CN102874805A - Method for preparing porous carbon for wastewater treatment - Google Patents
Method for preparing porous carbon for wastewater treatment Download PDFInfo
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- CN102874805A CN102874805A CN2012103465849A CN201210346584A CN102874805A CN 102874805 A CN102874805 A CN 102874805A CN 2012103465849 A CN2012103465849 A CN 2012103465849A CN 201210346584 A CN201210346584 A CN 201210346584A CN 102874805 A CN102874805 A CN 102874805A
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Abstract
The invention relates to a method for preparing porous carbon for wastewater treatment. The method comprises the following steps: (1) pretreating semi coke with the grain size of 5 to 18 mm and soaking in a mixed solution of organic matters and inorganic salts at certain concentration; (2) directly activating products which are dried and dehydrated at the temperature of between 750 and 850 DEG C for 60 to 180 minutes; and (3) performing acid treatment on the activated products, washing and drying to obtain the porous carbon. According to the scheme, the semi coke directly serves as a raw material and one-step activating treatment is adopted without the steps of crushing, deashing, kneading, forming, carbonizing and the like, so the process is simple, the cost is low, and the prepared porous carbon has abundant micropore-mesopore-macropore structures, can adsorb various metal ions and organic matters in sanitary wastewater and industrial wastewater and is widely applied.
Description
Technical field
The present invention relates to a kind of preparation method of porous charcoal, a kind ofly specifically prepare porous charcoal take blue charcoal as raw material, be mainly used in the processing trade effluent.
Background technology
Porous carbon material refers to have the Novel carbon material of different gap structures, its hole size from have can adsorbing metal ions micropore (＜2nm) to mesopore that can the adsorb organic compound molecule (2～50nm) and macropore (＞50nm).
Patent CN 102500319 has announced a kind of method that improves mesoporous rate in porous carbon.The porous charcoal that the method makes has good removal effect to organism in the sewage, helps the industrial applications of porous charcoal in water quality.But the method needs porous charcoal is carried out the hydrogen peroxide dipping, needs the secondary charing, re-activation, complex process.
Summary of the invention
It is lower to the purpose of this invention is to provide a kind of cost, and preparation technology is simple, has abundant micropore-mesopore-macroporous structure, can be used for the preparation method of the porous charcoal of sanitary wastewater and industrial waste water purifying.
A kind of preparation method of the porous charcoal for wastewater treatment mainly may further comprise the steps:
(1) the blue charcoal with 5～18mm particle diameter is immersed in certain density organism and the inorganic salt mixing solutions;
(2) to dried product direct activation;
(3) activation products are carried out acid treatment, through cleaning, drying obtains porous charcoal again.
A kind of preparation method's step (1) of the porous charcoal for wastewater treatment, organism kinds comprises citric acid, oxalic acid and polyacrylamide, inorganic salt comprise iron nitrate, nitrocalcite or Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES.
A kind of preparation method's step (2) of the porous charcoal for wastewater treatment, the temperature of product activation is 750～850 ℃, soak time 60～180min, 6～10 ℃ of temperature rise rates.
A kind of preparation method's step (3) of the porous charcoal for wastewater treatment, the kind of acid comprises hydrochloric acid, nitric acid, 60～100 ℃ of pickling temperatures, pickling time 30～90min, acid solution PH=2～5.
The present invention adopts cheap blue charcoal, and (particle diameter: 5～18mm) are raw material, adopt the direct activation method, do not need the steps such as fragmentation, moulding, granulation, charing, have reduced cost, and technique is simple; By pickling, can remove organic matter and micro-alkali soluble salt in the porous charcoal, impel the part micropore to move to mesopore, macropore direction.This porous charcoal has abundant pore structure: micropore-mesopore-macropore, can fully adsorb metal ion and the organism of waste water, and be suitable for various sanitary wastewaters and trade effluent.
Embodiment
Embodiment one:
(particle diameter: 5～18mm) are immersed in the citric acid and iron nitrate mixing solutions of 0.1mol/L soak time 20min, 90 ℃ of product drying temperatures with blue charcoal.Pour into after the drying in the activation furnace, at N
2Heat up under the atmosphere, 6 ℃/min of temperature rise rate, 750 ℃ of activation temperatures, soak time 60min when reaching activation temperature, closes the nitrogen valve, passes into high-pressure steam.Activation is oscillation cleaning 30min in the HCl of PH=5 solution afterwards, and the hydrochloric acid soln temperature 60 C cleans with boiling tap water, until about PH=7, oven dry just obtains porous charcoal.Through test, the intensity of porous charcoal is 93%, and iodine sorption value is 458mg/g, and methylene blue adsorption number matter 235mg/g, COD clearance are 91%.
Embodiment two:
(particle diameter: 5～18mm) are immersed in the oxalic acid acid and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES mixing solutions of 0.8mol/L time 30min, 90 ℃ of product drying temperatures with blue charcoal.Pour into after the drying in the activation furnace, at N
2Heat up under the atmosphere, 8 ℃/min of temperature rise rate, 800 ℃ of activation temperatures, soak time 180min when reaching activation temperature, closes the nitrogen valve, passes into high-pressure steam.The rear HNO at PH=3 of activation
3Oscillation cleaning 40min in the solution, 90 ℃ of hydrochloric acid soln temperature are cleaned with boiling tap water, until about PH=7, oven dry just obtains porous charcoal.Through test, the intensity of porous charcoal is 92%, and iodine sorption value is 489mg/g, and methylene blue adsorption number matter 318mg/g, COD clearance are 96%.
Embodiment three:
(particle diameter: 5～18mm) are immersed in the oxalic acid acid and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES mixing solutions of 1.2mol/L time 30min, 90 ℃ of product drying temperatures with blue charcoal.Pour into after the drying in the activation furnace, at N
2Heat up under the atmosphere, 10 ℃/min of temperature rise rate, 850 ℃ of activation temperatures, soak time 120min when reaching activation temperature, closes the nitrogen valve, passes into high-pressure steam.Activation is oscillation cleaning 60min in the HCl of PH=2 solution afterwards, and 90 ℃ of hydrochloric acid soln temperature are cleaned with boiling tap water, until about PH=7, oven dry just obtains porous charcoal.Through test, the intensity of porous charcoal is 90%, and iodine sorption value is 412mg/g, and methylene blue adsorption number matter 288mg/g, COD clearance are 92%.
Embodiment four:
(particle diameter: 5～18mm) are immersed in the oxalic acid acid and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES mixing solutions of 0.8mol/L time 30min, 90 ℃ of product drying temperatures with blue charcoal.Pour into after the drying in the activation furnace, at N
2Heat up under the atmosphere, 8 ℃/mmin of temperature rise rate, 800 ℃ of activation temperatures, soak time 150min when reaching activation temperature, closes the nitrogen valve, passes into high-pressure steam.The rear HNO at PH=4 of activation
3Oscillation cleaning 70min in the solution, 90 ℃ of hydrochloric acid soln temperature are cleaned with boiling tap water, until about PH=7, oven dry just obtains porous charcoal.Through test, the intensity of porous charcoal is 94%, and iodine sorption value is 373mg/g, and methylene blue adsorption number matter 247mg/g, COD clearance are 93%.
Embodiment five:
(particle diameter: 5～18mm) are immersed in the oxalic acid acid and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES mixing solutions of 2.0mol/L time 20min, 90 ℃ of product drying temperatures with blue charcoal.Pour into after the drying in the activation furnace, at N
2Heat up under the atmosphere, 9 ℃/min of temperature rise rate, 830 ℃ of activation temperatures, soak time 180min when reaching activation temperature, closes the nitrogen valve, passes into high-pressure steam.The rear HNO at PH=2.5 of activation
3Oscillation cleaning 90min in the solution, 85 ℃ of hydrochloric acid soln temperature are cleaned with boiling tap water, until about PH=7, oven dry just obtains porous charcoal.Through test, the intensity of porous charcoal is 93%, and iodine sorption value is 361mg/g, and methylene blue adsorption number matter 285mg/g, COD clearance are 91%.
Claims (4)
1. preparation method who is used for the porous charcoal of wastewater treatment is characterized in that its technique may further comprise the steps:
(1) pre-treatment is carried out in the blue charcoal of 5-18mm particle diameter, in certain density organism and inorganic salt mixing solutions, soak;
(2) product behind the drying and dehydrating is carried out direct activation;
(3) activation products are carried out acid treatment, obtain porous charcoal through cleaning, drying again.
2. the preparation method of a kind of porous charcoal for wastewater treatment according to claim 1, it is characterized in that: in described step (1), organic concentration is 0.1～2mol/L, organism kinds comprises polyacrylamide, oxalic acid, citric acid etc., and Inorganic Salts comprises iron nitrate, nitrocalcite, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES etc.
3. the preparation method of a kind of porous charcoal for wastewater treatment according to claim 1 is characterized in that: in described step (2), and 750～850 ℃ of product direct activation temperature, soak time 60～180min, 6～10 ℃ of temperature rise rates.
4. the preparation method of a kind of porous charcoal for wastewater treatment according to claim 1, it is characterized in that: in described step (3), the kind of acid comprises hydrochloric acid, nitric acid, 60～100 ℃ of pickling temperatures, pickling time 30～90min, acid solution PH=2～5.
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| CN2012103465849A CN102874805A (en) | 2012-09-17 | 2012-09-17 | Method for preparing porous carbon for wastewater treatment |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253776A (en) * | 2013-05-28 | 2013-08-21 | 武汉钢铁(集团)公司 | Semi-coke microbial carrier and preparation method thereof |
| CN105174350A (en) * | 2015-09-07 | 2015-12-23 | 延安大学 | Method of treating phenolic wastewater by adopting magnetic semicoke adsorbent |
| CN107176655A (en) * | 2017-04-11 | 2017-09-19 | 北京化工大学 | A kind of method of utilization block foam structure chelate synthesis multi-stage porous carbon electric adsorption electrode material and application |
| CN107879342A (en) * | 2017-11-21 | 2018-04-06 | 常州亚环环保科技有限公司 | A kind of preparation method of high absorbent-type porous activated carbon |
| CN109529770A (en) * | 2018-12-29 | 2019-03-29 | 中国科学院兰州化学物理研究所 | A method of porous carbon adsorbent material is prepared as template using the Pickering lotion that semicoke is stable |
| CN111518600A (en) * | 2019-12-23 | 2020-08-11 | 新疆中宇金盾碳基研究院(有限公司) | Saltpetering inhibitor, semi-coke type carbon containing saltpetering inhibitor and preparation method thereof |
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| CN1762575A (en) * | 2005-09-14 | 2006-04-26 | 东华大学 | Method for preparation of active carbon fibrous absorption material |
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| CN1762575A (en) * | 2005-09-14 | 2006-04-26 | 东华大学 | Method for preparation of active carbon fibrous absorption material |
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| 田宇红 等: "微波辐射-KOH活化兰炭粉制备活性炭", 《化学工程》 * |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253776A (en) * | 2013-05-28 | 2013-08-21 | 武汉钢铁(集团)公司 | Semi-coke microbial carrier and preparation method thereof |
| CN103253776B (en) * | 2013-05-28 | 2014-11-12 | 武汉钢铁(集团)公司 | Semi-coke microbial carrier and preparation method thereof |
| CN105174350A (en) * | 2015-09-07 | 2015-12-23 | 延安大学 | Method of treating phenolic wastewater by adopting magnetic semicoke adsorbent |
| CN105174350B (en) * | 2015-09-07 | 2017-10-24 | 延安大学 | Using the method for magnetic semi-coke adsorbent Phenol-Containing Wastewater Treatment |
| CN107176655A (en) * | 2017-04-11 | 2017-09-19 | 北京化工大学 | A kind of method of utilization block foam structure chelate synthesis multi-stage porous carbon electric adsorption electrode material and application |
| CN107176655B (en) * | 2017-04-11 | 2020-05-19 | 北京化工大学 | Method for synthesizing hierarchical porous carbon electro-adsorption electrode material by using block-shaped foam structure chelate and application |
| CN107879342A (en) * | 2017-11-21 | 2018-04-06 | 常州亚环环保科技有限公司 | A kind of preparation method of high absorbent-type porous activated carbon |
| CN107879342B (en) * | 2017-11-21 | 2020-12-18 | 宁夏浦士达环保科技有限公司 | Preparation method of high-adsorption type porous activated carbon |
| CN109529770A (en) * | 2018-12-29 | 2019-03-29 | 中国科学院兰州化学物理研究所 | A method of porous carbon adsorbent material is prepared as template using the Pickering lotion that semicoke is stable |
| CN109529770B (en) * | 2018-12-29 | 2021-09-14 | 中国科学院兰州化学物理研究所 | Method for preparing porous carbon adsorbent material by taking semicoke-stable Pickering emulsion as template |
| CN111518600A (en) * | 2019-12-23 | 2020-08-11 | 新疆中宇金盾碳基研究院(有限公司) | Saltpetering inhibitor, semi-coke type carbon containing saltpetering inhibitor and preparation method thereof |
| CN111518600B (en) * | 2019-12-23 | 2021-05-18 | 新疆中宇金盾碳基研究院(有限公司) | Saltpetering inhibitor, semi-coke type carbon containing saltpetering inhibitor and preparation method thereof |
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