CN103172063A - Method for preparing active carbon by using fullerene soot extraction residues - Google Patents
Method for preparing active carbon by using fullerene soot extraction residues Download PDFInfo
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- CN103172063A CN103172063A CN2011104364094A CN201110436409A CN103172063A CN 103172063 A CN103172063 A CN 103172063A CN 2011104364094 A CN2011104364094 A CN 2011104364094A CN 201110436409 A CN201110436409 A CN 201110436409A CN 103172063 A CN103172063 A CN 103172063A
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Abstract
The invention relates to a method for preparing active carbon by using fullerene soot extraction residues, belonging to the technical field of active carbon materials. According to the method for preparing active carbon, fullerene soot extraction residues as the material is directly activated by using a gas activation method and a chemical activation method to obtain excellent active carbon. The method has the advantages that the preparation process line of the method is simple, the consumption of activation agents is low, the prepared active carbon has high specific surface area and can be used as the capacitor electrode material, the catalyst carrier and the sorbent; and the method provides a convenient and feasible method for utilization of fullerene soot extraction residues.
Description
Technical field
The present invention relates to a kind of method that is prepared active carbon with high specific surface area by soccerballene cigarette ash extract remainder, belong to the absorbent charcoal material technical field.
Background technology
Since the people such as Kroto in 1985 find soccerballene, the concern that soccerballene enjoys the countries in the world scholar due to chemistry and the physical properties of its uniqueness.At present comparatively ripe preparation method is combustion method, arc evaporation, laser method etc., and still, the productive rate of the above-mentioned method for preparing soccerballene is all very low, is generally 10% left and right, and the cigarette ash extract remainder of residue 90% left and right often is taken as waste disposal.Along with developing rapidly of soccerballene industry, the problem of utilizing of soccerballene cigarette ash extract remainder more and more causes various countries scholar's concern.Cleveland etc. (Journal of Environmental Engineering, 1996,122:235-238) studies show that cigarette ash Pyrogentisinic Acid, trieline and benzene etc. after atmospheric oxidation have adsorptive power preferably.Chen (Journal of chromatography A, 2000,886:313-317) etc. reported that soccerballene cigarette ash extract remainder can be used for adsorbing 17 kinds of volatile organisms in atmosphere.Egashira (Journal of power sources, 2005,148:116-120) etc. the people after 900 ℃ of charings, is used for the test of organic system assembling ultracapacitor with the cigarette ash extract remainder, can reach 58Fg than electric capacity
-1
Gac has that pore texture prosperity, specific surface area are large, the surface carbon oxygen-containing functional group is abundant, heat and the characteristics such as chemical stability is good; be a kind of sorbent material and support of the catalyst of high-quality, be widely used in the fields such as industry, agricultural, national defence, medical and health, environment protection.The advantages such as the present invention take soccerballene cigarette ash extract remainder as raw material, adopts gas activation method and analysis for preparation of activated carbon by chemical activation take the preparation high grade activated carbon as purpose, and it is large that product has porosity, and specific surface area is high, and reactive behavior is large, and particle diameter is little.The present invention provides an a new direction for the utilization of soccerballene cigarette ash extract remainder.
Summary of the invention
In view of the defective that prior art exists, the purpose of this invention is to provide that a kind of technique is simple, activator level is few, productive rate is high, effectively utilize the waste that produces in the soccerballene preparation process to prepare the method for active carbon with high specific surface area.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac can adopt physical activation method and chemical activation method, its raw materials used soccerballene cigarette ash extract remainder for producing in the soccerballene preparation process.
Described its constituent content of soccerballene cigarette ash extract remainder is: carbon content: 40～98%, and oxygen level: 0～30%, hydrogen richness: 0～10%.
A kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac can be utilized the standby gac of gas activation legal system, comprises the steps:
A. raw material is passed into activated gas after being heated to activation temperature under inert atmosphere, heat temperature raising speed is 2～10 ℃/min, and activation temperature is 400～1000 ℃;
B. carry out activation treatment under activation temperature, the activation treatment time is 0.5～6h, and the activated gas flow is 50～300sccm;
C. above-mentioned product is cooled to room temperature and namely gets gac under inert atmosphere.
Described activated gas is water vapour, carbonic acid gas, oxygen, airborne one or more combination.
Inert atmosphere described in step a and step c is: rare gas element is nitrogen, argon gas or helium, and gas flow is 50～300sccm.
A kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac can be utilized analysis for preparation of activated carbon by chemical activation, comprises the steps:
A. with after raw material and activator mix, be heated to activation temperature under inert atmosphere, heat temperature raising speed is 2～10 ℃/min, and activation temperature is 400～1000 ℃;
B. carry out activation treatment under activation temperature, the activation treatment time is 0.5～6h;
C. above-mentioned product is cooled to room temperature under inert atmosphere, through pickling or be washed to neutrality, filters, namely get gac after drying.
Described activator is phosphoric acid, zinc chloride, potassium hydroxide or salt of wormwood, and the mass ratio of raw material and activator is 1: 0.5～8.
Inert atmosphere is: rare gas element is nitrogen, argon gas or helium, and gas flow is 50～300sccm.
During take phosphoric acid as activator, select deionized water to be washed till neutrality.During take zinc chloride, potassium hydroxide or salt of wormwood as activator, first pickling, then wash with water to neutrality.
Also comprise the step with the oven dry of soccerballene cigarette ash extract remainder before step a.
The invention has the beneficial effects as follows: raw materials size can make raw material fully mix with activator at nano level, and activator is fully used; Activator level is few, simple process, and productive rate high (more than 40%), resulting gac has chemical property and absorption property preferably.
Description of drawings
Accompanying drawing 5 width of the present invention,
Fig. 1 is the nitrogen adsorption desorption figure of embodiment 2 samples; (X-coordinate: relative pressure, ordinate zou: adsorptive capacity)
Fig. 2 is the nitrogen adsorption desorption figure of embodiment 9 samples; (X-coordinate: relative pressure, ordinate zou: adsorptive capacity)
Fig. 3 is embodiment 8 sample Pyrogentisinic Acids' sorption isotherm; (X-coordinate: Adsorption of Phenol equilibrium concentration, ordinate zou: the Adsorption of Phenol equilibrium adsorption capacity)
Fig. 4 is that embodiment 2 samples are at 10mV s
-1Cyclic voltammetry curve under scanning speed; (X-coordinate: sweep voltage, ordinate zou: current density)
Fig. 5 is that embodiment 8 samples are at 10mV s
-1Cyclic voltammetry curve under scanning speed.(X-coordinate: sweep voltage, ordinate zou: current density)
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
In the following embodiments, select arc process, combustion method and three kinds of soccerballene cigarette ash extract remainders of laser evaporation method, be labeled as respectively YH1, YH2 and YH3, its physical parameter is as shown in table 1.
The constituent content of three kinds of soccerballene cigarette ash extract remainders of table 1
| Sample | Carbon content (%) | Hydrogen richness (%) | Oxygen level (%) |
| YH1 | 92 | 3 | 5 |
| YH2 | 89 | 3 | 8 |
| YH3 | 94 | 4 | 2 |
Embodiment 1
Soccerballene cigarette ash extract remainder (YH1) is dried, at nitrogen flow rate 50sccm, under the condition of 2 ℃/min of heat-up rate, heating raw materials is passed into activated gas water vapour to 800 ℃ of activation temperatures, activated gas water vapour flow is 300sccm, and soak time is 6h.Subsequently, product is cooled to room temperature under nitrogen flow 50sccm.The Microstructure characterization of this gac sees Table 2.
Soccerballene cigarette ash extract remainder (YH2) is dried, at argon gas flow velocity 300sccm, under the condition of 10 ℃/min of heat-up rate, heating raw materials is passed into the activated gas carbonic acid gas to 1000 ℃ of activation temperatures, activated gas carbonic acid gas flow velocity is 50sccm, and soak time is 0.5h.Subsequently, product is cooled to room temperature under argon gas flow velocity 50sccm.The Microstructure characterization of this gac sees Table 2.
With soccerballene cigarette ash extract remainder (YH3) oven dry, at helium flow velocity 100sccm, under the condition of 5 ℃/min of heat-up rate, heating raw materials is passed into activated gas oxygen to 400 ℃ of activation temperatures, the activated gas oxygen gas flow rate is 100sccm, soak time is 1h.Subsequently, product is cooled to room temperature under helium flow velocity 100sccm.The Microstructure characterization of this gac sees Table 2.
Soccerballene cigarette ash extract remainder (YH1) is dried, at helium flow velocity 100sccm, under the condition of 5 ℃/min of heat-up rate, heating raw materials is passed into the activated gas air to 450 ℃ of activation temperatures, the activated gas air velocity is 100sccm, and soak time is 1.5h.Subsequently, product is cooled to room temperature under helium flow velocity 100sccm.The Microstructure characterization of this gac sees Table 2.
Embodiment 5
Soccerballene cigarette ash extract remainder (YH2) is dried; Activator is phosphoric acid.Soccerballene cigarette ash and phosphoric acid are mixed in mass ratio at 1: 6, dry in loft drier.Under nitrogen flow rate 50sccm, be warming up to 400 ℃ and carry out activation treatment 2h; Be cooled to room temperature under nitrogen flow rate 50sccm, be washed till neutrality with deionized water, can make gac after oven dry.The Microstructure characterization of this gac sees Table 2.
Embodiment 6
Soccerballene cigarette ash extract remainder (YH3) is dried; Activator is zinc chloride.Soccerballene cigarette ash and zinc chloride are mixed in mass ratio at 1: 0.5, dry in loft drier.Under helium flow velocity 300sccm, be warming up to 700 ℃ and carry out activation treatment 1h; Be cooled to room temperature under helium flow velocity 300sccm.Standing 24h after extremely acid with the hydrochloric acid neutralization solution of 1M is washed till neutrality with deionized water, can make gac after oven dry.The Microstructure characterization of this gac sees Table 2.
Embodiment 7
Soccerballene cigarette ash extract remainder (YH1) is dried; With above-mentioned soccerballene cigarette ash extract remainder and activator potassium hydroxide in mass ratio 1: 1 ratio mix, add deionized water that potassium hydroxide is all dissolved, after mixing, dry in loft drier.At argon gas flow velocity 100sccm, under 5 ℃/min of heat-up rate, be warming up to 700 ℃ of activation treatment 2h of temperature; Be cooled to room temperature under argon gas flow velocity 100sccm.Standing 24h after extremely acid with the hydrochloric acid neutralization solution of 1M, deionized water is washed till neutrality, can make gac after oven dry.The Microstructure characterization of this gac sees Table 2.
Embodiment 8
Soccerballene cigarette ash extract remainder (YH2) is dried; With above-mentioned soccerballene cigarette ash extract remainder and activator potassium hydroxide in mass ratio 1: 4 ratio mix, add deionized water that potassium hydroxide is all dissolved, after mixing, dry in loft drier.At argon gas flow velocity 150sccm, under 5 ℃/min of heat-up rate, be warming up to 800 ℃ of activation treatment 1h of temperature; Be cooled to room temperature under argon gas flow velocity 150sccm.Standing 24h after extremely acid with the hydrochloric acid neutralization solution of 1M, deionized water is washed till neutrality, can make gac after oven dry.The Microstructure characterization of this gac sees Table 2.
Embodiment 9
Soccerballene cigarette ash extract remainder (YH3) is dried; With above-mentioned soccerballene cigarette ash extract remainder and activator salt of wormwood in mass ratio 1: 8 ratio mix, add deionized water that salt of wormwood is all dissolved, after mixing, dry in loft drier.At nitrogen flow rate 300sccm, under 10 ℃/min of heat-up rate, be warming up to 1000 ℃ of activation treatment 0.5h of temperature; Be cooled to room temperature under nitrogen flow rate 300sccm.Standing 24h after extremely acid with the hydrochloric acid neutralization solution of 1M, deionized water is washed till neutrality, can make gac after oven dry.The Microstructure characterization of this gac sees Table 2.
Application example 1
The sample that precision takes 25mg embodiment 8 preparations is placed in respectively 25mL (0.05-0.8mgmL
-1) in phenol solution, 24h vibrates on vibrator under room temperature.Then it is filtered with funnel, get 1ml filtrate, be diluted to 25ml, ultraviolet method is measured the residual content of phenol in filtrate in maximum absorption wavelength 270nm, calculates the adsorptive capacity of the sample of embodiment 8 preparations with minusing.Calculate according to following equation:
q
e＝(C
0-C
e)V/W
In formula: q
e-equilibrium adsorption capacity, mgg
-1
C
0-initial concentration solution, mgmL
-1
C
e-solution absorbs equilibrium concentration, mgmL
-1
The volume of V-solution, L;
The W-adsorbent mass, g.
Finally obtain sample Pyrogentisinic Acid's sorption isotherm (as shown in Figure 3).But press the adsorptive value Da Keda 180mgg of the phenol of standard GB/T-T12496.12-1999 method mensuration
-1The left and right.The gac of the present invention's preparation is rich in certain mesopore, and Pyrogentisinic Acid's class material has adsorptive power preferably, also can be used for matching stain, the absorption of basic dyestuff.
Application example 2
The sample of embodiment 2 and embodiment 8 is scattered in to stir in a small amount of dehydrated alcohol with mass ratio with tetrafluoroethylene respectively at 90: 10 makes it to mix, after the gained slurry drying, be pressed into sheet on tabletting machine, then with punch tool, carbon plate to be cut into diameter be the 1cm disk.Gained disk and nickel collector are placed between two nickel foam are made into electrode of super capacitor.Utilize the chemical property of the electrical condenser of electrochemical workstation CHI660D test material assembling, testing method is cyclic voltammetry (as shown in Figure 4 and Figure 5).Land system testing constant current charge-discharge.Three-electrode system is adopted in test: the carbon electrode of preparation is working electrode, and the Pt electrode is to electrode, and mercury/mercuric oxide electrode is reference electrode.Ionogen is 6molL
-1KOH solution.Cyclic voltammetry curve-0.9～-test in the voltage range of 0.1V, the voltage range of Land system testing is-0.9～-0.1V.Cyclic voltammetry shows, material has good electrostatic double layer characteristic.The constant current charge-discharge test shows that in current density be 50mAg
-1The time, the quality of embodiment 2 and embodiment 8 gained samples can reach 140Fg than electric capacity
-1And 240Fg
-1
The Microstructure characterization of table 2 activated carbon
Claims (10)
1. a method of utilizing soccerballene cigarette ash extract remainder to prepare gac, is characterized in that: raw materials used soccerballene cigarette ash extract remainder for producing in the soccerballene preparation process.
2. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 1, is characterized in that, the constituent content of described soccerballene cigarette ash extract remainder is: carbon content: 40～98%, and oxygen level: 0～30%, hydrogen richness: 0～10%.
3. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 1, it is characterized in that: described preparation method is the gas activation method, comprises the steps:
A. raw material is heated to activation temperature under inert atmosphere;
B. pass into activated gas and carry out activation treatment under activation temperature;
C. above-mentioned product is cooled to room temperature and namely gets gac under inert atmosphere.
4. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 3, it is characterized in that: described activated gas is water vapour, carbonic acid gas, oxygen, airborne one or more combination, and the activated gas flow is 50～300sccm.
5. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 3, it is characterized in that: activation temperature is 400～1000 ℃, and heat temperature raising speed is 2～10 ℃/min, and soak time is 0.5～6h.
6. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 3, it is characterized in that: the inert atmosphere described in step a and step c is: rare gas element is nitrogen, argon gas or helium, gas flow is 50～300sccm.
7. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 1, it is characterized in that: described preparation method is chemical activation method, comprises the steps:
A. after raw material being mixed by required mass ratio with activator, be heated to activation temperature under inert atmosphere;
B. carry out activation treatment under activation temperature;
C. above-mentioned product is cooled to room temperature under inert atmosphere, through pickling or be washed to neutrality, filters, namely get gac after drying.
8. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 7, it is characterized in that: described activator is phosphoric acid, zinc chloride, potassium hydroxide or salt of wormwood; The mass ratio of described raw material and activator is 1: 0.5～8.
9. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 7, it is characterized in that: activation temperature is 400～1000 ℃, and heat temperature raising speed is 2～10 ℃/min, and soak time is 0.5～6h; Described inert atmosphere is: nitrogen, argon gas or helium, inert gas flow are 50～300sccm.
10. a kind of method of utilizing soccerballene cigarette ash extract remainder to prepare gac according to claim 7, is characterized in that: during take phosphoric acid as activator, select deionized water to be washed till neutrality; During take zinc chloride, potassium hydroxide or salt of wormwood as activator, first pickling, then wash with water to neutrality.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099589A (en) * | 2019-12-27 | 2020-05-05 | 肇庆学院 | Preparation of biochar by using coal fly ash as raw material and application of biochar as live bacteria carrier |
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| WO2006109690A1 (en) * | 2005-04-08 | 2006-10-19 | Matsushita Electric Industrial Co., Ltd. | Electrode material for electric double layer capacitor and process for producing the same, electrode for electric double layer capacitor, and electric double layer capacitor |
| CN101248143A (en) * | 2005-04-26 | 2008-08-20 | 特密高股份有限公司 | Method for further processing the residue obtained during the production of fullerene and carbon nanostructures |
-
2011
- 2011-12-22 CN CN2011104364094A patent/CN103172063A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006109690A1 (en) * | 2005-04-08 | 2006-10-19 | Matsushita Electric Industrial Co., Ltd. | Electrode material for electric double layer capacitor and process for producing the same, electrode for electric double layer capacitor, and electric double layer capacitor |
| CN101248143A (en) * | 2005-04-26 | 2008-08-20 | 特密高股份有限公司 | Method for further processing the residue obtained during the production of fullerene and carbon nanostructures |
Non-Patent Citations (2)
| Title |
|---|
| MINATO EGASHIRA等: "Toluene-insoluble fraction of fullerene-soot as the electrode of a double-layer capacitor", 《JOURNAL OF POWER SOURCES》 * |
| 李航等: "富勒烯烟灰的研究进展", 《炭素技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099589A (en) * | 2019-12-27 | 2020-05-05 | 肇庆学院 | Preparation of biochar by using coal fly ash as raw material and application of biochar as live bacteria carrier |
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Application publication date: 20130626 |