CN102107872A - Process for preparing active carbon by adding husks into chemical sludge - Google Patents

Process for preparing active carbon by adding husks into chemical sludge Download PDF

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CN102107872A
CN102107872A CN201110052074.6A CN201110052074A CN102107872A CN 102107872 A CN102107872 A CN 102107872A CN 201110052074 A CN201110052074 A CN 201110052074A CN 102107872 A CN102107872 A CN 102107872A
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sludge
drying
active carbon
technology according
washing
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徐炎华
胡俊
赵浩
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Nanjing Tech University
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Nanjing Tech University
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Abstract

The invention relates to a process for preparing active carbon by adding husks into chemical sludge. The process comprises the following steps of: drying residual sludge which is generated from sewage treatment in chemical industry and serves as a raw material; adding the husks; grinding; adding an activating agent; drying; performing carbonizing activation under the protection of inert gases; and cooling, washing and drying to prepare sludge-based active carbon. The active carbon is prepared from a great deal of the residual sludge which is generated from sewage treatment in chemical industry and serves as the raw material, so the discharge value of the residual sludge in the chemical industry is reduced, preparation cost of an active carbon adsorbent is reduced, and obvious environmental and economic benefits are achieved. The heavy metal concentration of the prepared active carbon is lower than the highest allowable leachate concentration stated in national standard GB 5085.3-2007 (hazardous waste identification standard leaching toxicity identification); and under a high-temperature pyrolysis condition, organic matters in the sludge can be completely mineralized. The active carbon prepared by the process can be applied in the fields of wastewater treatment, waste gas absorption and the like and has a wide market prospect.

Description

A kind of chemical engineering sludge adds the technology that shell prepares gac
Technical field
The present invention relates to a kind of disposal of resources of industrial solid castoff, relate in particular to a kind of chemical engineering sludge and add the technology that shell prepares gac.
Background technology
The mud of chemical industry is not only bulky, and organic poison content height, and particle is thin, is cotton-shaped colloidal structure, has high-hydrophilic.Surplus the existing big or small chemical industrial park 1000 of China, have family surplus the big or small chemical enterprise 100,000.These chemical enterprises produce tens thousand of tons excess sludge every day, and the water ratio of mud is up to more than 95%, and mud is after the belt press filtration, and water ratio reduces to 70~85%, because of it contains various organic poisons and heavy metal." national Hazardous wastes register " regulation according to the up-to-date promulgation of China, the excess sludge that produces in the industry wastewater treatment process such as chemical industry, medicine and agricultural chemicals is dangerous solid waste, must send the Hazardous wastes disposal center of qualification to focus on, about 2000 yuan/ton of disposal costs.
China's chemical engineering sludge burning disposal expense height, many chemical enterprises transfer to adopt landfill or compost treatment excess sludge, owing to contain a large amount of organic poisons in the mud, landfill or compost easily produce serious secondary pollution, the harm ecotope, and compost has taken a large amount of farmlands.How therefore research and development, more effectively dispose municipal sludge at the economy of toxicity mud, efficient treatment technology, and it is the problem that the environmental protection field presses for solution that municipal sludge is turned waste into wealth.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, and provide a kind of chemical engineering sludge to add the technology that shell prepares gac, in easy mode mud is carried out carbonization-activation and handle, the carbonization-activation material that obtains can substitute gac and use, and realizes the recycling sludge utilization.
Technical scheme of the present invention is: a kind of chemical engineering sludge adds the technology that shell prepares gac, and its concrete steps are as follows:
(1), with after the chemical engineering sludge drying behind the belt filter-press dehydration, obtain dewatered sludge;
(2), adding the dry fruit shell in dewatered sludge obtains mixture, grinding again;
(3), add activation solution, dipping activation under 50~100 ℃ temperature, soak time is 2~10h, the stirring while activate; Dry then;
(4), with rare gas element as the protection gas, at 600~900 ℃ of pyrolysis 0.5~5h;
(5), cooling, washing, drying, make active sludge carbon.
Drying temperature in preferred steps (1) and (3) is 105~120 ℃, and be 4~24h time of drying.Drying process in the step (5) is selected the ordinary method drying.
Preferred described dry fruit shell is at least a kind of in coconut husk, almond or the nut-shell; Wherein in the per kilogram dewatered sludge, the addition of dry fruit shell is 5~30g; Median size after mixture grinds is 0.15~1mm.
Preferred described activation solution is at least a kind of in zinc chloride, potassium hydroxide or the potassium sulfide aqueous solution; Wherein the concentration of activation solution is 1~5mol/L; In the per kilogram dewatered sludge, the add-on of activation solution is 0.5~2L.
Stir speed (S.S.) after the preferred adding activation solution is 100~200r/min.
Preferred described rare gas element is nitrogen, helium or argon gas; The purge rates of rare gas element is 100~200mL/min.
Temperature rise rate in the preferred described pyrolytic process is 10~20 ℃/min.
Preferred described washing process is earlier with the washing of 0.8~1.5mol/L hydrochloric acid soln, drying; Through washing, drying makes active sludge carbon again.
The present invention is the feedstock production gac with the chemical industry dewatered sludge, has broken through traditional prepare gac and prepare the technology of gac with the excess sludge of sanitary sewage with coal, timber.
Beneficial effect:
Compare with traditional sludge disposal and method for preparation of active carbon, have following advantage:
1, is the feedstock production gac with the chemical industry dewatered sludge, broken through and traditional prepare the technology of gac, also opened up the new way that solid waste is handled simultaneously with coal, timber with the excess sludge of sanitary sewage.
2, be the feedstock production gac with the chemical industry dewatered sludge, for the treatment and disposal of mud finds a way out, cheaply can get for Activated Carbon Production has found simultaneously, the raw material of wide material sources, can alleviate China's timber, energy starved contradiction.
3, prepare gac with mud and reached " turning waste into wealth ", " treatment of wastes with processes of wastes against one another " purpose, have good environment and social benefit.Under the high temperature pyrolysis condition, carbonaceous organic material in the mud issues estranged separating in the effect of heat, non-carbon is overflowed with the form of volatile matter, organism in the mud can obtain permineralization, and the heavy metal of gac leaches the leach liquor maximum permissible concentration of concentration far below regulation among the GB GB5085.3-2007 (the Hazardous wastes judging standard leaches toxicity and differentiates).
Embodiment
Embodiment 1:
Get the quality water ratio and be certain petrochemical plant excess sludge of 75%, 120 ℃ of dry 6h take by weighing the 1kg dewatered sludge, add the 5g coconut husk successively, and being ground to median size is 0.71mm, and adding 0.5L concentration again is the potassium hydroxide activation solution of 3mol/L; In 90 ℃ of dipping activation 4h, stir dry (120 ℃ of dry 4h) simultaneously in 150r/min in activation.600 ℃ (temperature rise rate be 15 ℃/min), the purge rates of nitrogen be 150mL/min protection down, pyrolysis 3h.Cooling is with 1mol/L salt acid elution, drying; Washing again gets gac after the drying.Recording specific surface area is: 441m 2/ g, its heavy metal leaches concentration and sees Table 1.
Embodiment 2:
Get the quality water ratio and be certain insecticide factory's sewage treatment plant residual mud of 80%, 110 ℃ of dry 8h take by weighing the 1kg dewatered sludge, add the 15g almond successively, being ground to median size is 0.50mm, adds potassium hydroxide and liquor zinci chloridi that 1L concentration is 3mol/L again; In 85 ℃ of dipping activation 6h, stir dry (110 ℃ of dry 8h) simultaneously in 100r/min in activation.700 ℃ (temperature rise rate be 10 ℃/min), the purge rates of helium be 100mL/min protection down, pyrolysis 2.5h.Cooling is with 0.8mol/L salt acid elution, drying; Washing again gets gac after the drying.Recording specific surface area is: 465m 2/ g, its heavy metal leaches concentration and sees Table 1.
Embodiment 3:
Get the quality water ratio and be certain medication chemistry factory sewage treatment plant residual mud of 85%, 105 ℃ of dry 24h take by weighing the 1kg dewatered sludge, add the 30g peach-pit successively, and being ground to median size is 0.15mm, adds the potassium sulfide solution that 2L concentration is 1mol/L again; In 75 ℃ of dipping activation 8h, activating the while in 200r/min, dry (105 ℃ of dry 24h).800 ℃ (temperature rise rate be 20 ℃/min), the purge rates of argon gas be 180mL/min protection down, pyrolysis 5h.Cooling is with 1.5mol/L salt acid elution, drying; Washing again gets gac after the drying.Recording specific surface area is: 510m 2/ g, its heavy metal leaches concentration and sees Table 1.
Table 1 gac leaches heavy metal content analysis in the leach liquor in the toxicity telling test
Figure BDA0000048844580000031

Claims (8)

1. a chemical engineering sludge adds the technology that shell prepares gac, and its concrete steps are as follows:
(1), with after the chemical engineering sludge drying behind the belt filter-press dehydration, obtain dewatered sludge;
(2), adding the dry fruit shell in dewatered sludge gets mixture, grinding again;
(3), add activation solution, dipping activation under 50~100 ℃ temperature, soak time is 2~10h, the stirring while activate; Dry then;
(4), with rare gas element as the protection gas, at 600~900 ℃ of pyrolysis 0.5~5h;
(5), cooling, washing, drying, make active sludge carbon.
2. technology according to claim 1 is characterized in that the drying temperature in step (1) and (3) is 105~120 ℃, and be 4~24h time of drying.
3. technology according to claim 1 is characterized in that described dry fruit shell is at least a kind of in coconut husk, almond or the nut-shell; Wherein in the per kilogram dewatered sludge, the addition of dry fruit shell is: 5~30g; Median size after mixture grinds is 0.15~1mm.
4. technology according to claim 1 is characterized in that described activation solution is at least a kind of in zinc chloride, potassium hydroxide or the potassium sulfide aqueous solution; Wherein the concentration of activation solution is 1~5mol/L; In the per kilogram dewatered sludge, the add-on of activation solution is 0.5~2L.
5. technology according to claim 1, the stir speed (S.S.) that it is characterized in that adding after the activation solution is 100~200r/min.
6. technology according to claim 1 is characterized in that described rare gas element is nitrogen, helium or argon gas; The purge rates of rare gas element is 100~200mL/min.
7. technology according to claim 1 is characterized in that the temperature rise rate in the described pyrolytic process is 10~20 ℃/min.
8. technology according to claim 1 is characterized in that described washing process is for washing drying earlier with 0.8~1.5mol/L hydrochloric acid soln; Through washing, drying makes active sludge carbon again.
CN201110052074.6A 2011-03-04 2011-03-04 Process for preparing active carbon by adding husks into chemical sludge Pending CN102107872A (en)

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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432007A (en) * 2011-09-23 2012-05-02 南京工业大学 Method for preparing activated carbon by physical activation of excess sludge
CN102530941A (en) * 2011-12-16 2012-07-04 北京工业大学 Sludge-based activated carbon and preparation method thereof
CN102698712A (en) * 2012-05-14 2012-10-03 北京工业大学 Surface modification method of sludge-activated carbon for treating dyeing wastewater
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
CN103435039A (en) * 2013-08-20 2013-12-11 西安工程大学 Method for preparing fallen phoenix tree leaf-doped muddy active carbon by microwave irradiation
CN104084142A (en) * 2014-07-04 2014-10-08 河海大学 Preparation method of physiochemically-modified macadimia nutshell adsorbing agent
CN104495841A (en) * 2014-12-09 2015-04-08 西南石油大学 Preparation method of walnut shell-doped sludge activated carbon
CN105731752A (en) * 2016-04-29 2016-07-06 东北大学 Method for preparing biochar by carrying out copyrolysis on excess sludge and hazelnut shell
CN107628619A (en) * 2017-09-15 2018-01-26 深圳市水务(集团)有限公司 A kind of preparation method of the rich nitrogen active sludge carbon of adulterated food leftover bits and pieces
CN108033448A (en) * 2018-01-31 2018-05-15 西南石油大学 A kind of coconut husk-sludge composite activated carbon and its preparation method and application
CN108046254A (en) * 2017-12-27 2018-05-18 济南大学 A kind of corncob derives active carbon electrode material and preparation method thereof
CN108423678A (en) * 2018-04-17 2018-08-21 华南农业大学 A kind of multistage porous carbon materials of superhigh specific surface area and the preparation method and application thereof
CN109019598A (en) * 2018-07-18 2018-12-18 华南农业大学 A kind of mixing biomass prepares the method and manufactured three-dimensional porous carbon material and its application of the three-dimensional porous carbon material of high specific capacitance
CN109174063A (en) * 2018-10-17 2019-01-11 肇庆市珈旺环境技术研究院 A kind of sludge base adsorbent and preparation method thereof
CN109317098A (en) * 2018-10-25 2019-02-12 肇庆市珈旺环境技术研究院 A kind of sludge base mixed adsorbing material and preparation method thereof
CN110078070A (en) * 2019-04-11 2019-08-02 西安石油大学 A kind of preparation method of the oily sludge base absorption carbon material for oily waste water treatment
CN110342605A (en) * 2019-07-30 2019-10-18 苏州飞辉环境科技有限公司 It is a kind of for adsorbing the sludge-based activated carbon composite material and preparation method of heavy metal in flying ash leachate
CN110526549A (en) * 2019-07-29 2019-12-03 安徽百和环境技术有限公司 A kind of betterment of land sludge organism charcoal and preparation method thereof
CN113184844A (en) * 2021-05-25 2021-07-30 马鞍山钢铁股份有限公司 Method for preparing activated carbon by using carbon-containing dust and mud
CN114749164A (en) * 2022-04-20 2022-07-15 江苏美亚科泽过滤技术有限公司 Preparation method of sulfur dioxide and hydrogen sulfide gas adsorbent

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CN1644495A (en) * 2004-12-14 2005-07-27 南开大学 Method for preparing active carbon from urban sewage treatment plant mud

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Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432007A (en) * 2011-09-23 2012-05-02 南京工业大学 Method for preparing activated carbon by physical activation of excess sludge
CN102530941A (en) * 2011-12-16 2012-07-04 北京工业大学 Sludge-based activated carbon and preparation method thereof
CN102698712A (en) * 2012-05-14 2012-10-03 北京工业大学 Surface modification method of sludge-activated carbon for treating dyeing wastewater
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
CN103435039A (en) * 2013-08-20 2013-12-11 西安工程大学 Method for preparing fallen phoenix tree leaf-doped muddy active carbon by microwave irradiation
CN104084142B (en) * 2014-07-04 2015-11-18 河海大学 A kind of preparation method of materialization modification macadamia shell adsorbent
CN104084142A (en) * 2014-07-04 2014-10-08 河海大学 Preparation method of physiochemically-modified macadimia nutshell adsorbing agent
CN104495841A (en) * 2014-12-09 2015-04-08 西南石油大学 Preparation method of walnut shell-doped sludge activated carbon
CN105731752A (en) * 2016-04-29 2016-07-06 东北大学 Method for preparing biochar by carrying out copyrolysis on excess sludge and hazelnut shell
CN105731752B (en) * 2016-04-29 2019-04-26 东北大学 A method of charcoal is prepared using excess sludge and hazelnut shell copyrolysis
CN107628619A (en) * 2017-09-15 2018-01-26 深圳市水务(集团)有限公司 A kind of preparation method of the rich nitrogen active sludge carbon of adulterated food leftover bits and pieces
CN108046254A (en) * 2017-12-27 2018-05-18 济南大学 A kind of corncob derives active carbon electrode material and preparation method thereof
CN108046254B (en) * 2017-12-27 2021-03-02 济南大学 Corncob-derived activated carbon electrode material and preparation method thereof
CN108033448A (en) * 2018-01-31 2018-05-15 西南石油大学 A kind of coconut husk-sludge composite activated carbon and its preparation method and application
CN108423678A (en) * 2018-04-17 2018-08-21 华南农业大学 A kind of multistage porous carbon materials of superhigh specific surface area and the preparation method and application thereof
CN109019598A (en) * 2018-07-18 2018-12-18 华南农业大学 A kind of mixing biomass prepares the method and manufactured three-dimensional porous carbon material and its application of the three-dimensional porous carbon material of high specific capacitance
CN109174063A (en) * 2018-10-17 2019-01-11 肇庆市珈旺环境技术研究院 A kind of sludge base adsorbent and preparation method thereof
CN109317098A (en) * 2018-10-25 2019-02-12 肇庆市珈旺环境技术研究院 A kind of sludge base mixed adsorbing material and preparation method thereof
CN110078070A (en) * 2019-04-11 2019-08-02 西安石油大学 A kind of preparation method of the oily sludge base absorption carbon material for oily waste water treatment
CN110526549A (en) * 2019-07-29 2019-12-03 安徽百和环境技术有限公司 A kind of betterment of land sludge organism charcoal and preparation method thereof
CN110526549B (en) * 2019-07-29 2021-08-24 安徽百和环保科技有限公司 Soil improvement sludge biochar and preparation method thereof
CN110342605A (en) * 2019-07-30 2019-10-18 苏州飞辉环境科技有限公司 It is a kind of for adsorbing the sludge-based activated carbon composite material and preparation method of heavy metal in flying ash leachate
CN113184844A (en) * 2021-05-25 2021-07-30 马鞍山钢铁股份有限公司 Method for preparing activated carbon by using carbon-containing dust and mud
CN114749164A (en) * 2022-04-20 2022-07-15 江苏美亚科泽过滤技术有限公司 Preparation method of sulfur dioxide and hydrogen sulfide gas adsorbent

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Application publication date: 20110629