CN101234332A - Method for using sewage sludge and waste graphite to prepare activated adsorption material - Google Patents
Method for using sewage sludge and waste graphite to prepare activated adsorption material Download PDFInfo
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Abstract
The invention relates to a method for preparing activated absorption materials by using sludge and waste graphite, belonging to environmental-protective field. The invention is characterized in that after getting, drying, grinding and sieving the residual sludge from a municipal wastewater treatment plant, adding zinc chloride and sulfuric acid solution according to a solid-liquid ratio of 1: (2.5 to 4.5) into the sludge, resting for 20 to 24 hours, baking for 20 to 24 hours and adding waste graphite into treated sludge with the amount of 3 to 10 percent of the total amount of sludge; then, putting the solution into a pyrolyzing furnace for pyrolysis, isolating the air with nitrogen, controlling the nitrogen flow in 0.4 to 0.5L/min, the heating rate of 10 to 15 DEG C/min and the pyrolysis temperature of 500 to 800 DEG C for 1.5 to 2.5 hours; rinsing the pyrolyzed products with hydrochloric acid solution with the concentration of 3mol/L to promote the oxides to dissolve completely and simultaneously, washing away the impurities in the carbon, and then washing with the deionized water under a temperature of 70 DEG C to remove the Cl <-1>, and making grinding and sieving after 24 hours of baking under a temperature of 105 DEG C to obtain the product with the particle size of 0.7 to 1.0mm which is sludge activated absorption material. Research on the application of the absorbent to the coking wastewater treatment application tests shows that the absorbent reaches CODcr removal rate of 41.23 percent, color removal rate of 70 percent and turbidity removal rate of 83.60 percent.
Description
Technical field:
The invention belongs to the environmental protection field, particularly a kind of waste material (excess sludge of municipal sewage plant and useless breeze, graphite etc.) that utilizes adopts suitable activating technology, the low-cost method for preparing high added value activated sludge absorption material.
Background technology:
Mud is the material that is rich in organic matter and carbonaceous.Therefore, carry out cracking or some chemical treatment of process under the condition of control, it might be converted into active carbon.This transforms the volume that not only can reduce mud, can also produce the sorbing material than commercial active carbon cheapness simultaneously.Feasibility (Beeckmans and Park, 1971 that many researchs are verified should transform; Bilitewski, 1 979; Chiang and You, 1987; JeyaseelanandLu, 1996; Martin et al, 1996).
In the document after 2000, have many about prepare the report of active carbon with mud.People's mud such as the Tay of Nanyang Technolohy University and Chen Xiaoge prepare active carbon and have done correlative study, from aspect analyses such as BET specific area, pore volume, phosphorus content, benzene adsorption capacities, active sludge carbon have been carried out the research of physicochemical characteristics.They have also explored the optimum condition for preparing active carbon with the digested sludge behind the interpolation cocoanut shell, and the BET specific area can reach 867.61m under this condition
2/ g is 57.99%. to the clearance of phenol
The adding of cocoanut shell makes the absorption property of sludge activity carbon that large increase arranged, and cocoanut shell is as the raw material of commercial active carbon, and price is higher, causes the active sludge carbon cost of this method preparation to increase to some extent, is unfavorable for promoting the use of of active sludge carbon.
Summary of the invention:
The objective of the invention is to utilize waste material (excess sludge of municipal sewage plant and useless breeze, graphite etc.), adopt suitable activating technology, low-cost preparation high added value activated sludge absorption material.
The industrial ecology recycling economy thought of resource-based comprehensive utilization and trashformation reuse, in the excess sludge of city, add a certain amount of barren rock China ink, broken breeze etc., adopt suitable activating means, improve the absorption property of active sludge carbon, make adsorbent and be successfully applied to the processing of high-enriched organics waste water.
A kind of mud and waste graphite to prepare activated adsorption material method utilized, get a certain amount of excess sludge from the municipal sewage plant, mummification, the back of grinding, sieve are by solid-to-liquid ratio 1: (2.5～4.5) add compound activator solution (zinc chloride and sulfuric acid solution), static placement 20～24h, baking 20～24h, mud after the processing adds the barren rock China ink, and addition is 3～10% of a mud total amount.Then, put into pyrolysis oven and carry out pyrolysis, utilize the nitrogen secluding air, nitrogen flow is controlled at 0.4～0.5L/min, and the rate of heat addition is controlled at 10～15 ℃/min, and pyrolysis temperature is 500～800 ℃, and the time is 1.5～2.5h.Product after the pyrolysis is the rinsing of 3mol/L hydrochloric acid solution with concentration earlier, impels wherein that oxide fully dissolves, and impurity in the wash-out carbon washs with 70 ℃ of deionized waters, to remove wherein Cl again simultaneously
-1, at 105 ℃ down behind the baking 24h, grind and sieve, obtain the product of 0.7mm～1.0mm particle diameter---sludge activity sorbing material.The waste gas utilization mass concentration that produces in the pyrolytic process is that 10% sodium hydroxide solution absorbs processing.
The sludge activity adsorbent specific area of developing with this method reaches 139.41m
2/ g, the aperture is 6.6nm, total pore volume 3.52cm
3/ g, the iodine absorption value is up to 513.80mg/g.Use this adsorbent and carry out the Treatment of Coking Effluent application test and studies show that the CODcr clearance reaches 41.23%, chroma removal rate reaches 70%, and turbidity removal rate can reach 83.60%, and certain application prospect is arranged.
Description of drawings
Fig. 1 is sludge activity sorbing material preparation flow figure
Fig. 2 is pyrolysis installation figure
1-nitrogen steel cylinder; The 2-spinner flowmeter; 3-high-temperature tubular resistance furnace; The 4-temperature controller; The 5-exhaust gas processing device
Fig. 3 is the influence of addition to the CODcr clearance
The specific embodiment:
Below in conjunction with embodiment the present invention is described further.
The present invention is raw materials used to be the excess sludge of municipal sewage plant.
The present invention has added graphite on traditional active sludge carbon preparation method's basis, resource is fully used, and also effectively raises the correlated performance of active sludge carbon.
(1) preparation dewatered sludge:
With the municipal sludge oven dry, the dewatered sludge that moisture content is 10wt% is made in dehydration.
(2) dipping, sludge-drying
Complex reagent dipping dewatered sludge with the concentrated sulfuric acid and zinc chloride, zinc chloride is 3: 1 with the ratio of the concentration of the concentrated sulfuric acid, the volume of complex reagent is that solid-to-liquid ratio is 4: 1 with the ratio of the quality of dewatered sludge, flood after 24 hours, dewatered sludge is dried processing, afterwards, adding mass fraction in the dry mud is 5% graphite.
(3) pyrolysis mud
Adopt pyrolysis installation shown in Figure 2 to carry out pyrolysis, utilize the nitrogen secluding air, nitrogen flow is controlled at 0.5L/min, and the rate of heat addition is controlled at 15 ℃/min, and pyrolysis temperature is 550 ℃, and the time is 2h.The waste gas utilization mass concentration that produces in the pyrolytic process is that 10% sodium hydroxide solution absorbs processing.
(4) washing, oven dry product
Product is earlier with the rinsing of 3mol/L hydrochloric acid solution, impels wherein that oxide fully dissolves, and impurity in the wash-out carbon washs with 70 ℃ of deionized waters, to remove wherein Cl again simultaneously
-1, at 105 ℃ down behind the baking 24h, grind and sieve, obtain the product of 0.7mm～1.0mm particle diameter.
The product of embodiment 1 sees Table 1 with the correlated performance that does not add the active sludge carbon of graphite
Table 1 correlated performance relatively
| Type | Specific area | Total pore volume | Mean pore size |
| The active sludge carbon of conventional method preparation | 117.28m 2/g | 2.91cm 3/g | 6.944nm |
| The sludge activity sorbing material that adds 5% graphite | 139.41m 2/g | 3.52cm 3/g | 6.578nm |
As can be seen from Table 1, this invention is compared with traditional preparation active sludge carbon method, has not only improved the performance of active sludge carbon, can also effectively utilize some the barren rock China inks in the industrial activity, and broken breeze is realized the comprehensive utilization of resource.
Claims (2)
1, a kind of mud and waste graphite to prepare activated adsorption material method utilized, it is characterized in that getting excess sludge from the municipal sewage plant, mummification, the back of grinding, sieve are by solid-to-liquid ratio 1: (2.5～4.5) add zinc chloride and sulfuric acid solution, static placement 20～24h, baking 20～24h, mud after the processing adds the barren rock China ink, and addition is 3～10% of a mud total amount; Then, put into pyrolysis oven and carry out pyrolysis, utilize the nitrogen secluding air, nitrogen flow is controlled at 0.4～0.5L/min, and the rate of heat addition is controlled at 10～15 ℃/min, and pyrolysis temperature is 500～800 ℃, and the time is 1.5～2.5h; Product after the pyrolysis is the rinsing of 3mol/L hydrochloric acid solution with concentration earlier, impels wherein that oxide fully dissolves, and impurity in the wash-out carbon washs with 70 ℃ of deionized waters, to remove wherein Cl again simultaneously
-1, at 105 ℃ down behind the baking 24h, grind and sieve, obtain the product of 0.7mm～1.0mm particle diameter---sludge activity sorbing material.
2, a kind of mud and waste graphite to prepare activated adsorption material method utilized according to claim 1 is characterized in that the waste gas utilization mass concentration that produces in the pyrolytic process is that 10% sodium hydroxide solution absorbs processing.
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| CNA200710177295XA CN101234332A (en) | 2007-11-14 | 2007-11-14 | Method for using sewage sludge and waste graphite to prepare activated adsorption material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102228821A (en) * | 2011-07-18 | 2011-11-02 | 殷衡 | Adsorbent and preparation method thereof |
| CN102284213A (en) * | 2011-08-09 | 2011-12-21 | 哈尔滨工业大学 | Composite filter material for sewage treatment and preparation method thereof |
| CN102745879A (en) * | 2012-07-05 | 2012-10-24 | 华中科技大学 | Sludge-based adsorbent used for desulfurization and demercuration of flue-gas and preparation method thereof |
| CN104084126A (en) * | 2014-07-09 | 2014-10-08 | 福建工程学院 | Preparation method of biomass-based ferroaluminium complex spherical carbon |
| CN104276619A (en) * | 2014-10-09 | 2015-01-14 | 常州大学 | Method for processing methylthionine chloride in printing and dyeing wastewater |
| CN105236592A (en) * | 2015-11-14 | 2016-01-13 | 黄海涛 | Water purification charcoal material as well as production method and application thereof |
| CN106622129A (en) * | 2016-12-17 | 2017-05-10 | 安徽师范大学 | Graphite/sludge composite adsorbent, and preparation method and application thereof |
| CN109694234A (en) * | 2019-02-26 | 2019-04-30 | 北京建筑大学 | The method for preparing water-permeable brick using waterworks sludge |
| WO2024055515A1 (en) * | 2022-09-15 | 2024-03-21 | 广东邦普循环科技有限公司 | Sludge-based hexavalent chromium composite adsorbent and preparation method therefor |
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2007
- 2007-11-14 CN CNA200710177295XA patent/CN101234332A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102228821A (en) * | 2011-07-18 | 2011-11-02 | 殷衡 | Adsorbent and preparation method thereof |
| CN102228821B (en) * | 2011-07-18 | 2013-02-06 | 殷衡 | Adsorbent and preparation method thereof |
| CN102284213A (en) * | 2011-08-09 | 2011-12-21 | 哈尔滨工业大学 | Composite filter material for sewage treatment and preparation method thereof |
| CN102284213B (en) * | 2011-08-09 | 2013-09-25 | 哈尔滨工业大学 | Composite filter material for sewage treatment and preparation method thereof |
| CN102745879A (en) * | 2012-07-05 | 2012-10-24 | 华中科技大学 | Sludge-based adsorbent used for desulfurization and demercuration of flue-gas and preparation method thereof |
| CN102745879B (en) * | 2012-07-05 | 2013-10-30 | 华中科技大学 | Sludge-based adsorbent used for desulfurization and demercuration of flue-gas and preparation method thereof |
| CN104084126A (en) * | 2014-07-09 | 2014-10-08 | 福建工程学院 | Preparation method of biomass-based ferroaluminium complex spherical carbon |
| CN104276619A (en) * | 2014-10-09 | 2015-01-14 | 常州大学 | Method for processing methylthionine chloride in printing and dyeing wastewater |
| CN104276619B (en) * | 2014-10-09 | 2016-03-09 | 常州大学 | A kind of method for the treatment of of dyeing and printing Methylene Blue |
| CN105236592A (en) * | 2015-11-14 | 2016-01-13 | 黄海涛 | Water purification charcoal material as well as production method and application thereof |
| CN106622129A (en) * | 2016-12-17 | 2017-05-10 | 安徽师范大学 | Graphite/sludge composite adsorbent, and preparation method and application thereof |
| CN109694234A (en) * | 2019-02-26 | 2019-04-30 | 北京建筑大学 | The method for preparing water-permeable brick using waterworks sludge |
| WO2024055515A1 (en) * | 2022-09-15 | 2024-03-21 | 广东邦普循环科技有限公司 | Sludge-based hexavalent chromium composite adsorbent and preparation method therefor |
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