CN104163427B - A kind of method that activated carbon is prepared using fuse salt activation - Google Patents

A kind of method that activated carbon is prepared using fuse salt activation Download PDF

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CN104163427B
CN104163427B CN201410350867.XA CN201410350867A CN104163427B CN 104163427 B CN104163427 B CN 104163427B CN 201410350867 A CN201410350867 A CN 201410350867A CN 104163427 B CN104163427 B CN 104163427B
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activated carbon
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activation
fuse salt
raw material
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CN104163427A (en
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李爱民
尹玉磊
高宁博
张雷
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The invention discloses a kind of method that activated carbon is prepared using fuse salt activation, raw material is crushed, drying is put into heating furnace the isothermal pyrolysis under the conditions of certain temperature, coke caused by pyrolysis being passed through is put into fuse salt, isothermal reaction is taken out after certain time, is heated to certain temperature constant temperature activation a period of time under an inert atmosphere.It is cooled to room temperature, gained material is soaked with certain density hydrochloric acid solution, it is washed to neutrality, it is activated carbon by gained material drying, the activated carbon prepared by the present invention utilizes permeability good under fuse salt hot conditions under the premise of high-quality is ensured, reduce conventional method salt caused by early-stage preparations are conciliate in thermal process to waste and volatilize, shorten and prepare time, significantly reduce the production cost of activated carbon, this technology is advantageous to promote the innovation of activated carbon process.

Description

A kind of method that activated carbon is prepared using fuse salt activation
Technical field
The invention belongs to activated carbon preparation field, is related to a kind of method that activated carbon is prepared using fuse salt activation.
Background of invention
Activated carbon is a kind of carbonaceous material with huge specific surface area and flourishing hole, possesses excellent energy of adsorption Power, there is the features such as chemical stability is high, adsorption capacity is strong, renewable to be widely used in liquid phase because it possesses in adsorption process The fields such as absorption, separation, purification and the storage of the energy with gaseous substance.
The preparation method of activated carbon has a variety of, and physical activation method, chemical activation method are broadly divided into according to the property of activator And physical chemistry activation method.The advantages of physical activation method is that technique is simple, prepares that cost is low, the pollution small later stage to environment without Need to wash, shortcoming is activation temperature height, and activated carbon quality is not relatively high, and economic value added is low, more commonly used physically activated examination Agent has vapor, carbon dioxide etc.;The advantages of chemical activation method is that preparation temperature is low with respect to physical activation method, energy requirement phase To less, the quality of activated carbon is higher, shortcoming be cost height, the pollution to environment is relatively serious, the later stage need washing procedure from Increase the waste of chemical reagent and secondary pollution to environment to a certain extent, relatively common chemical activation reagent have zinc chloride, Phosphoric acid, potassium hydroxide, potassium carbonate etc..Activated carbon quality that chemical activation is prepared due to it is high, adsorption capacity is strong therefore wider It is general to be applied among actual production.
Chinese patent, publication date:On 2 24th, 2010, publication number:CN101654247A application numbers: 200910195690.X patent of invention " preparation method of shaddock peel activated carbon ", propose by the use of various concentrations potassium hydroxide as Activator simultaneously activates the activated carbon that pomelo peel prepares high-quality under a certain pressure.The method can not avoid activated carbon quality and work Contradiction between agent dosage, process need a large amount of alkali lye to cause the corrosion of equipment as activator and prepare cost Greatly improve, and be pyrolyzed after caused by coke need it is polished again with potassium hydroxide admixture activation, process of lapping meeting Produce dust and problem of environmental pollution be present.
Chinese patent, publication date:On December 16th, 2012, publication number:The application numbers of CN 102249228: 201110158695.2 patent of invention " method that activated carbon is prepared with the pinecone " proposes to be mixed using the pinecone with potassium hydroxide Activation prepares high quality active carbon.The method raw material is cheap, reduces the production cost of activated carbon, promotes the hair of low-carbon economy Exhibition, is reasonable from principle, but potassium hydroxide needs static 20-30 hours after being mixed with the raw material pinecone, is answered from actual With setting out, it is prolonged it is static can not only cause preparation time cycle stretch-out, and man power and material's cost can be increased, and then The manufacturing cost of activated carbon is set to remain high.
There is chemical reagent to participate in problems being present during activation prepares activated carbon at present, wherein most important core One of problem:The contradiction of activator quality and activated carbon quality.The amount of chemical reagent is improved in order to improve activated carbon quality, this The individual generally existing in process for preparing active carbon, above way will certainly cause the exacerbation of raising and the pollution of cost.In activity There is most to be slatterned because of the volatilization of high temperature in charcoal actual fabrication process in chemical reagent, can not actual participation activation Process, cause the utilization rate of activating reagent low;Another key problem:Chemical reagent needs after being mixed with raw material and coke Chemical reagent is allowed to be sufficiently submerged in raw material and coke the regular hour, the cycle that this process can cause activated carbon to prepare prolongs Long, the covert cost and efficiency that add preparation.It is exactly the bottleneck place for restricting its development that these problems, which exist,.
The content of the invention
, can the invention provides a kind of method that activated carbon is prepared using fuse salt for overcome the deficiencies in the prior art To prepare activated carbon as raw material using materials such as coal, timber, biomass.On the one hand chemical reagent can effectively be controlled because volatilization Caused by waste, another aspect preparation process shortening manufacturing cycle, dropped without mix in advance by chemical reagent with raw material and coke Low activity charcoal production cost.
Raw material is crushed, after drying, the pyrolytic reaction 10-480min under the conditions of 300-800 DEG C, pyrolytic reaction will be passed through and produced Raw coke is added in fuse salt, is taken out after reacting 0.5-240min under the conditions of 200-1000 DEG C, under an inert atmosphere 400- 1200 DEG C of activation 0.5-10 hours.Product is cooled to room temperature, soaked with hydrochloric acid solution, is washed to neutrality, gained material is dried It is dry to produce activated carbon.
Raw material:Biomass material (such as:Wood chip, cocoanut shell, charcoal, bamboo, bark, walnut shell, fruit stone, boll hull, rice Shell, coffee bean stalk, oil palm shell, furfural dregs and spent pulping liquor etc.);Coal feedstock (such as:Anthracite, lignite, mud coal etc.);Plastics Class polyvinyl chloride, polypropylene, phenolic resin, furane resins, pollopas, furane resins, polytetrafluoroethylene (PTFE) etc.;Petroleum (such as:Contain carbon products and waste material in the petroleum refining process such as asphalt, petroleum coke, the oil dregs of fat).
It is preferred that raw material is crushed into 0.5-10mm, constant mass is dried at 80-120 DEG C;Further preferably raw material is broken 2mm is broken to, constant mass is dried at 105 DEG C.
The isothermal pyrolysis at 300-800 DEG C is preferably placed into heating furnace, is further preferably put into heating furnace at 500 DEG C Isothermal pyrolysis.
It is preferred that isothermal pyrolysis 10-480min, further preferred isothermal pyrolysis 25min.
It is preferred that the coke by pyrolysis is put into 200-1000 DEG C of fuse salt, further preferably by by pyrolysis Raw material is put into 400 DEG C of fuse salt.
It is preferred that being taken out after isothermal reaction 0.5-240min, taken out after further preferred isothermal reaction 2min.
It is preferred that be heated to 400-1200 DEG C under an inert atmosphere, be further preferably heated under an inert atmosphere 800 DEG C or 900℃。
It is preferred that activating 0.5-10 hours in constant temperature, further preferably 1-2 hours are activated in constant temperature.
The activated carbon prepared by the present invention is under the premise of activated carbon fine quality is ensured, using under fuse salt hot conditions Good permeability, the salt caused by during antipyretic that reduces conventional method wastes and volatilization.The method, without raw material and work Change reagent to mix in advance, time is shortened to by the 1-48 hours of conventional method within 30 minutes, significantly reduce and live Property charcoal production cycle, and then lower production cost, improve production efficiency.This technology is advantageous to promote the leather of activated carbon process Newly.
Brief description of the drawings
Accompanying drawing is the technological process of the present invention.
Embodiment
The embodiment of the present invention is further illustrated below in conjunction with technical scheme, is not intended to limit making for the present invention Use scope.
Embodiment 1
Using trade waste furfural dregs as raw material:Selection furfural dregs 100g is crushed to 1mmg and quality perseverance is dried at 120 DEG C It is fixed, the isothermal pyrolysis 25min under the conditions of 400 DEG C is put into heating furnace, coke caused by being pyrolyzed will be passed through and be put into 400 DEG C of meltings In salt, taken out after isothermal reaction 2min, be heated to 800 DEG C under an inert atmosphere and carry out 600 DEG C of constant temperature activation.It is cooled to room temperature, With 0.1mol/L hydrochloric acid solution immersion gained material, neutrality is washed to, is activated carbon by gained material drying.
Embodiment 2
Using agricultural wastes corncob as raw material:Selection corncob 100g is crushed to 1mm and quality perseverance is dried at 120 DEG C It is fixed, the isothermal pyrolysis 25min under the conditions of 350 DEG C is put into heating furnace, coke caused by being pyrolyzed will be passed through and be put into 400 DEG C of meltings In salt, taken out after isothermal reaction 2min, be heated to 700 DEG C under an inert atmosphere and carry out constant temperature activation 60min.It is cooled to room temperature, With 0.1mol/L hydrochloric acid solution immersion gained material, neutrality is washed to, is activated carbon by gained material drying.
Embodiment 3
Using coal as raw material:Selection coal 100g is crushed to 2mm and is dried to constant mass at 120 DEG C, is put into heating furnace 500 Isothermal pyrolysis 25min under the conditions of DEG C, will through coke caused by pyrolysis and be put into 400 DEG C of fuse salts, after isothermal reaction 2min Take out, be heated to 900 DEG C under an inert atmosphere and carry out constant temperature activation 60min.Room temperature is cooled to, with 0.1mol/L hydrochloric acid solution Immersion gained material, is washed to neutrality, is activated carbon by gained material drying.

Claims (5)

  1. A kind of 1. method that activated carbon is prepared using fuse salt activation, it is characterised in that step is as follows:
    Raw material is crushed, after drying, pyrolytic reaction 25min under the conditions of 500 DEG C, will be added to by coke caused by pyrolytic reaction In fuse salt, taken out after reacting 2min under the conditions of 400 DEG C, under an inert atmosphere 400-1200 DEG C of activation 0.5-10 hour;Will production Thing is cooled to room temperature, is soaked with hydrochloric acid solution, is then washed to neutrality, by gained material drying activated carbon;
    Described raw material is crushed to 0.5-10mm, is biomass material, coal feedstock, igelite, polypropylene, phenolic aldehyde tree One or both of fat, furane resins, pollopas, furane resins, polytetrafluoroethylene (PTFE), petroleum are mixed above.
  2. 2. according to the method for claim 1, it is characterised in that activate 1- at a temperature of 800 DEG C or 900 DEG C under an inert atmosphere 2 hours.
  3. 3. method according to claim 1 or 2, it is characterised in that described raw material is crushed to 2mm.
  4. 4. method according to claim 1 or 2, it is characterised in that dried under the conditions of 80-120 DEG C.
  5. 5. according to the method for claim 3, it is characterised in that dried under the conditions of 80-120 DEG C.
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CN105366658A (en) * 2015-11-13 2016-03-02 哈尔滨工程大学 Method for preparing porous carbon for super capacitor by waste plastic carbonization
CN105623687B (en) * 2016-03-02 2018-01-26 大连理工大学 A kind of fuse salt spray pyrolysis biomass joint prepares bio oil and the apparatus and method of multiporous biological charcoal
CN106865541A (en) * 2017-02-22 2017-06-20 李峰 A kind of Lauxite matrix activated carbon microballoon for coating polyacrylamide and preparation method thereof
CN106955668A (en) * 2017-04-01 2017-07-18 东北农业大学 A kind of method that fuse salt assisted with high-temperature charring prepares N doping multiporous biological charcoal
CN106865547A (en) * 2017-04-06 2017-06-20 合肥工业大学 A kind of preparation method of plastic biologic activated carbon and its activated carbon of acquisition
CN106938190A (en) * 2017-04-19 2017-07-11 东北农业大学 A kind of preparation method of the lamella multiporous biological charcoal with strong adsorption function
CN107492648B (en) * 2017-08-18 2019-12-27 湖北文理学院 Cotton-based carbon fiber/MnO/C material, preparation method and application
CN107434305B (en) * 2017-09-29 2020-10-23 福建省农业科学院农业工程技术研究所 Water purifying agent with defect-rich carbon carrier immobilized microorganisms and preparation method thereof
CN109161915B (en) * 2018-09-30 2020-07-14 东北大学 Method for preparing activated carbon powder for supercapacitor by utilizing coal based on molten salt
CN109530386B (en) * 2018-10-24 2020-05-08 华中科技大学 Method for multistage upgrading of mixed organic solid waste based on molten salt
CN111232973A (en) * 2020-03-06 2020-06-05 安徽马钢化工能源科技有限公司 Method for preparing coal tar pitch-based activated porous carbon through chloride mixture melting and alkali activation
CN111994905A (en) * 2020-08-14 2020-11-27 五邑大学 Preparation method of high-performance carbon material

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CN104085891A (en) * 2014-07-14 2014-10-08 武汉大学 Method for preparing carbon powder with high specific capacitance by using activated carbon activated by molten salt

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CN101112984A (en) * 2007-07-03 2008-01-30 四川大学 Method for preparing activated charcoal by using discarded jatropha curcas husk
CN101538039A (en) * 2009-04-17 2009-09-23 北京盖雅技术中心有限公司 Method for preparing active carbon by using side products of processing yellow ginger with catalysis-solvent method
CN101780954A (en) * 2010-01-22 2010-07-21 核工业西南勘察设计研究院有限公司 Carbon material with high surface activity and preparation method thereof
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CN104085891A (en) * 2014-07-14 2014-10-08 武汉大学 Method for preparing carbon powder with high specific capacitance by using activated carbon activated by molten salt

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