CN103436904A - Method for preparing carbide derived carbon by fused salt electrolysis method - Google Patents
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Abstract
The invention discloses a method for preparing carbide derived carbon by a fused salt electrolysis method. The method mainly comprises the steps that metal carbide serves as a raw material, and is subjected to die pressing sintering to form a metal carbide sheet to serve as an anode; by taking fused salt as an electrolyte, and a high-purity and high-density graphite rod as a cathode, fused salt electrolysis is performed in an electrolysis furnace in an argon atmosphere with the electrolysis temperature of 400-1300 DEG C, the electrolysis voltage of 1.8-3.2V, and the electrolysis time of 2-60h; after the electrolysis, an anode product is taken out, and subjected to water washing, ultrasonic-assisted pickling, water washing and drying treatment; and the carbide derived carbon is prepared. According to the method, the low-cost metal carbide can serve as the raw material for preparing the carbide derived carbon by the fused salt electrolysis method, so that a preparation technology is simplified; the cost is lowered; and the prepared carbide derived carbon serves as an electrode material of a supercapacitor, and has high specific capacity and good cycling stability.
Description
Technical field
The present invention relates to a kind of preparation method of carbide-derived carbon.
Technical background
Carbide-derived carbon has relatively high specific surface area and regulatable pore size distribution and the good excellent specific properties such as electron conduction, therefore at gas storage, molecular sieve, support of the catalyst, sorbent material, battery and electrode of super capacitor, the potential application in the fields such as water/air filtration and medical facilities and become extremely important.The main preparation methods of carbide-derived carbon has at present: high temperature thermal decomposition method, halogen etch method, supercutical fluid etch method etc.These methods are all intermittent, and complicated process of preparation, the production cycle is long and energy consumption is high; Environmental pollution is more serious; Thereby caused the price of carbide-derived carbon higher, limited the widespread use of carbide-derived carbon.
Summary of the invention
The object of the present invention is to provide a kind of method that preparation method is simple, cost is low, pollution-free, fused salt electrolysis process that be convenient to suitability for industrialized production prepares carbide-derived carbon.
The technical solution adopted in the present invention is as follows:
1, by metal carbide powders, it is titanium carbide, silicon carbide, norbide, wolfram varbide, chromium carbide etc., and preferably technical grade, mean particle size 2 μ m suppress in blocks with the pressure of 3-15MPa in mould.
2, under protection of inert gas with the temperature sintering 2-8h of 800-1000 ℃.
3, using the metallic carbide sheet of sintering as positive pole, with high-purity high-density degree graphite rod (carbon content>99.99%, density 1.5g/cm
3) as negative pole, positive and negative electrode is put into to ceramic crucible, using ceramic crucible as electrolyzer, heating installation is crucible electrical resistance furnace, power supply is D.C. regulated power supply, in the electrolytic furnace under argon shield, usings melting salt as ionogen, electrolysis temperature 400-1300 ℃, electrolysis voltage 1.8V-3.2V, electrolysis time 2-60 hour; Described melting salt is calcium chloride, magnesium chloride, Repone K, sodium-chlor and fused salt mixt thereof etc.
4, after electrolysis finishes, anodal electrolysate is taken out, be cooled to room temperature, the electrolysis whole process is by argon shield.Electrolysate is carried out to deionized water washing, 36% chlorohydric acid pickling successively, the preferably auxiliary pickling of ultrasonic wave, then deionized water washing, 120 ℃ of dryings in air, prepared product is carbide-derived carbon.
The present invention compared with prior art has following advantage:
1, the present invention is that a kind of to take cheap technical grade metallic carbide be raw material, has used preparation technology pollution-free, that simplify, and the purity of prepared carbide-derived carbon product is high, even aperture distribution, specific surface area is large, and chemical property is superior, has high specific storage.
2, electrolyzer of the present invention, can make electrolytic process stablize, be easy to control, and preparation cost is low.
The accompanying drawing explanation
Fig. 1 is that fused salt electrolysis equipment master of the present invention looks the section simplified schematic diagram.
Fig. 2 is that the XRD figure of carbide-derived carbon prepared as raw material by industrial titanium carbide is take in the present invention.
Fig. 3 is that the XRD figure of carbide-derived carbon prepared as raw material by industrial norbide is take in the present invention.
Fig. 4 is that the XRD figure of carbide-derived carbon prepared as raw material by industrial silicon carbide is take in the present invention.
Fig. 5 is that the XRD figure of carbide-derived carbon prepared as raw material by industrial wolfram varbide is take in the present invention.
Fig. 6 is that the XRD figure of carbide-derived carbon prepared as raw material by industrial chromium carbide is take in the present invention.
Fig. 7 is that the TEM figure of carbide-derived carbon prepared as raw material by industrial titanium carbide is take in the present invention.
Fig. 8 is that the TEM figure of carbide-derived carbon prepared as raw material by industrial norbide is take in the present invention
Fig. 9 is that the TEM figure of carbide-derived carbon prepared as raw material by industrial silicon carbide is take in the present invention.
Figure 10 is that the TEM figure of carbide-derived carbon prepared as raw material by industrial wolfram varbide is take in the present invention.
Figure 11 is that the TEM figure of carbide-derived carbon prepared as raw material by industrial chromium carbide is take in the present invention.
Figure 12 be take titanium carbide as raw material, the charging and discharging curve figure under the different current densities of the porous carbon that under 400 ℃ of argon shields prepared by 3.2V fused salt electrolysis 60h.
Figure 13 be take norbide as raw material, the charging and discharging curve figure under the different current densities of the porous carbon that under 750 ℃ of argon shields prepared by 3.0V fused salt electrolysis 45h.
Figure 14 be take silicon carbide as raw material, the charging and discharging curve figure under the different current densities of the porous carbon that under 900 ℃ of argon shields prepared by 2.6V fused salt electrolysis 30h.
Figure 15 be take wolfram varbide as raw material, the charging and discharging curve figure under the different current densities of the porous carbon that under 1100 ℃ of argon shields prepared by 2.2V fused salt electrolysis 15h.
Figure 16 be take chromium carbide as raw material, the charging and discharging curve figure under the different current densities of the porous carbon that under 1300 ℃ of argon shields prepared by 1.8V fused salt electrolysis 2h.
In figure: 1, crucible electrical resistance furnace, 2, graphite rod cathode, 3, molten salt electrolyte, 4, argon bottle, 5, under meter, 6, the argon inlet mouth, 7, water coolant, 8, the electrode extended line, 9, thermopair, 10, argon gas air outlet, 11, D.C. regulated power supply, 12, the stainless steel electrolytic stove, 13, cooling water jecket, 14, metallic carbide positive pole, 15, the ceramic crucible electrolyzer.
In the fused salt electrolysis equipment master shown in Fig. 1 looks the section simplified schematic diagram, be provided with the stainless steel electrolytic stove in crucible type resistance furnace stove, it has a upper shed trough-shaped housing, the opening of this housing is provided with the sealing upper cover connected by fastening piece, electrolytic furnace housing inner bottom part is provided with refractory brick, be equipped with the ceramic crucible electrolyzer above fire brick layer, be provided with metallic carbide positive pole, graphite rod cathode and molten salt electrolyte in groove.The wire be connected with above-mentioned positive and negative electrode is connected with D.C. regulated power supply through the through hole of electrolytic furnace upper cover respectively.Cover the inlet/outlet pipe that also is respectively equipped with argon gas on electrolytic furnace, wherein the inlet pipe of argon gas is connected with argon bottle by the pipeline that is provided with under meter.Cover on electrolytic furnace and also be provided with a part and be placed in the thermopair in electrolytic furnace.At the external chuck that is provided with the water coolant turnover of electrolytic furnace.
Take 1.5 gram titanium carbide powders (2 μ m, 98%), be molded into sheet under 3MPa pressure, then put into sintering oven, be filled with argon gas, be warming up to 800 ℃ of sintering 8h, the titanium carbide sheet after sintering is put into electronic conductive material and connected and draw as anodal, by high-purity high-density degree graphite rod (carbon content>99.99%, density 1.5g/cm
3) as negative pole, take ceramic crucible as electrolyzer in electrolytic furnace, take Repone K 48 grams, magnesium chloride 120 grams, (Repone K: magnesium chloride: sodium-chlor=0.2:0.5:0.3) gross weight 240 grams are put into ceramic crucible to sodium-chlor 72 grams, pass into argon gas in crucible electrical resistance furnace, heat up 400 ℃ and make its fusing, positive and negative electrode is put into to ceramic crucible, and D.C. regulated power supply connects positive and negative electrode energising 3.2V, carries out electrolysis 60 hours.After reaction finishes, the product that positive pole is obtained is washed with deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and the deionized water washing, in air, 120 ℃ of dryings, then tested.Fig. 2 is the XRD figure of the titanium carbide derived carbon of preparation.The TEM figure that Fig. 7 is the carbide-derived carbon of preparation, as can be seen from the figure sheet structure.Charging and discharging curve figure under the different current densities of the titanium carbide derived carbon that Figure 12 is preparation, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 circle specific discharge capacities of obtained sample are 110 F/g, under 500mA/g, the specific discharge capacity of obtained sample is 90F/g, under 1000mA/g, the specific discharge capacity of obtained sample is 75F/g; By nitrogen absorption under low temperature test b ET Surface Area=602.196m
2/ g.
Take 1.5 gram boron carbide powders (2 μ m, 98%), be molded into sheet under 5MPa pressure, then put into sintering oven, be filled with argon gas, be warming up to 850 ℃ of sintering 7h, the norbide sheet after sintering is put into to anodal basket as anodal, by high-purity high-density degree graphite rod (carbon content>99.99%, density 1.5g/cm
3) as negative pole, take ceramic crucible as electrolyzer in electrolytic furnace, take 240 gram magnesium chlorides and put into ceramic crucible, pass into argon gas in crucible electrical resistance furnace, be warming up to 750 ℃ and stable after, positive and negative electrode is put into to ceramic crucible, and D.C. regulated power supply connects positive and negative electrode energising 3.0V, carries out electrolysis 45 hours.After reaction finishes, the product that positive pole is obtained is washed with deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and the deionized water washing, in air, 120 ℃ of dryings, then tested.Fig. 3 is the XRD figure of the norbide derived carbon of preparation.The TEM figure that Fig. 8 is the norbide derived carbon of preparation, as can be seen from the figure sheet structure and pore structure.Charging and discharging curve figure under the different current densities of the norbide derived carbon that Figure 13 is preparation, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 circle specific discharge capacities of obtained sample are 123.5F/g, under 500mA/g, the specific discharge capacity of obtained sample is 102F/g, under 1000mA/g, the specific discharge capacity of obtained sample is 77.7F/g; By nitrogen absorption under low temperature test b ET Surface Area=763.843m
2/ g.
Embodiment 3
Take 1.5 gram silicon carbide powders (2 μ m, 98%), be molded into sheet under 8MPa pressure, then put into sintering oven, be filled with argon gas, be warming up to 900 ℃ of sintering 5h, the silicon carbide plate after sintering is put into to anodal basket as anodal, by high-purity high-density degree graphite rod (carbon content>99.99%, density 1.5g/cm
3) as negative pole, take ceramic crucible as electrolyzer in electrolytic furnace, take 240 gram calcium chloride and put into ceramic crucible, pass into argon gas in crucible electrical resistance furnace, be warming up to 900 ℃ and stable after, positive and negative electrode is put into to crucible, D.C. regulated power supply connects positive and negative electrode energising 2.6V, carries out electrolysis 30 hours.After reaction finishes, the product that positive pole is obtained is washed with deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and the deionized water washing, in air, 120 ℃ of dryings, then tested.Fig. 4 is the XRD figure of the silicon carbide derived carbon of preparation.The TEM figure that Fig. 9 is the silicon carbide derived carbon of preparation, can find out obvious pore structure.Charging and discharging curve figure under the different current densities of the silicon carbide derived carbon that Figure 14 is preparation, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 circle specific discharge capacities of obtained sample are 143.8F/g, under 500mA/g, the specific discharge capacity of obtained sample is 123F/g, under 1000mA/g, the specific discharge capacity of obtained sample is 97.2F/g; By nitrogen absorption under low temperature test b ET Surface Area=988.5522m
2/ g.
Take 1.5 gram tungsten-carbide powders (2 μ m, 98%), be molded into sheet under 10MPa pressure, then put into sintering oven, be filled with argon gas, be warming up to 950 ℃ of sintering 3h, the tungsten carbide chip after sintering is connected and draws as anodal with electronic conductive material, by high-purity high-density degree graphite rod (carbon content>99.99%, density 1.5g/cm
3) as negative pole, take ceramic crucible as electrolyzer in electrolytic furnace, the 240 gram Repone K of weighing are put into ceramic crucible, pass into argon gas in crucible electrical resistance furnace, be warming up to 1100 ℃ and stable after, positive and negative electrode is put into to crucible, and D.C. regulated power supply connects positive and negative electrode energising 2.2V, carries out electrolysis 15 hours.After reaction finishes, the product that positive pole is obtained is washed with deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and the deionized water washing, in air, 120 ℃ of dryings, then tested.Fig. 5 is the XRD figure of the wolfram varbide derived carbon of preparation.The TEM figure that Figure 10 is the wolfram varbide derived carbon of preparation, as can be seen from the figure obvious pore structure.Charging and discharging curve figure under the different current densities of the wolfram varbide derived carbon that Figure 15 is preparation, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 circle specific discharge capacities of obtained sample are 160F/g, under 500mA/g, the specific discharge capacity of obtained sample is 138.89F/g, under 1000mA/g, the specific discharge capacity of obtained sample is 111.1F/g; By nitrogen absorption under low temperature test b ET Surface Area=1137.7433m
2/ g.
Embodiment 5
Take 1.5 gram chromium carbide powders (2 μ m, 98%), be molded into sheet under 15MPa pressure, then put into sintering oven, be filled with argon gas, be warming up to 1000 ℃ of sintering 2h, the chromium carbide sheet after sintering is put into to anodal basket and draw as anodal, by high-purity high-density degree graphite rod (carbon content>99.99%, density 1.5g/cm
3) as negative pole, take ceramic crucible as electrolyzer in electrolytic furnace, the 240 gram sodium-chlor of weighing are put into ceramic crucible, pass into argon gas in crucible electrical resistance furnace, be warming up to 1300 ℃ and stable after, positive and negative electrode is put into to crucible, D.C. regulated power supply connects positive and negative electrode energising 1.8V, carries out electrolysis 2 hours.After reaction finishes, the product that positive pole is obtained is washed with deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and the deionized water washing, in air, 120 ℃ of dryings, tested.Fig. 6 is the XRD figure of the chromium carbide derived carbon of preparation.The TEM figure that Figure 11 is the chromium carbide derived carbon of preparation, as can be seen from the figure sheet structure and pore structure.Charging and discharging curve figure under the different current densities of the chromium carbide derived carbon that Figure 16 is preparation, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 circle specific discharge capacities of obtained sample are 114.22F/g, under 500mA/g, the specific discharge capacity of obtained sample is 88.89F/g, under 1000mA/g, the specific discharge capacity of obtained sample is 54.165F/g; By nitrogen absorption under low temperature test b ET Surface Area=640.6837m
2/ g.
Claims (7)
1. a fused salt electrolysis process prepares the method for carbide-derived carbon, it is characterized in that: metal carbide powders compression molding under 3-15MPa pressure is pressed into to sheet, under protection of inert gas with the temperature sintering 2-8 hour of 800-1000 ℃, using the metallic carbide sheet of sintering as positive pole, using high-purity high-density degree graphite rod as negative pole, using ceramic crucible as electrolyzer, heating installation is crucible electrical resistance furnace, power supply is D.C. regulated power supply, using melting salt as ionogen in the electrolytic furnace under argon shield, electrolysis temperature 400-1300 ℃, electrolysis voltage 1.8V-3.2V, electrolysis time 2-60 hour, after electrolysis finishes, anodal electrolysate is taken out, be cooled to room temperature, anodal electrolysate is washed successively, pickling, washing and drying and processing.
2. fused salt electrolysis process according to claim 1 prepares the method for carbide-derived carbon, it is characterized in that: described positive pole be using the metallic carbide sheet put into anodal basket or with electronic conductive material draw as positive pole.
3. fused salt electrolysis process according to claim 1 and 2 prepares the method for carbide-derived carbon, it is characterized in that: titanium carbide, norbide, silicon carbide, wolfram varbide, chromium carbide that described metallic carbide raw material is technical grade.
4. fused salt electrolysis process according to claim 3 prepares the method for carbide-derived carbon, it is characterized in that: described melting salt is calcium chloride, magnesium chloride, Repone K, sodium-chlor and fused salt mixt thereof.
5. fused salt electrolysis process according to claim 4 prepares the method for carbide-derived carbon, it is characterized in that: the powder that described metal carbide powders is 2 microns of technical grades, mean particle size.
6. fused salt electrolysis process according to claim 1 prepares the method for carbide-derived carbon, it is characterized in that: when anodal electrolysate is carried out to pickling, by ultrasonic, assisted.
7. the fused salt electrolysis process of claim 1 prepares the device of carbide-derived carbon, it is characterized in that: in crucible type resistance furnace stove, be provided with the stainless steel electrolytic stove, it has a upper shed trough-shaped housing, the opening of this housing is provided with the sealing upper cover connected by fastening piece, electrolytic furnace housing inner bottom part is provided with refractory brick, be equipped with the ceramic crucible electrolyzer above fire brick layer, be provided with metallic carbide positive pole, graphite rod cathode and molten salt electrolyte in groove.The wire be connected with above-mentioned positive and negative electrode is connected with D.C. regulated power supply through the through hole of electrolytic furnace upper cover respectively, cover the inlet/outlet pipe that also is respectively equipped with argon gas on electrolytic furnace, wherein the inlet pipe of argon gas is connected with argon bottle by the pipeline that is provided with under meter, cover on electrolytic furnace and also be provided with a part and be placed in the thermopair in electrolytic furnace, at the external chuck that is provided with the water coolant turnover of electrolytic furnace.
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| CN106082175A (en) * | 2016-08-25 | 2016-11-09 | 北京化工大学 | A kind of method that melted sodium carbonate high temperature prepares carbide-derived carbon |
| CN110459769A (en) * | 2019-07-17 | 2019-11-15 | 武汉大学 | A kind of silicon-carbon solid sols, preparation method and the application of high dispersive |
| US11489164B2 (en) | 2019-07-17 | 2022-11-01 | Wuhan University | Highly dispersed silicon-carbon solid sol, preparation method and application thereof |
| CN110459769B (en) * | 2019-07-17 | 2021-06-04 | 武汉大学 | High-dispersion silicon-carbon solid sol, preparation method and application thereof |
| CN111231137A (en) * | 2020-03-06 | 2020-06-05 | 中国工程物理研究院机械制造工艺研究所 | Cutting processing system and method for boron carbide-based ceramic material |
| CN112725817A (en) * | 2020-12-30 | 2021-04-30 | 重庆大学 | Method for preparing carbide ceramic coating by molten salt electrolysis |
| CN112921300A (en) * | 2021-03-04 | 2021-06-08 | 沈阳大学 | Method for in-situ generation of diamond-like film precursor |
| WO2024028216A1 (en) * | 2022-08-03 | 2024-02-08 | Skeleton Technologies GmbH | In-situ hot filtration for gas-solid-separation in carbide-derived carbon production |
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