CN102431992A - Method for preparing porous carbon material by using magnesium oxide template in cooperation with activation of potassium hydroxide - Google Patents
Method for preparing porous carbon material by using magnesium oxide template in cooperation with activation of potassium hydroxide Download PDFInfo
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Abstract
The invention discloses a method for preparing a porous carbon material by using a magnesium oxide template in cooperation with the activation of potassium hydroxide, and belongs to the technical field of carbon materials and microwave chemistry. The method comprises the following steps of: grinding coal tar pitch serving as a carbon source, nano magnesium oxide serving as a template and the potassium hydroxide serving as an activating agent; transferring the mixture to a corundum crucible; and putting into a microwave reactor, performing one-step microwave heating activation, and thus obtaining the porous carbon material for an electrochemical capacitor, wherein the specific surface area of the obtained porous carbon material is between 439 and 1,394m<2>/g, the total pore volume is between 0.23 and 0.94cm<3>, the average pore size is between 1.95 and 3.36mm, the ratio of the volume of a non-micro pore to the total pore volume is between 26.1 and 86.2 percent, and the porous carbon yield is between 37.8 and 84.9 percent. The invention has the advantages that: the method is quick and energy-saving; and the prepared porous carbon is used as an electrode material of the electrochemical capacitor and has extremely high stability and high comprehensive performance.
Description
Technical field
The invention belongs to raw material of wood-charcoal material and microwave chemical technical field, be specifically related to the method that the collaborative Pottasium Hydroxide activation of a kind of Natural manganese dioxide template prepares porous carbon material.
Background technology
Porous charcoal has flourishing pore texture and special surface chemistry, has a wide range of applications in fields such as metallurgy, chemical industry, the energy and environmental protection.The production and the applicating history of porous charcoal are long, are the electrode materialss that ultracapacitor adopts the earliest.The raw material of production porous charcoal mainly contains coal, oil and biomass etc.Coal-tar pitch is the by product in the coal tar course of processing, and China's coal-tar pitch output is very big, and existing coal-tar pitch is mid-temperature pitch mostly.Contain unsaturated aromatic hydrocarbon in the mid-temperature pitch; Aging faster under oxygen, water, sunlight, the action of ultraviolet ray in air than petroleum pitch; And the harmful composition that contains in the medium temperature coal pitch is many than petroleum pitch, therefore, and the limited use system of medium temperature coal pitch in urban construction such as super highway.The medium temperature coal pitch ash content is low, and is cheap, if can utilize medium temperature coal pitch to come the production porous charcoal, will help enlarging the purposes of medium temperature coal pitch, reduces the production cost of porous charcoal.
Adopt template or chemical activation method to prepare porous charcoal by coal-tar pitch.Mainly adopt hard template method such as silicon-dioxide in the template, the removal of hard template needs hydrofluoric acid wash, causes hard template technology environmental pollution serious.Be acvator mainly in the chemical activation method, adopt common tube furnace to heat with Pottasium Hydroxide, salt of wormwood, phosphoric acid and zinc chloride.The conventional chemical activation method not only heat-up time long, energy consumption is high, and used acvator large percentage, it is seriously polluted that washes causes, cost is high.Exploration prepares electrochemical capacitor by the collaborative Pottasium Hydroxide activation medium temperature coal pitch of Natural manganese dioxide template and has environmental protection and the double meaning that economizes on resources with porous carbon material.
Patent 200910043229.2 has been announced a kind of preparation method of porous carbon material used for storing energy.This method is that 6nm, specific surface area are 1100m with the mean pore size
2The silicon-dioxide of/g is template; Mesophase pitch is a carbon source; Pitch and silicon-dioxide are put into electric furnace after grinding mixing, under nitrogen protection, are incubated 8h after with the temperature rise rate of 5 ℃/min electric furnace being warming up to 300 ℃; Be incubated 1h after with the temperature rise rate of 10 ℃/min electric furnace being warming up to 900 ℃ then, under nitrogen protection, be cooled to room temperature at last; After hydrofluoric acid with 30% was removed silica template, washing, filtration, 100 ℃ of dryings, the specific surface area of the porous charcoal that makes was 600m
2/ g, mean pore size is 5.0nm, the specific volume of porous charcoal reaches 220F/g.Patent 03178572.7 has been announced a kind of preparation method who is rich in the asphalt-base globular active carbon of mesopore.This method is to be that 105 ℃ pitch is raw material with softening temperature, and preparing softening temperature 300 ℃ of following oxidations is 250 ℃ pitch.Behind the naphthalene of adding 15% under 270 ℃, cool to 180 ℃, add 2% heat-reactive phenolic resin, 1% polyethylene of dispersing agent alcohol stirs; The balling-up pitch of adding 5% is warming up to 200 ℃ under whipped state in 1% polyvinyl alcohol water solution, makes balling-up pitch after the cooling; The pitch protocorm is warming up to 300 ℃ with the temperature rise rate of 0.5 ℃/min obtains not molten drop in air; Will be not in activated reactor the molten asphalt ball be warming up to 850 ℃ of charings with the speed of 10 ℃/min; Feed steam activation simultaneously, the specific surface area of the spheric active carbon that makes is 1198m
2/ g, total pore volume is 0.79cm
3/ g, non-micropore pore volume is 0.32cm
3/ g, the ratio of non-micropore pore volume is 40%.Patent 98123530.1 has been announced a kind of preparation method of mesopore asphalt-base globular active carbon.This method be with the asphalt-base globular active carbon that an activation makes with certain specific surface area in solution of metal compound such as iron protochloride and NSC 51149, flood and drying after; Under 800-1000 ℃, carry out re-activation with water vapour or carbonic acid gas, the gac specific surface area that makes is at 1048-1650m
2Between/the g, the mesopore aperture concentrates between the 2-4nm, and total pore volume is between 0.22-0.58cm
3Between/the g, the ratio of mesopore volume reaches 70%.Patent 200810037093.X has announced a kind of preparation method of high-carbon yield asphalt group spherical absorbent charcoal.This method is passed through not molten asphalt ball and chemical activating agent zinc chloride or phosphoric acid solution mixing; Be heated to 300-800 ℃ then and carry out charing, activation; After pickling, washing, make asphalt-base spherical activated carbon, the specific surface area of gained gac is between 1100-1320m
2Between/the g, total pore volume is between 0.54-0.63cm
3Between/the g, the gac yield is between 32-90%.
It is carbon source that paper " preparation of mesophase pitch based mesoporous carbons using an imprinting method " (New carbon materials 22 (2007) 259-263) has proposed with the mesophase pitch; Use nanometer silica gel to adopt print process to prepare the mesopore charcoal as pore-forming material; Mesophase pitch and silica-gel mixture are after 5h stirs in the paper; Behind 340-400 ℃ of thermal treatment 2h at 900 ℃ of charing 2h; The gained mixture repeatedly washs 2h with the 3M sodium hydroxide solution in 94 ℃, and then at room temperature washs 12h to remove the silica gel template with 37% hydrofluoric acid, and the specific surface area of gained coal-tar pitch base mesopore charcoal is 140m
2/ g, its total pore volume is 0.31cm
3/ g.Paper " preparation and the chemical property thereof of template coal-tar pitch base mesopore charcoal " (novel charcoal material; 26 (2011) 187-191) having proposed with the coal-tar pitch is carbon source; Use silicon-dioxide to adopt vapor phase process to prepare the mesopore charcoal as template, coal-tar pitch heats mixture with six sections temperature programmings after 5h stirs than the mixture for 1:1.2 with the silicon-dioxide quality in the paper, subsequently; Feed dioxide gas at 900 ℃ and carry out activation, make the mesopore charcoal with the hydrofluoric acid wash activation products at last; Wherein, when soak time during between 90-150min, the specific surface area of gained mesopore charcoal is between 838-1360m
2Between/the g, its specific volume reaches 146F/g.
Can find out from above-mentioned document, be carbon source with the coal-tar pitch, adopts hard template or chemical activation method to add the technology of hot preparation porous charcoal through routine, and its soak time is long, and energy consumption is high, and the cost height is seriously polluted.Conventional heating is based on heat conduction and radiation theory, heats from the outside ecto-entad of material, and its firing rate is slow, and the internal and external temperature field of granule materials is inhomogeneous, needs could accomplish activation process through several hrs.And to obtain the high specific surface area porous charcoal, 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 cost is high.
Summary of the invention
The present invention is directed to the deficiency that exists in the existing porous carbon material technology of preparing, propose the method that the collaborative Pottasium Hydroxide activation of a kind of Natural manganese dioxide template prepares porous carbon material, these method concrete steps are following:
(1) pre-treatment of coal-tar pitch: coal-tar pitch is ground to particle diameter less than 74 μ m, obtains pretreated coal-tar pitch, the coal-tar pitch air-dried moisture is 1.13%, and ash content is 0.16%, and volatilization is divided into 57.5%, and fixed carbon is 41.21%, and softening temperature is 110 ℃;
(2) grinding of reactant: take by weighing the pretreated coal-tar pitch of a certain amount of step (1) gained and put into mortar; Add Natural manganese dioxide and a certain amount of solid potassium hydroxide that a certain amount of particle diameter is 50nm; Add coal-tar pitch, Natural manganese dioxide and Pottasium Hydroxide three mixture total mass be 27g, said coal-tar pitch quality is between 4.2-14.5g, the Natural manganese dioxide quality is between 0-16.8g; The Pottasium Hydroxide quality is between 6-12.5g, with obtaining reactant behind said three's mixture grinding 1h;
(3) preparation of porous charcoal: the reactant transfer that obtains step (2) is to corundum crucible; Place in the microwave reactor, the setting microwave power is 600W, carries out the microwave heating activation of 30min; With putting into beaker after the activation products cool to room temperature taking-up that obtains after the activation; The 2M dilute sulphuric acid that in beaker, adds certain volume stirs the ultrasonic concussion 30min in back, after beaker at room temperature leaves standstill 48h, obtains porous charcoal after using pH value that 70-80 ℃ distilled water wash activation products extremely filtrate as 6-7; Place loft drier behind 110 ℃ of freeze-day with constant temperature 24h, to be ground to 325 orders the porous charcoal after the washing, obtain electrochemical capacitor and use porous carbon material.
This method is carbon source with the coal-tar pitch, and nano magnesia is a template, and Pottasium Hydroxide is acvator, makes electrochemical capacitor through microwave heating and uses porous carbon material.Gained porous carbon material specific surface area is between 439-1394m
2Between/the g, total pore volume is between 0.23-0.94cm
3Between/the g, mean pore size is between 1.95-3.36nm, and the ratio that non-micropore pore volume accounts for total pore volume is between 26.1-86.2%, and the porous charcoal productive rate is between 37.8-84.9%.The porous charcoal that makes has good stability and excellent comprehensive performance as electrochemical capacitor electrode material.
The present invention has the following advantages:
1, coal-tar pitch is as the pyrogenic by product of coal, has that low ash, amount are easy to get greatly, inexpensive advantage.
2, used Natural manganese dioxide template is a soft template, can be easy to remove with common dilute acid soln.
3, utilize microwave that granule materials is heated and to the selectivity heat characteristic of polar material from molecular level; Overcome the internal temperature gradient of granule materials; Accelerate priming reaction speed, shortened soak time, promoted the formation of raw material hole; Improve the yield of porous charcoal, reached energy saving purposes.
4, Natural manganese dioxide and Pottasium Hydroxide synergy has the mesopore of controlled modulation porous carbon electrode material and the function of micropore ratio, can improve the cyclical stability of porous carbon electrode.
Description of drawings
Fig. 1 is the porous charcoal nitrogen adsorption desorption thermo-isopleth of the embodiment of the invention 2,3,5 preparations.
Fig. 2 is the main graph of pore diameter distribution of porous charcoal of the embodiment of the invention 2,3,5 preparations.
Fig. 3 is that the energy density of porous charcoal electrical condenser of the embodiment of the invention 2,3,5 preparation is with the variation diagram of cycle index.
Fig. 4 is energy density and the graph of a relation of average power density that the present invention implements the porous charcoal electrical condenser of 2,3,5 preparations.
Embodiment
Embodiment 1: porous charcoal PC
4.2-16.8-6Concrete preparation process is following:
(1) pre-treatment of coal-tar pitch: coal-tar pitch is ground to particle diameter less than 74 μ m, obtains pretreated coal-tar pitch, gained coal-tar pitch air-dried moisture is 1.13%, and ash content is 0.16%, and volatilization is divided into 57.5%, and fixed carbon is 41.21%, and softening temperature is 110 ℃.
(2) grinding of reactant: take by weighing the pretreated coal-tar pitch of 4.2g step (1) gained and put into mortar, adding the 16.8g particle diameter is the Natural manganese dioxide of 50nm, adds the 6g solid potassium hydroxide, and three's mixture obtains reactant after grinding 1h.
(3) preparation of porous charcoal: the reactant feed that step (2) is obtained moves in the corundum crucible; Corundum crucible is placed in the microwave chemical reactor, nitrogengas cylinder, quartzy protective guard, corundum crucible, thermopair, fluid collection vials and tail gas wash bottle are connected, open nitrogengas cylinder; With high pure nitrogen the air in the corundum crucible is purged; Behind the nitrogen purging 5min, setting microwave power is that 600W and soak time are 30min, carries out microwave heating activation and prepares porous charcoal; Microwave heating activation when the temperature of temperature indicator drops to 200 ℃, is closed nitrogengas cylinder after finishing, and obtains activation products behind the cool to room temperature.
(4) activation products that step (3) obtained are put into beaker; The dilute sulphuric acid that adds 360mL 2M in the beaker stirs the ultrasonic concussion 30min in back; After beaker at room temperature leaves standstill 48h; Obtain porous charcoal after using 70-80 ℃ distilled water wash activation products to pH value of filtrate as 6-7, place loft drier behind 110 ℃ of freeze-day with constant temperature 24h, to be ground to 325 orders the porous charcoal after the washing, the gained porous carbon material is labeled as PC
4.2-16.8-6
Embodiment 2: porous charcoal PC
7-14-6Concrete preparation process is following:
(1) pre-treatment of coal-tar pitch: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, difference is that the coal-tar pitch that takes by weighing is 7g, Natural manganese dioxide is 14g, Pottasium Hydroxide is 6g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement, difference be add the 2M dilute sulphuric acid amount be 300mL, the gained porous carbon material is labeled as PC
7-14-6
Embodiment 3: porous charcoal PC
9-12-6Concrete preparation process is following:
(1) pre-treatment of coal-tar pitch: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, difference is that the coal-tar pitch that takes by weighing is 9g, Natural manganese dioxide is 12g, Pottasium Hydroxide is 6g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement, difference be add the 2M dilute sulphuric acid amount be 270mL, the gained porous carbon material is labeled as PC
9-12-6
Embodiment 4: porous charcoal PC
14-7-6Concrete preparation process is following:
(1) pre-treatment of coal-tar pitch: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, difference is that the coal-tar pitch that takes by weighing is 14g, Natural manganese dioxide is 7g, Pottasium Hydroxide is 6g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement, difference be add the 2M dilute sulphuric acid amount be 170mL, the gained porous carbon material is labeled as PC
14-7-6
Embodiment 5: porous charcoal PC
14.5-0-12.5Concrete preparation process is following:
(1) pre-treatment of coal-tar pitch: according to embodiment 1 in the same method of step (1) implement.
(2) according to embodiment 1 in the same method of step (2) implement, difference is that the coal-tar pitch that takes by weighing is 14.5g, Natural manganese dioxide is 0g, Pottasium Hydroxide is 12.5g.
(3) according to embodiment 1 in the same method of step (3) implement.
(4) according to embodiment 1 in the same method of step (4) implement, difference be add the 2M dilute sulphuric acid amount be 85mL, the gained porous charcoal is labeled as PC
14.5-0-12.5
Embodiment 1-5 gained porous carbon material pore structure analysis result is listed in the table 1.
Claims (1)
1. a Natural manganese dioxide template is worked in coordination with the method that the Pottasium Hydroxide activation prepares porous carbon material, it is characterized in that these method concrete steps are following:
(1) pre-treatment of coal-tar pitch: coal-tar pitch is ground to particle diameter less than 74 μ m, obtains pretreated coal-tar pitch, the coal-tar pitch air-dried moisture is 1.13%, and ash content is 0.16%, and volatilization is divided into 57.5%, and fixed carbon is 41.21%, and softening temperature is 110 ℃;
(2) grinding of reactant: take by weighing the pretreated coal-tar pitch of a certain amount of step (1) gained and put into mortar; Add Natural manganese dioxide and a certain amount of solid potassium hydroxide that a certain amount of particle diameter is 50nm; Add coal-tar pitch, Natural manganese dioxide and Pottasium Hydroxide three mixture total mass be 27g, said coal-tar pitch quality is between 4.2-14.5g, the Natural manganese dioxide quality is between 0-16.8g; The Pottasium Hydroxide quality is between 6-12.5g, with obtaining reactant behind said three's mixture grinding 1h;
(3) preparation of porous charcoal: the reactant transfer that obtains step (2) is to corundum crucible; Place in the microwave reactor, the setting microwave power is 600W, carries out the microwave heating activation of 30min; With putting into beaker after the activation products cool to room temperature taking-up that obtains after the activation; The 2M dilute sulphuric acid that in beaker, adds certain volume stirs the ultrasonic concussion 30min in back, after beaker at room temperature leaves standstill 48h, obtains porous charcoal after using pH value that 70-80 ℃ distilled water wash activation products extremely filtrate as 6-7; Place loft drier behind 110 ℃ of freeze-day with constant temperature 24h, to be ground to 325 orders the porous charcoal after the washing, obtain electrochemical capacitor and use porous carbon material.
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| CN108975302A (en) * | 2018-07-05 | 2018-12-11 | 中冶焦耐(大连)工程技术有限公司 | A kind of preparation method and application of the low graphitized carbon material of asphaltic base |
| CN109133050A (en) * | 2018-09-25 | 2019-01-04 | 安徽工业大学 | The preparation method of acid dyes indyl porous charcoal nanometer sheet in a kind of absorption waste water |
| CN109279601A (en) * | 2018-11-27 | 2019-01-29 | 西安交通大学 | A kind of porous carbon materials and the preparation method and application thereof with carbonization structure |
| CN110127692A (en) * | 2019-05-24 | 2019-08-16 | 许皖 | A kind of preparation method of mesoporous heat-resistant activity charcoal |
| CN110683529A (en) * | 2019-11-26 | 2020-01-14 | 陕西延长石油（集团）有限责任公司 | Preparation method of coal-series one-dimensional porous carbon material |
| CN112850707A (en) * | 2021-02-05 | 2021-05-28 | 汪炜 | Preparation method of activated carbon |
| CN113184847A (en) * | 2021-04-15 | 2021-07-30 | 安徽工业大学 | Porous carbon material and preparation method and application thereof |
| CN113277509A (en) * | 2021-05-26 | 2021-08-20 | 中国科学技术大学 | Porous carbon nano material and preparation method thereof |
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