CN100581999C - Method for preparing coke breeze activated carbon from waste coke breeze - Google Patents
Method for preparing coke breeze activated carbon from waste coke breeze Download PDFInfo
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- CN100581999C CN100581999C CN200710017746A CN200710017746A CN100581999C CN 100581999 C CN100581999 C CN 100581999C CN 200710017746 A CN200710017746 A CN 200710017746A CN 200710017746 A CN200710017746 A CN 200710017746A CN 100581999 C CN100581999 C CN 100581999C
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Abstract
A method of preparing active carbon with waste coke powder is as follows: first, grinding the raw material of waste coke powder into 0.5-0.05mm, then mixing the coke powder with potassium nitrate with the mass ratio of 5:1, adding proper amount of water and uniformly stirring the mixture into paste, then moving the paste into a heating furnace and raising the temperature to 600 DEG C under the protection of nitrogen, after that, keeping the temperature for 30 minutes and then cooling to the room temperature to get pretreated coke powder; mixing the pretreated coke powder with activator with the mass ratio of 1:6, wherein, the activator consists of potassium hydroxide and calcium carbonate which have the mass ratio of 3:1, then adding proper amount of water and uniformly stirring the mixture, then moving the mixture into the heating furnace and raising the temperature to 650-900 DEG C under the protection of nitrogen, keeping the temperature for 40-100 minutes and then cooling to the room temperature to get crude active carbon; soaking the crude active carbon in 10% HF solution of 30ml for 3-4 hours, then washing and drying by hot deionized water to get the refined coke powder active carbon.
Description
Technical field
The present invention relates to the preparation technology of carbonaceous material.
Background technology
U.S. Pat 4082694 is to be raw material with refinery coke and coal, and having adopted potassium hydroxide is activator, in inert atmosphere, carries out precalcining between 350～400 ℃ and handles the activation that heats up again after 0.5～5.5 hour, has made the gac of high-specific surface area; Japanese Patent JP6144817 is to change the active carbon with high specific surface area that the activation temperature rise rate has made better adsorptivity; Chinese patent CN1186043A under 260～360 ℃, is an activator with potassium hydroxide with high softening point bitumen, activates in inert atmosphere, has obtained activated carbon with high specific surface area.These patents weak point aborning is that the activation yield is low, cost is high, adopts alkali burnt high, produces seriously pollutedly, and the gac pore size distribution is wide.
Summary of the invention
The purpose of this invention is to provide a kind of method with preparing coke breeze activated carbon from waste coke breeze.
The present invention prepares process of active carbon with discarded coke powder, carries out as follows:
(1) will discard coke powder raw material pulverizing to 0.5～0.05mm, coke powder is mixed with saltpetre, mass ratio is 5: 1, add suitable quantity of water, stir into a paste, move in the process furnace, be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling to room temperature gets pretreated coke powder;
(2) pretreated coke powder is mixed with the mass ratio of activator by 1: 6, wherein activator is made up of potassium hydroxide and lime carbonate, and mass ratio is 3: 1; stir with suitable quantity of water, move in the process furnace, under nitrogen protection, be warming up to 650～900 ℃; insulation 40-100min is cooled to room temperature.Promptly get rough coke powder gac.
(3) in rough gac, add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying promptly get and make with extra care the coke powder gac.
Compared with the prior art method of the present invention has following advantage:
1, be the feedstock production gac with discarded coke powder, favourable refuse is usefulness again, save energy, protection environment.
2, will discard the processing that stirs of coke powder, composite activating agent and water, and help activator and fully contact, make the reaction homogeneous, and reduce to pollute with coke powder.
3, this activator is KOH-K
2CO
3Mixture, its ratio is 3: 1.Use this activator to help reducing equipment contaminate and environmental pollution.
Embodiment
The present invention prepares process of active carbon with discarded coke powder, carries out as follows:
(1) will discard coke powder raw material pulverizing to 0.5～0.05mm, coke powder is mixed with saltpetre, mass ratio is 5: 1, add suitable quantity of water, stir into a paste, move in the process furnace, be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling to room temperature gets pretreated coke powder;
(2) pretreated coke powder is mixed with the mass ratio of activator by 1: 6, wherein activator is made up of potassium hydroxide and lime carbonate, and mass ratio is 3: 1; stir with suitable quantity of water, move in the process furnace, under nitrogen protection, be warming up to 650～900 ℃; insulation 40-100min is cooled to room temperature.Promptly get rough coke powder gac.
(3) in rough gac, add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying promptly get and make with extra care the coke powder gac.
It is 5: 1 that the mass ratio of coke powder and saltpetre is adopted in pre-treatment, 600 ℃ of following oxide treatment.Activator is made up of potassium hydroxide and lime carbonate, and mass ratio is 3: 1.Used process furnace is a retort furnace, and heat-up rate is 10～15 ℃/min, and activation temperature is 650 ℃-900 ℃.Washing is to wash with hydrofluoric acid earlier, the reusable heat washing.
Be several specific embodiments that the present invention is prepared below:
Embodiment 1:
To discard coke powder (moisture 2.46%, ash content 15.4%, volatile matter 3.57%, sulphur content 0.9%, fixed carbon 78.89%) fragmentation; be sized to 0.05mm; press coke powder: saltpetre=5: 1 (mass ratio); add suitable quantity of water; stir into a paste; be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling is to room temperature.Get the pre-treatment coke powder: composite activating agent=1/6 stirs with suitable quantity of water, moves in the retort furnace, is warming up to 850 ℃ under nitrogen protection, and insulation 100min is cooled to room temperature.Add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying get the coke powder gac.The activation productive rate is 39.8%, its methylene radical adsorptive value 270.0mg/g.
Embodiment 2:
To discard coke powder (moisture 2.46%, ash content 15.4%, volatile matter 3.57%, sulphur content 0.9%, fixed carbon 78.89%) fragmentation; be sized to 0.05-0.08mm; press coke powder: saltpetre=5: 1 (mass ratio); add suitable quantity of water; stir into a paste; be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling is to room temperature.Get the pre-treatment coke powder: composite activating agent=1/5 stirs with suitable quantity of water, moves in the retort furnace, is warming up to 750 ℃ under nitrogen protection, and insulation 80min is cooled to room temperature.Add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying get the coke powder gac.The activation productive rate is 46.4%, its methylene radical adsorptive value 172.5mg/g.
Embodiment 3:
To discard coke powder (moisture 2.46%, ash content 15.4%, volatile matter 3.57%, sulphur content 0.9%, fixed carbon 78.89%) fragmentation; be sized to 0.08-0.18mm; press coke powder: saltpetre=5: 1 (mass ratio); add suitable quantity of water; stir into a paste; be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling is to room temperature.Get the pre-treatment coke powder: composite activating agent=1/5 stirs with suitable quantity of water, moves in the retort furnace, is warming up to 850 ℃ under nitrogen protection, and insulation 80min is cooled to room temperature.Add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying get the coke powder gac.The activation productive rate is 48.6%, its methylene radical adsorptive value 198.0mg/g.
Embodiment 4:
To discard coke powder (moisture 2.46%, ash content 15.4%, volatile matter 3.57%, sulphur content 0.9%, fixed carbon 78.89%) fragmentation; be sized to 0.18-0.5mm; press coke powder: saltpetre=5: 1 (mass ratio); add suitable quantity of water; stir into a paste; be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling is to room temperature.Get the pre-treatment coke powder: composite activating agent=1/4 stirs with suitable quantity of water, moves in the retort furnace, is warming up to 850 ℃ under nitrogen protection, and insulation 60min is cooled to room temperature.Add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying get the coke powder gac.The activation productive rate is 40.6%, its methylene radical adsorptive value 148.5mg/g.
Embodiment 5:
To discard coke powder (moisture 2.46%, ash content 15.4%, volatile matter 3.57%, sulphur content 0.9%, fixed carbon 78.89%) fragmentation; be sized to 0.05mm; press coke powder: saltpetre=5: 1 (mass ratio); add suitable quantity of water; stir into a paste; be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling is to room temperature.Get the pre-treatment coke powder: composite activating agent=1/4 stirs with suitable quantity of water, moves in the retort furnace, is warming up to 750 ℃ under nitrogen protection, and insulation 40min is cooled to room temperature.Add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying get the coke powder gac.The activation productive rate is 45.9%, its methylene radical adsorptive value 186.0mg/g.
Embodiment 6:
To discard coke powder (moisture 2.46%, ash content 15.4%, volatile matter 3.57%, sulphur content 0.9%, fixed carbon 78.89%) fragmentation; be sized to 0.18-0.5mm; press coke powder: saltpetre=5: 1 (mass ratio); add suitable quantity of water; stir into a paste; be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling is to room temperature.Get the pre-treatment coke powder: composite activating agent=1/6 stirs with suitable quantity of water, moves in the retort furnace, is warming up to 750 ℃ under nitrogen protection, and insulation 80min is cooled to room temperature.Add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying get the coke powder gac.The activation productive rate is 48.0%, its methylene radical adsorptive value 120.0mg/g.
Claims (1)
1, prepare process of active carbon with discarded coke powder, it is characterized in that carrying out as follows:
(1) will discard coke powder raw material pulverizing to 0.5～0.05mm, coke powder is mixed with saltpetre, mass ratio is 5: 1, add suitable quantity of water, stir into a paste, move in the process furnace, be warming up to 600 ℃ under nitrogen protection, insulation 30min postcooling to room temperature gets pretreated coke powder;
(2) pretreated coke powder is mixed with the mass ratio of activator by 1: 6, wherein activator is made up of potassium hydroxide and lime carbonate, mass ratio is 3: 1, stir with suitable quantity of water, move in the process furnace, under nitrogen protection, be warming up to 650～900 ℃, insulation 40-100min, be cooled to room temperature, promptly get rough coke powder gac;
(3) in rough gac, add 30ml 10% hydrofluoric acid solution and soaked 3-4 hour, reusable heat deionized water wash, drying promptly get and make with extra care the coke powder gac.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710017746A CN100581999C (en) | 2007-04-19 | 2007-04-19 | Method for preparing coke breeze activated carbon from waste coke breeze |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710017746A CN100581999C (en) | 2007-04-19 | 2007-04-19 | Method for preparing coke breeze activated carbon from waste coke breeze |
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| CN101190789A CN101190789A (en) | 2008-06-04 |
| CN100581999C true CN100581999C (en) | 2010-01-20 |
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| CN200710017746A Expired - Fee Related CN100581999C (en) | 2007-04-19 | 2007-04-19 | Method for preparing coke breeze activated carbon from waste coke breeze |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434389B (en) * | 2008-12-10 | 2011-02-16 | 南京林业大学 | Preparation of super active carbon |
| CN101579536B (en) * | 2009-07-03 | 2012-07-25 | 遵化市春雨环保设备研究所 | Preparation method of an air freshener of activated carbon |
| CN102748949A (en) * | 2012-06-26 | 2012-10-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Powder material heating device and technology |
| CN103350997B (en) * | 2013-07-04 | 2015-05-27 | 陕西煤业化工技术研究院有限责任公司 | Technique for preparing activated carbon with powdered coal pyrolysis powdered coke |
| CN104692382B (en) * | 2014-12-10 | 2017-01-18 | 山东钢铁股份有限公司 | Method for preparing active carbon by using coke reactivity testing device |
| CN105480975A (en) * | 2016-02-25 | 2016-04-13 | 黑龙江省科学院大庆分院 | Method for preparing high-specific-surface-area porous carbon with hemp stems as carbon source |
| CN109835900A (en) * | 2019-03-21 | 2019-06-04 | 哈尔滨工业大学 | A kind of preparation method of the coal base porous carbon based on potassium carbonate cyclic activation and the preparation method of biomass-based porous carbon |
| CN115073138B (en) * | 2022-07-20 | 2023-07-21 | 俄源实业(上海)有限公司 | Preparation method of high-performance ceramic heat-insulating material and material prepared by same |
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2007
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Non-Patent Citations (2)
| Title |
|---|
| 用废弃的半焦焦粉制活性炭工业性试验研究. 张彩荣等.煤炭转化，第22卷第2期. 1999 |
| 用废弃的半焦焦粉制活性炭工业性试验研究. 张彩荣等.煤炭转化，第22卷第2期. 1999 * |
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| CN101190789A (en) | 2008-06-04 |
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