CN102757047A - Method for preparing cylindrical sludge-based activated carbon - Google Patents
Method for preparing cylindrical sludge-based activated carbon Download PDFInfo
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Abstract
本发明以城市污水厂剩余污泥为原料制备柱状污泥基活性炭，解决现有活性炭成型须粘结剂而引起环境污染问题。首先将已干燥的剩余污泥经30％的ZnCl2溶液或其它活化剂活化，置于105℃干燥箱烘干，用粉碎机粉碎过200目分样筛，制得的粉末污泥置于造粒机内，仅加入适量水，粉末污泥与水的质量比2.8∶1，无须加粘着剂，充分搅拌均匀，挤出柱状颗粒。通过马弗炉加热干燥脱水，再以炭化所需最佳温度炭化，制得柱状污泥基活性炭。本发明制得的柱状活性炭不易形成粉尘飞扬，且使用后易与溶液分离。与普通柱状活性炭相比，其表面含丰富的酸性官能团，可以高效去除水体中的有机污染物和重金属等污染物等。
The invention prepares columnar sludge-based activated carbon by using surplus sludge from urban sewage plants as a raw material, and solves the problem of environmental pollution caused by the need for binders in forming the existing activated carbon. First, activate the dried excess sludge with 30% ZnCl2 solution or other activators, dry it in a drying oven at 105°C, and crush it through a 200-mesh sieve with a pulverizer. In the granulator, only a proper amount of water is added, the mass ratio of powder sludge to water is 2.8:1, no adhesive is needed, and the columnar granules are extruded by fully stirring evenly. The columnar sludge-based activated carbon is obtained by heating, drying and dehydrating in a muffle furnace, and then carbonizing at the optimum temperature required for carbonization. The columnar activated carbon prepared by the invention is not easy to form dust and is easy to separate from the solution after use. Compared with ordinary columnar activated carbon, its surface is rich in acidic functional groups, which can efficiently remove organic pollutants, heavy metals and other pollutants in water.
Description
Technical field
The present invention relates to a kind of the excess sludge of municipal sewage plant prepared process of active carbon, especially relate to a kind of directly with the method for excess sludge preparative column shaped activated carbon.
Background technology
Gac is because characteristics such as its flourishing pore texture, huge specific surface area, stable chemical property, higher physical strength, recyclabilities; As a kind of sorbent material of excellent property, be widely used aspect the removal of atmospheric polluting material and water pollutant.
At present, the traditional raw material of preparation gac is wood chip, charcoal and coal.Because timber regeneration is slow, the mass consumption of timber is restricted the development of wood activated charcoal in addition.Production cost constantly increases and coal mass active carbon is owing to the minimizing of coal resources.Therefore, seeking traditional raw materials such as other resource replacing woods, coal prepares gac and becomes in many ways the focus of paying close attention to.The excess sludge of municipal sewage plant is produced gac as raw material, both can find a way out, effectively reduce the running cost of sewage work, solve and deal with the environmental problem of bringing improperly for the processing of excess sludge; Can prepare again be widely used, well behaved gac resource, turn waste into wealth, for the preparation of gac provides an approach, have good benefits in environment and economic benefit, meet trend and requirement that changing waste into resources utilizes.
Meanwhile, consider that the Powdered Activated Carbon that utilizes the excess sludge of municipal sewage plant to make is difficult for and water sepn in application process, and form dust from flying easily, cause the serious environmental pollution problem.
In addition; Existing columnar activated carbon all is with coal tar or adopts coal tar to add the working method as sticker such as pitch that the coal tar adding proportion is bigger, and adopts hydraulic pressure or other high-tension apparatus moulding; Exist many defectives following: the coal tar consumption is big; Make production cost improve, and rise steadily that the profit margin of whole industry is progressively dwindled along with the rise of coal tar price; Coal tar can decompose generation some harmful, toxic substances in process of production, and smell is abominable, and environment is caused severe contamination; Coal tar must carry out under the uninterrupted heating condition of steam in storage, transportation, and heat energy consumption is bigger; Adopt hydraulic pressure or high-tension apparatus during moulding, energy expenditure is high.
Summary of the invention
The objective of the invention is to strictness and carry out 12 planning requirements and the development trend of recycling, Sustainable development, overcome above-mentioned Powdered Activated Carbon and be difficult for and water sepn, and be prone to form dust from flying; Overcome cost raising that the utilization of adopting coal tar wet goods sticker causes and the problem of environmental pollution problems such as height that consume energy with molding device simultaneously.
The present invention provides a kind of method of directly excess sludge of municipal sewage plant being processed columnar activated carbon.This method is a main raw material with the excess sludge of municipal sewage plant, it is characterized in that comprising following process:
(a) excess sludge of municipal wastewater treatment plant is dried (24h) in 105 ℃ of loft drier, add the chemical activating agent solution soaking of preparation, chemical activation is 24 hours under the normal temperature, puts into 105 ℃ of loft drier oven dry (24h), is crushed to 200 order sub-sieves with kibbler then;
(b) the mud powder that makes in (a) is placed in the kneading cylinder of granulating equipment, add an amount of tap water, the mass ratio of mud powder and tap water 2.8: 1; Stir; Put into the extrusion cylinder again, material is squeezed into the smooth bar of diameter 1--10mm, and be cut into long 5--40mm cylindrical particle;
(c) the column mud granule is put into the retort furnace temperature programming, the fs is warming up to 105 ℃ and dehydrates, and subordinate phase continues to be warming up to the required optimum temps charing of charing 60 minutes, makes column mud matrix activated carbon.
In (a) of the present invention step, described chemical activating agent is the prerequisite of Preparation of Activated Carbon, and the gac activation has physical activation method and chemical activation method, and the present invention adopts the method for chemical activation.It is for the moisture removal with excess sludge that activation is prepended to 105 ℃ of loft drier oven dry (24h), not influence chemical activation effect afterwards; It is in order to be crushed to 200 purpose powder more easily that activation is placed on 105 ℃ of loft drier oven dry (24h).
In (b) of the present invention step, add and can extrude smooth bar after tap water fully stirs, this is because excess sludge itself has stronger tackiness; Need not extra interpolation tackiness agent; Meanwhile, do not have at pressure under the situation of particular requirement, can satisfy mud moulding desirable strength.
Granulating equipment is selected the extrusion shaping machine that columnar mould is housed for use, and material is squeezed into bar through the forcing machine template, and according to different purposes, the diameter range that is extruded into bar is 1mm～10mm, and bar is cut into cutting knife the cylindrical particle of length-specific in the extruding back.
In (c) of the present invention step is the high temperature carbonization stage, makes the column sludge carbonization that makes, and becomes columnar activated carbon.
The present invention adopts twin screw to mediate the extrusion shaping machine that the extruding all-in-one perhaps is equipped with columnar mould; At lower pressure and do not add any tackiness agent; And under above-mentioned optimum condition, make and excess sludge moulding and activation charing finally obtain column mud matrix activated carbon.Have the following advantages:
1, the excess sludge of municipal sewage plant is produced gac as raw material, turn waste into wealth, both can find a way out, effectively reduce the running cost of sewage work again, solved the improper environmental problem of bringing of sludge treatment for the processing of excess sludge.The recycling of national proposition, the requirement and the trend of Sustainable development have been carried out.
2, make full use of the tackiness of mud itself, broken away from the method that adopts coal tar wet goods tackiness agent to produce columnar activated carbon fully, made technology easy; Reduced environmental pollution; Practiced thrift heat energy, production cost reduces greatly, meets the requirement of national energy-saving and emission-reduction fully.
3, adopt such granulating equipment, forming pressure is lower, and operational condition is gentle, has improved throughput greatly.
4, compare with Powdered Activated Carbon, the dust from flying phenomenon can not occur, and in water treatment applications, easy and water sepn has improved environmental benefit greatly the time simple to operate.
Description of drawings
Fig. 1 is a mud pilum shaped activated carbon pictorial diagram.
Fig. 2 is that mud pilum shaped activated carbon ESEM (does not filter ZnCl
2Amplify 2000 times) figure.
Embodiment
Embodiment 1:
The method of manufacture of column mud matrix activated carbon, this method are main raw material with the excess sludge of municipal sewage plant, it is characterized in that comprising following process:
(a) excess sludge of municipal wastewater treatment plant is dried (24h) in 105 ℃ of loft drier, the adding massfraction is 30% ZnCl
2Solution soaks as acvator, and chemical activation is 24 hours under the normal temperature, puts into 105 ℃ of loft drier oven dry (24h), is crushed to 200 order sub-sieves with kibbler then;
(b) place twin screw to mediate in the kneading cylinder of extruding integral type granulating equipment in the mud powder that makes in (a); Add an amount of tap water; The mass ratio of mud powder and tap water 2.8: 1 stirs, and puts into the extrusion cylinder again; Material is squeezed into the smooth bar of diameter 4mm, and is cut into long 20mm cylindrical particle;
(c) the column mud granule is put into the retort furnace temperature programming, the fs is warming up to 105 ℃ and dehydrates, and subordinate phase continued to be warming up to 600 ℃ of high temperature carbonizations 60 minutes, makes column mud matrix activated carbon.
Through test, the average compressive strength of this mud pilum shaped activated carbon is 100.23N, and iodine sorption value is 415.62, and long period of soaking can not caved in or disperse in the water of room temperature, has stability preferably.
Embodiment 2
The method of manufacture of column mud matrix activated carbon, this method are main raw material with the excess sludge of municipal sewage plant, it is characterized in that comprising following process:
(a) excess sludge of municipal wastewater treatment plant is dried (24h) in 105 ℃ of loft drier, the adding massfraction is 30% ZnCl
2Solution soaks as acvator, and chemical activation is 24 hours under the normal temperature, and acvator is filtered, and puts into 105 ℃ of loft drier oven dry (24h), is crushed to 200 order sub-sieves with kibbler then;
(b) place twin screw to mediate in the kneading cylinder of extruding integral type granulating equipment in the mud powder that makes in (a); Add an amount of tap water; The mass ratio of mud powder and tap water 2.8: 1 stirs, and puts into the extrusion cylinder again; Material is squeezed into the smooth bar of diameter 4mm, and is cut into long 20mm cylindrical particle;
(c) the column mud granule is put into the retort furnace temperature programming, the fs is warming up to 105 ℃ and dehydrates, and subordinate phase continued to be warming up to 600 ℃ of high temperature carbonizations 60 minutes, makes column mud matrix activated carbon.
Through test, the average compressive strength of this mud pilum shaped activated carbon is 141.91N, and iodine sorption value is 279.20, and long period of soaking can not caved in or disperse in the water of room temperature.
Embodiment 3
The method of manufacture of column mud matrix activated carbon, this method are main raw material with the excess sludge of municipal sewage plant, it is characterized in that comprising following process:
(a) excess sludge of municipal wastewater treatment plant is dried (24h) in 105 ℃ of loft drier, the adding massfraction is 30% ZnCl
2Solution soaks as acvator, and chemical activation is 24 hours under the normal temperature, and acvator is filtered, and puts into 105 ℃ of loft drier oven dry (24h), is crushed to 200 order sub-sieves with kibbler then;
(b) place twin screw to mediate in the kneading cylinder of extruding integral type granulating equipment in the mud powder that makes in (a); Add an amount of tap water; The mass ratio of mud powder and tap water 2.8: 1 stirs, and puts into the extrusion cylinder again; Material is squeezed into the smooth bar of diameter 4mm, and is cut into long 20mm cylindrical particle;
(c) the column mud granule is put into the retort furnace temperature programming, the fs is warming up to 105 ℃ and dehydrates, and subordinate phase continued to be warming up to 500 ℃ of high temperature carbonizations 60 minutes, makes column mud matrix activated carbon.
Through test, the average compressive strength of this mud pilum shaped activated carbon is 133.81N, and iodine sorption value is 329.49, and long period of soaking can not caved in or disperse in the water of room temperature.
Embodiment 4
The method of manufacture of column mud matrix activated carbon, this method are main raw material with the excess sludge of municipal sewage plant, it is characterized in that comprising following process:
(a) excess sludge of municipal wastewater treatment plant is dried (24h) in 105 ℃ of loft drier, the adding massfraction is 30% ZnCl
2Solution soaks as acvator, and chemical activation is 24 hours under the normal temperature, and acvator is filtered, and puts into 105 ℃ of loft drier oven dry (24h), is crushed to 200 order sub-sieves with kibbler then;
(b) place twin screw to mediate in the kneading cylinder of extruding integral type granulating equipment in the mud powder that makes in (a); Add an amount of tap water; The mass ratio of mud powder and tap water 2.8: 1 stirs, and puts into the extrusion cylinder again; Material is squeezed into the smooth bar of diameter 4mm, and is cut into long 20mm cylindrical particle;
(c) the column mud granule is put into the retort furnace temperature programming, the fs is warming up to 105 ℃ and dehydrates, and subordinate phase continued to be warming up to 700 ℃ of high temperature carbonizations 60 minutes, makes column mud matrix activated carbon.
Through test, the average compressive strength of this mud pilum shaped activated carbon is 142.81N, and iodine sorption value is 327.49, and long period of soaking can not caved in or disperse in the water of room temperature.
Embodiment 5
According to process step and the processing parameter of embodiment 1, in the step (b), granulating equipment is selected the extrusion shaping machine that columnar mould is housed for use, and the column mud matrix activated carbon absorption index that makes is suitable with embodiment 1,2,3,4.
Embodiment 6
According to the process step of embodiment 1, in the step (a), chemical activating agent is selected certain density KOH solution for use; In the step (c), carbonization temperature is made as 800--900 ℃, and other step and processing parameter are constant, and the column mud matrix activated carbon that obtains has more flourishing micropore and bigger specific surface area, and reaction is very fast, and long period of soaking can not caved in or disperse in the water of room temperature.
Embodiment 7
According to the process step of embodiment 1, in the step (a), chemical activating agent is selected certain density H for use
3PO
4Solution; In the step (c), carbonization temperature is made as 400--600 ℃, and other step and processing parameter are constant, and the column mud matrix activated carbon aperture that obtains is less, but mesopore is flourishing, and long period of soaking can not caved in or disperse in the water of room temperature.
Embodiment 8
According to the process step of embodiment 1, in the step (a), chemical activating agent is selected certain density NH for use
3H
2O solution; In the step (c), carbonization temperature is made as 800--900 ℃, and other step and processing parameter are constant, and nitrogen-containing functional group has been added on the column mud matrix activated carbon surface that obtains, and its desulfidation obviously strengthens, and long period of soaking can not caved in or disperse in the water of room temperature.
Embodiment 9
According to process step and the processing parameter of embodiment 1, the mud powder after the activation is put into the extrusion cylinder after adding the water stirring, uses the mould of different diameter instead, can material be squeezed into the smooth bar of diameter 1mm--4mm, and can be cut into long 5mm--40mm cylindrical particle.
Claims (5)
1. the preparation method of a column mud matrix activated carbon, this method is a main raw material with the excess sludge of municipal sewage plant, it is characterized in that comprising following process:
(a) excess sludge of municipal wastewater treatment plant is dried (24h) in 105 ℃ of loft drier, add the chemical activating agent solution soaking of preparation, chemical activation is 24 hours under the normal temperature, puts into 105 ℃ of loft drier oven dry (24h), is crushed to 200 order sub-sieves with kibbler then;
(b) the mud powder that makes in (a) is placed in the kneading cylinder of granulating equipment, add an amount of tap water, the mass ratio of mud powder and tap water 2.8: 1; Stir; Put into the extrusion cylinder again, material is squeezed into the smooth bar of diameter 1--10mm, and be cut into long 5--40mm cylindrical particle;
(c) the column mud granule is put into the retort furnace temperature programming, the fs is warming up to 105 ℃ and dehydrates, and subordinate phase continues to be warming up to the required optimum temps charing of charing 60 minutes, makes column mud matrix activated carbon.
2. the preparation method of a kind of column mud matrix activated carbon as claimed in claim 1 is characterized in that the mud of used municipal wastewater treatment plant itself has stronger tackiness, can directly be squeezed into bar, and need not add tackiness agent.
3. the preparation method of a kind of column mud matrix activated carbon as claimed in claim 1 is characterized in that described chemical activating agent is the ZnCl of massfraction 30%
2Solution, KOH solution, H
3PO
4Solution or NH
3H
2O solution.
4. the preparation method of a kind of column mud matrix activated carbon as claimed in claim 1 is characterized in that described granulating equipment is that twin screw is mediated extruding integral type granulating equipment or other are equipped with the extrusion shaping machine of columnar mould.
5. the preparation method of a kind of column mud matrix activated carbon as claimed in claim 1 is characterized in that the required optimum temps of described charing depends on activator species, like ZnCl
2It is 600 ℃; KOH and NH
3H
2O is 800--900 ℃; H
3PO
4Be 400--600 ℃.
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| CN2012101736583A CN102757047A (en) | 2012-05-31 | 2012-05-31 | Method for preparing cylindrical sludge-based activated carbon |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556030A (en) * | 2014-12-31 | 2015-04-29 | 安徽工业大学 | Control method for preparing active carbon with large specific surface by sludge |
| CN106111142A (en) * | 2016-06-21 | 2016-11-16 | 西安汉术化学工程股份有限公司 | A kind of being electrically excited processes the preparation method of filler catalyst used by high-concentration waste water device |
| 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 |
| 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 |
| CN107824158A (en) * | 2017-10-11 | 2018-03-23 | 上海市政工程设计研究总院（集团）有限公司 | A kind of method that sewage treatment plant's dewatered sludge prepares active sludge carbon |
| CN107934957A (en) * | 2017-10-17 | 2018-04-20 | 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 |
| CN108298576A (en) * | 2018-03-07 | 2018-07-20 | 福建工程学院 | A kind of preparation method of antibacterial granule activated carbon |
| CN110436461A (en) * | 2018-05-02 | 2019-11-12 | 新奥科技发展有限公司 | A kind of active carbon and preparation method thereof |
| CN116253322A (en) * | 2023-05-15 | 2023-06-13 | 山西新辉活性炭有限公司 | Mesoporous columnar activated carbon preparation equipment and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556030A (en) * | 2014-12-31 | 2015-04-29 | 安徽工业大学 | Control method for preparing active carbon with large specific surface by sludge |
| CN106111142A (en) * | 2016-06-21 | 2016-11-16 | 西安汉术化学工程股份有限公司 | A kind of being electrically excited processes the preparation method of filler catalyst used by high-concentration waste water device |
| 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 |
| 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 |
| CN107824158A (en) * | 2017-10-11 | 2018-03-23 | 上海市政工程设计研究总院（集团）有限公司 | A kind of method that sewage treatment plant's dewatered sludge prepares active sludge carbon |
| CN107934957A (en) * | 2017-10-17 | 2018-04-20 | 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 |
| CN108298576A (en) * | 2018-03-07 | 2018-07-20 | 福建工程学院 | A kind of preparation method of antibacterial granule activated carbon |
| CN110436461A (en) * | 2018-05-02 | 2019-11-12 | 新奥科技发展有限公司 | A kind of active carbon and preparation method thereof |
| CN116253322A (en) * | 2023-05-15 | 2023-06-13 | 山西新辉活性炭有限公司 | Mesoporous columnar activated carbon preparation equipment and preparation method thereof |
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Application publication date: 20121031 |