CN104692359A - Porous carbon with part of graphene and preparation method of porous carbon - Google Patents
Porous carbon with part of graphene and preparation method of porous carbon Download PDFInfo
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- CN104692359A CN104692359A CN201510092424.XA CN201510092424A CN104692359A CN 104692359 A CN104692359 A CN 104692359A CN 201510092424 A CN201510092424 A CN 201510092424A CN 104692359 A CN104692359 A CN 104692359A
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Abstract
The invention discloses porous carbon with part of graphene. The porous carbon structurally comprises an irregular-layer graphite micro crystal and few-layer graphene which is uniformly dispersed on the surface of the graphite microcrystal. The graphene is uniformly dispersed on the structural surface of microcrystal carbon, so that the conductivity and the specific discharge capacity of the material are greatly improved. Compared with a method for independently producing graphene, a preparation method of the porous carbon with part of graphene has the advantage that the cost is greatly reduced; compared with the active carbon applied to super capacitors in the market, the porous carbon has the obvious performance advantages.
Description
Technical field
A kind of part graphite of the present invention alkylene porous charcoal and preparation method thereof, belongs to field of charcoal material, especially relates to a kind of working method of Carbon Materials.
Background technology
Carbon, one of element abundant on the earth, has multiple allotropic substance.According to the difference of hybridized orbital, carbon homojunction crystalline state can be divided into the Linear Carbon of the graphite of the diamond of SP3 hydridization, SP2 hydridization, Graphene, carbon nanotube, soccerballene and SP hydridization.Gac, from microtexture, gac is made up of the turbostratic of graphite microcrystal body and decolorizing carbon with graphite SP2 hydridization, and turbostratic makes gac have very large specific surface area, and the π key that SP2 is formed makes gac have good electroconductibility.The existence form that the another kind of carbon is important is crystallite charcoal, is the structure of short range order longrange disorder.
Because stability is high, electric conductivity is high and density is little etc., characteristic has a wide range of applications Carbon Materials in electrochemical energy storage device.
In double layer capacitor, lithium-ion capacitor and other electrochemical energy storage devices, the Carbon Materials gac with vesicular structure is as electrode active material commercial applications widely.Current energy storage device Activated Carbon Production producer mainly contains Kuraray, the Wu Yu chemistry of Japan, and the EnerG2 of the U.S., the Jacobi of Sweden, the conjunction of China reaches the producers such as charcoal element, Fu Laisen, Hua County gac.Wherein Kuraray company is good due to stability of material, occupies most of market share.But at present activated carbon electrodes is in specific conductivity, but its specific discharge capacity only has in 110-120 F/g energy density and need to improve.
Crystallite charcoal or be called that nanometer door charcoal has unique structure, a kind of special gac can be thought, compared with conventional carbon, it has relatively low specific surface area, and the d002 interlamellar spacing of graphite microcrystal is approximately between 0.365-0.085nm, is greater than the 0.335nm of conventional graphite, thus there is the characteristic of " electrochemical activation ", namely, in electrolytic solution under high voltages, electrolytic solution solute ions and solvent can be embedded into the interlayer of graphite microcrystal, thus have the characteristic of heavy body.
Graphene has higher specific surface area and high specific conductivity because of it, and therefore as having the character more excellent than conventional porous carbon material during capacitor material, but Graphene is expensive, can't be applied in the middle of super capacitor material completely at present.There are hexa-atomic element, the organic institute in Chinese Academy of Sciences Chengdu, Nanjing Xian Feng nano material etc. in the domestic producer that can manufacture Graphene at present, but because the production technique of energy storage material Graphene also has bottleneck, more Graphene application is in fields such as thin-film material, optical material, coating.
The electrode having research to attempt gac to mix with Graphene compound to be used for ultracapacitor, certain lifting is served really to the performance of ultracapacitor, but the dispersiveness of Graphene and cost are still the reason of its large-scale application of restriction, and short-term is difficult to universal.
Summary of the invention
The object of the invention is the Carbon Materials inferior position on cost and performance for current energy storage field especially electrostatic double layer energy storage field, the present invention proposes a kind of specific conductivity of material and mass ratio significantly improves, lower-cost part graphite alkylene porous charcoal and this part graphite alkylene porous charcoal preparation method.
The present invention for achieving the above object, adopts following technical scheme:
A kind of part graphite alkylene porous charcoal, is characterized in that: its structure comprises the graphite microcrystal of random layer and is scattered in homodisperse few layer graphene on graphite microcrystal surface.
It is further characterized in that: described porous charcoal specific surface area is 50-3500m
2/ g.
The common graphite crystallite of the graphite microcrystal of described random layer to be d002 interlamellar spacing be 0.335nm, or d002 interlamellar spacing is the large interlamellar spacing graphite microcrystal of 0.365-0.385nm.
The preparation method of above-mentioned part graphite alkylene porous charcoal, comprises the steps:
(1) precursor power: carbonized by carbon feedstock, or/and reactivate forms the graphite microcrystal of random layer;
(2) part graphite alkylene: carry out part graphite alkylene to presoma, or/and reactivate forming section graphite alkylene porous charcoal;
(3) part graphite alkylene porous charcoal is cleaned, purifying, complete preparation.
A kind of preferred mode: first carry out activation to the material after charing and form crystallite charcoal, then carry out part graphite alkylene formation graphite alkylene porous charcoal porous charcoal, finally carries out cleaning, purifying, completes preparation.
Another kind of preferred mode: first carry out part graphite alkylene to the material after charing, then carry out activation forming section graphite alkylene porous charcoal, finally carries out cleaning, purifying, completes preparation.
Another preferred mode: first carry out pre-activate to the material of charing, then carry out part graphite alkylene and obtain surface for the pre-activate charcoal of graphene oxide layer, more again activate, finally carries out cleaning, purifying, completes preparation.
Above-mentioned carbon feedstock is resol, xylogen, organism fiber or refinery coke.
It is further characterized in that: described part graphite olefination procedure is electrochemical intercalation, solvent-thermal method or chemistry redox method.
A kind of part graphite of the present invention alkylene porous charcoal, its structure comprises the graphite microcrystal of random layer and is scattered in homodisperse few layer graphene on graphite microcrystal surface.Because graphene uniform is scattered in the body structure surface of crystallite charcoal, the specific conductivity of material and specific discharge capacity have had and have significantly improved.A preparation method for part graphite alkylene porous charcoal, and produces separately compared with Graphene, and cost significantly reduces.Compared with the activated carbon for super capacitors on market, there is obvious performance advantage.
Embodiment
A preparation method for part graphite alkylene porous charcoal, first carbonizes carbon feedstock, then carries out activating the graphite microcrystal forming random layer; Part graphite alkylene is carried out to the graphite microcrystal of random layer, forming section graphite alkylene porous charcoal; Part graphite alkylene porous charcoal is cleaned, purifying, complete preparation.Final finished structure is the graphite microcrystal of random layer and is scattered in homodisperse few layer graphene on graphite microcrystal surface.
The preparation process of a kind of part graphite of the present invention alkylene porous charcoal is further illustrated below by embodiment.
Embodiment 1:
1. be presoma with resol, carry out under nitrogen hydrogen mixeding gas (N2:H2=95:5) protection, carbonization temperature 550 degrees Celsius, carbonization time 5 hours.
2. below material use crusher in crushing to 100 order after charing.
3. the material after fragmentation carries out mixing 30 minutes according to the ratio of 1:2 with KOH in mixed powder machine.
4. the powder mixed is put into revolving activation furnace and is activated, activation temperature 750 degrees Celsius, soak time 2 hours.
5. activator mixture discharging in aqueous, obtains crystallite charcoal through multiple tracks pickling, washing, drying, and this crystallite charcoal graphite layers distance is 0.367-0.378 nm.
6. crystallite powdered carbon body and Stainless Steel Ball being mixed according to the mode of volume ratio 1:1 is placed in fine and close stainless steel electrolytic basket, electrolysis basket aperture is less than the D50 of crystallite powdered carbon body, electrolysis basket is placed in anode and cathode electrolytic cell, anode and cathode electrolyzer is separated by the isolated body of electronic isolation ion conducting, and electrolytic solution is the carbonic allyl ester solution of 1 Mol/L tetraethyl-ammonium tetrafluoroborate.Electrolyzer and the external world are completely airtight, apply electric field in anode and cathode, and electrolysis basket rolls and makes crystallite powdered carbon body have uniform current potential and its graphite microcrystalline structure by electrolyte solution and solute ions intercalation, and the voltage of electrochemical intercalation is 4V.Electrolyzer temperature controls at 20 degrees Celsius.
7. in same airtight electrolyzer, temperature is increased to 50 degrees Celsius, and utilize hyperacoustic energy to carry out the stripping of graphene layer part, ultrasonic frequency controls at 40kHz, splitting time 3 hours.
8. be separated the crystallite charcoal of Stainless Steel Ball and generating portion Graphene, and carry out cleaning, dry and remove the operations such as functional group, forming section graphite alkylene crystallite charcoal product.
Through test, part graphite alkylene crystallite charcoal specific surface area 97 m2/g of embodiment 1 gained, in the organic electrolyte system of tetraethyl-Tetrafluoroboric acid amine, (propylene carbonate) is 180 F/g, operating voltage 3.5V Absorbable organic halogens circulation 10000 weeks as super capacitor material specific storage.
Embodiment 2:
1. be presoma with refinery coke, carry out under nitrogen hydrogen mixeding gas (N2:H2=95:5) protection, carbonization temperature 800 degrees Celsius, carbonization time 5 hours.
2. below material use crusher in crushing to 100 order after charing.
3. the material after fragmentation is put into revolving activation furnace and is carried out steam activation, activation temperature 900 degrees Celsius, soak time 4 hours.
4. activator mixture is through multiple tracks pickling, washing, drying until be satisfied with and utilize micronizer mill that the crystallite powdered carbon after activation is broken to D50 between 6-8 micron, and this crystallite charcoal graphite layers distance is 0.373-0.382 nm.。
5. crystallite powdered carbon body, graphitized carbon black and binding agent (easily carbonizing thermosetting adhesive) are made positive pole and the negative pole of self-supporting respectively according to the ratio of 90:10:10.The acetonitrile solution of positive pole, negative pole and the tetraethyl-ammonium tetrafluoroborate containing 1.2 Mol/L is utilized to make simulation ultracapacitor electrolysis pond as electrolytic solution (electrolytic solution is excessive) far away.Apply the Multiple-Scan voltage of 3.5-4.0V, and at room temperature electrolyzer is applied to ultrasonic 0.5 hour of 40kHz.
6. self-supporting positive pole and negative pole pulverized again, clean, high temperature sintering remove functional group obtain part graphite alkylene crystallite powdered carbon body.
Through test, part graphite alkylene crystallite charcoal specific surface area 123 m2/g of embodiment 2 gained, in the organic electrolyte system of tetraethyl-Tetrafluoroboric acid amine, (acetonitrile) is 195 F/g, operating voltage 3.5V Absorbable organic halogens circulation 10000 weeks as super capacitor material specific storage.
Embodiment 3:
1. be presoma with xylogen, carry out under nitrogen hydrogen mixeding gas (N2:H2=95:5) protection, carbonization temperature 550 degrees Celsius, carbonization time 5 hours.
2. below material use crusher in crushing to 100 order after charing.
3. the material after fragmentation carries out mixing 30 minutes according to the ratio of 1:4 with NaOH in mixed powder machine.
4. the powder mixed is put into revolving activation furnace and is activated, activation temperature 800 degrees Celsius, soak time 4 hours.
5. activator mixture discharging in aqueous, obtains crystallite charcoal through multiple tracks pickling, washing, drying, and the graphite microcrystal interlamellar spacing in this crystallite charcoal is 0.334-0.337 nm.
6. the crystallite charcoal obtained in step 5 is mixed in the ratio of 1:40:3 with the vitriol oil, potassium permanganate, temperature controls to react 2 hours below 5 degrees Celsius, after this thin up 20 times, stir and add excessive hydrogen peroxide termination reaction after 30 minutes, after multiple tracks pickling, washing, drying, obtain the crystallite charcoal that surface is graphene oxide layer.
7. by gained surface for the crystallite charcoal of graphene oxide layer is dispersed in water, with the supersound process 1 hour of 40kHz, centrifugal, washing, dry, obtain the crystallite carbon powder of surface for few layer graphene oxide.
8. previous materials and xitix are mixed with the ratio of 1:1 the aqueous solution that concentration is 10%, carry out reduction reaction, reduction temperature is 80 degrees Celsius, and the recovery time is 3 hours.
9. by reduzate through washing, dry, obtain graphite alkylene porous charcoal powder.
Through test, part graphite alkylene porous charcoal specific surface area 1896 m2/g of embodiment 3 gained, in the organic electrolyte system of tetraethyl-Tetrafluoroboric acid amine, (acetonitrile) is 172 F/g, operating voltage 2.7V Absorbable organic halogens circulation 100000 weeks as super capacitor material specific storage.
Embodiment 4:
1. be presoma with coconut husk, carry out under nitrogen hydrogen mixeding gas (N2:H2=95:5) protection, carbonization temperature 450 degrees Celsius, carbonization time 5 hours.
2. below material use crusher in crushing to 100 order after charing.
3. the material after fragmentation carries out mixing 30 minutes according to the ratio of 1:2 with KOH in mixed powder machine.
4. the powder mixed is put into revolving activation furnace and is activated, activation temperature 700 degrees Celsius, soak time 2.5 hours.
5. activator mixture discharging in aqueous, obtains crystallite charcoal through multiple tracks pickling, washing, drying, and the graphite microcrystal interlamellar spacing in this crystallite charcoal is 0.334-0.337 nm.
6. crystallite charcoal step 5 obtained mixes in the ratio of 1:40:3 with the vitriol oil, potassium permanganate, temperature controls to react 2 hours below 5 degrees Celsius, after this thin up 20 times, stir and add excessive hydrogen peroxide termination reaction after 30 minutes, after multiple tracks pickling, washing, drying, obtain the crystallite charcoal that surface is graphene oxide layer.
7. by gained surface for the crystallite charcoal of graphene oxide layer is dispersed in water, with the ultrasonic stripping 1 hour of 40kHz, centrifugal, washing, dry, obtain the crystallite carbon powder of surface for few layer graphene oxide.
8. previous materials is sintered under hot conditions under reducing gas protection and remove functional group, obtain graphite alkylene porous charcoal powder.
Through test, part graphite alkylene porous charcoal specific surface area 1709 m2/g of embodiment 4 gained, in the organic electrolyte system of tetraethyl-Tetrafluoroboric acid amine, (acetonitrile) is 165 F/g, operating voltage 2.7V Absorbable organic halogens circulation 100000 weeks as super capacitor material specific storage.
Embodiment 5:
1. be presoma with refinery coke, carry out under nitrogen hydrogen mixeding gas (N2:H2=95:5) protection, carbonization temperature 750 degrees Celsius, carbonization time 5 hours.
2. below material use crusher in crushing to 100 order after charing.
3. material clean after fragmentation is dried, and mix according to ratio and the vitriol oil of 1:20:3, potassium permanganate, react 4 hours at 60 degrees Celsius, after this thin up 20 times, stirs and add excessive hydrogen peroxide termination reaction after 30 minutes.After multiple tracks pickling, washing, drying, obtain the charcoal material that surface is graphene oxide layer.
4. above-mentioned charcoal material is carried out mixing 30 minutes according to the ratio of 1:2 with KOH in mixed powder machine.
5. the powder mixed is put into revolving activation furnace and is activated, activation temperature 700 degrees Celsius, soak time 2.5 hours.
6. activator mixture discharging in aqueous, obtain the crystallite charcoal of surface for graphene oxide layer through multiple tracks pickling, washing, drying, the graphite microcrystal interlamellar spacing in this crystallite charcoal is 0.334-0.337 nm.
7. the crystallite charcoal of gained is dispersed in water, with the ultrasonic stripping 1 hour of 40kHz, centrifugal, washing, dry, obtain the crystallite carbon powder of surface for few layer graphene oxide.
8. previous materials is sintered under hot conditions under reducing gas protection and remove functional group, obtain graphite alkylene porous charcoal powder.
Through test, part graphite alkylene porous charcoal specific surface area 1920 m2/g of embodiment 5 gained, in the organic electrolyte system of tetraethyl-Tetrafluoroboric acid amine, (acetonitrile) is 183 F/g, operating voltage 2.7V Absorbable organic halogens circulation 100000 weeks as super capacitor material specific storage.
Embodiment 6:
1. be presoma with resol, carry out under nitrogen hydrogen mixeding gas (N2:H2=95:5) protection, carbonization temperature 550 degrees Celsius, carbonization time 5 hours.
2. below material use crusher in crushing to 100 order after charing.
3. the material after fragmentation carries out mixing 30 minutes according to the ratio of 1:2 with KOH in mixed powder machine.
4. the powder mixed is put into revolving activation furnace and is carried out pre-activate, activation temperature 400 degrees Celsius, soak time 3 hours.
5. pre-activate mixture discharging in aqueous, obtains pre-activate charcoal through multiple tracks pickling, washing, drying.
6. pre-activate charcoal is mixed in the ratio of 1:20:3 with the vitriol oil, potassium permanganate, temperature controls to react 4 hours below 60 degrees Celsius, after this thin up 20 times, stir and add excessive hydrogen peroxide termination reaction after 30 minutes, after multiple tracks pickling, washing, drying, obtain the pre-activate charcoal that surface is graphene oxide layer.
7. gained pre-activate charcoal is divided and carry out mixing 30 minutes according to the ratio of 1:2 in mixed powder machine with KOH.
8. the powder mixed is put into revolving activation furnace and is activated, activation temperature 800 degrees Celsius, soak time 1 hour.
9. activator mixture discharging in aqueous, obtains the crystallite charcoal of surface for graphene oxide structure through multiple tracks pickling, washing, drying.
10. previous materials and xitix are mixed with the ratio of 1:1 the aqueous solution that concentration is 10%, carry out reduction reaction, reduction temperature is 80 degrees Celsius, and the recovery time is 3 hours.
11. by reduzate through washing, dry, obtain graphite alkylene porous charcoal powder.
Through test, part graphite alkylene porous charcoal specific surface area 1835 m2/g of embodiment 6 gained, in the organic electrolyte system of tetraethyl-Tetrafluoroboric acid amine, (acetonitrile) is 175 F/g, operating voltage 2.7V Absorbable organic halogens circulation 100000 weeks as super capacitor material specific storage.
Claims (9)
1. a part graphite alkylene porous charcoal, is characterized in that: its structure comprises the graphite microcrystal of random layer and is scattered in homodisperse few layer graphene on graphite microcrystal surface.
2. part graphite alkylene porous charcoal according to claim 1, is characterized in that: described porous charcoal specific surface area is 50-3500m
2/ g.
3. part graphite alkylene porous charcoal according to claim 1 and 2, is characterized in that: the common graphite crystallite of the graphite microcrystal of described random layer to be d002 interlamellar spacing be 0.335nm, or d002 interlamellar spacing is the large interlamellar spacing graphite microcrystal of 0.365-0.385nm.
4. a preparation method for the part graphite alkylene porous charcoal described in claim 1-3, comprises the steps:
(1) precursor power: carbonized by carbon feedstock, or/and reactivate forms the graphite microcrystal of random layer;
(2) part graphite alkylene: carry out part graphite alkylene to presoma, or/and reactivate forming section graphite alkylene porous charcoal;
(3) part graphite alkylene porous charcoal is cleaned, purifying, complete preparation.
5. the preparation method of graphite alkylene porous charcoal according to claim 4, it is characterized in that: activation is first carried out to the material after charing and forms crystallite charcoal, carry out part graphite alkylene again and form graphite alkylene porous charcoal porous charcoal, finally carry out cleaning, purifying, complete preparation.
6. the preparation method of graphite alkylene porous charcoal according to claim 4, is characterized in that: first carry out part graphite alkylene to the material after charing, then carry out activation forming section graphite alkylene porous charcoal, finally carries out cleaning, purifying, completes preparation.
7. the preparation method of graphite alkylene porous charcoal according to claim 4, it is characterized in that: first pre-activate is carried out to the material of charing, then carry out the pre-activate charcoal that part graphite alkylene acquisition surface is graphene oxide layer, more again activate, finally carry out cleaning, purifying, complete preparation.
8. the preparation method of the graphite alkylene crystallite charcoal according to any one of claim 4-7, is characterized in that: described carbon feedstock is resol, xylogen, organism fiber or refinery coke.
9. the preparation method of the part graphite alkylene porous charcoal according to any one of claim 4-7, is characterized in that: described part graphite olefination procedure is electrochemical intercalation, solvent-thermal method or chemistry redox method.
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Cited By (5)
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| CN108134085A (en) * | 2018-01-10 | 2018-06-08 | 福州大学 | The graphite lithium ion battery negative material and preparation method of a kind of surface multi-layer graphite alkylene |
| CN108298525A (en) * | 2018-03-19 | 2018-07-20 | 广西科学院 | A kind of graphene microcrystal and preparation method thereof |
| WO2018225670A1 (en) * | 2017-06-05 | 2018-12-13 | 積水化学工業株式会社 | Carbon material-containing dispersion liquid, slurry for electrode formation, and method for producing electrode for nonaqueous electrolyte secondary batteries |
| CN110054177A (en) * | 2018-03-20 | 2019-07-26 | 南方科技大学 | Graphene multi-stage porous carbon material and preparation method thereof and lithium ion battery |
| CN115074694A (en) * | 2022-07-01 | 2022-09-20 | 常州第六元素半导体有限公司 | Graphene film preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018225670A1 (en) * | 2017-06-05 | 2018-12-13 | 積水化学工業株式会社 | Carbon material-containing dispersion liquid, slurry for electrode formation, and method for producing electrode for nonaqueous electrolyte secondary batteries |
| JPWO2018225670A1 (en) * | 2017-06-05 | 2020-04-02 | 積水化学工業株式会社 | Method for producing carbon material-containing dispersion, electrode forming slurry, and electrode for non-aqueous electrolyte secondary battery |
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| CN108298525A (en) * | 2018-03-19 | 2018-07-20 | 广西科学院 | A kind of graphene microcrystal and preparation method thereof |
| CN110054177A (en) * | 2018-03-20 | 2019-07-26 | 南方科技大学 | Graphene multi-stage porous carbon material and preparation method thereof and lithium ion battery |
| CN115074694A (en) * | 2022-07-01 | 2022-09-20 | 常州第六元素半导体有限公司 | Graphene film preparation method |
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