CN102658084B - Preparation method of nickel nitrate modified sludge activated carbon - Google Patents
Preparation method of nickel nitrate modified sludge activated carbon Download PDFInfo
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- CN102658084B CN102658084B CN2012101548048A CN201210154804A CN102658084B CN 102658084 B CN102658084 B CN 102658084B CN 2012101548048 A CN2012101548048 A CN 2012101548048A CN 201210154804 A CN201210154804 A CN 201210154804A CN 102658084 B CN102658084 B CN 102658084B
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- sludge
- nickel nitrate
- activated carbon
- carbon
- absorbent charcoal
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Abstract
The invention discloses a preparation method of nickel nitrate modified sludge activated carbon, which comprises the following steps: 1) drying wet sludge with the water content of 82-87% with a fluidized bed until the water content of the sludge is reduced to 5-15%, thereby obtaining dry sludge; 2) putting the dry sludge particles in a high-temperature pipe furnace, and carbonizing at 400-600 DEG C for 0.5-2 hours; 3) impregnating the sludge carbonized material with isometric 45 wt% concentrated nitric acid for 5 hours, standing at room temperature over night, and washing with deionized water to obtain sludge activated carbon; 4) impregnating the sludge activated carbon in a modifier nickel nitrate for 24 hours, and stirring for 4 hours until the nickel nitrate is supported onto the sludge activated carbon; and 5) heat activating treatment on nickel nitrate supported sludge activated carbon: heating to 300-400 DEG C in a high-purity nitrogen atmosphere, continuing for several minutes until no oxynitride is detected in exhaust gas, continuing purging with high-purity nitrogen, cooling to room temperature, and taking out the sample, thereby obtaining the nickel nitrate modified sludge activated carbon.
Description
Technical field
The invention relates to the active carbon of flue gas desulfurization, relate in particular to the modified sewage sludge absorbent charcoal of desulfurizing low concentration fume.
Background technology
Along with the fast development of urbanization and the carrying out of national energy-saving emission reduction work, the quantity of national sewage treatment plant is in continuous increase, as the output of the product mud after sewage disposal, also just continues to increase thereupon.The mode of sludge treatment has landfill, Fertilizer Transformed utilization, burning and burning electricity generation etc., and Sludge landfill is had relatively high expectations for the soil mechanical properties of mud, the addressing difficulty; The development of green agriculture and the raising of Public environmental attitude make sludge manure recycling difficulty; Sludge incineration residue-slag and the flying dust problem of storing up also is difficult to solve.Therefore in the urgent need to a kind of effective ways, process these a large amount of mud now.
In recent years, the Main Ingredients and Appearance in municipal sludge be content of organics also in continuous increase, this just for effectively prepare active carbon provide may.At present, researchers to utilize mud prepare active carbon carrying out many research.But the active sludge carbon aperture of making at present is larger, and specific area is little, is more suitable for macromolecular absorption, and its desulfuration efficiency is also lower.Can consider active sludge carbon is carried out to surface modification treatment, because the chemism of nickel is large, make the surface of active sludge carbon be loaded with the oxide of nickel, and using this as catalyst, thereby improve desulfuration efficiency.Have not yet to see and nickel nitrate is carried out to the report of desulfurization for modified sewage sludge absorbent charcoal.Therefore, with the nickel nitrate modified sewage sludge absorbent charcoal, improving desulfurization performance, is very necessary to the application that promotes active sludge carbon.
Summary of the invention
technical problem:the objective of the invention is to disclose a kind of preparation method who removes the nickel nitrate modified sewage sludge absorbent charcoal of sulfur dioxide in flue gas, is poor in view of the desulfurization performance of existing active sludge carbon, adopts nickel nitrate pair
Its modification, to improve its desulfurization performance.
technical scheme:the present invention is achieved by following technical proposals.
Be used for the preparation method of the nickel nitrate modified sewage sludge absorbent charcoal of desulfurizing low concentration fume, comprise the steps:
1. the preparation method of a nickel nitrate modified sewage sludge absorbent charcoal, is characterized in that nickel nitrate modified sewage sludge absorbent charcoal material component is Ni (NO
3) 26H
2the wet mud of O and sewage treatment plant, making step is as follows:
1) by the wet mud fluidized bed drying of moisture content 82% ~ 87%, make the moisture content of mud be reduced to 5% ~ 15%, obtain dewatered sludge; Dewatered sludge is sieved, obtain the dewatered sludge particle of particle diameter at 0.6 ~ 3mm;
2) the dewatered sludge particle is put into to high temperature process furnances, at 400 ~ 600 ℃ of lower charing 0.5 ~ 2h, the rate of heat addition is controlled at 5 ~ 15 ℃/min, obtains the sludge carbon material;
3) the red fuming nitric acid (RFNA) incipient impregnation 5h that is 45% by the sludge carbon material by mass concentration, ambient temperature overnight, then wash by deionized water, by the PH detection paper, reach till 6 ~ 7, again it is fully ground and sieve after 80 ℃ of oven dry, get and be less than 200 purpose particles, obtain active sludge carbon;
4) active sludge carbon step 3) obtained is put into as the nickel nitrate of modifier and is flooded 24h, stirs 4h, nickel nitrate is loaded on active sludge carbon, then 50 ℃ of oven dry;
5) active sludge carbon of load nickel nitrate carried out to the heat-activated processing: it is warming up to 300 ~ 400 ℃ under the protection of high pure nitrogen; then continue several minutes until can't detect nitrogen oxide in tail gas; finally with high pure nitrogen, continue to purge; be cooled to room temperature and take out sample, obtain the nickel nitrate modified sewage sludge absorbent charcoal.
In described nickel nitrate the quality of nickel account for active sludge carbon mass percentage content 5% ~ 15%.
The moisture content of the dewatered sludge that described step 1 is made is 9%.
The carbonization temperature of described step 2 is 550 ℃, and the time is 1h, and the rate of heat addition is controlled at 10 ℃/min.
In described step 4 nickel nitrate, to account for the degree of active sludge carbon be 10% to the quality of nickel.
Described step 5 modified sewage sludge absorbent charcoal is warming up to 380 ℃ under the protection of high pure nitrogen, continues 0.5h.
beneficial effect:the preparation for modified sewage sludge absorbent charcoal by nickel nitrate first, effective desulphurizing ability that must improve active sludge carbon.Nickel nitrate modified sewage sludge absorbent charcoal of the present invention is mainly used in desulfurizing low concentration fume.
The specific embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The present invention is for the nickel nitrate modified sewage sludge absorbent charcoal of desulfurizing low concentration fume, and raw materials used is Ni (NO
3)
2.6H
2the excess sludge of O and sewage treatment plant.
(1) by the mud fluidized bed drying, make the moisture content of mud be reduced to 5% ~ 15%, obtain dewatered sludge; Dewatered sludge is sieved, make its particle diameter at 0.6 ~ 3mm.
(2) mud step 1 made is put into high temperature process furnances, adopts nitrogen protection, and at 550 ℃ of lower charing 1h, the rate of heat addition is controlled at 10 ℃/min, obtains carbonized material.
(3) 45% red fuming nitric acid (RFNA) incipient impregnation 5h for sludge carbon material step 2 made, ambient temperature overnight, then wash by deionized water, by the PH detection paper, reach till 6 ~ 7, again it is fully ground and sieve after 80 ℃ of oven dry, get and be less than 200 purpose particles, obtain active sludge carbon.
(4) getting the degree that the quality of nickel in nickel nitrate accounts for active sludge carbon is 10%, a certain amount of modifier is loaded on active sludge carbon: the active sludge carbon that step 3 is made floods 24h in nickel nitrate solution (50mL), wherein stir 4h, then 50 ℃ of oven dry.
(5) the heat-activated processing is carried out in the active sludge carbon of modification: the modified sewage sludge absorbent charcoal that step 4 is made is warming up to 380 ℃ under the protection of high pure nitrogen; then continue several minutes until can't detect nitrogen oxide in tail gas; finally with high pure nitrogen, continue to purge; be cooled to room temperature and take out sample, obtain the nickel nitrate modified sewage sludge absorbent charcoal.
To nickel nitrate modified sewage sludge absorbent charcoal and common unmodified active sludge carbon physicochemical data tested, in Table 1.
The nickel nitrate modified sewage sludge absorbent charcoal that the present invention is made and business active carbon carry out desulfurization.The present invention is by 800ppmSO
2, 8%O
2, and N
2mix rear conduct and process source of the gas, adopt moral figure instrument International Trading Company Ltd (Testo 350-XL) to detect the concentration of the sulfur dioxide in the mist of differential responses condition front and back.According to calculating, the nickel nitrate modified sewage sludge absorbent charcoal that the present invention makes and the desulfurization degree of business active carbon are respectively 93.94% and 97.88%.
Embodiment 2
Except (4): getting the degree that the quality of nickel in nickel nitrate accounts for active sludge carbon is: 5%, all the other each steps are all identical with embodiment 1.
Embodiment 3
Except (4): getting the degree that the quality of nickel in nickel nitrate accounts for active sludge carbon is: 15%, all the other each steps are all identical with embodiment 1.
The physical property of table 1 nickel nitrate modified sewage sludge absorbent charcoal and common unmodified active sludge carbon
| ? | The nickel nitrate modified sewage sludge absorbent charcoal | Common unmodified active sludge carbon |
| Iodine number (mg/g) | 273.56 | 162.14 |
| Surface nickel content (%) | 7.36 | 0 |
| BET surface area (m 2/g） | 62.09 | 66.66 |
| Total pore volume (cm 3/g） | 0.0805 | 0.1073 |
| Micropore volume (cm 3/g） | 0.012645 | 0.008954 |
| Average pore size (nm) | 5.18 | 6.44 |
Claims (2)
1. the preparation method of a nickel nitrate modified sewage sludge absorbent charcoal, is characterized in that nickel nitrate modified sewage sludge absorbent charcoal material component is Ni (NO
3) 26H
2the wet mud of O and sewage treatment plant, making step is as follows:
1) by the wet mud fluidized bed drying of moisture content 82%～87%, make the moisture content of mud be reduced to 5%～15%, obtain dewatered sludge; Dewatered sludge is sieved, obtain the dewatered sludge particle of particle diameter at 0.6～3mm;
2) the dewatered sludge particle is put into to high temperature process furnances, at 400～600 ℃ of lower charing 0.5～2h, the rate of heat addition is controlled at 5～15 ℃/min, obtains the sludge carbon material;
3) the red fuming nitric acid (RFNA) incipient impregnation 5h that is 45% by the sludge carbon material by mass concentration, ambient temperature overnight, then wash by deionized water, by the pH detection paper, reach till 6～7, again it is fully ground and sieve after 80 ℃ of oven dry, get and be less than 200 purpose particles, obtain active sludge carbon;
4) active sludge carbon step 3) obtained is put into as the nickel nitrate of modifier and is flooded 24h, stirs 4h, nickel nitrate is loaded on active sludge carbon, then 50 ℃ of oven dry;
5) active sludge carbon of load nickel nitrate carried out to the heat-activated processing: it is warming up to 300～400 ℃ under the protection of high pure nitrogen; then continue several minutes until can't detect nitrogen oxide in tail gas; finally with high pure nitrogen, continue to purge; be cooled to room temperature and take out sample, obtain the nickel nitrate modified sewage sludge absorbent charcoal.
2. the preparation method of nickel nitrate modified sewage sludge absorbent charcoal according to claim 1, the quality that it is characterized in that nickel in described nickel nitrate account for active sludge carbon mass percentage content 5%～15%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103553040B (en) * | 2013-11-15 | 2015-06-17 | 中国石油大学(华东) | Method for preparing porous carbon through co-pyrolysis of petroleum coke and oily sludge |
| CN103848420A (en) * | 2013-11-28 | 2014-06-11 | 天津大学 | Amination-acidification modified activated carbon material |
| CN104926073A (en) * | 2015-06-03 | 2015-09-23 | 东南大学 | Method for preparing desulfurizer by utilizing municipal sludge |
| CN106219545A (en) * | 2016-07-25 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of preparation method of sucrose base grading-hole activated carbon |
| CN107876011A (en) * | 2017-11-07 | 2018-04-06 | 常州布奇纺织有限公司 | A kind of sulfur-bearing industrial waste gas processing method |
| CN112755961B (en) * | 2020-12-31 | 2023-12-01 | 中国科学院城市环境研究所 | MgO-loaded activated carbon and preparation method and application thereof |
| CN112919466A (en) * | 2021-03-02 | 2021-06-08 | 北海艾米碳材料技术研发有限公司 | Active carbon graphene modification method for preparing super capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000072427A (en) * | 1998-09-03 | 2000-03-07 | Kawasaki City | Production of active carbon by sludge |
| JP2000169130A (en) * | 1998-12-08 | 2000-06-20 | Masanami Tekko:Kk | Production of granular organic sludge carbon from activated sludge |
| ES2233164A1 (en) * | 2003-02-10 | 2005-06-01 | Soluciones Termicas Aplicadas, S.L. | Integral cleaning of high organics content effluent comprises controlled coagulation and centrifugation, with acidity control and disinfection |
| CN1644495A (en) * | 2004-12-14 | 2005-07-27 | 南开大学 | Method for preparing active carbon from urban sewage treatment plant mud |
| CN1973995A (en) * | 2006-11-02 | 2007-06-06 | 上海交通大学 | Prepn of wet sludge carbonizing adsorbent |
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| JPS4986291A (en) * | 1972-12-21 | 1974-08-19 | ||
| JP3181496B2 (en) * | 1995-09-27 | 2001-07-03 | 河西工業株式会社 | Automotive roof console box |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000072427A (en) * | 1998-09-03 | 2000-03-07 | Kawasaki City | Production of active carbon by sludge |
| JP2000169130A (en) * | 1998-12-08 | 2000-06-20 | Masanami Tekko:Kk | Production of granular organic sludge carbon from activated sludge |
| ES2233164A1 (en) * | 2003-02-10 | 2005-06-01 | Soluciones Termicas Aplicadas, S.L. | Integral cleaning of high organics content effluent comprises controlled coagulation and centrifugation, with acidity control and disinfection |
| CN1644495A (en) * | 2004-12-14 | 2005-07-27 | 南开大学 | Method for preparing active carbon from urban sewage treatment plant mud |
| CN1973995A (en) * | 2006-11-02 | 2007-06-06 | 上海交通大学 | Prepn of wet sludge carbonizing adsorbent |
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