CN101962184A - Method for preparing active carbon by mechanical-chemical method - Google Patents
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Abstract
The invention relates to a method for preparing active carbon by a mechanical-chemical method. The method comprises the following specific steps of: (1) putting a dried carbon source material into 10 to 70 mass percent of solution of a pure aid in a mass ratio of 3:1-1, uniformly stirring and soaking at room temperature for 2 to 8 hours; (2) charging the material into grinding equipment, continuously grinding until average particle size is between 1 and 2 mu m and thermally treating at the temperature of between 300 and 700 DEG C for 30 to 60 minutes; and (3) washing the treated material with 10 percent solution of hydrochloric acid for 30 minutes, washing with deionized water until pH value is between 6 and 7 and transferring the material into a drying oven for drying after water washing is qualified so as to obtain powder active carbon. The method has the advantages of low reaction temperature, short time and low energy consumption. The prepared active carbon has the advantages of developed micropores, large specific surface area, rich surface functional group, higher pollutant adsorption efficiency, higher environmental compatibility, higher uniformity and low cost, and is convenient to operate and easy to regenerate.
Description
Technical field
The invention belongs to the chemical industry field, more specifically relate to a kind of mechanochemical method and prepare process of active carbon.
Background technology
In modern production and life, industry " three wastes " and urban life " three wastes " all must could discharge through purifying.Gac is widely used in industrial or agricultural and the field of environment protection as a kind of adsorption cleaning material.Yet at present the gac industry remains problems such as being easy to generate pollution in, the production process higher at production cost, therefore seeking new preparation method reduces production costs to reach, reduce secondary pollution in the production process, improve Properties of Activated Carbon simultaneously, enlarge the focus that its range of application just becomes present research tackling key problem.Some investigators have carried out the research of some low cost active charcoals, but this respect mainly is to utilize on the low-cost raw materials such as agriculture and industry waste, municipal wastes, as G ü lbeyi Dursun etc.
[1]Utilize beet pulp to produce gac and be used for adsorbing phenol, Amit Bhatnagar for raw material
[2]Utilize trade waste to produce the low cost active charcoal and be used for absorption removal water agricultural chemicals bromofos, full in summer should wait
[3]With the tobacco rod waste is that raw material, wood tar oil are that cakingagent, carbonic acid gas are that activator prepares the particle charcoal.
Traditionally, the generation of novel substance, crystal formation transform or lattice deformability is all realized by high temperature (heat energy) or chemical transformation, and mechanical force and chemical technology (Mechanochemical Process) is to utilize mechanical energy induced chemical reaction and induced material tissue, structure and changes of properties, carries out the modification processing with the preparation novel material or to material.In the last few years, many investigators had carried out big quantity research to aspects such as the theory of this emerging cross discipline of mechanical force and chemical, application, as, Jeong etc.
[4]Adopt mechanochemical method with LiOH.H
2O and Co (OH)
2Synthesize LiCoO with good electrical chemical property for raw material
2Powder.This method is simple to operate, and cost is low, and temperature of reaction is low, the preparation efficiency height, and the material particle of preparation is little, specific surface area is big, but size distribution is inhomogeneous, and purity is lower.Obrovac etc.
[5]With mechanochemical method made laminate structure LiMO2 (M=Ti, Mn, Fe, Co, Ni).The result shows that the material of preparation has bigger specific surface area and better electrochemical activity.S.Franger etc.
[6]Utilize physics and chemical means to existing several preparation LiFePO
4Method, as high temperature solid-state method, coprecipitation method, hydrothermal synthesis method and mechanochemical method, compare.The result shows that mechanochemical method can make temperature, granularity, crystalline structure and the composition of reactant and product even, thereby makes when synthetic target product that required Heating temperature reduces greatly, significantly reduce heat-up time.The product purity of Huo Deing is higher like this, the well-crystallized, and particle diameter is also less relatively, so the specific storage of material is higher, and chemical property is better.
Publication number is that the patent of invention of CN 1746107A discloses a kind of chestnut shell preparation method of active carbon, after this method is soaked chestnut shell and liquor zinci chloridi, need earlier under 380-680 ℃ of oxygen barrier condition charing 200-240 minute, in activation furnace 550-650 ℃ afterwards, pressure is to activate 30-45 minute in the 0.08-0.15MPa superheated vapour air-flow, through overpickling, obtain gac after the washing.Publication number be CN 101817524 A patent disclosure a kind of technology of utilizing physical activation method to produce gac, this method is the particulate material with compression moulding, sends in the special external-heating revolving activation furnace, activation temperature is at 800-900 degree centigrade.Above-mentioned technological process is all comparatively complicated, and temperature of reaction is higher, and it is bigger to consume energy.
Summary of the invention
The object of the present invention is to provide a kind of mechanochemical method to prepare process of active carbon, the mechanical force that this method utilizes grinding plant to produce, simultaneously under the acting in conjunction of chemical reagent and heating power, the physico-chemical property and the structure of carbon source material are had greatly changed, improved reactive behavior, thereby excite and quickened charing, reactivation process, reach many, fast, good thus, economize the purpose that ground prepares gac.
A kind of mechanochemical method prepares process of active carbon, and the concrete steps of this method are:
(1) weight ratio according to pure auxiliary agent and over dry carbon source material is the ratio of 1～3:1, and it is that 10～70% the compounding agent solution back that stirs is soaked under room temperature and put 2～8 hours that carbon source material is placed massfraction;
(2) above-mentioned material is packed into grinding plant, continuously grinding 30～60 minutes, to median size be 1～2 μ m, under 300～700 ℃ temperature, heat-treated 30～60 minutes then;
(3) the material massfraction after will handling again is 10% hydrochloric acid soln pickling 30 minutes; Being washed till the pH value with deionized water then is 6～7, washes to move to after qualified in the baking oven dryly, promptly obtains powdered carbon.Wherein said drying temperature is 105-120 ℃, time of drying 1-2h.
The described carbon source material of this method comes from plant material, coal and shell, and wherein plant material comprises all carbonaceous roots of plants, stem, materials such as leaf.Auxiliary agent described in the step (1) is a kind of in acid assistant, base agent, the salt assitant, acid assistant be liquid mineral acid phosphoric acid, vitriolic one or more; Base agent is one or more of alkali metal compound potassium hydroxide, sodium hydroxide; Salt assitant is one or more of metal salt compound zinc chloride, volatile salt, ammonium nitrate, salt of wormwood, yellow soda ash.Described grinding plant is ball mill, stir a kind of in mill, vibration mill, centrifugal grinding mills, basket shredder, horizontal mill, the colloidal mill.
The ultimate principle of this method is a mechanical force of utilizing grinding plant to produce, simultaneously under the acting in conjunction of chemical reagent and heating power, the physico-chemical property and the structure of carbon source material are had greatly changed, as cause the fracture of chemical bond, produce new surface, cause variations such as lattice imperfection, make in the material and can increase, make it be in a kind of unsettled chemical activity state, thereby catalysis has excited the generation of priming reaction, the reactive behavior of system is improved, has quickened charing, the reactivation process of preparation gac.
Remarkable advantage of the present invention: the original production process of active carbon of the present invention has shortened the reaction times greatly, reduced temperature of reaction, reduced energy consumption, the activated carbon capillary prosperity of preparing simultaneously, the specific surface area height is rich in surface functional group, has higher absorb polluted matter efficient, Environmental compatibility and homogeneity preferably, and easy to operate, cost is low, easy regeneration.
Description of drawings
Fig. 1 prepares the process flow sheet of gac for mechanochemical method.
Embodiment
A kind of mechanochemical method prepares process of active carbon, and the concrete steps of this method are:
(1) weight ratio according to pure auxiliary agent and over dry carbon source material is the ratio of 1～3:1, and it is that 10～70% the compounding agent solution back that stirs is soaked under room temperature and put 2～8 hours that carbon source material is placed massfraction;
(2) above-mentioned material is packed into grinding plant, continuously grinding 30～60 minutes, to median size at 1～2 μ m, under 300～700 ℃ temperature, heat-treated 30～60 minutes then;
(3) material after will handling again was with 10% hydrochloric acid soln pickling 30 minutes; Being washed till the pH value with deionized water then is 6～7, wash move to after qualified in the baking oven in 105 ℃-120 ℃ dry 1-2 hours down, can obtain the powdered carbon of well behaved micropore prosperity.
Embodiment 1
A kind of mechanochemical method prepares process of active carbon, and the concrete steps of this method are:
(1) weight ratio according to pure phosphoric acid and dry cedar sawdust is the ratio of 1:1, and it is that placed 8 hours under room temperature 60% the phosphoric acid solution back that stirs that cedar sawdust is placed massfraction;
(2) above-mentioned material is packed into ball mill, continuously grinding 30 minutes, to median size at 1～2 μ m, under 300 ℃ temperature, heat-treated 60 minutes then;
(3) material after will handling again was with 10% hydrochloric acid soln pickling 30 minutes; Being washed till the pH value with deionized water then is 6, wash move to after qualified in the baking oven in 120 ℃ dry 1 hour down, can obtain the powdered carbon of well behaved micropore prosperity.
Embodiment 2
A kind of mechanochemical method prepares process of active carbon, and the concrete preparation process of this method is:
(1) weight ratio according to pure zinc chloride and over dry pine sawdust is the ratio of 2:1, and it is that placed 5 hours under room temperature 45% the liquor zinci chloridi back that stirs that pine sawdust is placed massfraction;
(2) above-mentioned material is packed into vibration mill, continuously grinding 40 minutes, to median size at 1～2 μ m, under 500 ℃ temperature, heat-treated 45 minutes then;
(3) material after will handling again was with 10% hydrochloric acid soln pickling 30 minutes; Being washed till the pH value with deionized water then is 6.5, wash move to after qualified in the baking oven in 105 ℃ dry 1.5 hours down, can obtain the powdered carbon of well behaved micropore prosperity.
Embodiment 3
A kind of mechanochemical method prepares process of active carbon, and the concrete preparation process of this method is:
(1) weight ratio according to pure cerium hydroxide potassium and dry shell is the ratio of 3:1, and it is that placed 2 hours under room temperature 70% the potassium hydroxide back that stirs that shell is placed massfraction;
(2) above-mentioned material is packed into grinding plant, continuously grinding 60 minutes, to median size at 1～2 μ m, under 700 ℃ temperature, heat-treated 30 minutes then;
(3) material after will handling again was with 10% hydrochloric acid soln pickling 30 minutes; Being washed till the pH value with deionized water then is 7, wash move to after qualified in the baking oven in 110 ℃ dry 2 hours down, can obtain the powdered carbon of well behaved micropore prosperity.
Embodiment 4
A kind of mechanochemical method prepares process of active carbon, and the concrete preparation process of this method is:
(1) weight ratio according to pure cerium hydroxide potassium and over dry coal is the ratio of 3:1, and it is that placed 8 hours under room temperature 10% the potassium hydroxide back that stirs that shell is placed massfraction;
(2) above-mentioned material is packed into grinding plant, continuously grinding 40 minutes, to median size at 1～2 μ m, under 700 ℃ temperature, heat-treated 30 minutes then;
(3) material after will handling again was with 10% hydrochloric acid soln pickling 30 minutes; Being washed till the pH value with deionized water then is 7, wash move to after qualified in the baking oven in 110 ℃ dry 1.5 hours down, can obtain the powdered carbon of well behaved micropore prosperity.
The above only is preferred embodiment of the present invention, and all equalizations of being done according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Reference
[1]Gülbeyi?Dursun，Handan
，Arzu?Y.?Dursun．Adsorption?of?phenol?from?aqueous?solution?by?using?carbonised?beet?pulp[J]．Journal?of?Hazardous?Materials，2005，B125：175–182.
[2]Amit?Bhatnagar．Removal?of?bromophenols?from?water?using?industrial?wastes?as?low?cost?adsorbents[J]．Journal?of?Hazardous?Materials，2007，139（1，?2?）：93–102．
[3] full in summer is answered, Peng Jinhui, Zhang Libo. the research [J] of carbonic acid gas activation preparation tobacco rod base granulated active carbon. and gold, 2006, (27) 7:38 – 41.
[4]Jeong?W?T，Lee?K?S．Electrochemical?cycling?behavior?of?LiCoO
2?cathode?prepared?by?mechanical?alloying?of?hydroxides[J]．Journal?of?Power?Sources，2002，104：195—200．
[5]Obrovac?M?N，Mao?O，Dahn?J?R．Structure?and?electrochemistry?of?LiMO
2(M=?Ti，Mn，Fe，Co，Ni)prepared?by?mechanochemical?synthesis[J]．Solid?State?Ionics．，1998，112(2)：9-19．
[6]Franger?S，Bourbon?C，Rouauh?H，et?a1．Comparison?between?different?LiFePO
4?synthesis?routes?and?their?influence?on?its?physico—chemical?properties[J]．Journal?of?Power?Sources，2003，119：252—257．
Claims (5)
1. a mechanochemical method prepares process of active carbon, it is characterized in that, the concrete steps of this method are:
(1) mass ratio according to pure auxiliary agent and dried carbon source material is the ratio of 1～3:1, and it is that 10～70% the compounding agent solution back that stirs is soaked under room temperature and put 2～8 hours that carbon source material is placed massfraction;
(2) above-mentioned material is packed into grinding plant, continuously grinding 30～60 minutes, to median size be 1～2 μ m, thermal treatment 30～60 minutes under 300～700 ℃ temperature then;
(3) the material massfraction after will handling again is 10% hydrochloric acid soln pickling 30min minute; Being washed till the pH value with deionized water then is 6～7, washes to move to after qualified in the baking oven dryly, promptly obtains powdered carbon.
2.. a kind of mechanochemical method as claimed in claim 1 prepares process of active carbon, it is characterized in that: carbon source material is plant material, coal or shell.
3. a kind of mechanochemical method as claimed in claim 1 prepares process of active carbon, it is characterized in that: auxiliary agent described in the step (1) is a kind of in acid assistant, base agent, the salt assitant; Acid assistant be liquid mineral acid phosphoric acid, vitriolic one or more; Base agent is one or more of alkali metal compound potassium hydroxide, sodium hydroxide; Salt assitant is one or more of metal salt compound zinc chloride, volatile salt, ammonium nitrate, salt of wormwood, yellow soda ash.
4. a kind of mechanochemical method as claimed in claim 1 prepares process of active carbon, it is characterized in that: the described drying temperature of step (3) is 105-120 ℃, time of drying 1-2h.
5. a kind of mechanochemical method as claimed in claim 1 prepares process of active carbon, it is characterized in that: grinding plant is ball mill, stir a kind of in mill, vibration mill, centrifugal grinding mills, basket shredder, horizontal mill and the colloidal mill.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275911A (en) * | 2011-06-03 | 2011-12-14 | 中国林业科学研究院林产化学工业研究所 | Microporous active carbon and preparation method by chemical agent aperture regulation and control |
| CN102311113A (en) * | 2011-06-17 | 2012-01-11 | 深圳市今朝时代新能源技术有限公司 | Tobacco stalk based porous carbon material for electrodes of super capacitor and preparation method thereof |
| CN102826547A (en) * | 2012-08-08 | 2012-12-19 | 临沂胜兴活性炭有限公司 | Preparation method of peach pit activated carbon |
| CN103172064A (en) * | 2013-04-12 | 2013-06-26 | 宁夏大学 | Low-ash coal-based activated carbon quick activation production technology |
| CN103588201A (en) * | 2013-11-15 | 2014-02-19 | 白银海博生化科技有限公司 | Method for preparing activated carbon by using sunflower stalks |
| CN104760948A (en) * | 2015-04-22 | 2015-07-08 | 燕山大学 | Preparation method for high-performance porous carbon electrode material for super capacitor |
| CN104843704A (en) * | 2015-04-30 | 2015-08-19 | 大连理工大学 | Activated carbon comprising hierarchical hole channel and production method thereof |
| CN105236402A (en) * | 2015-10-30 | 2016-01-13 | 上海市政工程设计研究总院（集团）有限公司 | Method for preparing three-dimensional multilevel-pore activated carbon |
| CN109081343A (en) * | 2012-04-25 | 2018-12-25 | 卡尔冈碳素公司 | Reduce the leaching of arsenic and antimony from active carbon |
| CN109745948A (en) * | 2019-03-07 | 2019-05-14 | 中国科学院过程工程研究所 | One kind except cadmium adsorbent, and its preparation method and application |
| CN109865508A (en) * | 2019-04-09 | 2019-06-11 | 福建农林大学 | A kind of method of ultrasonic wave added melting eutectic alkali regenerating waste active carbon |
| CN109876785A (en) * | 2019-04-09 | 2019-06-14 | 福建农林大学 | A kind of method of ultrasonic wave added low melting point solid peracid regeneration waste active carbon |
| CN110182805A (en) * | 2019-06-22 | 2019-08-30 | 合肥煜创碳业有限公司 | A kind of preparation method of active carbon |
| CN113858010A (en) * | 2021-10-27 | 2021-12-31 | 湖南白绿林环保科技有限公司 | Modified activated carbon and preparation method thereof |
| CN115007214A (en) * | 2022-06-20 | 2022-09-06 | 鄂尔多斯市瀚博科技有限公司 | Copper-containing metal organic framework catalyst prepared by mechanochemical method and preparation method thereof |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275911A (en) * | 2011-06-03 | 2011-12-14 | 中国林业科学研究院林产化学工业研究所 | Microporous active carbon and preparation method by chemical agent aperture regulation and control |
| CN102311113A (en) * | 2011-06-17 | 2012-01-11 | 深圳市今朝时代新能源技术有限公司 | Tobacco stalk based porous carbon material for electrodes of super capacitor and preparation method thereof |
| CN109081343A (en) * | 2012-04-25 | 2018-12-25 | 卡尔冈碳素公司 | Reduce the leaching of arsenic and antimony from active carbon |
| CN102826547A (en) * | 2012-08-08 | 2012-12-19 | 临沂胜兴活性炭有限公司 | Preparation method of peach pit activated carbon |
| CN103172064A (en) * | 2013-04-12 | 2013-06-26 | 宁夏大学 | Low-ash coal-based activated carbon quick activation production technology |
| CN103588201B (en) * | 2013-11-15 | 2015-12-30 | 白银海博生化科技有限公司 | Sunflower straw is utilized to prepare active carbon method |
| CN103588201A (en) * | 2013-11-15 | 2014-02-19 | 白银海博生化科技有限公司 | Method for preparing activated carbon by using sunflower stalks |
| CN104760948A (en) * | 2015-04-22 | 2015-07-08 | 燕山大学 | Preparation method for high-performance porous carbon electrode material for super capacitor |
| CN104843704B (en) * | 2015-04-30 | 2017-05-24 | 大连理工大学 | Activated carbon comprising hierarchical hole channel and production method thereof |
| CN104843704A (en) * | 2015-04-30 | 2015-08-19 | 大连理工大学 | Activated carbon comprising hierarchical hole channel and production method thereof |
| CN105236402A (en) * | 2015-10-30 | 2016-01-13 | 上海市政工程设计研究总院（集团）有限公司 | Method for preparing three-dimensional multilevel-pore activated carbon |
| CN109745948A (en) * | 2019-03-07 | 2019-05-14 | 中国科学院过程工程研究所 | One kind except cadmium adsorbent, and its preparation method and application |
| CN109865508A (en) * | 2019-04-09 | 2019-06-11 | 福建农林大学 | A kind of method of ultrasonic wave added melting eutectic alkali regenerating waste active carbon |
| CN109876785A (en) * | 2019-04-09 | 2019-06-14 | 福建农林大学 | A kind of method of ultrasonic wave added low melting point solid peracid regeneration waste active carbon |
| CN109876785B (en) * | 2019-04-09 | 2022-03-08 | 福建农林大学 | Method for regenerating waste activated carbon by using ultrasonic-assisted low-melting-point solid acid |
| CN110182805A (en) * | 2019-06-22 | 2019-08-30 | 合肥煜创碳业有限公司 | A kind of preparation method of active carbon |
| CN113858010A (en) * | 2021-10-27 | 2021-12-31 | 湖南白绿林环保科技有限公司 | Modified activated carbon and preparation method thereof |
| CN113858010B (en) * | 2021-10-27 | 2023-10-13 | 湖南白绿林环保科技有限公司 | Modified activated carbon and preparation method thereof |
| CN115007214A (en) * | 2022-06-20 | 2022-09-06 | 鄂尔多斯市瀚博科技有限公司 | Copper-containing metal organic framework catalyst prepared by mechanochemical method and preparation method thereof |
| CN115007214B (en) * | 2022-06-20 | 2024-01-09 | 鄂尔多斯市瀚博科技有限公司 | Copper-based metal organic framework catalyst prepared by mechanochemical method and preparation method |
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Application publication date: 20110202 |