CN102701200A - Method for preparing active carbon from municipal sludge by two-step thermal decomposition - Google Patents
Method for preparing active carbon from municipal sludge by two-step thermal decomposition Download PDFInfo
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Abstract
The invention provides a method for preparing active carbon from municipal sludge by two-step thermal decomposition, belonging to the technical field of active carbon. The method comprises the following steps of: thermally decomposing and carbonizing dried municipal sludge for 30-90 minutes at 400-550 DEG C, and then adding an activator in an amount of 2-4mol/l into the carbonized sample, impregnating and activating, and then thermally decomposing and activating at high temperature of 450-600 DEG C to obtain the sludge-activated carbon. According to the method provided by the invention, the sludge is carbonized and activated by the two-step thermal decomposition and then the carbonized sludge is activated by the activator, so that the demand of the activator is greatly decreased and a way of recycling the sludge is provided to realize harmless, reduction and reclamation of the waste treatment.
Description
Technical field
The present invention relates to a kind of is the preparation method of the active sludge carbon of main raw material(s) with the excess sludge of municipal sewage plant, is applicable to the removal of COD, coloring matter in removal and the sewage of various toxic gases, belongs to the activated carbon technology field.
Background technology
In recent years, along with the municipal sewage treatment industrial expansion, municipal sludge output sharply increases, and the big and complicated component of sludge yield will bring serious environmental to pollute as not dealing carefully with.The treatment and disposal of mud is a problem demanding prompt solution, and recycling sludge more and more receives people's concern.The researcher utilizes the characteristics that contain large amount of organic in the mud both at home and abroad, and mud is prepared into carbon-bearing adsorbent.Present mud prepares process of active carbon and mainly contains physical activation method, chemical activation method and microwave activation method, and wherein chemical activation method is higher relatively because of the gac quality that makes, and uses more.Chemical activation method mainly adopts one section pyrolysis activation method to prepare gac, and the mud of oven dry is directly carried out acvator dipping, and carries out the pyrolysis activation and prepare gac.Therefore research and develop a kind of low acvator demand, and have the preparation method of the active sludge carbon of high adsorption capacity, the extensive industrialization utilization for preparing gac for mud has directive significance.
Summary of the invention
The purpose of this invention is to provide a kind of is the preparation technology of two step pyrolysis active sludge carbons of main raw material(s) with the excess sludge of municipal sewage plant, and the gained active sludge carbon is applicable to removes COD, coloring matter in various toxic gases and the sewage.
A kind of city provided by the present invention two step pyrolysis prepare the method for mud matrix activated carbon, it is characterized in that, may further comprise the steps:
1) sludge from wastewater treatment plant is dried to water ratio below 10%, grinds, sieve, keep particle size range 20 orders-100 purpose mud granule;
2), this mud granule is warming up to 400-550 ℃ of carbonization 30-90min with the temperature rise rate of 10-20 ℃/min, carbonization process is protection gas with nitrogen;
3) with step 2) carbide that obtains mixes by mass ratio 1:1-1:4 with the activator solution of 2-4mol/l, in normal temperature dipping 12-24h down, is dried to constant weight afterwards, obtains activation appearance;
4) activation appearance is warming up to 450-600 ℃ with the temperature rise rate of 10-20 ℃/min, behind the pyrolysis activation 30-90min, in nitrogen, cools off, the distilled water wash of then using hydrochloric acid and 70-80 ℃ successively is to neutral, and oven dry promptly obtains active sludge carbon.
Said acvator is preferably ZnCl
2, H
3PO
4, a kind of among the KOH.
The invention has the advantages that the excess sludge of having recycled sewage work, appearance after the carbonization is carried out the acvator activation, practiced thrift the use of acvator, the gac specific surface area of the inventive method preparation is not less than 425m
2/ g has improved its absorption property greatly, and productive rate and one section pyrolysis that two sections pyrolysis prepare gac prepare the gac productive rate and be more or less the same.With the activated gac that generated of excess sludge, make waste sludge obtain resource utilization, solved the problem of outlet of excess sludge greatly.Therefore, this sorbent material has the simple and low characteristics of cost of preparation.
Below in conjunction with embodiment the present invention is described further.
Embodiment
Employed mud is the excess sludge of sewage work's second pond among the following embodiment.
Embodiment 1
1) drying sludge to water ratio below 10%, is ground, sieves, keeping particle size range is 20-100 purpose mud granule;
2) this mud granule is warming up to 400 ℃ of carbonization 60min with the temperature rise rate of 10 ℃/min, carbonization process is protection gas with nitrogen;
3) be after 1:2 mixes with the liquor zinci chloridi of this carbonization appearance and 4mol/l by mass ratio again,, then be dried to constant weight, obtain activation appearance in normal temperature dipping 12h down;
4) activation appearance is warming up to 450 ℃ with the temperature rise rate of 10 ℃/min, behind the pyrolysis activation 90min, in nitrogen, cools off, then use the distilled water wash of hydrochloric acid and 70 ℃ successively, oven dry promptly obtains active sludge carbon;
The specific surface area of active sludge carbon is 425m
2/ g, productive rate are 37.02%.
Embodiment 2
1) drying sludge to water ratio below 10%, is ground, sieves, keeping particle size range is the mud granule below the 20-100 order;
2) this mud granule is warming up to 450 ℃ of carbonization 90min with the temperature rise rate of 15 ℃/min, carbonization process is protection gas with nitrogen;
3) liquor zinci chloridi with carbonization appearance and 3mol/l is after 1:3 mixes by mass ratio, in normal temperature dipping 24h down, then is dried to constant weight, obtains the activated sludge particle;
3) the activated sludge particle is warming up to 500 ℃ with the temperature rise rate of 15 ℃/min, behind the pyrolysis activation 30min, in nitrogen, cools off, then use the distilled water wash of hydrochloric acid and 80 ℃ successively, oven dry promptly obtains active sludge carbon;
The specific surface area of active sludge carbon is 485m
2/ g, productive rate are 40.12%.
Embodiment 3
1) drying sludge to water ratio below 10%, is ground, sieves, keeping particle size range is the mud granule below the 20-100 order;
2) this mud granule is warming up to 500 ℃ of carbonization 30min with the temperature rise rate of 20 ℃/min, carbonization process is protection gas with nitrogen;
3) liquor zinci chloridi with this carbonization appearance and 2mol/l is after 1:1 mixes by mass ratio, in normal temperature dipping 24h down, then is dried to constant weight, obtains activation appearance;
4) activation appearance is warming up to 550 ℃ with the temperature rise rate of 20 ℃/min, behind the pyrolysis activation 60min, in nitrogen, cools off, then use the distilled water wash of hydrochloric acid and 75 ℃ successively, oven dry promptly obtains active sludge carbon;
The specific surface area of active sludge carbon is 470.64m
2/ g, productive rate are 37.26%.
Embodiment 4
1) drying sludge to water ratio below 10%, is ground, sieves, keeping particle size range is the mud granule below the 20-100 order;
2) this mud granule is warming up to 550 ℃ of carbonization 30min with the temperature rise rate of 10 ℃/min, carbonization process is protection gas with nitrogen;
3) liquor zinci chloridi with this carbonization appearance and 4mol/l is after 1:4 mixes by mass ratio, in normal temperature dipping 24h down, then is dried to constant weight, obtains activation appearance;
4) activation appearance is warming up to 600 ℃ with the temperature rise rate of 10 ℃/min, behind the pyrolysis activation 60min, in nitrogen, cools off, then use the distilled water wash of hydrochloric acid and 70 ℃ successively, oven dry promptly obtains active sludge carbon;
The specific surface area of active sludge carbon is 470.64m
2/ g, productive rate are 37.26%.
Comparative Examples 1
1) drying sludge to water ratio below 10%, is ground, sieves, keeping particle size range is the mud granule below the 20-100 order;
2) liquor zinci chloridi with this mud granule sample and 4mol/l is after 1:4 mixes by mass ratio, in normal temperature dipping 24h down, then is dried to constant weight, obtains the activated sludge particle;
3) the activated sludge particle is warming up to 600 ℃ with the temperature rise rate of 10 ℃/min, behind the pyrolysis activation 60min, in nitrogen, cools off, then use the distilled water wash of hydrochloric acid and 70 ℃ successively, oven dry promptly obtains active sludge carbon;
The specific surface area of active sludge carbon is 251m
2/ g, productive rate are 39.10%.
Can find out that from above Comparative Examples and embodiment the present invention has practiced thrift the use of acvator, and the gac specific surface area that obtains is much larger than single stage method.
Claims (2)
1. municipal sludge two step pyrolysis prepare process of active carbon, it is characterized in that, may further comprise the steps:
1) sludge from wastewater treatment plant is dried to water ratio below 10%, grinds, sieve, keep particle size range 20 orders-100 purpose mud granule;
2) this mud granule is warming up to 400-550 ℃ of carbonization 30-90min with the temperature rise rate of 10-20 ℃/min, carbonization process is protection gas with nitrogen;
3) with step 2) carbide that obtains mixes by mass ratio 1:1-1:4 with the activator solution of 2-4mol/l, in normal temperature dipping 12-24h down, is dried to constant weight afterwards, obtains activation appearance;
4) activation appearance is warming up to 450-600 ℃ with the temperature rise rate of 10-20 ℃/min, behind the pyrolysis activation 30-90min, in nitrogen, cools off, the distilled water wash of then using hydrochloric acid and 70-80 ℃ successively is to neutral, and oven dry promptly obtains active sludge carbon.
2. according to the method for claim 1, it is characterized in that said acvator is ZnCl
2, H
3PO
4, a kind of among the KOH.
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Cited By (20)
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|---|---|---|---|---|
| CN103130223A (en) * | 2013-03-25 | 2013-06-05 | 东南大学 | Method for preparing activated carbon by using municipal solid waste as raw material |
| CN103357379A (en) * | 2013-08-14 | 2013-10-23 | 山东建筑大学 | Method for preparing arsenic removal adsorbent from water plants |
| CN103394325A (en) * | 2013-08-14 | 2013-11-20 | 山东建筑大学 | Method for preparing arsenic removal adsorbent by use of marine product waste |
| CN103951153A (en) * | 2014-05-14 | 2014-07-30 | 中国科学院城市环境研究所 | Method and system for preparing carbon adsorbent material by mixing waste plastics with sludge |
| CN104258808A (en) * | 2014-09-02 | 2015-01-07 | 中国科学院城市环境研究所 | Method and system for increasing specific surface area of sludge biochar |
| CN105016336A (en) * | 2015-07-13 | 2015-11-04 | 安徽成方新材料科技有限公司 | Environmental-friendly type asphalt resin mixed base spherical activated carbon obtained through utilization of waste and preparation method of environmental-friendly type asphalt resin mixed base spherical activated carbon |
| CN106348291A (en) * | 2016-10-13 | 2017-01-25 | 华北电力大学（保定） | Method for preparing active carbon by utilizing urban sludge |
| CN106495153A (en) * | 2016-10-31 | 2017-03-15 | 新奥生态环境治理有限公司 | The method of production material with carbon element |
| CN106732360A (en) * | 2016-12-21 | 2017-05-31 | 福建师范大学 | A kind of preparation method of the sludge base charcoal of the crust that adulterates |
| CN106986339A (en) * | 2017-04-24 | 2017-07-28 | 句容市百诚活性炭有限公司 | A kind of preparation method of active sludge carbon |
| CN107434251A (en) * | 2017-05-24 | 2017-12-05 | 山东圣坤环保科技有限公司 | A kind of preparation method of active sludge carbon |
| CN107758658A (en) * | 2017-10-11 | 2018-03-06 | 上海市政工程设计研究总院（集团）有限公司 | One kind shaping active sludge carbon preparation method |
| CN108529622A (en) * | 2018-07-10 | 2018-09-14 | 南京林业大学 | A method of utilizing bamboo matter building waste modified sewage sludge matrix activated carbon |
| CN110092557A (en) * | 2019-06-12 | 2019-08-06 | 大连大学 | A kind of recycling sludge utilizes processing system and method |
| CN110310844A (en) * | 2019-06-28 | 2019-10-08 | 华中科技大学 | Sludge utilizes method and the nickel foam-nitrogen-doped nanometer carbon composite prepared by this method |
| CN111268880A (en) * | 2020-02-26 | 2020-06-12 | 徐州工程学院 | Preparation method and application of metal ion modified sludge-based biochar |
| CN111285370A (en) * | 2020-02-20 | 2020-06-16 | 南京工业大学 | Comprehensive utilization method of organic hazardous waste salt residues |
| CN112142153A (en) * | 2019-06-26 | 2020-12-29 | 万华化学集团股份有限公司 | Dephosphorizing and organic matter removing reagent and method for treating phosphorus-containing organic matter-containing wastewater |
| CN112479204A (en) * | 2020-12-09 | 2021-03-12 | 青岛理工大学 | Process and method for preparing active carbon by hydrothermal co-carbonization of enteromorpha and municipal sludge |
| CN113548751A (en) * | 2021-08-04 | 2021-10-26 | 浙江欧德利科技有限公司 | Process for removing COD (chemical oxygen demand) in high-salinity wastewater |
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| CN103130223A (en) * | 2013-03-25 | 2013-06-05 | 东南大学 | Method for preparing activated carbon by using municipal solid waste as raw material |
| CN103394325B (en) * | 2013-08-14 | 2015-04-15 | 山东建筑大学 | Method for preparing arsenic removal adsorbent by use of marine product waste |
| CN103357379A (en) * | 2013-08-14 | 2013-10-23 | 山东建筑大学 | Method for preparing arsenic removal adsorbent from water plants |
| CN103394325A (en) * | 2013-08-14 | 2013-11-20 | 山东建筑大学 | Method for preparing arsenic removal adsorbent by use of marine product waste |
| CN103357379B (en) * | 2013-08-14 | 2015-06-03 | 山东建筑大学 | Method for preparing arsenic removal adsorbent from water plants |
| CN103951153A (en) * | 2014-05-14 | 2014-07-30 | 中国科学院城市环境研究所 | Method and system for preparing carbon adsorbent material by mixing waste plastics with sludge |
| CN103951153B (en) * | 2014-05-14 | 2016-03-30 | 中国科学院城市环境研究所 | A kind of waste plastics and mud are mixed with the method and system of charcoal sorbing material |
| CN104258808A (en) * | 2014-09-02 | 2015-01-07 | 中国科学院城市环境研究所 | Method and system for increasing specific surface area of sludge biochar |
| CN104258808B (en) * | 2014-09-02 | 2017-01-25 | 中国科学院城市环境研究所 | Method and system for increasing specific surface area of sludge biochar |
| CN105016336A (en) * | 2015-07-13 | 2015-11-04 | 安徽成方新材料科技有限公司 | Environmental-friendly type asphalt resin mixed base spherical activated carbon obtained through utilization of waste and preparation method of environmental-friendly type asphalt resin mixed base spherical activated carbon |
| CN106348291A (en) * | 2016-10-13 | 2017-01-25 | 华北电力大学（保定） | Method for preparing active carbon by utilizing urban sludge |
| CN106495153A (en) * | 2016-10-31 | 2017-03-15 | 新奥生态环境治理有限公司 | The method of production material with carbon element |
| CN106495153B (en) * | 2016-10-31 | 2019-05-28 | 新奥生态环境治理有限公司 | The method for producing carbon material |
| CN106732360A (en) * | 2016-12-21 | 2017-05-31 | 福建师范大学 | A kind of preparation method of the sludge base charcoal of the crust that adulterates |
| CN106986339A (en) * | 2017-04-24 | 2017-07-28 | 句容市百诚活性炭有限公司 | A kind of preparation method of active sludge carbon |
| CN107434251A (en) * | 2017-05-24 | 2017-12-05 | 山东圣坤环保科技有限公司 | A kind of preparation method of active sludge carbon |
| CN107758658A (en) * | 2017-10-11 | 2018-03-06 | 上海市政工程设计研究总院（集团）有限公司 | One kind shaping active sludge carbon preparation method |
| CN108529622A (en) * | 2018-07-10 | 2018-09-14 | 南京林业大学 | A method of utilizing bamboo matter building waste modified sewage sludge matrix activated carbon |
| CN110092557A (en) * | 2019-06-12 | 2019-08-06 | 大连大学 | A kind of recycling sludge utilizes processing system and method |
| CN112142153A (en) * | 2019-06-26 | 2020-12-29 | 万华化学集团股份有限公司 | Dephosphorizing and organic matter removing reagent and method for treating phosphorus-containing organic matter-containing wastewater |
| CN110310844A (en) * | 2019-06-28 | 2019-10-08 | 华中科技大学 | Sludge utilizes method and the nickel foam-nitrogen-doped nanometer carbon composite prepared by this method |
| CN111285370A (en) * | 2020-02-20 | 2020-06-16 | 南京工业大学 | Comprehensive utilization method of organic hazardous waste salt residues |
| CN111268880A (en) * | 2020-02-26 | 2020-06-12 | 徐州工程学院 | Preparation method and application of metal ion modified sludge-based biochar |
| CN112479204A (en) * | 2020-12-09 | 2021-03-12 | 青岛理工大学 | Process and method for preparing active carbon by hydrothermal co-carbonization of enteromorpha and municipal sludge |
| CN113548751A (en) * | 2021-08-04 | 2021-10-26 | 浙江欧德利科技有限公司 | Process for removing COD (chemical oxygen demand) in high-salinity wastewater |
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Application publication date: 20121003 |