CN102001656A - Method for preparing high-adsorbability activated carbon by using rice hulls as raw material - Google Patents
Method for preparing high-adsorbability activated carbon by using rice hulls as raw material Download PDFInfo
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- CN102001656A CN102001656A CN 201010586233 CN201010586233A CN102001656A CN 102001656 A CN102001656 A CN 102001656A CN 201010586233 CN201010586233 CN 201010586233 CN 201010586233 A CN201010586233 A CN 201010586233A CN 102001656 A CN102001656 A CN 102001656A
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- filter residue
- zinc chloride
- mass concentration
- repone
- rice husk
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Abstract
The invention relates to a method for preparing high-adsorbability activated carbon by using rice hulls as a raw material. The method comprises the following steps of: providing rice hulls, carrying out acid and alkali treatment and washing the rice hulls to obtain neutral filter residue; drying the filter residue, soaking in an eutectic solution of zinc chloride and potassium chloride at 70-80 DEG C for not less than 9h; taking out the filter residue, pouring into a porcelain crucible, putting into a muffle furnace to activate at 400-800 DEG C for 1-2h; washing, filtering and washing with water to be neutral; and drying and grinding to obtain the product, wherein in the eutectic solution of the zinc chloride and the potassium chloride, the mass concentration of the zinc chloride is 20-60 percent, and the mass concentration of the potassium chloride is 2-10 percent. The invention is easy to form a thin hole structure and can manufacture activated carbon with robust holes and better adsorbability, and the activating method has less carbon loss and relative high carbon yield.
Description
Technical field
The present invention relates to a kind of preparation method of active carbon, is a kind of method with rice husk feedstock production high-adsorption active carbon specifically.
Background technology
Gac is a kind of porous carbon material, and early oneself is widely used in fields such as chemical industry, food-processing, transportation and energy, health care, agricultural, national defence.
Known employing rice husk is in the feedstock production process of active carbon, and chemical activation method can produce void ratio prosperity, the reasonable gac of absorption property than gas activation method, and the activation of chemical activation method can be carried out under low relatively temperature.
Usually the chemical activation method that adopts is through acid treatment (removing impurity such as little metal) with rice husk, filter residue is washed to neutrality, then through alkaline purification (removing silicon), filter residue is washed to neutrality again, pharmaceutical chemicals is added in the filter residue with certain proportion, in the rare gas element medium, heat then, carry out charing and activation simultaneously, again the chemical agent that adds is reclaimed at last.In reactivation process, with chemical agent etching carbonaceous material, and make wherein hydrogen and element such as oxygen mainly with H
2O, CH
4Overflow Deng the small molecules form, suppress the formation of by product tar, can improve the gac yield, the main chemical agent of use has KOH, H
3PO
4, H
2SO
4, ZnCl
2, NaOH etc.
More than two kinds of methods to prepare gac table of equipment cover many, accuracy requirement height, cost height, energy consumption are big, the technology relative complex, pollute problems such as big.
Summary of the invention
The purpose of this invention is to provide a kind of method, adopt this method can produce that hole is more flourishing, the better gac of absorption property, and the charcoal loss is little, relatively the yield height with rice husk feedstock production high-adsorption active carbon.
Provided by the invention a kind of be the method for feedstock production high-adsorption active carbon with the rice husk, this method provide rice husk through acid-alkali treatment again through being washed to the neutral filter residue, with this filter residue and drying, be total to solution immersion under 70～80 ℃ with zinc chloride and Repone K and be not less than 9 hours; The filter residue taking-up is poured in the porcelain crucible, put retort furnace into and activate 1～2 hour down at 400～800 ℃; Through washing, filter, be washed to neutrality, drying is ground promptly again; The mass concentration that described zinc chloride and Repone K are total to zinc chloride in the solution is 20～60%, and the mass concentration of Repone K is 2～10%.
Solution is as activator altogether for zinc chloride and Repone K, and in this common solution, zinc chloride is main activator, and Repone K is activator promotor.Because of potassium ion in the Repone K is gone out the potassium metal by aquagenic hydrogen exchange under the high temperature, when activation temperature surpassed 762 ℃ of potassium metal boiling points, the potassium metal can diffuse into the charcoal layer and stay micropore, thereby improves the gac activity greatly.So the charcoal absorption performance prepared than the activator of single component of the absorption property of the gac prepared as activator of solution is higher altogether for zinc chloride and Repone K.
In the present invention, the time of solution soaking can not be too short altogether with zinc chloride and Repone K, lacked very much can infiltration insufficiently, and the part rice husk can not be activated, thereby causes productive rate to descend, and is also not too long, preferably 10～20 hours.
Filter residue after activated need wash it, and to remove deactivator, in the present invention, washings is the hydrochloric acid of mass concentration 8～12% preferably.
In above-mentioned, the temperature of oven dry is 105～120 ℃.
The said filter residue of the present invention, this filter residue prepares according to a conventional method, is about to rice husk through acid treatment (removing impurity such as little metal), and filter residue is washed to neutrality, and through alkaline purification (removing silicon), filter residue is washed to neutrality again and obtains then.In addition, also can make as follows:
A certain amount of rice husk through washing, with certain density acid soak regular hour (or refluxing 1～4 hour under 100 ℃), is filtered, and filtrate uses it for anything else in addition, and filter residue is washed to neutrality.
This filter residue is put into the there-necked flask of 500ml, and adding concentration is KOH solution or the NaOH solution of 1～4mol/L, and 85～120 ℃ of following back flow reaction 1～4h filter, and filtrate uses it for anything else in addition, and filter residue is washed to neutrality.
For the gac of the present invention's preparation, adopt the GB7702-87 standard, with the adsorptive value test sample of iodine, the result shows: the gac of this method preparation has very high absorption property, and possesses higher purity.These product performance have also directly been verified in specific surface and porosity test.
The present invention compared with prior art; carbonization-activation is once finished; need under the protection of rare gas element etc., not activate; the carbonization-activation temperature is low; help forming the less carbon crystallite of size, form thin pore texture easily, can produce that hole is more flourishing, the better gac of absorption property; and the loss of this activation method carbon is little, the relative yield height of charcoal.In addition, table of equipment required for the present invention cover is few, invests for a short time, and technology is simple, realizes suitability for industrialized production easily.
Embodiment
In order better to understand the present invention, below in conjunction with embodiment the present invention is described in further detail, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Raw material filter residue in the following example all adopts the method for prior art to obtain, and is about to rice husk through acid treatment (removing impurity such as little metal), and filter residue is washed to neutrality, and through alkaline purification (removing silicon), filter residue is washed to neutrality more then.
Embodiment 1
With filter residue and drying, be total to solution with zinc chloride and Repone K and soaked 20 hours down at 70 ℃, the mass concentration that wherein is total to zinc chloride in the solution is 20%, the mass concentration of Repone K is 10%; The filter residue taking-up is poured in the porcelain crucible, put retort furnace into and activate 2 hours down at 400 ℃; With the washings salt acid elution of mass concentration 8%, filter, be washed to neutrality, 120 ℃ of oven dry down, grind promptly.
Embodiment 2
With filter residue and drying, be total to solution with zinc chloride and Repone K and soaked 10 hours down at 80 ℃, the mass concentration that wherein is total to zinc chloride in the solution is 60%, the mass concentration of Repone K is 2%; The filter residue taking-up is poured in the porcelain crucible, put retort furnace into and activate 1 hour down at 800 ℃; With the washings salt acid elution of mass concentration 12%, filter, be washed to neutrality, 105 ℃ of oven dry down, grind promptly.
Embodiment 3
With filter residue and drying, be total to solution with zinc chloride and Repone K and soaked 15 hours down at 75 ℃, the mass concentration that wherein is total to zinc chloride in the solution is 40%, the mass concentration of Repone K is 5%; The filter residue taking-up is poured in the porcelain crucible, put retort furnace into and activate 1.5 hours down at 600 ℃; With the washings salt acid elution of mass concentration 10%, filter, be washed to neutrality, 112 ℃ of oven dry down, grind promptly.
Embodiment 4
With filter residue and drying, be total to solution with zinc chloride and Repone K and soaked 10 hours down at 80 ℃, the mass concentration that wherein is total to zinc chloride in the solution is 50%, the mass concentration of Repone K is 10%; The filter residue taking-up is poured in the porcelain crucible, put retort furnace into and activate 1 hour down at 800 ℃; With the washings salt acid elution of mass concentration 12%, filter, be washed to neutrality, 105 ℃ of oven dry down, grind promptly.
Claims (4)
1. one kind is the method for feedstock production high-adsorption active carbon with the rice husk, it is characterized in that, provide rice husk through acid-alkali treatment again through being washed to the neutral filter residue, with this filter residue and drying, with zinc chloride and Repone K altogether solution soak down at 70～80 ℃ and be not less than 9 hours; The filter residue taking-up is poured in the porcelain crucible, put retort furnace into and activate 1～2 hour down at 400～800 ℃; Through washing, filter, be washed to neutrality, drying is ground and is promptly got product again; The mass concentration that described zinc chloride and Repone K are total to zinc chloride in the solution is 20～60%, and the mass concentration of Repone K is 2～10%.
2. according to claim 1 a kind of be the method for feedstock production high-adsorption active carbon with the rice husk, it is characterized in that washing used washings is the hydrochloric acid of mass concentration 8～12%.
3. according to claim 1 a kind of be the method for feedstock production high-adsorption active carbon with the rice husk, it is characterized in that the temperature of oven dry is 105～120 ℃.
4. according to claim 1 a kind of be the method for feedstock production high-adsorption active carbon with the rice husk, it is characterized in that the time of solution soaking is 10～20 hours altogether with zinc chloride and Repone K.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010586233 CN102001656A (en) | 2010-12-14 | 2010-12-14 | Method for preparing high-adsorbability activated carbon by using rice hulls as raw material |
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|---|---|---|---|
| CN 201010586233 CN102001656A (en) | 2010-12-14 | 2010-12-14 | Method for preparing high-adsorbability activated carbon by using rice hulls as raw material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614829A (en) * | 2012-03-20 | 2012-08-01 | 江南大学 | Method for preparing mycotoxin adsorbent for efficient carbon silicon feed by taking rice hulls as raw materials |
| CN102786052A (en) * | 2012-07-16 | 2012-11-21 | 太仓市联林活性炭厂 | Method for preparation of activated carbon through rice hull desilication |
| CN102847512A (en) * | 2012-09-27 | 2013-01-02 | 江南大学 | Preparation method of rice husk based porous carbon fungaltoxin adsorbent |
| CN103539119A (en) * | 2013-10-30 | 2014-01-29 | 中国第一汽车股份有限公司 | Preparation method of activated carbon for electrochemical energy storage device |
| CN103566880A (en) * | 2013-09-29 | 2014-02-12 | 安徽金叶炭素科技有限公司 | Rice hull modified active carbon adsorption desulfurizing agent and preparation method thereof |
| CN103566903A (en) * | 2013-09-29 | 2014-02-12 | 安徽金叶炭素科技有限公司 | Attapulgite clay modified active carbon and preparation method thereof |
| CN104163427A (en) * | 2014-07-21 | 2014-11-26 | 大连理工大学 | Method utilizing melt salt activation to prepare active carbon |
| CN104437361A (en) * | 2014-10-24 | 2015-03-25 | 东华大学 | Method for preparing functional biological carbon by in-situ impregnation |
| CN104709905A (en) * | 2013-12-16 | 2015-06-17 | 中国科学院兰州化学物理研究所 | Method for preparing supercapacitor-dedicated active carbon by using mixed molten salts as activator |
| CN107188170A (en) * | 2017-06-01 | 2017-09-22 | 镇江四联机电科技有限公司 | A kind of use mixed base activation prepares the production technology of activated carbon |
| CN110294475A (en) * | 2019-06-06 | 2019-10-01 | 中国林业科学研究院林产化学工业研究所 | Zinc chloride process active carbon and preparation method thereof |
-
2010
- 2010-12-14 CN CN 201010586233 patent/CN102001656A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《粮食与饲料工业》 20051231 左秀凤等 氯化锌活化稻壳制备活性炭的研究 第5-7页 1-4 , 第12期 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614829A (en) * | 2012-03-20 | 2012-08-01 | 江南大学 | Method for preparing mycotoxin adsorbent for efficient carbon silicon feed by taking rice hulls as raw materials |
| CN102786052A (en) * | 2012-07-16 | 2012-11-21 | 太仓市联林活性炭厂 | Method for preparation of activated carbon through rice hull desilication |
| CN102847512B (en) * | 2012-09-27 | 2015-09-02 | 江南大学 | A kind of rice husk base porous charcoal mycotoxin absorbant preparation method |
| CN102847512A (en) * | 2012-09-27 | 2013-01-02 | 江南大学 | Preparation method of rice husk based porous carbon fungaltoxin adsorbent |
| CN103566880A (en) * | 2013-09-29 | 2014-02-12 | 安徽金叶炭素科技有限公司 | Rice hull modified active carbon adsorption desulfurizing agent and preparation method thereof |
| CN103566903A (en) * | 2013-09-29 | 2014-02-12 | 安徽金叶炭素科技有限公司 | Attapulgite clay modified active carbon and preparation method thereof |
| CN103566903B (en) * | 2013-09-29 | 2016-01-27 | 安徽金叶炭素科技有限公司 | A kind of Concave-convex clay rod modified activated carbon and preparation method thereof |
| CN103566880B (en) * | 2013-09-29 | 2016-01-27 | 安徽金叶炭素科技有限公司 | A kind of rice husk modified activated carbon adsorption desulfurizing agent and preparation method thereof |
| CN103539119A (en) * | 2013-10-30 | 2014-01-29 | 中国第一汽车股份有限公司 | Preparation method of activated carbon for electrochemical energy storage device |
| CN104709905A (en) * | 2013-12-16 | 2015-06-17 | 中国科学院兰州化学物理研究所 | Method for preparing supercapacitor-dedicated active carbon by using mixed molten salts as activator |
| CN104163427A (en) * | 2014-07-21 | 2014-11-26 | 大连理工大学 | Method utilizing melt salt activation to prepare active carbon |
| CN104437361A (en) * | 2014-10-24 | 2015-03-25 | 东华大学 | Method for preparing functional biological carbon by in-situ impregnation |
| CN107188170A (en) * | 2017-06-01 | 2017-09-22 | 镇江四联机电科技有限公司 | A kind of use mixed base activation prepares the production technology of activated carbon |
| CN110294475A (en) * | 2019-06-06 | 2019-10-01 | 中国林业科学研究院林产化学工业研究所 | Zinc chloride process active carbon and preparation method thereof |
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Application publication date: 20110406 |