CN104709905A - Method for preparing supercapacitor-dedicated active carbon by using mixed molten salts as activator - Google Patents
Method for preparing supercapacitor-dedicated active carbon by using mixed molten salts as activator Download PDFInfo
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- CN104709905A CN104709905A CN201310685936.8A CN201310685936A CN104709905A CN 104709905 A CN104709905 A CN 104709905A CN 201310685936 A CN201310685936 A CN 201310685936A CN 104709905 A CN104709905 A CN 104709905A
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Abstract
The invention discloses a method for preparing supercapacitor-dedicated active carbon by using mixed molten salts as an activator. According to the method, asphalt or coal tar which is used as a raw material is uniformly mixed with mixed molten salts; under protection of argon or nitrogen, the mixture is placed in a carbonization furnace to be carbonized; and finally, the carbonized product is crushed, washed and dried to obtain active carbon. The active carbon has high specific surface area and effective mesopore-micropore pore size distribution, and has high electrochemical specific capacity and good high-current charge discharge capability and cycling stability.
Description
Technical field
The present invention relates to a kind of fused salt mixt that utilizes and prepare the method for activated carbon for super capacitors for activator.
Background technology
Industrial production and the applicating history of gac are long, and absorbent charcoal material is not agraphitic carbon in general sense, neither complete crystalline carbon as diamond, but have the laminate structure of the basic crystallite of similar graphite.Gac, based on carbon, combines with hydrogen, oxygen, nitrogen etc., has good adsorption.Gac wide material sources, there is high specific surface area, excellent conductivity, fabulous chemical stability and the lower coefficient of expansion, and the features such as variform can be made as required, make it be widely used in the field such as liquid phase adsorption, Gas Phase Adsorption, catalyzer and carrier thereof, blood purification, car carbon tank, and become ultracapacitor and use maximum a kind of electrode materialss.Research shows, high specific surface area and effective pore size distribution are the principal elements that absorbent charcoal material produces high electrochemical specific capacity.
At present, prepare active carbon method and can be divided into physical activation method, chemical activation method and fly ash method.Chemical activation is large to equipment corrosion, contaminate environment, and residual chemicals activator in its obtained gac, application aspect is restricted.The yield of physically activated production gac is not high, and activation temperature is higher, first need carry out charing reactivate.Current countries in the world all in research, inquire into chemical activation method and physical activation method combined, by novel production technique, produce pore texture more rationally, flourishing, absorption property is more superior, purposes activated carbon product widely.
Conventional activated carbon is generally prepared by raw material with coal, impurity ash oontent due to coal is high causes that the impurity ash oontent of gac is high, specific surface area is low, absorption property is not good, chemical property is poor, and this just directly affects gac application in a lot of fields.In addition, mostly adopt KOH to be activator when preparing gac, this just increases the corrosion to activation equipment, adds production cost, is also unfavorable for its widespread use.China is coke production big country of the world, pitch and tar resource enrich, and impurity ash oontent is lower, if a kind of simple, controlled, quick, efficient, less energy-consumption, corrosion-free, pollution-free and the method for constant product quality prepares gac on a large scale by pitch or coal tar can be invented, very important meaning will be produced to its further development and application.
Summary of the invention
The object of the present invention is to provide a kind of is activator with fused salt mixt; the method of gac prepared by pitch or coal tar one step carbonization-activation; this method preparation technology is simple; with low cost; and process safety is controlled; be applicable to large-scale production absorbent charcoal material, and the gac specific surface area of preparation is high, is applicable to prepare activated carbon for super capacitors.
The present invention adopts pitch or coal tar to be raw material, is mixed together evenly, under argon gas or nitrogen protection, mixture is placed in itself and fused salt mixt charring furnace and carbonizes, washs drying, namely obtain gac after finally the product after charing being pulverized.
Utilize fused salt mixt to prepare a method for activated carbon for super capacitors for activator, it is characterized in that the method step is:
1) with pitch or coal tar for raw material, by its with by LiCl and ZnCl
2composition fused salt mixt or by NaCl and ZnCl
2composition fused salt mixt or by KCl and ZnCl
2the fused salt mixt of composition mixes, and obtains mixture;
2) under argon gas or nitrogen protection, mixture is carbonized 0.5 h ~ 5 h at 600 DEG C ~ 1200 DEG C;
3) again with clear water washing after being pulverized by the product after charing, the absorbent charcoal material of black after oven dry, is obtained.
Of the present invention by LiCl and ZnCl
2the fused salt mixt of composition consists of LiCl 15 ~ 45 wt%, ZnCl
255 ~ 85 wt%.
Of the present invention by NaCl and ZnCl
2the fused salt mixt of composition consists of NaCl 15 ~ 45 wt%, ZnCl
255 ~ 85 wt%.
Of the present invention by KCl and ZnCl
2the fused salt mixt of composition consists of KCl 15 ~ 45 wt%, ZnCl
255 ~ 85 wt%.
The mass ratio of fused salt mixt of the present invention and pitch or coal tar is 6:1 ~ 1:1.
The temperature rise rate of charing of the present invention is 0.5 DEG C/min ~ 10 DEG C/min, and carbonization temperature is preferably 800 DEG C ~ 1000 DEG C, and carbonization time is preferably 1 h ~ 2 h.
Feature of the present invention and beneficial effect are:
Cost of the present invention is low, a step carbonization process is simple, can prepare in a large number and process safety is controlled, the gac prepared has very high specific surface area and effectively mesoporous-micropore size distribution, has high electrochemical specific capacity, good high rate during charging-discharging and cyclical stability.
Utilize fused salt mixt for activator, a step carbonization-activation preparation has the absorbent charcoal material of excellent chemical property, is an effective way of development high specific energy, low-cost super electrical condenser.In addition, the added value of high performance active carbon material is high, also can be used for the industry such as industrial adsorbents and lithium ion battery.
Accompanying drawing explanation
Fig. 1 is with KCl and ZnCl
2mixture be fused salt mixt, pitch is carbon source, carbonization at 1000 DEG C, when fused salt mixt and pitch content are 3:1, the N of gained gac
2adsorption/desorption curve
Fig. 2 is the graph of pore diameter distribution corresponding with Fig. 1.
Fig. 3 is with KCl and ZnCl
2mixture be fused salt mixt, pitch is carbon source, carbonization at 1000 DEG C, when fused salt mixt and pitch content are 3:1, the scanning electron microscope (SEM) photograph of gained gac.
Fig. 4 is with NaCl and ZnCl
2mixture be fused salt mixt, coal tar is carbon source, carbonization at 800 DEG C, when fused salt mixt and coal tar ratio are 4:1, the N of gained gac
2adsorption/desorption curve.
Fig. 5 is the graph of pore diameter distribution corresponding with Fig. 4.
Fig. 6 is with LiCl and ZnCl
2mixture be fused salt mixt, coal tar is carbon source, carbonization at 1200 DEG C, when fused salt mixt and coal tar ratio are 2:1, the N of gained gac
2adsorption/desorption curve.
Fig. 7 is the graph of pore diameter distribution corresponding with Fig. 6.
Embodiment
Embodiment 1
Employing pitch is carbon source, KCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 35 wt% KCl and 65 wt% ZnCl
2mix, after pitch is added, the ratio of mixing salt and pitch is 3:1.Bulk material after mixing is placed in tube furnace, under Ar gas shielded, is heated to 1000 DEG C of charing 1 h with the temperature rise rate of 5 DEG C/min and obtains sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption curve and pore size distribution curve (Fig. 1 and Fig. 2) result show: its specific surface area reaches 1500 m
2/ g, pore volume reaches 1.19 cm
3/ g, pore size distribution is in the scope of 2.5 nm ~ 16 nm.
Show in electron microscopic observation result (Fig. 3): the gac prepared under such condition is spherical, spherical diameter, probably between 10 ~ 30 nm, is very beneficial for industrial application.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 180 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 2
Employing pitch is carbon source, KCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 15 wt% KCl and 85 wt% ZnCl
2mix, after pitch is added, the ratio of mixing salt and pitch is 6:1.Bulk material after mixing is placed in tube furnace, under Ar gas shielded, is heated to 800 DEG C of charing 2 h with the temperature rise rate of 2 DEG C/min and obtains sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2absorption ~ desorption curve result shows: the specific surface area of the gac obtained under such condition is 2000 m
2/ g, pore volume is 1.4 cm
3/ g.The hole dimension of absorbent charcoal material still remains in the scope of 2.5 nm ~ 16 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 240 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 3
Employing pitch is carbon source, KCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 25 wt% KCl and 75 wt% ZnCl
2mix, after pitch is added, the ratio of mixing salt and pitch is 1:1.Bulk material after mixing is placed in tube furnace, at N
2under gas shielded, be heated to 900 DEG C of charing 1.5 h with the temperature rise rate of 10 DEG C/min and obtain sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption Dependence Results shows: the specific surface area of the gac obtained under such condition is 1000 m
2/ g, pore volume is 1.0 cm
3/ g.The hole dimension of absorbent charcoal material still remains in the scope of 2.5 nm ~ 16 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 160 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 4
Employing coal tar is carbon source, NaCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 35 wt% NaCl and 65 wt% ZnCl
2mix, after coal tar is added, the ratio of mixing salt and coal tar is 2:1.Bulk material after mixing is placed in tube furnace, at N
2under gas shielded, be heated to 1200 DEG C of charing 0.5 h with the temperature rise rate of 0.5 DEG C/min and obtain sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption Dependence Results shows: the specific surface area of the gac obtained under such condition is 2100 m
2/ g, pore volume is 1.5 cm
3/ g.The hole dimension of absorbent charcoal material still remains in the scope of 2.5 nm ~ 16 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 259 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 5
Employing coal tar is carbon source, NaCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 45 wt% NaCl and 55 wt% ZnCl
2mix, after coal tar is added, the ratio of mixing salt and coal tar is 5:1.Bulk material after mixing is placed in tube furnace, under Ar gas shielded, is heated to 700 DEG C of charing 4 h with the temperature rise rate of 1 DEG C/min and obtains sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption Dependence Results shows: the specific surface area of the gac obtained under such condition is 1200 m
2/ g, pore volume is 1.04 cm
3/ g.The hole dimension of absorbent charcoal material still remains in the scope of 2.5 nm ~ 16 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 165 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 6
Employing coal tar is carbon source, NaCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 25 wt% NaCl and 75 wt% ZnCl
2mix, after coal tar is added, the ratio of mixing salt and coal tar is 4:1.Bulk material after mixing is placed in tube furnace, under Ar gas shielded, is heated to 800 DEG C of charing 5 h with the temperature rise rate of 8 DEG C/min and obtains sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption curve and pore size distribution curve (Fig. 4 and Fig. 5) result show: its specific surface area reaches 2225 m
2/ g, pore volume reaches 1.3 cm
3/ g, pore size distribution is in the scope of 1.0 nm ~ 8 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is up to 320 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 7
Employing pitch is carbon source, LiCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 35 wt% LiCl and 65 wt% ZnCl
2mix, after pitch is added, the ratio of mixing salt and pitch is 6:1.Bulk material after mixing is placed in tube furnace, under Ar gas shielded, is heated to 900 DEG C of charing 2 h with the temperature rise rate of 5 DEG C/min and obtains sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption Dependence Results shows: the specific surface area of gac is 2800 m under such condition
2/ g, pore volume is 1.5 cm
3/ g.The hole dimension of absorbent charcoal material still remains in the scope of 1.0 nm ~ 8 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 350 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 8
Employing pitch is carbon source, LiCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 45 wt% LiCl and 55 wt% ZnCl
2mix, after pitch is added, the ratio of mixing salt and pitch is 1:1.Bulk material after mixing is placed in tube furnace, at N
2under gas shielded, be heated to 600 DEG C of charing 5 h with the temperature rise rate of 1 DEG C/min and obtain sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption Dependence Results shows: the specific surface area of gac is 1800 m under such condition
2/ g, pore volume is 1.0 cm
3/ g.The hole dimension of absorbent charcoal material still remains in the scope of 1.0 nm ~ 8 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 220 F/g, and has good high rate during charging-discharging and cyclical stability.
Embodiment 9
Employing coal tar is carbon source, LiCl and ZnCl
2mixture be fused salt mixt, a step carbonization-activation legal system is for gac.First by 25 wt% LiCl and 75 wt% ZnCl
2mix, after coal tar is added, the ratio of mixing salt and coal tar is 2:1.Bulk material after mixing is placed in tube furnace, at N
2under gas shielded, be heated to 1200 DEG C of charing 1 h with the temperature rise rate of 10 DEG C/min and obtain sample.By dry for washing after the sample comminution after charing, thus the gac of the black obtained.
N
2adsorption-desorption curve and pore size distribution curve (Fig. 6 and Fig. 7) result show: its specific surface area reaches 1400 m
2/ g, pore volume reaches 0.7 cm
3/ g, in the scope of pore size distribution 1 nm ~ 4 nm.
In this example, the ratio capacitance of absorbent charcoal material in aqueous electrolyte is 162 F/g, and has good high rate during charging-discharging and cyclical stability.
As shown in Fig. 1, Fig. 2, employing pitch is carbon source, KCl and ZnCl
2mixture be fused salt mixt, utilize a step carbonization-activation legal system for gac, the activated carbon pore size of gained is between 2.5 ~ 16 nm.
As shown in Figure 3, the gac adopting fused salt mixt carborization to prepare is spherical.
As shown in Figure 4 and Figure 5, employing coal tar is carbon source, NaCl and ZnCl
2mixture be fused salt mixt, utilize a step carbonization-activation legal system for gac, the hole dimension of gained Carbon Materials is between 1.0 ~ 8 nm.
Coal tar is adopted to be carbon source as shown in Figure 6 and Figure 7, LiCl and ZnCl
2mixture be fused salt mixt, utilize a step carbonization-activation legal system for gac, the hole dimension of gained Carbon Materials is between 1 ~ 4 nm.
Claims (6)
1. utilize fused salt mixt to prepare a method for activated carbon for super capacitors for activator, it is characterized in that the method step is:
1) with pitch or coal tar for raw material, by its with by LiCl and ZnCl
2composition fused salt mixt or by NaCl and ZnCl
2composition fused salt mixt or by KCl and ZnCl
2the fused salt mixt of composition mixes, and obtains mixture;
2) under argon gas or nitrogen protection, mixture is carbonized 0.5 h ~ 5 h at 600 DEG C ~ 1200 DEG C;
3) again with clear water washing after being pulverized by the product after charing, the absorbent charcoal material of black after oven dry, is obtained.
2. the method for claim 1, is characterized in that described by LiCl and ZnCl
2the fused salt mixt of composition consists of LiCl 15 ~ 45 wt%, ZnCl
255 ~ 85 wt%.
3. the method for claim 1, is characterized in that described by NaCl and ZnCl
2the fused salt mixt of composition consists of NaCl 15 ~ 45 wt%, ZnCl
255 ~ 85 wt%.
4. the method for claim 1, is characterized in that described by KCl and ZnCl
2the fused salt mixt of composition consists of KCl 15 ~ 45 wt%, ZnCl
255 ~ 85 wt%.
5. the method for claim 1, is characterized in that the mass ratio of described fused salt mixt and pitch or coal tar is 6:1 ~ 1:1.
6. the method for claim 1, it is characterized in that the temperature rise rate of described charing is 0.5 DEG C/min ~ 10 DEG C/min, carbonization temperature is preferably 800 DEG C ~ 1000 DEG C, and carbonization time is preferably 1 h ~ 2 h.
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| CN105384170A (en) * | 2015-10-28 | 2016-03-09 | 武汉纺织大学 | Method for preparing activated charcoal by utilizing waste textile fiber material in molten-salt medium |
| CN106010468A (en) * | 2016-06-22 | 2016-10-12 | 黄毅 | Low-melting-point mixed molten salt as heat transfer and storage medium |
| CN106206076A (en) * | 2016-06-24 | 2016-12-07 | 安徽江威精密制造有限公司 | Electrode material that the mechanical performance of a kind of modified Nano carbon fiber doping vario-property is excellent and preparation method thereof |
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| CN105384170A (en) * | 2015-10-28 | 2016-03-09 | 武汉纺织大学 | Method for preparing activated charcoal by utilizing waste textile fiber material in molten-salt medium |
| CN106010468A (en) * | 2016-06-22 | 2016-10-12 | 黄毅 | Low-melting-point mixed molten salt as heat transfer and storage medium |
| CN106206076A (en) * | 2016-06-24 | 2016-12-07 | 安徽江威精密制造有限公司 | Electrode material that the mechanical performance of a kind of modified Nano carbon fiber doping vario-property is excellent and preparation method thereof |
| CN106698427A (en) * | 2017-03-09 | 2017-05-24 | 深圳市贝特瑞新能源材料股份有限公司 | Activated carbon, preparation method thereof, and application of activated carbon in supercapacitor electrode |
| CN107043098A (en) * | 2017-03-27 | 2017-08-15 | 中南大学 | A kind of application for the method and carbon nano rod that carbon nano rod is prepared based on molten-salt growth method |
| CN111263731B (en) * | 2017-10-26 | 2022-12-23 | 浦项化学株式会社 | Preparation method of porous carbon material by using coal tar generated in COG (chemical oxygen demand) process |
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| CN109161915A (en) * | 2018-09-30 | 2019-01-08 | 东北大学 | The method for preparing activated carbon for super capacitors powder using coal based on fused salt |
| CN110697708A (en) * | 2019-10-31 | 2020-01-17 | 华南理工大学 | Nitrogen-doped porous carbon material for lithium ion capacitor and efficient preparation method of low-temperature co-molten solvent activated biomass waste of nitrogen-doped porous carbon material |
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| CN111186839A (en) * | 2020-02-27 | 2020-05-22 | 中国科学院化学研究所 | Reaction system and method for preparing nano-pore carbon material by using ternary low-temperature molten salt |
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