CN101092239A - Method for preparing super active carbon based on hickory with coal being adulterated - Google Patents
Method for preparing super active carbon based on hickory with coal being adulterated Download PDFInfo
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Abstract
This invention relates to a method for preparing coal-doped Carya cathayensis shell-based super activated carbon. The method solves the problem of low specific volumetric capacity of activated carbon prepared by using one raw material as the carbon precursor. The method also addresses the problem that coconut shell or walnut shell and solid KOH are difficult to be activated in microwave oven. Besides, KOH has a high cost, and activation at 800 deg.C may generate K vapor. The method comprises: pulverizing carbonized coal and Carya cathayensis shell in fine pulverizers, mixing uniformly according to a certain ratio, mixing the mixture with NaOH and ethanol uniformly, heating the mixture in an activation furnace, activating, cooling, washing with HCl, rinsing with tap water, filtering and drying to obtain coal-doped Carya cathayensis shell-based super activated carbon.
Description
Technical field
The present invention relates to a kind of gac, especially relate to the super active carbon based preparation method of a kind of coal doping pecan shell.
Background technology
At present, the research of ultracapacitor mainly concentrates on several aspects such as carbon electrode material, electrolytic solution and structure design, and wherein carbon electrode material is considered to the key that capacitive property improves, energy density, power density and the cycle performance etc. of decision ultracapacitor.Current, as electrode of super capacitor the raw material of wood-charcoal material package draw together super-activated carbon, active carbon fiber fabrics, charcoal-aero gel, carbon nanotube etc.The ultracapacitor that adopts charcoal-aero gel and carbon nanotube to make electrode has excellent capacitive property, but because complicated process of preparation, with high costs is difficult to carry out large-scale production.Active carbon fiber fabrics need pass through many steps such as spinning, braiding, charing and activation, and complicated process of preparation, cycle are long, and causes volumetric capacitance little because electrode density is low, is substituted by more high performance super-activated carbon just gradually.The carbon precursor of preparation super-activated carbon is divided into coal, refinery coke, resol, shell, pitch etc.The super-activated carbon of patent disclosure and bibliographical information generally all adopts a kind of as its carbon precursor in the above-mentioned materials, and the super-activated carbon of preparation all has its defective.With macropore proportion height in the super-activated carbon of common coal preparation,, be not suitable as electrode material for super capacitor so its specific surface is lower.Pitch is because of the complete processing complexity, and the product of preparation is few with the coal poor performance, does not have advantage so industrialness is promoted.Resol is because its complete processing complexity, as also needing technology such as curings before the carbon precursor, adds the material expensive of resin own, is difficult to reduce cost, and is easy to produce formaldehyde etc. in the solidification process and makes cancer gas, and workman's health is had certain nocuity.The super-activated carbon of refinery coke preparation though can reach very high specific surface area, owing to itself material density is lower, so the super-activated carbon bulk density that causes it to make is lower, influences the volumetric capacitance amount of ultracapacitor.Shell is because its material is hard, and the super-activated carbon bulk density of preparation is higher, but specific surface area is lower.The termination capacity of ultracapacitor depends on its volume and capacity ratio, large-scale promotion application depends on the cost of electrode materials, especially in modern society, under all very nervous situation of the energy, resource, seek a kind of high-volume and capacity ratio, it is particularly important that the super-activated carbon of low price becomes.
The Chinese invention patent publication number be CN1218004 disclosed be to reach 3130m2/g with the active carbon with high specific surface area specific surface area that Fugu, Shaanxi coal prepares according to a certain percentage with KOH, but its industrialized shortcoming is a KOH cost height, 800 ℃ of activation have potassium vapor to run out, safety problem is a bottleneck that influences industrialization, Fugu, Shaanxi calorific value of coal generally is not more than 6500 kilocalories in addition, if adopt NaOH can't prepare the super-activated carbon that volume and capacity ratio reaches 320F/ml as activator.The Chinese invention patent publication number is that disclosed being blended in the microwave oven with coconut husk or nut-shell and solid potassium hydroxide of CN1736859A activates, and the activator of employing also is KOH, and microwave method is difficult to realize industrialization.
Summary of the invention
The purpose of this invention is to provide the super active carbon based preparation method of a kind of coal doping pecan shell, it mainly is to solve existing in prior technology only to utilize a kind of starting material to be difficult to reach the problem of the super-activated carbon of high-volume and capacity ratio as carbon precursor; The present invention has also solved to be blended in the microwave oven with coconut husk or nut-shell and solid potassium hydroxide and has activated, and microwave method is difficult to realize industrialization, and KOH cost height has potassium vapor to run out after 800 ℃ of activation, and the technical problem of big potential safety hazard etc. is arranged.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
The super active carbon based preparation method of a kind of coal doping pecan shell of the present invention is characterized in that:
A. coal after the charing and the pecan shell after the charing are crushed to D respectively on pulverising mill
50To 500 orders, coal dust after will pulverizing then end and pecan shell powder are by mass ratio 5～1: 1 mixes at 300 orders;
B. mixture and NaOH, ethanol mix in proportion, and the mass ratio of mixture and NaOH is 1: 2～5, and mixture and alcoholic acid mass ratio be 1: 0.05～0.2;
C. above-mentioned solidliquid mixture is warming up to 300～450 ℃ in activation furnace, stops;
D. be warming up to 700～850 ℃, and stop activation;
E. activator is to be cooled after below 50 ℃, with behind the chlorohydric acid pickling again with tap water wash to pH value be 6～7, filter, oven dry promptly.
Pecan shell can be the pecan shell of Linan, Hangzhou institute special product.Coal and pecan shell all must be through charing, pulverizing back uniform mixing on double-cone dryer.The mixture of step b and sodium hydroxide are NaOH, ethanol can be even by 1: 3 mixed.The concentration of hydrochloric acid of step e can be 10wt%.
As preferably, described coal is the coal of thermal value greater than 7500 kilocalories.Because the thermal value of coal itself is big, so just can play abundant activatory effect before not reaching the sodium Metal 99.5 boiling point.
As preferably, described step b mixture soaked 12～36 hours add dissolve with ethanol with the warm water of NaOH equivalent and the water yield 5% with NaOH, when water mixes after.
As preferably, described activation furnace is a rotary kiln.Use rotary kiln can make material activating more even.
As preferably, described activation furnace rotating speed was 2 commentariess on classics/min before 320 degree, and 320 degree are later to be 5 commentaries on classics/min.Because bigger at 320 ℃ of vapour quantities, rotating speed is difficult for too fast, otherwise can also bring out powdered carbon.After 320 ℃ there be not basically steam, revving up to make material that better flowability is arranged.
As preferably, the coal of described step a be with the coarse particles coal under the protection of inert gas condition, with temperature rise rate to 350～450 of 5 ℃/min ℃ and stopped 4～6 hours, be warming up to 500～700 ℃ of charings then and formed in 1～3 hour.
As preferably, the solidliquid mixture of described step c temperature rise rate with 3 ℃/min in activation furnace rises to 320 degree, stops 2～5 hours.
As preferably, it is 1～5 hour that described steps d stops soak time.
As preferably, the concentration of hydrochloric acid among the step e is 8wt%～15wt%.
As preferably, being filtered among the described step e with deionized water filter 23～5 times.
Therefore, the present invention has with NaOH just can reach KOH activatory effect as activator, adding two kinds of carbon precursor mixtures has complementary advantages, the feasible super-activated carbon that makes, specific discharge capacity value and electrode density value reach ideal value, be that volume and capacity ratio reaches ideal value, cost is comparatively saved, and has avoided characteristics such as potassium vapor discharging.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1: the super active carbon based preparation method of a kind of coal doping pecan shell of this example the steps include:
A. the coarse particles coal under the protection of inert gas condition, with the temperature rise rate to 430 of 5 ℃/min ℃ and stop 5h, be warming up to 600 ℃ of charings 2 hours then; Coal after the charing and the pecan shell after the charing are crushed to D respectively on pulverising mill
50, mixed on the usefulness double-cone dryer than 1: 1 with the pecan shell powder quality by the coal dust end after pulverizing then to about 500 orders at 300 orders;
B. mixture and sodium hydroxide are that NaOH, ethanol are even by 1: 3 mixed, and soak 24 hours behind the dissolve with ethanol of the warm water of adding and NaOH equivalent and the water yield 5%;
C. above-mentioned solidliquid mixture temperature rise rate with 3 ℃/min in rotary kiln is risen to 320 degree, stopped 2～5 hours, this stage rotary kiln speed is made as 2 commentaries on classics/min;
D. continue to be warming up to 820 ℃ with the speed of 3 ℃/min, and stop activation 2 hours, this moment, rotary kiln speed was made as 5 commentaries on classics/min;
E. activator is to be cooled after below 50 ℃, with behind the 10wt% chlorohydric acid pickling again with tap water wash to pH value be 6～7, use deionized water filter 23～5 time at last, oven dry promptly.
The super active carbon based specific discharge capacity of preparing of coal doping pecan shell is 320F/g, and electrode density is 1g/ml, and volume and capacity ratio is 320F/ml.
Embodiment 2: the super active carbon based preparation method of a kind of coal doping pecan shell of this example the steps include:
A. the coarse particles coal under the protection of inert gas condition, with the temperature rise rate to 350 of 5 ℃/min ℃ and stopped 5 hours, be warming up to 500 ℃ of charings 2 hours then; Coal after the charing and the pecan shell after the charing are crushed to D respectively on pulverising mill
50, mixed on the usefulness double-cone dryer than 5: 1 with the pecan shell powder quality by the coal dust end after pulverizing then to about 500 orders at 300 orders;
B. mixture and sodium hydroxide are that NaOH is even by 1: 2 mixed, and soak 24 hours behind the dissolve with ethanol of the warm water of adding and NaOH equivalent and the water yield 5%;
C. above-mentioned solidliquid mixture temperature rise rate with 3 ℃/min in rotary kiln is risen to 320 degree, stopped 2～5 hours, this stage rotary kiln speed is made as 2 commentaries on classics/min;
D. continue to be warming up to 820 ℃ with the speed of 3 ℃/min, and stop activation 2 hours, this moment, rotary kiln speed was made as 5 commentaries on classics/min;
E. activator is to be cooled after below 50 ℃, with behind the 10wt% chlorohydric acid pickling again with tap water wash to pH value be 6～7, use deionized water filter 23～5 time at last, oven dry promptly.
The super active carbon based specific discharge capacity of preparing of coal doping pecan shell is 150F/g, and electrode density is 1.2g/ml, and volume and capacity ratio is 180F/ml.
Embodiment 3: the super active carbon based preparation method of a kind of coal doping pecan shell of this example the steps include:
A. the coarse particles coal under the protection of inert gas condition, with the temperature rise rate to 350 of 5 ℃/min ℃ and stopped 5 hours, be warming up to 500 ℃ of charings 2 hours then; Coal after the charing and the pecan shell after the charing are crushed to D respectively on pulverising mill
50, mixed on the usefulness double-cone dryer than 3: 1 with the pecan shell powder quality by the coal dust end after pulverizing then to about 500 orders at 300 orders;
B. mixture and sodium hydroxide are that NaOH is even by 1: 5 mixed, and soak 24 hours behind the dissolve with ethanol of the warm water of adding and NaOH equivalent and the water yield 5%;
C. above-mentioned solidliquid mixture temperature rise rate with 3 ℃/min in rotary kiln is risen to 320 degree, stopped 2～5 hours, this stage rotary kiln speed is made as 2 commentaries on classics/min;
D. continue to be warming up to 820 ℃ with the speed of 3 ℃/min, and stop activation 2 hours, this moment, rotary kiln speed was made as 5 commentaries on classics/min;
E. activator is to be cooled after below 50 ℃, with behind the 10wt% chlorohydric acid pickling again with tap water wash to pH value be 6～7, use deionized water filter 23～5 time at last, oven dry promptly.
The super active carbon based specific discharge capacity of preparing of coal doping pecan shell is 220F/g, and electrode density is 1.1g/ml, and volume and capacity ratio is 242F/ml.
Embodiment 4: the super active carbon based preparation method of a kind of coal doping pecan shell of this example the steps include:
A. the coarse particles coal under the protection of inert gas condition, with the temperature rise rate to 400 of 5 ℃/min ℃ and stopped 5 hours, be warming up to 700 ℃ of charings 2 hours then coal after the charing and the pecan shell after the charing are crushed to D respectively on pulverising mill
50, mixed on the usefulness double-cone dryer than 4: 1 with the pecan shell powder quality by the coal dust end after pulverizing then to about 500 orders at 300 orders;
B. mixture and sodium hydroxide are that NaOH is even by 1: 3 mixed, and soak 24 hours behind the dissolve with ethanol of the warm water of adding and NaOH equivalent and the water yield 5%;
C. above-mentioned solidliquid mixture temperature rise rate with 3 ℃/min in rotary kiln is risen to 320 degree, stopped 2～5 hours, this stage rotary kiln speed is made as 2 commentaries on classics/min;
D. continue to be warming up to 700 ℃ with the speed of 3 ℃/min, and stop activation 2 hours, this moment, rotary kiln speed was made as 5 commentaries on classics/min;
E. activator is to be cooled after below 50 ℃, with behind the 10wt% chlorohydric acid pickling again with tap water wash to pH value be 6～7, use deionized water filter 23～5 time at last, oven dry promptly.
The super active carbon based specific discharge capacity of preparing of coal doping pecan shell is 200F/g, and electrode density is 1.1g/ml, and volume and capacity ratio is 220F/ml.
Claims (10)
1. super active carbon based preparation method of coal doping pecan shell is characterized in that:
A. coal after the charing and the pecan shell after the charing are crushed to D respectively on pulverising mill
50To 500 orders, coal dust after will pulverizing then end and pecan shell powder are by mass ratio 5～1: 1 mixes at 300 orders;
B. mixture and NaOH, ethanol mix in proportion, and the mass ratio of mixture and NaOH is 1: 2～5, and mixture and alcoholic acid mass ratio be 1: 0.05～0.2;
C. above-mentioned solidliquid mixture is warming up to 300～450 ℃ in activation furnace, stops;
D. be warming up to 700～850 ℃, and stop activation;
E. activator is to be cooled after below 50 ℃, with behind the chlorohydric acid pickling again with tap water wash to pH value be 6～7, filter, oven dry promptly.
2. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that described coal is the coal of thermal value greater than 7500 kilocalories.
3. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that described step b mixture and NaOH, soaked 12～36 hours after adding the dissolve with ethanol with the warm water of NaOH equivalent and the water yield 5% when water mixes.
4. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that described activation furnace is a rotary kiln.
5. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that described activation furnace rotating speed was 2 commentaries on classics/min before 320 degree, 320 degree are 5 commentaries on classics/min later.
6. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1; the coal that it is characterized in that described step a is to use the coarse particles coal under the protection of inert gas condition; with temperature rise rate to 350～450 of 5 ℃/min ℃ and stopped 4～6 hours, be warming up to 500～700 ℃ of charings then and formed in 1～3 hour.
7. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that solidliquid mixture temperature rise rate with 3 ℃/min in activation furnace of described step c rises to 320 degree, stops 2～5 hours.
8. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that it is 1～5 hour that described steps d stops soak time.
9. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that the concentration of hydrochloric acid among the described step e is 8wt%～15wt%.
10. the super active carbon based preparation method of a kind of coal doping pecan shell according to claim 1 is characterized in that being filtered into deionized water filter 23～5 times among the described step e.
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| CN102602930A (en) * | 2012-03-22 | 2012-07-25 | 西安科技大学 | Method for preparing activated carbon by aid of compound activators |
| CN102633252A (en) * | 2012-04-26 | 2012-08-15 | 合肥工业大学 | Method for producing porous carbon for super capacitor by utilizing lignosulfonate |
| CN103682345A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院长春应用化学研究所 | Carbon-based electrode material, preparation method of carbon-based electrode material and energy storage device |
| CN103979536A (en) * | 2014-05-16 | 2014-08-13 | 宁夏宝塔石化科技实业发展有限公司 | Preparation method of special active carbon for adsorbing dioxin |
| CN104891492A (en) * | 2015-06-15 | 2015-09-09 | 威海文隆电池有限公司 | Preparation method for activated carbon with medium pore radii |
| CN105883799A (en) * | 2016-04-25 | 2016-08-24 | 贵州安凯达实业股份有限公司 | Method for improving activity of activated carbon |
| CN105923634A (en) * | 2016-05-06 | 2016-09-07 | 海南大学 | Coconut-shell fiber-based activated carbon for supercapacitor and preparation method of activated carbon |
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| CN109012602A (en) * | 2018-09-30 | 2018-12-18 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of cocoanut active charcoal |
| CN109205618A (en) * | 2018-11-27 | 2019-01-15 | 佛山市光烨环保科技有限公司 | A method of super capacitor active carbon is prepared using acid-sludge pitch |
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- 2007-06-25 CN CNB2007100697063A patent/CN100560483C/en not_active Expired - Fee Related
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| CN102602930A (en) * | 2012-03-22 | 2012-07-25 | 西安科技大学 | Method for preparing activated carbon by aid of compound activators |
| CN102633252A (en) * | 2012-04-26 | 2012-08-15 | 合肥工业大学 | Method for producing porous carbon for super capacitor by utilizing lignosulfonate |
| CN103682345A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院长春应用化学研究所 | Carbon-based electrode material, preparation method of carbon-based electrode material and energy storage device |
| CN103979536A (en) * | 2014-05-16 | 2014-08-13 | 宁夏宝塔石化科技实业发展有限公司 | Preparation method of special active carbon for adsorbing dioxin |
| CN104891492A (en) * | 2015-06-15 | 2015-09-09 | 威海文隆电池有限公司 | Preparation method for activated carbon with medium pore radii |
| CN107244670A (en) * | 2016-03-29 | 2017-10-13 | 四川大学 | A kind of bigger serface carbon material and preparation method thereof and for super capacitor material |
| CN105883799A (en) * | 2016-04-25 | 2016-08-24 | 贵州安凯达实业股份有限公司 | Method for improving activity of activated carbon |
| CN105883799B (en) * | 2016-04-25 | 2018-06-29 | 贵州安凯达实业股份有限公司 | A kind of activity carbon activity improves method |
| CN105923634A (en) * | 2016-05-06 | 2016-09-07 | 海南大学 | Coconut-shell fiber-based activated carbon for supercapacitor and preparation method of activated carbon |
| CN105923634B (en) * | 2016-05-06 | 2019-01-15 | 海南大学 | Supercapacitor coir fibre matrix activated carbon and preparation method thereof |
| CN106673477A (en) * | 2016-12-25 | 2017-05-17 | 常州创索新材料科技有限公司 | Preparation method of green concrete duct grouting material |
| CN107381572A (en) * | 2017-08-30 | 2017-11-24 | 章德恩 | A kind of capacitor bio-coal matrix activated carbon material and preparation method thereof |
| CN109012602A (en) * | 2018-09-30 | 2018-12-18 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of cocoanut active charcoal |
| CN109364874A (en) * | 2018-10-12 | 2019-02-22 | 南京航空航天大学溧水仿生产业研究院有限公司 | The preparation method of porous charing shell adsorbent material |
| CN109205618A (en) * | 2018-11-27 | 2019-01-15 | 佛山市光烨环保科技有限公司 | A method of super capacitor active carbon is prepared using acid-sludge pitch |
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