CN103436904B - A kind of fused salt electrolysis process is prepared the method for carbide-derived carbon - Google Patents
A kind of fused salt electrolysis process is prepared the method for carbide-derived carbon Download PDFInfo
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Abstract
A kind of fused salt electrolysis process is prepared the method for carbide-derived carbon, it is mainly: using metal carbides as raw material, make metal carbides sheet as positive pole through molding sintering, using fuse salt as electrolyte, using high-purity high-density degree graphite rod as negative pole, in the electrolytic furnace of argon gas atmosphere, carry out molten-salt electrolysis, 400-1300 DEG C of electrolysis temperatures, decomposition voltage 1.8V-3.2V, electrolysis time 2-60 hours, after electrolysis finishes, anodal product is taken out, wash-ultrasonic wave is assisted pickling-washing-drying and processing, makes carbide-derived carbon. The present invention is by the method for molten-salt electrolysis, the metal carbides of available cheapness are that raw material is prepared carbide-derived carbon, have simplified preparation technology, have reduced cost, the carbide-derived carbon of preparation has height ratio capacity as electrode material for super capacitor, and stable circulation performance is good.
Description
Technical field
The present invention relates to a kind of preparation method of carbide-derived carbon.
Technical background
Carbide-derived carbon has the excellences such as relatively high specific area and regulatable pore-size distribution and good electron conductionCharacteristic, therefore at gas storage, molecular sieve, catalyst carrier, adsorbent, battery and electrode of super capacitor, water/air mistakeThe potential application in filter and the fields such as Medical Devices and become extremely important. The main preparation methods of carbide-derived carbon has at present: heightWarm decomposition method, halogen etching, supercritical fluid etching etc. These methods are all intermittent, complicated process of preparation,Production cycle is long and energy consumption is high; Environmental pollution is more serious; Thereby cause the price of carbide-derived carbon higher, limited carbonThe extensive use of compound derived carbon.
Summary of the invention
The object of the present invention is to provide that a kind of preparation method is simple, cost is low, pollution-free, the fused salt electricity of being convenient to suitability for industrialized productionSolution is prepared the method for carbide-derived carbon.
The technical solution adopted in the present invention is as follows:
1,, by metal carbide powders, it is titanium carbide, carborundum, boron carbide, tungsten carbide, chromium carbide etc., best technical grade,Particle mean size 2 μ m, the pressure compacting with 3-15MPa in mould is in blocks.
2, under inert gas shielding with the temperature sintering 2-8h of 800-1000 DEG C.
3, using the metal carbides sheet of sintering as positive pole, with high-purity high-density degree graphite rod (phosphorus content > 99.99%, density1.5g/cm3) as negative pole, both positive and negative polarity is put into ceramic crucible, using ceramic crucible as electrolytic cell, firing equipment is crucible electricityResistance stove, power supply is D.C. regulated power supply, in the electrolytic furnace under argon shield using fuse salt as electrolyte, electrolysis temperature400-1300 DEG C, decomposition voltage 1.8V-3.2V, electrolysis time 2-60 hour; Described fuse salt is calcium chloride, magnesium chloride, chlorineChange potassium, sodium chloride and fused salt mixt thereof etc.
4, after electrolysis finishes, anodal electrolysate is taken out, be cooled to room temperature, electrolysis overall process is by argon shield. To electrolysisProduct carries out deionized water washing, 36% chlorohydric acid pickling successively, and the preferably auxiliary pickling of ultrasonic wave, then deionized water washing, at skyIn gas, 120 DEG C are dried, and prepared product is carbide-derived carbon.
The present invention compared with prior art tool has the following advantages:
1, the present invention is a kind of taking cheap technical grade metal carbides as raw material, has used preparation technology pollution-free, that simplify,The purity of prepared carbide-derived carbon product is high, even aperture distribution, and specific area is large, and chemical property is superior, toolThere is high specific capacity.
2, electrolysis installation of the present invention, can make electrolytic process stablize, be easy to control, and preparation cost is low.
Brief description of the drawings
Fig. 1 is that molten-salt electrolysis equipment master of the present invention looks section simplified schematic diagram.
Fig. 2 is the XRD figure of the carbide-derived carbon prepared taking industrial titanium carbide as raw material of the present invention.
Fig. 3 is the XRD figure of the carbide-derived carbon prepared taking industrial boron carbide as raw material of the present invention.
Fig. 4 is the XRD figure of the carbide-derived carbon prepared taking industrial carborundum as raw material of the present invention.
Fig. 5 is the XRD figure of the carbide-derived carbon prepared taking industrial tungsten carbide as raw material of the present invention.
Fig. 6 is the XRD figure of the carbide-derived carbon prepared taking industrial chromium carbide as raw material of the present invention.
Fig. 7 is the TEM figure of the carbide-derived carbon prepared taking industrial titanium carbide as raw material of the present invention.
Fig. 8 is the TEM figure of the carbide-derived carbon prepared taking industrial boron carbide as raw material of the present invention
Fig. 9 is the TEM figure of the carbide-derived carbon prepared taking industrial carborundum as raw material of the present invention.
Figure 10 is the TEM figure of the carbide-derived carbon prepared taking industrial tungsten carbide as raw material of the present invention.
Figure 11 is the TEM figure of the carbide-derived carbon prepared taking industrial chromium carbide as raw material of the present invention.
Figure 12 is taking titanium carbide as raw material, the different electric currents of the porous carbon that under 400 DEG C of argon shields prepared by 3.2V molten-salt electrolysis 60hCharging and discharging curve figure under density.
Figure 13 is taking boron carbide as raw material, the different electric currents of the porous carbon that under 750 DEG C of argon shields prepared by 3.0V molten-salt electrolysis 45hCharging and discharging curve figure under density.
Figure 14 is taking carborundum as raw material, the different electric currents of the porous carbon that under 900 DEG C of argon shields prepared by 2.6V molten-salt electrolysis 30hCharging and discharging curve figure under density.
Figure 15 is taking tungsten carbide as raw material, the difference electricity of the porous carbon that under 1100 DEG C of argon shields prepared by 2.2V molten-salt electrolysis 15hCharging and discharging curve figure under current density.
Figure 16 is taking chromium carbide as raw material, the different electric currents of the porous carbon that under 1300 DEG C of argon shields prepared by 1.8V molten-salt electrolysis 2hCharging and discharging curve figure under density.
In figure: 1, crucible electrical resistance furnace, 2, graphite rod cathode, 3, molten salt electrolyte, 4, argon bottle, 5, flowmeter, 6,Argon inlet mouth, 7, cooling water, 8, electrode extended line, 9, thermocouple, 10, argon gas gas outlet, 11, DC voltage-stabilizing electricitySource, 12, stainless steel electrolytic stove, 13, cooling water jecket, 14, metal carbides positive pole, 15, ceramic crucible electrolytic cell.
Look in section simplified schematic diagram the molten-salt electrolysis equipment master shown in Fig. 1, in crucible type resistance furnace stove, be provided with stainless steel electrolytic stove,It has a upper shed trough-shaped housing, and the opening of this housing is provided with the sealing upper cover being connected by securing member, the end in electrolytic furnace housingPortion is provided with refractory brick, is equipped with ceramic crucible electrolytic cell above fire brick layer, in groove, be provided with metallic carbide positive pole, graphite rod cathode andMolten salt electrolyte. The wire being 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.On electrolytic furnace, cover the inlet/outlet pipe that is also respectively equipped with argon gas, wherein the inlet tube of argon gas is by being provided with pipeline and the argon of flowmeterGas cylinder is connected. On electrolytic furnace, cover and be also provided with a part and be placed in the thermocouple in electrolytic furnace. At the external cooling water that is provided with of electrolytic furnaceThe chuck of turnover.
Embodiment 1
Take 1.5 grams of titanium carbide powders (2 μ m, 98%), under 3MPa pressure, be molded into sheet, then put into sintering furnace,Be filled with argon gas, be warming up to 800 DEG C of sintering 8h, the titanium carbide sheet after sintering is put into electronic conductive material and connected and draw as justThe utmost point, by high-purity high-density degree graphite rod (phosphorus content > 99.99%, density 1.5g/cm3) as negative pole, in electrolytic furnace with ceramic earthenwareCrucible is electrolytic cell, take 72 grams, 48 grams, potassium chloride, 120 grams, magnesium chloride, sodium chloride (potassium chloride: magnesium chloride: sodium chloride=0.2:0.5:0.3) 240 grams of gross weights are put into ceramic crucible, in crucible electrical resistance furnace, pass into argon gas, heat up 400 DEG C and make its fusing, willBoth positive and negative polarity is put into ceramic crucible, and D.C. regulated power supply connects both positive and negative polarity energising 3.2V, carries out electrolysis 60 hours. Reaction finishesAfter, the product that positive pole is obtained is washed by deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and deionized water washing, at skyIn gas, 120 DEG C are dried, and then test. Fig. 2 is the XRD figure of the titanium carbide derived carbon of preparation. Fig. 7 is the carbonization of preparationThe TEM figure of thing derived carbon, as can be seen from the figure laminated structure. Figure 12 is the different current densities of the titanium carbide derived carbon of preparationUnder charging and discharging curve figure, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 of obtained sampleCircle specific discharge capacity is 110F/g, and under 500mA/g, the specific discharge capacity of obtained sample is 90F/g, at 1000mA/gUnder, the specific discharge capacity of obtained sample is 75F/g; By nitrogen absorption under low temperature test b ETSurfaceArea=602.196m2/g。
Embodiment 2
Take 1.5 grams of boron carbide powders (2 μ m, 98%), under 5MPa pressure, be molded into sheet, then put into sintering furnace,Be filled with argon gas, be warming up to 850 DEG C of sintering 7h, the boron carbide sheet after sintering is put into anodal basket as anodal, by high-purity high-densityDegree graphite rod (phosphorus content > 99.99%, density 1.5g/cm3) as negative pole, in electrolytic furnace, taking ceramic crucible as electrolytic cell, claimGet 240 grams of magnesium chlorides and put into ceramic crucible, in crucible electrical resistance furnace, pass into argon gas, be warming up to 750 DEG C and stable after, will be justNegative pole is put into ceramic crucible, and D.C. regulated power supply connects both positive and negative polarity energising 3.0V, carries out electrolysis 45 hours. After reaction finishes,The product that positive pole is obtained is washed by deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and deionized water washing, in air120 DEG C dry, then tests. Fig. 3 is the XRD figure of the boron carbide derived carbon of preparation. Fig. 8 is that the boron carbide of preparation spreads outThe TEM figure of raw carbon, as can be seen from the figure laminated structure and pore structure. Figure 13 is the different electric currents of the boron carbide derived carbon of preparationCharging and discharging curve figure under density, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation of obtained sample10 circle specific discharge capacities are 123.5F/g, and under 500mA/g, the specific discharge capacity of obtained sample is 102F/g, at 1000mA/gUnder, the specific discharge capacity of obtained sample is 77.7F/g; By nitrogen absorption under low temperature test b ETSurfaceArea=763.843m2/g。
Embodiment 3
Take 1.5 grams of silicon carbide powders (2 μ m, 98%), under 8MPa pressure, be molded into sheet, then put into sintering furnace,Be filled with argon gas, be warming up to 900 DEG C of sintering 5h, the silicon carbide plate after sintering is put into anodal basket as anodal, by high-purity high-densityDegree graphite rod (phosphorus content > 99.99%, density 1.5g/cm3) as negative pole, in electrolytic furnace, taking ceramic crucible as electrolytic cell, claimGet 240 grams of calcium chloride and put into ceramic crucible, in crucible electrical resistance furnace, pass into argon gas, be warming up to 900 DEG C and stable after, will be justNegative pole is put into crucible, and D.C. regulated power supply connects both positive and negative polarity energising 2.6V, carries out electrolysis 30 hours. After reaction finishes, willThe product that positive pole obtains is successively with deionized water washing, ultrasonic auxiliary 36% chlorohydric acid pickling, and deionized water washing, in air 120DEG C dry, then test. Fig. 4 is the XRD figure of the carborundum derived carbon of preparation. Fig. 9 is the carborundum derived carbon of preparationTEM figure, can find out obvious pore structure. Figure 14 is discharging and recharging under the different current densities of the carborundum derived carbon of preparationCurve map, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 circle electric discharge specific volumes of obtained sampleAmount is 143.8F/g, and under 500mA/g, the specific discharge capacity of obtained sample is 123F/g, under 1000mA/g, madeThe specific discharge capacity that obtains sample is 97.2F/g; By nitrogen absorption under low temperature test b ETSurfaceArea=988.5522m2/g。
Embodiment 4
Take 1.5 grams of tungsten-carbide powders (2 μ m, 98%), under 10MPa pressure, be molded into sheet, then put into sintering furnace,Be filled with argon gas, be warming up to 950 DEG C of sintering 3h, the tungsten carbide chip after sintering is connected and drawn as positive pole with electronic conductive material,By high-purity high-density degree graphite rod (phosphorus content > 99.99%, density 1.5g/cm3) as negative pole, in electrolytic furnace taking ceramic crucible asElectrolytic cell, the 240 grams of potassium chloride of weighing are put into ceramic crucible, in crucible electrical resistance furnace, pass into argon gas, are warming up to 1100 DEG C and steadyAfter fixed, both positive and negative polarity is put into crucible, D.C. regulated power supply connects both positive and negative polarity energising 2.2V, carries out electrolysis 15 hours. ReactionAfter end, the product that positive pole is obtained is washed by deionized water successively, ultrasonic auxiliary 36% chlorohydric acid pickling, and deionized water washing,In air, 120 DEG C are dried, and then test. Fig. 5 is the XRD figure of the tungsten carbide derived carbon of preparation. Figure 10 is preparationThe TEM figure of tungsten carbide derived carbon, as can be seen from the figure obvious pore structure. Figure 15 be preparation tungsten carbide derived carbon notWith the charging and discharging curve figure under current density, as can be seen from the figure: under the charge-discharge test of 300mA/g, obtained sampleCirculation 10 to enclose specific discharge capacity be 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 ETSurfaceArea=1137.7433m2/g。
Embodiment 5
Take 1.5 grams of chromium carbide powders (2 μ m, 98%), under 15MPa pressure, be molded into sheet, then put into sintering furnace,Be filled with argon gas, be warming up to 1000 DEG C of sintering 2h, the chromium carbide sheet after sintering is put into anodal basket and draw as positive pole, by high-purityHigh-density graphite rod (phosphorus content > 99.99%, density 1.5g/cm3) as negative pole, in electrolytic furnace taking ceramic crucible as electrolytic cell,The 240 grams of sodium chloride of weighing are put into ceramic crucible, in crucible electrical resistance furnace, pass into argon gas, be warming up to 1300 DEG C and stable after, willBoth positive and negative polarity is put into crucible, and D.C. regulated power supply connects both positive and negative polarity energising 1.8V, carries out electrolysis 2 hours. After reaction finishes, willThe product that positive pole obtains is successively with deionized water washing, ultrasonic auxiliary 36% chlorohydric acid pickling, deionized water washing, in air 120 DEG CDry, test. Fig. 6 is the XRD figure of the chromium carbide derived carbon of preparation. Figure 11 is the TEM of the chromium carbide derived carbon of preparationFigure, as can be seen from the figure laminated structure and pore structure. Figure 16 is charging and discharging under the different current densities of the chromium carbide derived carbon of preparationElectricity curve map, as can be seen from the figure: under the charge-discharge test of 300mA/g, the circulation 10 circle electric discharge ratios of obtained sampleCapacity is 114.22F/g, and 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 ETSurfaceArea=640.6837m2/g。
Claims (4)
1. fused salt electrolysis process is prepared a method for carbide-derived carbon, it is characterized in that: by metal carbide powders at 3-15MPaUnder pressure, compression molding is pressed into sheet, under inert gas shielding with the temperature sintering 2-8 hour of 800-1000 DEG C, by sinteringMetal carbides sheet, as positive pole, using high-purity high-density degree graphite rod as negative pole, is made electrolytic cell with ceramic crucible, and firing equipment isCrucible electrical resistance furnace, power supply is D.C. regulated power supply, in the electrolytic furnace under argon shield using fuse salt as electrolyte, electrolysis temperatureDegree 400-1300 DEG C, decomposition voltage 1.8V-3.2V, electrolysis time 2-60 hour, after electrolysis finishes, gets anodal electrolysateGo out, be cooled to room temperature, to anodal electrolysate wash successively, pickling, washing and drying and processing, prepared product isCarbide-derived carbon.
2. fused salt electrolysis process according to claim 1 is prepared the method for carbide-derived carbon, it is characterized in that: described positive poleBe using metal carbides 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 is prepared the method for carbide-derived carbon, it is characterized in that: describedMetallic carbide raw material is titanium carbide, boron carbide, carborundum, tungsten carbide, the chromium carbide of technical grade.
4. the fused salt electrolysis process of claim 1 is prepared the device of carbide-derived carbon, it is characterized in that: in crucible type resistance furnace stove, establishHave stainless steel electrolytic stove, it has a upper shed trough-shaped housing, and the opening of this housing is provided with the sealing upper cover being connected by securing member,Electrolytic furnace housing inner bottom part is provided with refractory brick, is equipped with ceramic crucible electrolytic cell above fire brick layer, is provided with metal carbides sheet in grooveAs positive pole, graphite rod cathode and molten salt electrolyte, the wire being connected with above-mentioned positive and negative electrode is leading to through electrolytic furnace upper cover respectivelyHole is connected with D.C. regulated power supply, covers the inlet/outlet pipe that is also respectively equipped with argon gas on electrolytic furnace, and wherein the inlet tube of argon gas is logicalCross the pipeline that is provided with flowmeter and be connected with argon bottle, on electrolytic furnace, cover and be also provided with a part and be placed in the thermocouple in electrolytic furnace,At the external chuck that is provided with cooling water turnover of electrolytic furnace.
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| US9764958B2 (en) | 2013-03-15 | 2017-09-19 | West Virginia University Research Corporation | Process for pure carbon production, compositions, and methods thereof |
| CN104099632B (en) * | 2014-06-03 | 2016-08-17 | 河北联合大学 | The method that the carbon thermal reduction metal sulfide that electrochemistry promotes prepares metal carbides |
| CN104018190B (en) * | 2014-06-17 | 2016-06-08 | 北京工业大学 | A kind of method that reclaims hard alloy scraps |
| WO2016064713A2 (en) | 2014-10-21 | 2016-04-28 | West Virginia University Research Corporation | Methods and apparatuses for production of carbon, carbide electrodes, and carbon compositions |
| CN104726890B (en) * | 2015-02-09 | 2017-07-04 | 银基烯碳新材料股份有限公司 | A kind of method that active carbon nanoparticles liquid is prepared based on electrolysis |
| CN105200458B (en) * | 2015-10-27 | 2017-09-29 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method for preparing titanium carbide |
| CN109312479B (en) * | 2016-04-20 | 2021-07-13 | 西弗吉尼亚大学研究公司 | Method, device and electrode for carbide-to-carbon conversion with nanostructured carbide compounds |
| CN106011943B (en) * | 2016-05-30 | 2017-12-15 | 安徽工业大学 | A kind of method that pure ferroalloy and carbide-derived carbon are prepared using carbon ferroalloy simultaneously as raw material |
| CN106082175B (en) * | 2016-08-25 | 2019-09-17 | 北京化工大学 | A method of melting sodium carbonate high temperature prepares carbide-derived carbon |
| CN110459769B (en) | 2019-07-17 | 2021-06-04 | 武汉大学 | High-dispersion silicon-carbon solid sol, preparation method and application thereof |
| CN111231137B (en) * | 2020-03-06 | 2022-06-03 | 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 |
| DE102022119516B3 (en) * | 2022-08-03 | 2024-02-01 | Skeleton Technologies GmbH | PRODUCTION OF POROUS CARBON FROM METAL CARBIDE |
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| GB777824A (en) * | 1952-11-13 | 1957-06-26 | Horizons Titanium Corp | Improvements in the electrolytic production of titanium |
| GB844587A (en) * | 1959-03-10 | 1960-08-17 | American Potash And Chemical C | Improvements in the production of boron |
| CN101914788A (en) * | 2010-07-26 | 2010-12-15 | 攀钢集团有限公司 | Method for preparing metallic titanium |
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| US8951401B2 (en) * | 2010-05-28 | 2015-02-10 | Toyota Boshoku Kabushiki Kaisha | Method for electrochemically depositing carbon film on a substrate |
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| GB777824A (en) * | 1952-11-13 | 1957-06-26 | Horizons Titanium Corp | Improvements in the electrolytic production of titanium |
| GB844587A (en) * | 1959-03-10 | 1960-08-17 | American Potash And Chemical C | Improvements in the production of boron |
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