CN1857998A - Method for preparing carbon nano material by micro wave radiation of coal - Google Patents
Method for preparing carbon nano material by micro wave radiation of coal Download PDFInfo
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- CN1857998A CN1857998A CN 200610031127 CN200610031127A CN1857998A CN 1857998 A CN1857998 A CN 1857998A CN 200610031127 CN200610031127 CN 200610031127 CN 200610031127 A CN200610031127 A CN 200610031127A CN 1857998 A CN1857998 A CN 1857998A
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Abstract
The present invention discloses microwave irradiation process of preparing nanometer carbon material, including great specific surface area active carbon and quasi one-dimensional nanometer carbon material. The preparation process of great specific surface area active carbon includes the steps of: mixing washed coal and activator in certain ratio and milling, irradiating in a microwave oven to heat, burn and arc, water washing and recovering activator, acid pickling, water washing and stoving. The preparation process of quasi one-dimensional nanometer carbon material includes the steps of: mixing washed coal and catalyst in certain ratio and milling, irradiating in a microwave oven to heat, burn and arc, and purifying. The present invention has short preparation period, low power consumption, low cost, less pollution and easy use in industrial production.
Description
Technical field
The invention belongs to nano material technology and microwave chemical field, relate to a kind of method for preparing carbon nanomaterial, particularly the microwave exposure coal prepares active carbon with high specific surface area and accurate one-dimensional carbon nano material.
Background technology
Gac is widely used at aspects such as water treatment, purifying air, precious metal extractions, and active carbon with high specific surface area also can be used for aspects such as ultracapacitor energy storage except that above-mentioned application.Traditional Activated Carbon Production method energy consumption height, seriously polluted, many countries have limited its application.Patent 931146937.2 has been announced the method for a kind of " manufacturing powdered activated carbon with microwave radiation method ", it is with wood chip and phosphoric acid or liquor zinci chloridi dipping, make gac with microwave radiation again, but this method is raw material with the wood chip, and the wood chip source is wideless, need to consume the forest reserves, this has limited the application of this method.Patent 02113270.4 has been announced a kind of " microwave radiation tobacco rod solid waste is made the method for powdered carbon ", this method is pulverized the back with the tobacco rod solid waste and is carried out carrying out carry out microwave radiation heating behind the hybrid infusion with solder(ing)acid, after pickling, oven dry, obtain gac, this method energy consumption is low, material cost is low, but, the tobacco rod solid waste needs the long period dipping, and zinc chloride has more serious pollution, and method is only at this special material of tobacco rod solid waste.Patent 2004100220085.X has announced " a kind of with brown coal slag production process of active carbon ", this is a kind of way that turns waste into wealth, but, brown coal slag carbon content is lower, the gac yield is lower, there is more activator to be taken away in the production process, and produces the high performance active carbon difficulty by non-carbon species.Develop efficient, energy-conservation, few free of contamination method for preparation of active carbon and be necessary greatly, especially efficient, energy-conservation, few pollution-free preparation method of high-performance, active carbon with high specific surface area has important use to be worth.
Accurate one-dimensional carbon nano material has unique physics and chemical property, be with a wide range of applications at aspects such as energy storage device, Field Emission Display, One-dimensional Quantum lead, support of the catalyst, matrix material enhancings, but, so far accurate one-dimensional carbon nano material still can not be with acceptable price scale production, and this becomes the bottleneck problem of its widespread usage.The preparation of accurate one-dimensional carbon nano material mainly contains arc discharge method, laser ablation method and chemical Vapor deposition process at present.Arc discharge method and laser ablation method are to generate accurate one-dimensional carbon nano material by the high temperature evaporation carbon material, and its yield is low, are difficult to produce in batches; Chemical Vapor deposition process is that hydrocarbon polymer is decomposed the accurate one-dimensional carbon nano material of generation through elevated temperature heat under the effect of transition metal catalyst, and these carbon sources are gaseous matter, stores and transport all difficulties; In addition, the capacity usage ratio in the preparation process is low, output is also lower.
Coal is as a kind of abundant and cheap raw material of nature, can be for the accurate one-dimensional carbon nano material required carbon source of growing.Patent 01122772.9 has been announced " preparation of carbon nanomaterial and device ", be carbonaceous materials such as coal and catalyzer directly to be sprayed into prepare carbon nanomaterial in the plasma jet, this method raw materials cost is low, but the price of plasma generator is expensive, the production cost height; Patent 200310105047 has announced that " a kind of method and device that is prepared carbon nanomaterial by coal continuously ", patent 20031010532 announced " a kind of method that is prepared carbon nano fiber by coal ", these two kinds of methods are to handle coal dust and catalyzer by arc plasma, and feed water vapor as promotor, prepare accurate one-dimensional carbon nano material, but there is electrode erosion in this method, causes cost to increase; Prepare accurate one-dimensional carbon nano material low-costly and in high volume important and practical meanings is arranged.
Summary of the invention
The purpose of this invention is to provide a kind of efficient, energy-saving and environmental protection, low cost and prepare the method for carbon nanomaterial in large quantity, comprise preparing active carbon with high specific surface area and accurate one-dimensional carbon nano material.
Particular content of the present invention is:
1. the microwave exposure coal prepares the method for active carbon with high specific surface area;
Coal and a certain proportion of activator mix mill of washing is even, put into microwave oven and carry out irradiation, make it heating, burning and play electric arc, wash and reclaim activator then, will wash product pickling, washing, oven dry again, promptly get active carbon with high specific surface area.Described coal is hard coal, bituminous coal, brown coal or mud coal; Described activator is sodium hydroxide or potassium hydroxide; The mass ratio of described activator and coal is 1～5: 1; The power input of described microwave oven is adjustable continuously, and the atmosphere in the microwave oven is adjustable; The time of described microwave exposure is 3～60 minutes.
2. the microwave exposure coal prepares the method for accurate one-dimensional carbon nano material;
It is even to add a certain proportion of catalyst mix mill in the coal of washing, puts into microwave oven and carries out irradiation, makes it heating, burning and plays electric arc, carries out purifying then, promptly gets accurate one-dimensional carbon nano material, and described coal is hard coal, bituminous coal, brown coal or mud coal; Described catalyzer is Fe, Co, Ni and alloy thereof, and they are reduced in preparation process by corresponding acetate, oxide compound, oxyhydroxide and generate, or add with the nano-powder metal; The massfraction that described catalyzer adds is 0.5%～5%; The power input of described microwave oven is adjustable continuously, and the atmosphere in the microwave oven is adjustable; The time of described microwave exposure is 3～60 minutes.Described accurate one-dimensional carbon nano material comprises carbon nanotube and carbon nanofiber.
Chemical Vapor deposition process, arc discharge method, combustion flame method are the typical methods for preparing accurate one-dimensional carbon nano material at present, the present invention organically combines three's advantage, but do not had the original limitation of three, and the raw material that uses is cheap and enrich.
The beneficial effect that the present invention obtains is that (1) employing coal is a main raw material(s), cheap, the wide material sources of coal; (2) in the process of preparing carbon nano material by micro wave radiation of coal, committed step and main power consumption step are heating, burning and the electric arc that microwave causes coal, reaction by coal and activator or catalyzer, generate active carbon with high specific surface area or accurate one-dimensional carbon nano material, preparation cycle is short, energy consumption is low; (3) present method facility investment is few, simple to operate, is easy to accomplish scale production; (4) few, the yield height that changes carbon nanomaterial into of the scaling loss of coal, few pollution-free to environment.
Description of drawings
Fig. 1 prepares the schema of active carbon with high specific surface area for the microwave exposure coal;
Fig. 2 prepares the schema of accurate one-dimensional carbon nano material for the microwave exposure coal;
Fig. 3 is the transmission electron microscope photo of the accurate one-dimensional carbon nano material of microwave exposure coal preparation.
Embodiment
Embodiment 1:
Is to mix at 1: 4 the bituminous coal of washing and potassium hydroxide by mass ratio, with stirring the mill mill evenly, puts into the microwave oven that power is 700W, and irradiation 20min in nitrogen atmosphere takes out the back water and cleans.Water lotion enters accumulator tank; Add massfraction in the solids after the washing and be 10% hydrochloric acid soln and carry out pickling, through washing, oven dry, get final product to such an extent that specific surface area is 3000m again
2The active carbon with high specific surface area that/g is above.
Embodiment 2:
Adding mass ratio and be 2% nano level Fe powder in the hard coal of washing mixes, with stirring the mill mill evenly, put into the microwave oven that power is 1000W, in air atmosphere, make it heating, burning and play electric arc, irradiation time is 15min, taking out the back is that 98% concentrated sulfuric acid solution carries out the pickling purifying with massfraction, get final product the mixture of carbon nanotube and carbon nanofiber.
Claims (12)
1, a kind of microwave exposure coal prepares the method for active carbon with high specific surface area, it is characterized in that comprising the process of being prepared as follows: coal and a certain proportion of activator mix mill of washing is even, put into microwave oven and carry out irradiation, make it heating, burning and play electric arc, wash and reclaim activator then, to wash product pickling, washing, oven dry again, promptly get active carbon with high specific surface area.
2, microwave exposure coal according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: described coal is hard coal, bituminous coal, brown coal or mud coal.
3, microwave exposure coal according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: described activator is sodium hydroxide or potassium hydroxide.
4, microwave exposure coal according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: the mass ratio of described activator and coal is 1～5: 1.
5, microwave exposure coal according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: the power input of described microwave oven is adjustable continuously, and the atmosphere in the microwave oven is adjustable.
6, microwave exposure coal according to claim 1 prepares the method for active carbon with high specific surface area, it is characterized in that: the time of described microwave exposure is 3～60 minutes.
7, a kind of microwave exposure coal prepares the accurate one-dimensional carbon nano material method of (accurate one-dimensional carbon nano material described here comprises carbon nanotube and carbon nanofiber), it is characterized in that comprising the process of being prepared as follows: in the coal of washing, add a certain proportion of catalyst mix mill and spare, put into microwave oven and carry out irradiation, make it heating, burning and play electric arc, carry out purifying then, promptly get accurate one-dimensional carbon nano material.
8, microwave exposure coal according to claim 7 prepares the method for accurate one-dimensional carbon nano material, it is characterized in that: described coal is hard coal, bituminous coal, brown coal or mud coal.
9, microwave exposure coal according to claim 7 prepares the method for accurate one-dimensional carbon nano material, it is characterized in that: described catalyzer is Fe, Co, Ni and alloy thereof, they are reduced in preparation process by corresponding acetate, oxide compound, oxyhydroxide and generate, or add with the nano-powder metal.
10, microwave exposure coal according to claim 7 prepares the method for accurate one-dimensional carbon nano material, it is characterized in that: the massfraction that described catalyzer adds is 0.5%～5%.
11, microwave exposure coal according to claim 7 prepares the method for accurate one-dimensional carbon nano material, it is characterized in that: the power input of described microwave oven is adjustable continuously, and the atmosphere in the microwave oven is adjustable.
12, microwave exposure coal according to claim 7 prepares the method for accurate one-dimensional carbon nano material, it is characterized in that: the time of described microwave exposure is 3～60 minutes.
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| CN 200610031127 CN1857998A (en) | 2006-01-10 | 2006-01-10 | Method for preparing carbon nano material by micro wave radiation of coal |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100447076C (en) * | 2007-04-20 | 2008-12-31 | 北京交通大学 | Method of preparing multi-wall carbon nano-tube from coal |
| CN102602931A (en) * | 2012-03-27 | 2012-07-25 | 武汉纺织大学 | Method for preparing medical active carbon tube by utilizing hairs |
| CN103265029A (en) * | 2013-05-02 | 2013-08-28 | 石河子大学 | Mesoporous coal-based active carbon and microwave heating oriented preparation method thereof |
| TWI508917B (en) * | 2012-06-18 | 2015-11-21 | Univ Nat Yunlin Sci & Tech | Method of Activating Waste Carbon Fiber by Microwave |
| CN105239092A (en) * | 2015-10-13 | 2016-01-13 | 河北工程大学 | Microwave-chemical-synthesized high-activity catalyst and preparation method thereof |
| CN107986260A (en) * | 2018-01-08 | 2018-05-04 | 匡玉华 | A kind of microwave-heating formula coal carbon nanotube device |
| CN110562960A (en) * | 2019-09-05 | 2019-12-13 | 太原理工大学 | preparation and purification method of coal-based carbon nano tube |
| CN110713179A (en) * | 2019-10-10 | 2020-01-21 | 太原理工大学 | Coal-based carbon nanotube for deoxidizing low-concentration coal bed gas and preparation and purification methods thereof |
-
2006
- 2006-01-10 CN CN 200610031127 patent/CN1857998A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100447076C (en) * | 2007-04-20 | 2008-12-31 | 北京交通大学 | Method of preparing multi-wall carbon nano-tube from coal |
| CN102602931A (en) * | 2012-03-27 | 2012-07-25 | 武汉纺织大学 | Method for preparing medical active carbon tube by utilizing hairs |
| TWI508917B (en) * | 2012-06-18 | 2015-11-21 | Univ Nat Yunlin Sci & Tech | Method of Activating Waste Carbon Fiber by Microwave |
| CN103265029A (en) * | 2013-05-02 | 2013-08-28 | 石河子大学 | Mesoporous coal-based active carbon and microwave heating oriented preparation method thereof |
| CN105239092A (en) * | 2015-10-13 | 2016-01-13 | 河北工程大学 | Microwave-chemical-synthesized high-activity catalyst and preparation method thereof |
| CN105239092B (en) * | 2015-10-13 | 2017-12-22 | 河北工程大学 | Microwave chemical synthesis high activated catalyst and preparation method thereof |
| CN107986260A (en) * | 2018-01-08 | 2018-05-04 | 匡玉华 | A kind of microwave-heating formula coal carbon nanotube device |
| CN110562960A (en) * | 2019-09-05 | 2019-12-13 | 太原理工大学 | preparation and purification method of coal-based carbon nano tube |
| CN110562960B (en) * | 2019-09-05 | 2022-08-02 | 太原理工大学 | Preparation and purification method of coal-based carbon nano tube |
| CN110713179A (en) * | 2019-10-10 | 2020-01-21 | 太原理工大学 | Coal-based carbon nanotube for deoxidizing low-concentration coal bed gas and preparation and purification methods thereof |
| CN110713179B (en) * | 2019-10-10 | 2023-02-28 | 太原理工大学 | Coal-based carbon nano tube for deoxidizing low-concentration coal bed gas and preparation and purification methods thereof |
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