CN101830460A - Active carbon particles and preparation method thereof - Google Patents
Active carbon particles and preparation method thereof Download PDFInfo
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- CN101830460A CN101830460A CN201010183314A CN201010183314A CN101830460A CN 101830460 A CN101830460 A CN 101830460A CN 201010183314 A CN201010183314 A CN 201010183314A CN 201010183314 A CN201010183314 A CN 201010183314A CN 101830460 A CN101830460 A CN 101830460A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses active carbon particles and a preparation method thereof. The method comprises the following steps of: (1) cutting dried straws into fragments, soaking for 3-5 h in ferric trichloride water solution, taking out and baking; (2) placing the straw fragments baked in the step (1) into a ceramic tube and then placing into a high temperature burning carbon determining furnace, introducing nitrogen gas to the ceramic tube, raising the temperature of the high temperature burning carbon determining furnace from room temperature to 350 DEG C, and maintaining for 1 h in the atmosphere of nitrogen gas to finish a carbonization stage; (3) raising the temperature of the high temperature burning carbon determining furnace from 350 DEG C to 850 DEG C, closing nitrogen gas, introducing carbon dioxide gas to the ceramic tube, and maintaining for 1 h in the atmosphere of carbon dioxide gas to finish the activation stage; and (4) after the activation stage finishes, closing carbon dioxide, introducing nitrogen gas to the ceramic tube again, reducing the temperature to room temperature and taking out to obtain the active carbon particles. The active carbon particle prepared by the method has low cost, large specific area and magnetism.
Description
Technical field
The present invention relates to a kind of activated carbon granule and preparation method thereof.
Background technology
In China, after the farm crop harvesting, produce a large amount of stalks, the annual stalk output of China is up to 700,000,000 tons according to incompletely statistics.But existing to stalk utilize technology very limited, most of stalk is all directly burned in the field by the peasant after results.The Office of the State Council of General Office of the State Council's issue in 2008 sends out some area burning agricultural crop straws of China rural area according to the document (2008) No. 105, and phenomenon is commonplace, and not only contaminate environment, serious threat traffic safety are also wasted resource.Promptly avoided the waste of resource to avoid contaminate environment again so be badly in need of seeking a kind of method of stalk of can efficiently utilizing.
Gac is traditional and modern artificial material, comes out one certainly over 100 years, and Application Areas is expanded day by day, and number of applications also constantly increases progressively.Usually can be used to purify air, handle aspects such as the poison sewage of difficult for biological degradation or purified tap water, its huge specific surface area has very strong adsorption potential, in the planar water or airborne particle or molion composition, reaches the purpose of purification rapidly.Present commercially available activated carbon granule mainly obtains through activation under 1000 ℃ of hot conditionss by raw materials such as charcoal or coals.Advantage is that productive rate is higher, and technology is comparatively ripe, and is high but starting material are worth, and also increased production cost greatly, and when utilizing gac to carry out sewage disposal or tap water purification, sorbent material is difficult to be reclaimed, and has also increased the cost of treatment process in addition.Therefore, how to utilize the low value starting material to produce high-quality activated carbon granule, and simplify follow-up purification process technique and also become one of focus of present research.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of gac and preparation method thereof.Utilize agricultural crop straw material cheap and easy to get, preparation high-specific surface area and activated carbon granule with magnetic.Both can provide a feasible scheme for the wasting of resources and the environmental pollution that present crop straw burning problem is brought, also, also simplified the technological process of utilizing activated carbon treatment waste water or purifying drinking water in addition for the material cost that reduces Preparation of Activated Carbon provides possibility.
The preparation method of activated carbon granule provided by the invention comprises the steps:
1) early-stage preparations process: with the exsiccant stalk, cut into fragment, in ferric chloride aqueous solutions, soaked 3～5 hours, take out, oven dry, wherein the concentration of ferric chloride aqueous solutions is 5～50g/L;
2) carbonization process: after the stalk fragment after the step 1) oven dry put into vitrified pipe, put into high-temp combustion and decide the charcoal stove, feed nitrogen in described vitrified pipe, the temperature of high-temp combustion being decided the charcoal stove rises to 350 ℃ from room temperature, and under nitrogen atmosphere, keep 1h, finish carbonation stage;
3) reactivation process: the temperature of high-temp combustion being decided the charcoal stove rises to 850 ℃ from 350 ℃, closes nitrogen, feeds carbon dioxide in described vitrified pipe, keeps 1h under the carbon dioxide atmosphere, finishes activation stage;
4) temperature-fall period: the stage to be activated finishes, and closing carbon dioxide feeds nitrogen again in described vitrified pipe, takes out after reducing to room temperature, can obtain activated carbon granule.
The present invention also provides a kind of activated carbon granule according to method for preparing.
Technical scheme provided by the invention has following beneficial effect:
1) starting material adopt farm crop harvesting back depleted stalk, and cost is low, and is cheap and easy to get, and the wasting of resources and the environmental pollution of having avoided the existing burn processing in rural area to bring.
2) activated carbon granule for preparing is measured through specific surface area measuring instrument, and specific surface area is 930m
2/ g, specific surface area is bigger;
3) activated carbon granule for preparing has magnetic preferably, can be easy to remove from the aqueous solution behind the adsorption treatment pollutent by attraction, and handled easily is avoided secondary pollution;
4), find to concentration to be that the methylene blue solution adsorptive capacity of 50mg/l can reach 250mg/g with the activated carbon granule adsorptive capacity of methylene blue solution checking preparation.
5) iron on the activated carbon granule for preparing mainly is the iron of oxidation state, in adsorbent solution, seldom discharge, after adsorption process finishes, reach national drinking water quality standard less than 0.1mg/l by iron concentration in inductively coupled plasma-atomic emission spectrum mensuration solution.
Embodiment
The invention will be further described below in conjunction with specific embodiment, can be implemented so that those skilled in the art can better understand the present invention also, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1:
Get harvested rape stalk stem, after the oven dry, get 10g, cut into the long fragment of about 0.25cm with instrument, fully soak 4h in the liquor ferri trichloridi with gauze parcel back input 200ml 10g/l, put into B after the taking-up, bottom pad is gone up middling speed filter paper, take out 5-10min with the recirculated water vacuum pump after, put into baking oven and dry 2h for 105 ℃, take by weighing 1.5g after the taking-up respectively and put into two vitrified pipe middle parts that internal diameter is 1.8cm, vitrified pipe is inserted high-temp combustion decide in the stove case of charcoal stove (SK2-205-13, Longkou City electric furnace head factory), two ends soft rubber ball are beyond the Great Wall avoided contacting with air, plug conduit on the soft rubber ball, in order to feeding gas.Vitrified pipe is connected (nitrogen valve is connected by Y-tube with the carbonic acid gas valve, and it is convenient to be convenient to ventilation) by conduit with reducing valve on the gas bomb, flow director on the indirect (0-50ml, LZB-2, the rich glad flow instrument in Shanghai company limited).Utilize temperature housing (708P-k1-40A, Xiamen space electric automation Science and Technology Ltd.) to set and control the temperature of carbon-determining stove.
Open the nitrogen reducing valve, the adjusting flow is 15ml/min, and design temperature rises to 350 ℃ with 10 ℃/min from room temperature, and keeps 1h, finishes carbonation stage.And then rise to 850 ℃ with 10 ℃/min.After arriving 850 ℃, temperature closes nitrogen valve; open the carbon dioxide gas valve door; flow velocity is constant; make the stalk after the carbonization finish activation stage under carbon dioxide, soak time is 1h, after the stage to be activated finishes; closing carbon dioxide gas; again feed nitrogen, and drop to room temperature in nitrogen protection, it is standby to put into moisture eliminator after the taking-up.
The activated carbon granule for preparing is measured through specific surface area measuring instrument, and specific surface area is 930m
2/ g.
Get the activated carbon granule 0.02g that preparation is finished, add in the methylene blue solution of 100ml 50mg/l, whole system is put into 25 ℃ of 150rpm reactions of constant temperature oscillator 10h, reaction finishes back water sampling 5ml, on ultraviolet-visible pectrophotometer, detect residue methylene blue concentration 0.52mg/l is only arranged, adsorptive capacity reaches 248mg/g, and commercially available activated carbon granule is 150～200mg/g to the adsorptive capacity of above-mentioned methylene blue, is lower than the activated carbon granule that the present invention makes.Iron concentration in use inductively coupled plasma-Atomic Emission Spectral Analysis solution is less than 0.1mg/l.
In addition, after adsorption test finishes, magnet on the container underneath, pouring soln finds that activated carbon granule all is attracted on the magnet then, and is residual considerably less in the solution, realized solid-liquid separation very simply.
Embodiment 2:
Maize straw prepares the process such as the embodiment 1 of magnetic active carbon.Get the magnetic active carbon particle 0.02g that preparation is finished, add 25ml 10mg/l Cr
6+Potassium bichromate solution in, whole system is put into 25 ℃ of 150rpm reactions of constant temperature oscillator 10h, reaction finishes back water sampling 1ml, on inductively coupled plasma-Atomic Emission Spectral Analysis instrument, detect the concentration of chromium ion, drawing adsorptive capacity at last is 17mg/g, and commercially available gac to the adsorptive capacity of chromium ion less than 10mg/g.
In addition, after adsorption test finishes, magnet on the container underneath, pouring soln finds that activated carbon granule all is attracted on the magnet then, and is residual considerably less in the solution, realized solid-liquid separation very simply.
The above embodiment is the preferred embodiment that proves absolutely that the present invention lifts, and protection scope of the present invention is not limited thereto.Being equal to that those skilled in the art are done on basis of the present invention substitutes or conversion, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (7)
1. the preparation method of an activated carbon granule is characterized in that, comprises the steps:
1) early-stage preparations process: with the exsiccant stalk, cut into fragment, in ferric chloride aqueous solutions, soaked 3～5 hours, take out, oven dry;
2) carbonization process: after the stalk fragment after the step 1) oven dry put into vitrified pipe, put into high-temp combustion and decide the charcoal stove, feed nitrogen in described vitrified pipe, the temperature of high-temp combustion being decided the charcoal stove rises to 350 ℃ from room temperature, and under nitrogen atmosphere, keep 1h, finish carbonation stage;
3) reactivation process: the temperature of high-temp combustion being decided the charcoal stove rises to 850 ℃ from 350 ℃, closes nitrogen, feeds carbon dioxide in described vitrified pipe, keeps 1h under the carbon dioxide atmosphere, finishes activation stage;
4) temperature-fall period: the stage to be activated finishes, and closing carbon dioxide feeds nitrogen again in described vitrified pipe, takes out after reducing to room temperature, can obtain the magnetic active carbon particle.
2. preparation method according to claim 1 is characterized in that, the concentration of the described ferric chloride aqueous solutions of step 1) is 5～50g/L.
3. preparation method according to claim 1 is characterized in that, the described stalk of step 1) is rape or maize straw.
4. preparation method according to claim 1 is characterized in that step 2) flow velocity of described feeding nitrogen is 5～15ml/min.
5. preparation method according to claim 1 is characterized in that step 2) the described high-temp combustion temperature of deciding the charcoal stove rises to 350 ℃ from room temperature, and heat-up rate is 10 ℃/min.
6. preparation method according to claim 1 is characterized in that, the flow velocity of the described feeding carbonic acid gas of step 3) is 15ml/min.
7. according to the activated carbon granule of the described method of claim 1 preparation.
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Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583333A (en) * | 2012-01-18 | 2012-07-18 | 黑龙江大学 | Method for synthesizing porous nanographite flakes by using corn stalks as carbon source |
| CN102992319A (en) * | 2012-12-05 | 2013-03-27 | 浙江大学 | Efficient and safe preparation method for active carbon material for adsorbing phosphorus in water body |
| CN103316636A (en) * | 2013-07-05 | 2013-09-25 | 河南农业大学 | Method for preparing biomass-based magnetic activated carbon |
| CN103663824A (en) * | 2012-09-14 | 2014-03-26 | 苏州工业园区七星电子有限公司 | Wastewater treatment method and device |
| CN104138743A (en) * | 2014-07-23 | 2014-11-12 | 河海大学 | Method for preparing algae base magnetic activated carbon material and application of algae base magnetic activated carbon material |
| CN104891479A (en) * | 2015-05-26 | 2015-09-09 | 中国林业科学研究院林产化学工业研究所 | Plant-based graphene and preparation method thereof |
| RU2562984C1 (en) * | 2014-07-02 | 2015-09-10 | Открытое акционерное общество "Электростальское научно-производственное объединение "Неорганика" (ОАО "ЭНПО "Неорганика") | Method of production of activated carbon from plant material - straw of cruciferous oil crops |
| CN105457594A (en) * | 2015-11-13 | 2016-04-06 | 无锡清杨机械制造有限公司 | Preparation method of hydrophilic magnetic activated carbon |
| CN105536700A (en) * | 2015-12-22 | 2016-05-04 | 国家***天津海水淡化与综合利用研究所 | Method for preparing magnetic biochar from straw |
| CN107151016A (en) * | 2017-06-28 | 2017-09-12 | 宿州市逢源生物科技有限公司 | A kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere |
| CN107215869A (en) * | 2017-06-28 | 2017-09-29 | 淮阴工学院 | A kind of biomass pyrolytic prepares magnetic active carbon and the method rich in synthesis gas gas |
| CN107337204A (en) * | 2017-06-28 | 2017-11-10 | 淮阴工学院 | Biomass pyrolytic, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas |
| CN107488519A (en) * | 2017-07-24 | 2017-12-19 | 北京科技大学 | A kind of method that acid-base catalysis Bio-Diesel Fuels are loaded using magnetic charcoal |
| CN107900092A (en) * | 2017-10-30 | 2018-04-13 | 常州大学 | A kind of arid area lead cadmium pollution soil repair system |
| CN108424303A (en) * | 2018-06-11 | 2018-08-21 | 孙永妮 | A method of preparing pest-resistant organic composite fertilizer using agriculture wastes |
| CN108671886A (en) * | 2018-04-25 | 2018-10-19 | 中国矿业大学 | A kind of magnetic active carbon adsorbent and the preparation method and application thereof based on abandoned biomass |
| CN110065942A (en) * | 2019-04-12 | 2019-07-30 | 华南理工大学 | A kind of rice base graininess micropore/ultramicropore carbon material and preparation method thereof |
| CN110075795A (en) * | 2019-04-26 | 2019-08-02 | 福建工程学院 | A kind of preparation method having magnetic tubulose active carbon |
| CN110342510A (en) * | 2018-04-02 | 2019-10-18 | 兰固 | A kind of production method of corn stalk active carbon |
| CN111420635A (en) * | 2020-03-31 | 2020-07-17 | 武汉理工大学 | Preparation method and application of nitrogen-sulfur co-doped waste biomass activated carbon |
| CN112551502A (en) * | 2020-12-21 | 2021-03-26 | 长沙工研院环保有限公司 | Method for recycling ferroelectrolytic phosphorus removal precipitate |
| CN113053675A (en) * | 2021-03-11 | 2021-06-29 | 冷春丽 | Preparation method of electrode composite material applied to supercapacitor |
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| CN101074096A (en) * | 2007-06-22 | 2007-11-21 | 山东大学 | Production of sand-grass straw activated carbon |
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Cited By (27)
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| CN102583333A (en) * | 2012-01-18 | 2012-07-18 | 黑龙江大学 | Method for synthesizing porous nanographite flakes by using corn stalks as carbon source |
| CN103663824A (en) * | 2012-09-14 | 2014-03-26 | 苏州工业园区七星电子有限公司 | Wastewater treatment method and device |
| CN102992319A (en) * | 2012-12-05 | 2013-03-27 | 浙江大学 | Efficient and safe preparation method for active carbon material for adsorbing phosphorus in water body |
| CN102992319B (en) * | 2012-12-05 | 2014-08-06 | 浙江大学 | Efficient and safe preparation method for active carbon material for adsorbing phosphorus in water body |
| CN103316636A (en) * | 2013-07-05 | 2013-09-25 | 河南农业大学 | Method for preparing biomass-based magnetic activated carbon |
| RU2562984C1 (en) * | 2014-07-02 | 2015-09-10 | Открытое акционерное общество "Электростальское научно-производственное объединение "Неорганика" (ОАО "ЭНПО "Неорганика") | Method of production of activated carbon from plant material - straw of cruciferous oil crops |
| CN104138743A (en) * | 2014-07-23 | 2014-11-12 | 河海大学 | Method for preparing algae base magnetic activated carbon material and application of algae base magnetic activated carbon material |
| CN104891479A (en) * | 2015-05-26 | 2015-09-09 | 中国林业科学研究院林产化学工业研究所 | Plant-based graphene and preparation method thereof |
| CN104891479B (en) * | 2015-05-26 | 2017-02-01 | 中国林业科学研究院林产化学工业研究所 | Plant-based graphene and preparation method thereof |
| CN105457594A (en) * | 2015-11-13 | 2016-04-06 | 无锡清杨机械制造有限公司 | Preparation method of hydrophilic magnetic activated carbon |
| CN105536700A (en) * | 2015-12-22 | 2016-05-04 | 国家***天津海水淡化与综合利用研究所 | Method for preparing magnetic biochar from straw |
| CN107215869A (en) * | 2017-06-28 | 2017-09-29 | 淮阴工学院 | A kind of biomass pyrolytic prepares magnetic active carbon and the method rich in synthesis gas gas |
| CN107337204A (en) * | 2017-06-28 | 2017-11-10 | 淮阴工学院 | Biomass pyrolytic, which is combined, prepares magnetic active carbon and the method rich in synthesis gas gas |
| CN107151016A (en) * | 2017-06-28 | 2017-09-12 | 宿州市逢源生物科技有限公司 | A kind of preparation method that straw biomass charcoal is prepared under carbon dioxide atmosphere |
| CN107488519A (en) * | 2017-07-24 | 2017-12-19 | 北京科技大学 | A kind of method that acid-base catalysis Bio-Diesel Fuels are loaded using magnetic charcoal |
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| CN110342510A (en) * | 2018-04-02 | 2019-10-18 | 兰固 | A kind of production method of corn stalk active carbon |
| CN108671886A (en) * | 2018-04-25 | 2018-10-19 | 中国矿业大学 | A kind of magnetic active carbon adsorbent and the preparation method and application thereof based on abandoned biomass |
| CN108424303A (en) * | 2018-06-11 | 2018-08-21 | 孙永妮 | A method of preparing pest-resistant organic composite fertilizer using agriculture wastes |
| CN110065942A (en) * | 2019-04-12 | 2019-07-30 | 华南理工大学 | A kind of rice base graininess micropore/ultramicropore carbon material and preparation method thereof |
| CN110065942B (en) * | 2019-04-12 | 2022-08-12 | 华南理工大学 | Rice-based granular microporous/ultramicroporous carbon material and preparation method thereof |
| CN110075795A (en) * | 2019-04-26 | 2019-08-02 | 福建工程学院 | A kind of preparation method having magnetic tubulose active carbon |
| CN111420635A (en) * | 2020-03-31 | 2020-07-17 | 武汉理工大学 | Preparation method and application of nitrogen-sulfur co-doped waste biomass activated carbon |
| CN112551502A (en) * | 2020-12-21 | 2021-03-26 | 长沙工研院环保有限公司 | Method for recycling ferroelectrolytic phosphorus removal precipitate |
| CN113053675A (en) * | 2021-03-11 | 2021-06-29 | 冷春丽 | Preparation method of electrode composite material applied to supercapacitor |
| CN113053675B (en) * | 2021-03-11 | 2023-07-28 | 深圳今为科技有限公司 | Preparation method of electrode composite material applied to super capacitor |
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