is that：（1）The raw materials used present invention is that common biomass is discarded
Thing, wide material sources are cheap, and method for pyrolysis is simple, easy to operate.It may be seen that the carbon composite prepared by
In the addition of binding agent, the function served as bridge of two kinds of carbon materials of connection is not only acted as, while also logically with two kinds of carbon materials ingenious
The connection for crossing C-C keys forms three-dimensional network structure, and close uniform, and specific surface area is big, with porous channel structure, Ke Yiti
High embedding lithium capacity and charge-discharge performance.
（2）Prepare carbon and its composite is used as lithium ion battery negative material, capacity density is up to 600mAh/g
, coulomb efficiency high is circulated first up to 92%, and after circulation 100 weeks, capability retention is more than 90%；Super capacitor prepared therefrom
The characteristics of electrode material of device has big specific volume, good cycling stability, the specific volume in 0.5A/g is up to 340F/g, circulation
Specific capacity conservation rate after 10000 times is more than 94%.
Simply, easily operation, cost are relatively low for the preparation method technique of the present invention, to obtain the electrode material of above-mentioned function admirable
Material provides effective way.
Embodiment
The invention will be further described by the following examples.
Embodiment 1
The soybean residue impregnated with dust technology is cleaned by ultrasonic 2h under 50KHz high frequencies, is then placed in air dry oven and does
Dry 12h.Dried soybean residue is put into tube furnace again, under nitrogen protection 500 DEG C of burning 6h.The soybean residue carbon of gained is first single
Only ball milling 4h, adds ball milling 2h after graphene mixing, then adds 5% sucrose solution as binding agent ball milling 1h again, finally
The complete carbon composite of ball milling is cleaned by ultrasonic to liquid evaporation at 60 DEG C, obtained solid matter is ground to form with agate mortar
After powder, as lithium ion battery and electrode material for super capacitor.Wherein, the rotating speed of ball milling is 400r/min, and graphene exists
First in 10ml alcohol and the mixed solution of water before addition（Volume ratio is 1:1）In be uniformly dispersed.
After tested, the carbon composite of gained is used as electric discharge of the lithium ion battery negative material after first charge-discharge circulation
Specific capacity reaches 570mAh/g, and first charge-discharge efficiency is 88%, and after 500 times circulate, capability retention is 94.4%；By it
The characteristics of electrode material for super capacitor of preparation has big specific volume, good cycling stability, the specific volume in 0.5A/g is reachable
340F/g, the specific capacity conservation rate after circulating 10000 times is more than 95%.
Embodiment 2
The red bean slag impregnated with dust technology is cleaned by ultrasonic 4h under 60KHz high frequencies, is then placed in air dry oven and does
Dry 12h.Dried soybean residue is put into tube furnace again, under nitrogen protection 700 DEG C of burning 6h.The red bean slag carbon of gained is first single
Only ball milling 2h, adds ball milling 2h after CNT mixing, then adds 3% glucose solution as binding agent ball milling 1h again,
Finally the complete carbon composite of ball milling is cleaned by ultrasonic to liquid evaporation at 60 DEG C, obtained solid matter is ground with agate mortar
After claying into power, as lithium ion battery and electrode material for super capacitor.Wherein, the rotating speed of ball milling is 400r/min, and carbon is received
Mitron is before addition first in 10ml alcohol and the mixed solution of water（Volume ratio is 1:2）In be uniformly dispersed.
After tested, the carbon composite of gained is used as electric discharge of the lithium ion battery negative material after first charge-discharge circulation
Specific capacity reaches 600mAh/g, and first charge-discharge efficiency is 90%, and after 500 times circulate, capability retention is 95.2%；By it
The characteristics of electrode material for super capacitor of preparation has big specific volume, good cycling stability, the specific volume in 0.5A/g is reachable
420F/g, the specific capacity conservation rate after circulating 10000 times is more than 98%.
Embodiment 3
The mung bean slag impregnated with dust technology is cleaned by ultrasonic 6h under 50KHz high frequencies, is then placed in air dry oven and does
Dry 12h.Dried soybean residue is put into tube furnace again, under nitrogen protection 900 DEG C of burning 10h.The mung bean slag carbon of gained is first
Independent ball milling 3h, adds ball milling 2h after carbon black mixing, then adds 4% polyglycol solution as binding agent ball milling 1h again,
Finally the complete carbon composite of ball milling is cleaned by ultrasonic to liquid evaporation at 60 DEG C, obtained solid matter is ground with agate mortar
After claying into power, as lithium ion battery and electrode material for super capacitor.Wherein, the rotating speed of ball milling is 400r/min, carbon black
Before addition first in 10ml alcohol and the mixed solution of water（Volume ratio is 1:3）In be uniformly dispersed.
After tested, the carbon composite of gained is used as electric discharge of the lithium ion battery negative material after first charge-discharge circulation
Specific capacity reaches 520mAh/g, and first charge-discharge efficiency is 91.2%, and after 1000 times circulate, capability retention is 93.2%；
The characteristics of electrode material for super capacitor prepared therefrom has big specific volume, good cycling stability, the specific volume in 0.5A/g can
Up to 440F/g, the specific capacity conservation rate after circulating 10000 times is more than 95%.
Embodiment 4
The pea slag impregnated with dust technology is cleaned by ultrasonic 8h under 70KHz high frequencies, is then placed in air dry oven and does
Dry 12h.Dried soybean residue is put into tube furnace again, under nitrogen protection 900 DEG C of burning 10h.The pea slag carbon of gained is first
Independent ball milling 3h, adds ball milling 2h after fullerene mixing, then adds 8% poly-vinyl alcohol solution as binding agent ball milling again
The complete carbon composite of ball milling, is finally cleaned by ultrasonic to liquid evaporation, obtained solid matter is ground with agate by 1h at 60 DEG C
Alms bowl pulverize it is last, as lithium ion battery and electrode material for super capacitor.Wherein, the rotating speed of ball milling is 400r/min,
Fullerene is before addition first in 20ml alcohol and the mixed solution of water（Volume ratio is 1:4）In be uniformly dispersed.
After tested, the carbon composite of gained is used as electric discharge of the lithium ion battery negative material after first charge-discharge circulation
Specific capacity reaches 480mAh/g, and first charge-discharge efficiency is 93.2%, and after 1000 times circulate, capability retention is 94.2%；
The characteristics of electrode material for super capacitor prepared therefrom has big specific volume, good cycling stability, the specific volume in 0.5A/g can
Up to 450F/g, the specific capacity conservation rate after circulating 10000 times is more than 96%.
Embodiment 5
The black soya bean slag impregnated with dust technology is cleaned by ultrasonic 6h under 50KHz high frequencies, is then placed in air dry oven and does
Dry 12h.Dried soybean residue is put into tube furnace again, under nitrogen protection 1200 DEG C of burning 8h.The black soya bean slag carbon of gained is first
Independent ball milling 5h, adds ball milling 3h after graphene mixing, then adds 10% sucrose solution as binding agent ball milling 2h again,
Finally the complete carbon composite of ball milling is cleaned by ultrasonic to liquid evaporation at 60 DEG C, obtained solid matter is ground with agate mortar
After claying into power, as lithium ion battery and electrode material for super capacitor.Wherein, the rotating speed of ball milling is 400r/min, graphite
Alkene is before addition first in 10ml alcohol and the mixed solution of water（Volume ratio is 2:3）In be uniformly dispersed.
After tested, the carbon composite of gained is used as electric discharge of the lithium ion battery negative material after first charge-discharge circulation
Specific capacity reaches 510mAh/g, and first charge-discharge efficiency is 92.2%, and after 1000 times circulate, capability retention is 93.4%；
The characteristics of electrode material for super capacitor prepared therefrom has big specific volume, good cycling stability, the specific volume in 0.5A/g can
Up to 465F/g, the specific capacity conservation rate after circulating 10000 times is more than 97%.
Embodiment 6
The green soya bean slag impregnated with dust technology is cleaned by ultrasonic 4h under 80KHz high frequencies, is then placed in air dry oven and does
Dry 12h.Dried soybean residue is put into tube furnace again, under nitrogen protection 700 DEG C of burning 12h.The green soya bean slag carbon of gained is first
Independent ball milling 6h, adds ball milling 4h after acetylene black mixing, then adds 4% glucose solution as binding agent ball milling 4h again,
Finally the complete carbon composite of ball milling is cleaned by ultrasonic to liquid evaporation at 60 DEG C, obtained solid matter is ground with agate mortar
After claying into power, as lithium ion battery and electrode material for super capacitor.Wherein, the rotating speed of ball milling is 400r/min, acetylene
It is black first in 8ml alcohol and the mixed solution of water before addition（Volume ratio is 2:5）In be uniformly dispersed.
After tested, the carbon composite of gained is used as electric discharge of the lithium ion battery negative material after first charge-discharge circulation
Specific capacity reaches 530mAh/g, and first charge-discharge efficiency is 95.2%, and after 1000 times circulate, capability retention is 96.4%；
The characteristics of electrode material for super capacitor prepared therefrom has big specific volume, good cycling stability, the specific volume in 0.5A/g can
Up to 480F/g, the specific capacity conservation rate after circulating 10000 times is more than 96%.
Inventor states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, do not mean that the present invention has to rely on above-mentioned detailed
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (10)
1. a kind of carbon composite comprises the following steps as the preparation method of electrode material：(1) bean dregs are immersed in dust technology
In solution, and cleaned through high frequency ultrasound；(2) bean dregs after cleaning are put into tube furnace, be carbonized under inert gas shielding
Processing；(3) carbon material obtained is pulverized, and last ball milling is sufficiently mixed and obtained in the presence of binding agent with other carbon materials
Carbon composite.
2. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Electrode
Material is the electrode material of lithium ion battery negative material and ultracapacitor.
3. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Bean dregs
One or more in soya bean, green soya bean, mung bean, red bean, black soya bean, broad bean and pea.
4. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Bean dregs
Impregnated, and be cleaned by ultrasonic 0.5~20 hour under 40~100KHz high frequencies with dust technology.
5. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Carbonization
The temperature of processing is 400-1500 DEG C, and the time is 1-20 hours.
6. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Carbonization
Carbon dust after processing with other carbon material ball milling mixings before first independent ball milling 1~20 hour, then add other carbon
Material ball milling 0.5~10 hour again, finally adds binding agent ball milling 0.5~5 hour.
7. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Other
Carbon material is the one or more in graphene, fullerene, carbon fiber, graphite, carbon black, acetylene black, and its consumption is bean dregs quality
1~20%.
8. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Addition
Binding agent be sucrose solution, glucose solution, polyethylene glycol, polyvinyl alcohol in one or more, its consumption is bean dregs matter
The 0.1~20% of amount.
9. a kind of carbon composite according to claim 1 is used as the preparation method of electrode material, it is characterised in that：Addition
Other carbon materials be first dissolved in 1~50 milliliter of mixed solution of distilled water and alcohol, the ratio of distilled water and alcohol is 1:1~
1:20, and adding surfactant makes it be uniformly dispersed, it is then ultrasonic 0.5~24 hour.
10. a kind of carbon composite according to claim 9 is used as the preparation method of electrode material, it is characterised in that：Table
Face activating agent is lauryl sodium sulfate, cetyl trimethylammonium bromide, DTAB and dodecyl
One or more in benzene sulfonic acid sodium salt.
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| CN108862276A (en) * | 2018-06-29 | 2018-11-23 | 桑顿新能源科技有限公司 | A kind of preparation method and product of lithium ion battery biomass carbon negative electrode material |
| CN110797512B (en) * | 2018-08-02 | 2020-11-06 | 多氟多化工股份有限公司 | Silicon-carbon negative electrode material, lithium ion battery negative electrode and lithium ion battery |
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