CN102658084A - 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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- CN102658084A CN102658084A CN2012101548048A CN201210154804A CN102658084A CN 102658084 A CN102658084 A CN 102658084A CN 2012101548048 A CN2012101548048 A CN 2012101548048A CN 201210154804 A CN201210154804 A CN 201210154804A CN 102658084 A CN102658084 A CN 102658084A
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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 carrying out of fast development of urbanization and national energy-saving and emission-reduction work, the quantity of national sewage treatment plant is in continuous increase, also just continues to increase as the output of the product mud after the sewage disposal thereupon.The mode of sludge treatment has landfill, fertilizer utilization, burning and burning electricity generation or the like, and the mud landfill is had relatively high expectations for the soil mechanical properties of mud, the addressing difficulty; The raising of the development of green agriculture and public's environmental consciousness makes sludge manureization utilize difficulty again; Sludge incineration residue-slag and the flying dust problem of storing up also is difficult to solve.So pressing for a kind of effective ways now handles these a large amount of mud.
In recent years, the Main Ingredients and Appearance in the municipal sludge be content of organics also in continuous increase, this just provides possible for preparing active carbon effectively.At present, researchers to utilize mud prepare active carbon carrying out many researchs.But the active sludge carbon aperture of making at present is bigger, 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 surface modification treatment,, make the surface of active sludge carbon be loaded with the oxide of nickel because the chemism of nickel is big, and with this as catalyst, thereby improve desulfuration efficiency.Do not see as yet at present nickel nitrate is used for the report that modified sewage sludge absorbent charcoal comes desulfurization.Therefore, improving desulfurization performance with the nickel nitrate modified sewage sludge absorbent charcoal, 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 relatively poor in view of the desulfurization performance of existing active sludge carbon, adopts nickel nitrate right
Its modification is to improve its desulfurization performance.
Technical scheme:The present invention is achieved through 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 following:
1) the wet mud of moisture content 82% ~ 87% is used fluidized bed drying, 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 high temperature process furnances, at 400 ~ 600 ℃ of following charing 0.5 ~ 2h, the rate of heat addition is controlled at 5 ~ 15 ℃/min, obtains the sludge carbonization material;
3) the sludge carbonization material being used mass concentration is 45% red fuming nitric acid (RFNA) incipient impregnation 5h, and ambient temperature overnight spends deionised water then; Reach till 6 ~ 7 with the PH detection paper; Again it is fully ground after 80 ℃ of oven dry and sieve, get, obtain active sludge carbon less than 200 purpose particles;
4) nickel nitrate that the active sludge carbon that step 3) is obtained is put into as modifier floods 24h, stirs 4h, nickel nitrate is loaded on the active sludge carbon, then 50 ℃ of oven dry;
5) active sludge carbon to the load nickel nitrate carries out the heat-activated processing: it is warming up to 300 ~ 400 ℃ under the protection of high pure nitrogen; In tail gas, detected in lasting several minutes then less than till the nitrogen oxide; Continue to purge with high pure nitrogen at last; Be cooled to room temperature and take out sample, obtain the nickel nitrate modified sewage sludge absorbent charcoal.
In the said nickel nitrate quality of nickel account for active sludge carbon mass percentage content 5% ~ 15%.
The moisture content of the dewatered sludge that said step 1 is processed is 9%.
The carbonization temperature of said step 2 is 550 ℃, and the time is 1h, and the rate of heat addition is controlled at 10 ℃/min.
To account for the degree of active sludge carbon be 10% to the quality of nickel in said step 4 nickel nitrate.
Said step 5 modified sewage sludge absorbent charcoal is warming up to 380 ℃ under the protection of high pure nitrogen, continue 0.5h.
Beneficial effect:First nickel nitrate is used for the preparation of modified sewage sludge absorbent charcoal, 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 present invention is described further.
Embodiment 1
The present invention is used 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) mud is used 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 that step 1 is made is put into high temperature process furnances, adopts nitrogen protection, and at 550 ℃ of following charing 1h, the rate of heat addition is controlled at 10 ℃/min, obtains carbonized material.
(3) the sludge carbonization material that step 2 is made is with 45% red fuming nitric acid (RFNA) incipient impregnation 5h, and ambient temperature overnight spends deionised water then; Reach till 6 ~ 7 with the PH detection paper; Again it is fully ground after 80 ℃ of oven dry and sieve, get, obtain active sludge carbon less than 200 purpose particles.
(4) getting the degree that the quality of nickel in the nickel nitrate accounts for active sludge carbon is 10%; A certain amount of modifier is loaded on the 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) active sludge carbon to modification carries out the heat-activated processing: the modified sewage sludge absorbent charcoal that step 4 is made is warming up to 380 ℃ under the protection of high pure nitrogen; In tail gas, detected in lasting several minutes then less than till the nitrogen oxide; Continue to purge with high pure nitrogen at last; 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 test, see table 1.
Nickel nitrate modified sewage sludge absorbent charcoal that the present invention is made and commercial active carbon carry out desulfurization.The present invention is with 800ppmSO
2, 8%O
2, and N
2As handling 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 after mixing.According to calculating, the nickel nitrate modified sewage sludge absorbent charcoal that the present invention makes and the desulfurization degree of commercial active carbon are respectively 93.94% and 97.88%.
Embodiment 2
Except (4): getting the degree that the quality of nickel in the 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 the 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 pore 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 following:
1) the wet mud of moisture content 82% ~ 87% is used fluidized bed drying, 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 high temperature process furnances, at 400 ~ 600 ℃ of following charing 0.5 ~ 2h, the rate of heat addition is controlled at 5 ~ 15 ℃/min, obtains the sludge carbonization material;
3) the sludge carbonization material being used mass concentration is 45% red fuming nitric acid (RFNA) incipient impregnation 5h, and ambient temperature overnight spends deionised water then; Reach till 6 ~ 7 with the PH detection paper; Again it is fully ground after 80 ℃ of oven dry and sieve, get, obtain active sludge carbon less than 200 purpose particles;
4) nickel nitrate that the active sludge carbon that step 3) is obtained is put into as modifier floods 24h, stirs 4h, nickel nitrate is loaded on the active sludge carbon, then 50 ℃ of oven dry;
5) active sludge carbon to the load nickel nitrate carries out the heat-activated processing: it is warming up to 300 ~ 400 ℃ under the protection of high pure nitrogen; In tail gas, detected in lasting several minutes then less than till the nitrogen oxide; Continue to purge with high pure nitrogen at last; 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 the said nickel nitrate account for active sludge carbon mass percentage content 5% ~ 15%.
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| CN2012101548048A CN102658084B (en) | 2012-05-18 | 2012-05-18 | Preparation method of nickel nitrate modified sludge activated carbon |
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| CN2012101548048A CN102658084B (en) | 2012-05-18 | 2012-05-18 | Preparation method of nickel nitrate modified sludge activated carbon |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553040A (en) * | 2013-11-15 | 2014-02-05 | 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 |
| CN112755961A (en) * | 2020-12-31 | 2021-05-07 | 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 |
| CN114763264A (en) * | 2021-01-11 | 2022-07-19 | 中国石油化工股份有限公司 | Process for preparing activated carbon by alkali activation method |
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Patent Citations (7)
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553040A (en) * | 2013-11-15 | 2014-02-05 | 中国石油大学(华东) | Method for preparing porous carbon through co-pyrolysis of petroleum coke and oily sludge |
| 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 |
| CN112755961A (en) * | 2020-12-31 | 2021-05-07 | 中国科学院城市环境研究所 | MgO-loaded activated carbon and preparation method and application thereof |
| 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 |
| CN114763264A (en) * | 2021-01-11 | 2022-07-19 | 中国石油化工股份有限公司 | Process for preparing activated carbon by alkali activation method |
| 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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Granted publication date: 20131211 Termination date: 20180518 |