CN102205962A - Device and method for preparing activated carbon material for electrochemical capacitor - Google Patents
Device and method for preparing activated carbon material for electrochemical capacitor Download PDFInfo
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Abstract
The invention provides a device and method for preparing an activated carbon material for an electrochemical capacitor, belonging to the technical fields of coal chemical industry and microwave chemistry. The method comprises the following preparation processes of: deashing coal particles serving as raw materials by using hydrochloric acid and hydrofluoric acid, modifying the deashed coal by using nitric acid in an auxiliary way, mixing the modified coal serving as a carbon source with potassium hydroxide and deionized water, stirring to obtain a mixture, stirring and evaporating the mixture to obtain a solid mixture, and then performing microwave-assisted activating, washing, drying and grinding on the solid mixture to obtain the activated carbon. The invention has the advantages that the activation time is only 20-30 minutes, the mass ratio of potassium hydroxide to coal is (0.5-3):1, the preparation process is simple, the microwave-assisted heating is uniform, efficient and energy-saving, the consumption of the potassium hydroxide is reduced, and the activation process has the advantages of uniformity and high efficiency. The prepared activated carbon is used as an electrode material of the electrochemical capacitor and has better stability and excellent comprehensive property.
Description
Technical field:
The invention belongs to Coal Chemical Industry and microwave chemical technical field, be specifically related to a kind of device and method for preparing electrochemical capacitor with absorbent charcoal material.
Background technology:
Gac has flourishing pore texture and special surface chemistry, has a wide range of applications in fields such as metallurgy, chemical industry, electronics, the energy and environmental protection.The raw material of producing gac mainly contains ature of coal, wooden and other carbon raw material.Wherein, wood material mainly is timber and all kinds of shell.Timber is cost to cut down forest, and the source of shell is limited.Rich coal resources in China accounts for 75% of the disposable energy.Wherein, the price of bottle coal is owing to be lower than coking coal and extremely people's favor.
The gac activation method mainly is divided into: physically activated and chemical activation method.The former is an activator with carbonic acid gas or water vapour; The latter is an activator with zinc chloride, phosphoric acid, potassium hydroxide or sodium hydroxide.Zinc chloride and phosphoric acid are usually used in containing the activation of cellulosic material; Potassium hydroxide is mainly used in the activation of coal and refinery coke.Present commercially available coal measures ash of active carbon content is higher, can only belong to low-quality gac as handling waste water and waste gas usefulness.High-quality coal measures gac on the market, main mode by routine heating potassium hydroxide activates and makes, and its soak time is longer, and activation temperature is higher, and the potassium hydroxide consumption is bigger.Patent CN200610123444.X has announced a kind of preparation method of high specific area anthrax active carbon.In this method, when the mass ratio of potassium hydroxide and coal is 4, adopt conventional heating method can make active carbon with high specific surface area at 900 ℃ of activation 2.5h.But its soak time is long, the energy consumption height, and the potassium hydroxide consumption is bigger, thus the production cost and the detergent active charcoal that have increased gac form the secondary pollution that waste water causes.Patent CN201010188981.9 has announced and has been used to gac for preparing carbon electrode of super capacitor and preparation method thereof.Wherein, after the needle coke process concentrated nitric acid and the vitriol oil are handled, when the needle coke mass ratio after potassium hydroxide and the processing is 4, mixture passes through the 1.5h stir process in 120 ℃ of baking ovens after, behind adopt that conventional heating means are heated to 100 ℃/min 800 ℃ and the constant temperature 1h, can make the gac of high-specific surface area and high specific volume.But in the above-mentioned patent, the quality of the potassium hydroxide that uses also is 4 times of carbon raw material, and the price of potassium hydroxide reaches 10,000 yuan/ton, thereby causes the increase of Activated Carbon Production cost.Simultaneously, aforesaid method also is to adopt conventional type of heating to prepare active carbon electrode material.Conventional heating is according to thermal conduction and radiation theory, heats from the outside ecto-entad of material, and rate of heating is slow, and the internal and external temperature field of granule materials is inhomogeneous, needs just can finish reactivation process through several hrs.And to obtain the high specific surface area gac, after having only the top layer hole of granule materials to be activated to collapse, granule materials central porisity could form.On the whole, conventional activation method length consuming time, power consumption is high, and alkali consumption is big.In addition, also need after the activation product is carried out pickling and washing, more residue alkali brings secondary pollutions such as waste water.Patent CN201010177879.9 has announced a kind of microwave complex activation method for preparing super porous carbon, this preparation method has used catalyzer iron powder and cobalt powder etc., there is microburst reaction to take place, makes microwave activation process instability, and increased the cost of activated carbon product.
Summary of the invention:
The present invention is directed to the deficiencies in the prior art, propose a kind of device and method for preparing electrochemical capacitor with absorbent charcoal material.
Device provided by the present invention comprises: microwave chemical reactor 1, microwave source 2, reactant 3, corundum crucible 4, quartzy protective guard 5, thermopair 6, temperature indicator 7, arm 8, nitrogengas cylinder 9, fluid collection vials 10, tail gas wash bottle 11; Described microwave source 2 is positioned at the Right Inboard of microwave chemical reactor 1, described quartzy protective guard 5 places in the microwave chemical reactor 1, described corundum crucible 4 places in the quartzy protective guard 5, and reactant 3 is positioned at corundum crucible 4, and described thermopair 6 is connected with reactant 3 and temperature indicator 7 respectively; An inlet is arranged at described microwave chemical reactor top, and nitrogengas cylinder 9 is introduced the nitrogen that discharges in the quartzy protective guard 5 by this inlet by pipeline; Described arm 8 links to each other with the pipeline on microwave chemical reactor 1 top, and these arm 8 mouths of pipe are downward-sloping to be connected with fluid collection vials 10, and described tail gas wash bottle 11 is connected with arm 8 by pipeline.
The temperature of corundum crucible 4 internal reaction things 3 is measured by thermopair 6, and the temperature of thermocouple measurement is shown by temperature indicator 7.An inlet is arranged at microwave chemical reactor top, has a pipeline to introduce the quartzy protective guard 5 from the nitrogen that nitrogengas cylinder 9 discharges in the inlet.The water vapour that nitrogen gas stream is carried secretly etc. is drawn by being installed in arm 8 microwave chemical reactor top, that the mouth of pipe is downward-sloping, and liquid product flows in the fluid collection vials 10 because of condensation in arm, and gaseous constituent enters tail gas wash bottle 11 and discharges after purifying.
Said apparatus is used to prepare the method for electrochemical capacitor with absorbent charcoal material, and these method concrete steps are as follows:
(1) preparation of de-ash coal: taking by weighing granularity is 180 purpose coal sample 100g, place the 1000mL glass beaker, the hydrochloric acid 500mL that slowly adds 6M, add the 2ml dehydrated alcohol then, stirring makes coal sample and solution thorough mixing, and sonic oscillation 30min is then in 55-60 ℃ of water bath with thermostatic control behind the heating 1h, to neutral, obtain the hydrochloric acid de-ash coal with the hot distilled water washing in 110 ℃ of vacuum-drying 2h; Above-mentioned hydrochloric acid de-ash coal is divided equally, place the 500mL plastic cup respectively, the hydrofluoric acid that adds 400mL 40% respectively, add the 2ml dehydrated alcohol then, stirring makes coal sample and solution thorough mixing, and sonic oscillation 30min is then in 55-60 ℃ of water bath with thermostatic control behind the heating 1h, to neutral, obtain the hydrofluoric acid de-ash coal with the hot distilled water washing in 110 ℃ of vacuum-drying 2h; Above-mentioned hydrofluoric acid de-ash coal is divided equally, place the big glass beaker of 1000mL respectively, the nitric acid that adds 500mL 2M respectively, add the 2ml dehydrated alcohol then, stirring makes coal sample and solution thorough mixing, and sonic oscillation 30min then heats 1h in 55-60 ℃ of water bath with thermostatic control, to neutral, obtain de-ash coal with the hot distilled water washing in 110 ℃ of vacuum-drying 2h;
(2) measure deionized water 30mL and place the 100mL beaker, 6-36g potassium hydroxide solid is dissolved in the deionized water, stir up to normal temperature fast, make alkali lye; Take by weighing the de-ash coal that 12g step (1) obtains and mix with described alkali lye, add the 5ml dehydrated alcohol then, stirring and evenly mixing obtains mixture; This mixture heated and stirred on the magnetic force heating stirrer is moved to this mashed prod in the ceramic mortar until forming mashed prod, and dry 1h in 110 ℃ of vacuum drying ovens obtains coal and alkali blended reactant;
(3) coal that step (2) is obtained and alkali blended reactant move in the corundum crucible 4, corundum crucible 4 is put into quartzy protective guard 5, quartzy protective guard 5 is placed in the microwave chemical reactor 1, with nitrogengas cylinder 9, quartzy protective guard 5, thermopair 6, fluid collection vials 10 and tail gas wash bottle 11 connect, open nitrogengas cylinder 9, with high pure nitrogen the air in the quartzy protective guard 5 is purged, behind the nitrogen purging 5min, set microwave power and be 700W and time between 20-30min, carry out microwave-assisted activation preparation gac, after the microwave-assisted activation finishes, when the temperature of temperature indicator 7 drops to below 200 ℃, close nitrogengas cylinder, gac head product cool to room temperature under air-proof condition that this step is made;
(4) the gac head product that makes with hot distilled water and dilute hydrochloric acid difference washing step (3), pH value until filtrate is 6-8, gac head product after will washing then is dry 1h in 110 ℃ of vacuum drying ovens, dried gac is ground to 325 orders, obtains the electrochemical capacitor absorbent charcoal material.
The gac that above-mentioned microwave-assisted potassium hydroxide activated coal makes all can obtain the alkaline solution that 71.8%-96.1% content does not wait in the washing link, and this solution is through can be used for the occasion of other needs after the simple process.
This method is carbon source with the de-ash coal, and potassium hydroxide is activator, and the mass ratio of potassium hydroxide and de-ash coal is 0.5-3: 1.Prepare absorbent charcoal material by microwave-assisted heating potassium hydroxide activation de-ash coal, the gained absorbent charcoal material is stayed in the corundum crucible, and prepared gac specific surface area is 834-1511m
2/ g, micropore pore volume are 0.34-0.60cm
3/ g.The gac that makes has stability and excellent comprehensive performance preferably as electrochemical capacitor electrode material.
The present invention has the following advantages:
1, adopts hydrochloric acid, hydrofluoric acid to the raw coal immersion treatment, can remove its ash content, and in raw coal, produce corresponding micropore; Then, utilize nitric acid dousing, can carry out modification, help activation pore-creating subsequently the coal behind the deliming.
2, utilize microwave that material is heated and to the selectivity heat characteristic of polar material from molecular level, overcome material temperature inside gradient, accelerated activator in material diffusion and react at active site, promoted the formation of raw material hole, shortened soak time, accelerate speed of response, improved the yield of gac, reached purpose energy-saving and cost-reducing and that reduce discharging.
3, the relative mass of used potassium hydroxide is less, has reduced the Activated Carbon Production cost.Simultaneously, reduced the secondary pollution that the activated carbon product washing water cause.
Description of drawings:
Fig. 1 is the device synoptic diagram of the embodiment of the invention 1,2,3,4 preparation absorbent charcoal materials.
Fig. 2 is the gac nitrogen suction-desorption isotherm of the embodiment of the invention 1,2,3,4 preparations.
Fig. 3 is that the specific volume of activated carbon electrodes of the embodiment of the invention 1,2,3,4 preparation is with the variation diagram of cycle index.
Among the figure: 1: microwave chemical reactor; 2: microwave source; 3: reactant; 4: corundum crucible; 5: quartzy protective guard; 6: thermopair; 7: temperature indicator; 8: arm; 9: nitrogengas cylinder; 10: fluid collection vials; 11: the tail gas wash bottle.
Embodiment:
Embodiment 1: be raw material with bituminous coal, concrete preparation process is as follows:
(1) 500mL hydrochloric acid (6M) is added 100g and cross in the 180 purpose bituminous coal, add the 2mL dehydrated alcohol again, stir and sonic oscillation mixture 30min; Mixture heats 1h in 55-60 ℃ of water bath with thermostatic control, extremely neutral with the hot distilled water washing, in 110 ℃ of following vacuum-drying 2h.Above-mentioned coal sample is divided into two parts places plastic beaker, add the hydrofluoric acid of 400mL 40% respectively, add the 2mL dehydrated alcohol, stir and sonic oscillation mixture 30min; In 55-60 ℃ of water bath with thermostatic control, heat 1h, extremely neutral with the hot distilled water washing, in 110 ℃ of following vacuum-drying 2h.Above-mentioned coal sample is divided into two parts places glass beaker, add the nitric acid of 500mL2M, add the 2mL dehydrated alcohol again, stir and sonic oscillation mixture 30min; In 55-60 ℃ of water bath with thermostatic control, heat 1h, to neutral,, promptly get de-ash coal in 110 ℃ of vacuum-drying 2h with the hot distilled water washing.Gained deliming pit ash is less than 0.2%.
(2) get de-ash coal 12g and the 6g potassium hydroxide that step (1) makes and be dissolved in the 30mL deionized water, stir fast and place the water cooling until returning to normal temperature with glass stick; Add the 5mL dehydrated alcohol again, use the glass stick stirring and evenly mixing; With this homomixture on the magnetic force heating stirrer heated and stirred until forming mashed prod; Mashed prod is transferred in the ceramic mortar, behind 110 ℃ of following vacuum-drying 1h, this mixture is transferred in the corundum crucible.Corundum crucible places the quartzy protective guard in the microwave chemical reactor, carries out the microwave-assisted heat-activated and prepare gac under 700W, 20min condition; Naturally cooling to room temperature, respectively with the distilled water and the dilute hydrochloric acid washing of heat, is 6-8 until the pH value of filtrate with the product after the activation.Behind 110 ℃ of following vacuum-drying 1h, be ground to 325 orders again, promptly get absorbent charcoal material and (be labeled as AC
0.5-700-20).The nitrogen absorption result shows, AC
0.5-700-20Specific surface area be 834m
2/ g, micropore pore volume are 0.34cm
3/ g.
(3) get the gac that step (2) makes, according to mass ratio be 89: 5: 6 with gac: carbon black: tetrafluoroethylene mixes.The gained homomixture is pressed onto thin slice on the nickel foam collector with 20MPa pressure after being pressed into uniform thin slice on the flour stranding machine, makes the electrode for electrochemical capacitor sheet; Electrode slice is behind 110 ℃ of following vacuum-drying 1h, at water system KOH and LiOH mixed electrolytic solution (H
2O: KOH: the LiOH mass ratio is 135: 50: 1) in vacuum be assembled into the button electrical condenser after soaking 1h.The constant current charge-discharge test result shows, under the 50mA/g discharge current density, and after 10 charge and discharge cycles, AC
0.5-700-20Specific volume be 198.0F/g, behind 1000 cycle charge-discharges, its specific volume is 181.8F/g, the specific volume conservation rate is 91.8%.
Embodiment 2: be raw material with bituminous coal, concrete preparation process is as follows:
(1) treatment process of feed coal and feed coal is with (1) among the embodiment 1, and pit ash is less than 0.2%.
(2) get de-ash coal 12g and the 24g potassium hydroxide that step (1) makes and be dissolved in the 30mL deionized water, stir fast and place the water cooling until returning to normal temperature with glass stick; Add the 5mL dehydrated alcohol again, use the glass stick stirring and evenly mixing; With this homomixture on the magnetic force heating stirrer heated and stirred until forming mashed prod; Mashed prod is transferred in the ceramic mortar, behind 110 ℃ of following vacuum-drying 1h, this mixture is transferred in the corundum crucible.Corundum crucible places the quartzy protective guard in the microwave chemical reactor, carries out the microwave-assisted heat-activated and prepare gac under 700W, 20min condition; Naturally cooling to room temperature, respectively with the distilled water and the dilute hydrochloric acid washing of heat, is 6-8 until the pH value of filtrate with the product after the activation.Behind 110 ℃ of following vacuum-drying 1h, be ground to 325 orders again, promptly get absorbent charcoal material and (be labeled as AC
2-700-20).The nitrogen absorption result shows, AC
2-700-20Specific surface area be 927m
2/ g, micropore pore volume are 0.36cm
3/ g.
(3) get the gac that step (2) makes, according to mass ratio be 89: 5: 6 with gac: carbon black: tetrafluoroethylene mixes.The gained homomixture is pressed onto thin slice on the nickel foam collector with 20MPa pressure after being pressed into uniform thin slice on the flour stranding machine, makes the electrode for electrochemical capacitor sheet; Electrode slice is behind 110 ℃ of following vacuum-drying 1h, at water system KOH and LiOH mixed electrolytic solution (H
2O: KOH: the LiOH mass ratio is 135: 50: 1) in vacuum be assembled into the button electrical condenser after soaking 1h.The constant current charge-discharge test result shows, under the 50mA/g discharge current density, and after 10 charge and discharge cycles, AC
2-700-20Specific volume be 283.9F/g, behind 1000 cycle charge-discharges, its specific volume is 245.9F/g, the specific volume conservation rate is 86.6%.
Embodiment 3: be raw material with bituminous coal, concrete preparation process is as follows:
(1) treatment process of feed coal and feed coal is with (1) among the embodiment 1, and pit ash is less than 0.2%.
(2) get de-ash coal 12g and the 36g potassium hydroxide that step (1) makes and be dissolved in the 30mL deionized water, stir fast and place the water cooling until returning to normal temperature with glass stick; Add the 5mL dehydrated alcohol again, use the glass stick stirring and evenly mixing; With this homomixture on the magnetic force heating stirrer heated and stirred until forming mashed prod; Mashed prod is transferred in the ceramic mortar, behind 110 ℃ of following vacuum-drying 1h, this mixture is transferred in the corundum crucible.Corundum crucible places the quartzy protective guard in the microwave chemical reactor, carries out the microwave-assisted heat-activated and prepare gac under 700W, 20min condition; Naturally cooling to room temperature, respectively with the distilled water and the dilute hydrochloric acid washing of heat, is 6-8 until the pH value of filtrate with the product after the activation.Behind 110 ℃ of following vacuum-drying 1h, be ground to 325 orders again, promptly get absorbent charcoal material and (be labeled as AC
3-700-20).The nitrogen absorption result shows, AC
3-700-20Specific surface area be 1365m
2/ g, micropore pore volume are 0.52cm
3/ g.
(3) get the gac that step (2) makes, according to mass ratio be 89: 5: 6 with gac: carbon black: tetrafluoroethylene mixes.The gained homomixture is pressed onto thin slice on the nickel foam collector with 20MPa pressure after being pressed into uniform thin slice on the flour stranding machine, makes the electrode for electrochemical capacitor sheet; Electrode slice is behind 110 ℃ of following vacuum-drying 1h, at water system KOH and LiOH mixed electrolytic solution (H
2O: KOH: the LiOH mass ratio is 135: 50: 1) in vacuum be assembled into the button electrical condenser after soaking 1h.The constant current charge-discharge test result shows, under the 50mA/g discharge current density, and after 10 charge and discharge cycles, AC
3-700-20Specific volume be 305.2F/g, behind 1000 cycle charge-discharges, its specific volume is 260.4F/g, the specific volume conservation rate is 85.3%.
Embodiment 4: be raw material with bituminous coal, concrete preparation process is as follows:
(1) treatment process of feed coal and feed coal is with (1) among the embodiment 1, and pit ash is less than 0.2%.
(2) get de-ash coal 12g and the 36g potassium hydroxide that step (1) makes and be dissolved in the 30mL deionized water, stir fast and place the water cooling until returning to normal temperature with glass stick; Add the 5mL dehydrated alcohol again, use the glass stick stirring and evenly mixing; With this homomixture on the magnetic force heating stirrer heated and stirred until forming mashed prod; Mashed prod is transferred in the ceramic mortar, behind 110 ℃ of following vacuum-drying 1h, this mixture is transferred in the corundum crucible.Corundum crucible places the quartzy protective guard in the microwave chemical reactor, carries out the microwave-assisted heat-activated and prepare gac under 700W, 30min condition; Naturally cooling to room temperature, respectively with the distilled water and the dilute hydrochloric acid washing of heat, is 6-8 until the pH value of filtrate with the product after the activation treatment.Behind 110 ℃ of following vacuum-drying 1h, be ground to 325 orders again, promptly get absorbent charcoal material and (be labeled as AC
3-700-30).The nitrogen absorption result shows, AC
3-700-30Specific surface area be 1511m
2/ g, micropore pore volume are 0.60cm
3/ g.
(3) get the gac that step (2) makes, according to mass ratio be 89: 5: 6 with gac: carbon black: tetrafluoroethylene mixes.Mixture is pressed onto thin slice on the nickel foam collector with 20MPa pressure after being pressed into uniform thin slice on the flour stranding machine, makes the electrode for electrochemical capacitor sheet; Electrode slice is behind 110 ℃ of following vacuum-drying 1h, at water system KOH and LiOH mixed electrolytic solution (H
20: KOH: the LiOH mass ratio is 135: 50: 1) in vacuum be assembled into the button electrical condenser after soaking 1h.The constant current charge-discharge test result shows, under the 50mA/g discharge current density, and after 10 charge and discharge cycles, AC
3-700-30Specific volume be 266.2F/g, behind 1000 cycle charge-discharges, its specific volume is 230.3F/g, the specific volume conservation rate is 86.5%.
Claims (2)
1. a device for preparing electrochemical capacitor with absorbent charcoal material is characterized in that this device comprises microwave chemical reactor (1), microwave source (2), reactant (3), corundum crucible (4), quartzy protective guard (5), thermopair (6), temperature indicator (7), arm (8), nitrogengas cylinder (9), fluid collection vials (10), tail gas wash bottle (11); Described microwave source (2) is positioned at the Right Inboard of microwave chemical reactor (1), described quartzy protective guard (5) places in the microwave chemical reactor (1), described corundum crucible (4) places in the quartzy protective guard (5), reactant (3) is positioned at corundum crucible (4), and described thermopair (6) is connected with reactant (3) and temperature indicator (7) respectively; An inlet is arranged at described microwave chemical reactor top, and nitrogengas cylinder (9) is introduced the nitrogen that discharges in the quartzy protective guard (5) by this inlet by pipeline; Described arm (8) links to each other with the pipeline on microwave chemical reactor (1) top, and this arm (8) mouth of pipe is downward-sloping to be connected with fluid collection vials (10), and described tail gas wash bottle (11) is connected with arm (8) by pipeline.
2. the described device of claim 1 is used to prepare the method for electrochemical capacitor with absorbent charcoal material, it is characterized in that these method concrete steps are as follows:
(1) preparation of de-ash coal: taking by weighing granularity is 180 purpose coal sample 100g, place the 1000mL glass beaker, the hydrochloric acid 500mL that slowly adds 6M, add the 2ml dehydrated alcohol then, stirring makes coal sample and solution thorough mixing, and sonic oscillation 30min is then in 55-60 ℃ of water bath with thermostatic control behind the heating 1h, to neutral, obtain the hydrochloric acid de-ash coal with the hot distilled water washing in 110 ℃ of vacuum-drying 2h; Above-mentioned hydrochloric acid de-ash coal is divided equally, place the 500mL plastic cup respectively, the hydrofluoric acid that adds 400mL 40% respectively, add the 2ml dehydrated alcohol then, stirring makes coal sample and solution thorough mixing, and sonic oscillation 30min is then in 55-60 ℃ of water bath with thermostatic control behind the heating 1h, to neutral, obtain the hydrofluoric acid de-ash coal with the hot distilled water washing in 110 ℃ of vacuum-drying 2h; Above-mentioned hydrofluoric acid de-ash coal is divided equally, place the big glass beaker of 1000mL respectively, the nitric acid that adds 500mL 2M respectively, add the 2ml dehydrated alcohol then, stirring makes coal sample and solution thorough mixing, and sonic oscillation 30min then heats 1h in 55-60 ℃ of water bath with thermostatic control, to neutral, obtain de-ash coal with the hot distilled water washing in 110 ℃ of vacuum-drying 2h;
(2) measure deionized water 30mL and place the 100mL beaker, 6-36g potassium hydroxide solid is dissolved in the deionized water, stir up to normal temperature fast, make alkali lye; Take by weighing the de-ash coal that 12g step (1) obtains and mix with described alkali lye, add the 5ml dehydrated alcohol then, stirring and evenly mixing obtains mixture; This mixture heated and stirred on the magnetic force heating stirrer is moved to this mashed prod in the ceramic mortar until forming mashed prod, and dry 1h in 110 ℃ of vacuum drying ovens obtains coal and alkali blended reactant;
(3) coal that step (2) is obtained and alkali blended reactant move in the corundum crucible (4), corundum crucible (4) is put into quartzy protective guard (5), quartzy protective guard (5) is placed in the microwave chemical reactor (1), with nitrogengas cylinder (9), quartzy protective guard (5), thermopair (6), fluid collection vials (10) and tail gas wash bottle (11) connect, open nitrogengas cylinder (9), with high pure nitrogen the air in the quartzy protective guard (5) is purged, behind the nitrogen purging 5min, set microwave power and be 700W and time between 20-30min, carry out microwave-assisted activation preparation gac, after the microwave-assisted activation finishes, when the temperature of temperature indicator (7) drops to below 200 ℃, close nitrogengas cylinder, gac head product cool to room temperature under air-proof condition that this step is made;
(4) the gac head product that makes with hot distilled water and dilute hydrochloric acid difference washing step (3), pH value until filtrate is 6-8, gac head product after will washing then is dry 1h in 110 ℃ of vacuum drying ovens, dried gac is ground to 325 orders, obtains the electrochemical capacitor absorbent charcoal material.
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| CN114823160A (en) * | 2022-04-11 | 2022-07-29 | 中国石油大学(华东) | Coal/heavy oil hydrogenation co-refining residue-based porous carbon electrode material and preparation method and application thereof |
| CN115974217A (en) * | 2022-12-28 | 2023-04-18 | 天津大学 | Deashing biochar composite electrode and preparation method and application thereof |
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