CN107473222A - A kind of method and device that active sludge carbon is prepared using potassium acetate - Google Patents

A kind of method and device that active sludge carbon is prepared using potassium acetate Download PDF

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Publication number
CN107473222A
CN107473222A CN201710832065.6A CN201710832065A CN107473222A CN 107473222 A CN107473222 A CN 107473222A CN 201710832065 A CN201710832065 A CN 201710832065A CN 107473222 A CN107473222 A CN 107473222A
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sludge
semicoke
potassium acetate
carbon
hydrochloric acid
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邵敬爱
金前争
王贤华
曾阔
张�雄
张世红
陈汉平
张俊杰
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing

Abstract

The invention belongs to sewage treatment area, and in particular to a kind of method that active sludge carbon is prepared using potassium acetate, specifically include following steps：Mud granule is carried out pyrolysis processing and cooled down by S1, collects thermal decomposition product sludge semicoke；S2 carries out activation process after sludge semicoke is uniformly mixed with potassium acetate powder, the mass ratio of potassium acetate and sludge semicoke is (0.5~3)：1；Sludge semicoke is put into hydrochloric acid solution and washs and filter by S3, cleans and obtains active sludge carbon after drying, wherein, concentration of hydrochloric acid is 1~3mol/L, and the quality of sludge semicoke and the volume ratio of hydrochloric acid are 1g：(2ml~10ml).The invention also discloses a kind of heavy metal adsorption device.The present invention can improve the physico-chemical structure of active sludge carbon, be prepared activated carbon best in quality, and will not cause secondary pollution in whole technical process, while it is low, non-toxic and the advantages that be easy to manipulation high efficiency, high quality, cost to be present.

Description

A kind of method and device that active sludge carbon is prepared using potassium acetate
Technical field
The invention belongs to sewage treatment area, and in particular to a kind of method and dress that active sludge carbon is prepared using potassium acetate Put.
Background technology
Environmental pollution has had become the urgent problem to be solved that our times faces, especially heavy metal pollution Seriously affect the physical and mental health of the mankind.Heavy metal can and human body in various protein interactions and make its inactivation, gradually exist Enrichment causes human body to be poisoned in human body, causes such as minamata disease, Itai-itai diseases etc..And lead is the Heavy Metals species in industrial wastewater One of, it is mainly derived from the industry such as battery, coating, fuel oil, paint, smelting, plating, machinery, hardware, hair dye, cosmetics Production, lead mainly exist in the form of soluble state in human body, can be directly absorbed by the body.It can enter people by skin etc. Body organ, anemia, nervous function imbalance and injury of kidney etc. are caused when serious.The discharge beyond standards of heavy metal lead, drinking-water can be passed through And food chain eventually enters into human body, it is detrimental to health.
At present the processing method of heavy metal lead mainly include the precipitation method, ion-exchange, electrolysis, membrane separation technique, Biological treatment etc., but these technical costs are higher, the cycle is long, processing environment requires harsh, is difficult to reach discharge standard.And inhale Attached method is that a kind of effective method of heavy metal in water is removed using porous solid material, and cost is low, and removal efficiency is high. Sludge-based activated carbon, which has been studied confirmation, can be used as a kind of effective adsorbent, can not only solve the disposal of sludge, and Reach the purpose of recycling.Sludge is a kind of cheap material as adsorbent, can effectively remove the pollutant in the aqueous solution, especially It can solidify the heavy metal in liquid.
The preparation method of active sludge carbon is broadly divided into physically activated and chemical activation at present.The activation of physically activated use Agent is carbon dioxide, air, vapor, and the ash content of the high content contained in sludge hinders the effect of activator and charcoal skeleton, It is hardly formed the pore structure of prosperity.And conventional chemical activating agent, such as zinc chloride, sulfuric acid, phosphoric acid, sulfuric acid, potassium hydroxide. Wherein zinc chloride produces toxic gaseous hydrochlorides etc. in activation process is pyrolyzed, and the effect of sulfuric acid, phosphoric acid to sludge semicoke is smaller, Hardly result in active sludge carbon best in quality.Potassium hydroxide has good activation, can obtain the hole knot of prosperity Structure, but corrosion of the highly basic to pyrolysis plant is more serious, increases the input cost of equipment.Therefore needing to probe into a kind of can both carry The physicochemical characteristic of high active sludge carbon, cost can be reduced again, reduce the preparation method of equipment corrosion, be easy to industrialized answer With.
Due to drawbacks described above and deficiency be present, this area is needed badly to make and further improved, prepared by design one kind The method of active sludge carbon, the pollution for environment and the corrosion of equipment can be avoided, while solve existing activator Activation does not reach the problem of effect.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, sludge work is prepared using potassium acetate the invention provides a kind of Property charcoal method, sylvite activator for using has pollution environment when it is prepared for existing active sludge carbon and activated carbon produces Measure the features such as small, accordingly research and propose and activator is used as using potassium acetate prepares active sludge carbon, wherein by being used as pass The potassium acetate and mud component and proportioning of key participation thing are designed, and additionally enter the hand-manipulating of needle to the important technical parameter of subsequent technique Property is designed, can accordingly be improved the physico-chemical structure of active sludge carbon preferably with the good activity function of potassium acetate, prepared Obtain activated carbon best in quality, and secondary pollution will not be caused in whole technical process, while high efficiency, high-quality be present Amount, cost be low, non-toxic and the advantages that be easy to manipulation, is therefore particularly suitable for the application occasion of large-scale mass production.
To achieve the above object, according to one aspect of the present invention, there is provided one kind prepares sludge activity using potassium acetate The method of charcoal, it is characterised in that mainly include the following steps that：
S1 by dewatered sludge it is dry, crush and sieved, obtained mud granule will be sieved and carry out pyrolysis processing, then Cool down under an inert atmosphere, collect thermal decomposition product sludge semicoke；
S2 uniformly mixes sludge semicoke with potassium acetate powder, then is to slowly warm up to activate from room temperature under an inert atmosphere Temperature carries out activation process, wherein, the mass ratio of the potassium acetate and sludge semicoke is (0.5~3)：1；
Sludge semicoke is put into hydrochloric acid solution and washs and filter by S3, wherein, concentration of hydrochloric acid is 1~3mol/L, and sludge is partly Burnt quality and the volume ratio of hydrochloric acid are 1g：(2ml~10ml), cleaned and dried with deionized water after filtration, obtain sludge Activated carbon.
Specifically, the present invention prepares activated carbon by using potassium acetate as activator, and potassium acetate can be with sludge half Carbon reaction in Jiao, is advantageous to the reaming of active sludge carbon, improves porosity.The active principles of potassium acetate are such as：
CH3COOK+C→CO2+K2O+H2O↑
CH3COOK→K2CO3+H2O↑
K2CO3+C→K2O+H2O↑
The activation of sludge can be realized using the good activity function of potassium acetate, meanwhile, by controlling second in preparation process The ratio and concentration of the key reaction things such as sour potassium, sludge semicoke and hydrochloric acid solution, improve the physico-chemical structure of active sludge carbon, make it Possesses the pore structure of prosperity, so as to obtain heavy metal adsorption active sludge carbon of good performance.
Preferably, in the step S1, drying temperature is 105 DEG C~108 DEG C, and drying time is 24h~48h；At pyrolysis Reason is heated to 500 DEG C~700 DEG C with 20~30 DEG C/min heating rate, residence time 1h-3h.
Preferably, the collection process of the sludge semicoke in the step S1 uses circulating water.By using recirculated water Cooling, make the cooling of sludge semicoke be easy to collect, while ensure that its performance by high temperature, is not easy to subsequently carry out activation process.
Preferably, in the step S1, the screen size used when being sieved to sludge is 30~120 mesh；It is described The activator potassium acetate grind into powder that is used in step S2 simultaneously sieves, and screen size is 30~120 mesh.Mud granule and acetic acid The particle size of potassium influences it in pyrolysis and the influence of activation process, by the control of its screen size in 30~120 mesh, so as to control The particle size of mud granule and potassium acetate powder, it is heated evenly and activates during beneficial to subsequent treatment completely, it is final so as to improve The quality of activated carbon.
Preferably, the heating rate in the step S2 is 10 DEG C/min~20 DEG C/min；Activation temperature be 700 DEG C~ 850 DEG C, soak time is 1h~2h.
Preferably, the mixed liquor of sludge semicoke and hydrochloric acid is placed on gyroscope in the step S3 and carries out washup Reason, the rotating speed of the gyroscope is 100~200 turns, and rotational time is 12h~24h.
Preferably, the drying temperature in the step S3 is 105 DEG C~108 DEG C, and the time is 24h~36h.
By the way that the key parameters such as activation temperature, soak time are controlled in above range, sludge semicoke is enabled in second It can be activated under the active function of sour potassium completely, and avoid potassium acetate to cause to inactivate because of heated.
Given up it is another aspect of this invention to provide that providing the active sludge carbon prepared according to upper methods described and being applied to removing Heavy metal lead in water.
It is another aspect of this invention to provide that provide a kind of heavy metal adsorption device, it is characterised in that it includes injection Pump, adsorption tube and sampler, it is connected between the syringe pump and adsorption tube by feed tube, the other end of the adsorption tube is with taking It is connected between sample device by drain pipe, the other end of the sampler is provided with pipeline and waste liquid, the suction are obtained from waste liquid pool Attached pipe is placed with the obtained active sludge carbon of method preparation as described above as adsorbent, and the sampler is from waste liquid pool The waste liquid of extraction, heavy metal is removed after the active sludge carbon absorption in adsorption tube, is finally entered in syringe pump.
Specifically, by centering syringe pump, adsorption tube and sampler in heavy metal adsorption dress so that waste water is adsorbing Circulate in device, and the heavy metal in waste water is adsorbed by the active sludge carbon in adsorption tube, realize useless to working The processing of water.
In general, by the contemplated above technical scheme of the present invention compared with prior art, have advantages below and Beneficial effect：
(1) method that active sludge carbon is prepared using potassium acetate of the invention, it is prepared for existing active sludge carbon Shi Caiyong sylvite activator has the characteristics that to pollute environment and active carbon yield is small, accordingly researchs and proposes using potassium acetate to make Active sludge carbon is prepared for activator, wherein by being set to being used as the crucial potassium acetate for participating in thing and mud component and proportioning Meter, targeted design additionally is carried out to the important technical parameter of subsequent technique, accordingly can be good preferably with potassium acetate Activity function, improve the physico-chemical structure of active sludge carbon, activated carbon best in quality, and whole technical process be prepared In will not cause secondary pollution, while it is low, non-toxic and the advantages that be easy to manipulation high efficiency, high quality, cost to be present, thus especially It is applied to the application occasion of large-scale mass production.
(2) present invention prepares activated carbon by using potassium acetate as activator, utilizes the good reactivity of potassium acetate The activation of sludge can be realized, meanwhile, by controlling the key reactions such as potassium acetate in preparation process, sludge semicoke and hydrochloric acid solution The ratio and concentration of thing, the physico-chemical structure of active sludge carbon is improved, it is possessed the pore structure of prosperity, so as to obtain heavy metal The good active sludge carbon of absorption property.Active sludge carbon prepared by the present invention possesses the pore structure of prosperity, and contains one Quantitative functional group, such as carboxyl, carbonyl, hydroxyl, ester functional groups, be advantageous to the absorption of heavy metal cation.
(3) particle size of mud granule of the invention and potassium acetate influences it in pyrolysis and the influence of activation process, general The control of its screen size is in 30~120 mesh, so as to control the particle size of mud granule and potassium acetate powder, beneficial to subsequent treatment When be heated evenly and activate completely, so as to improve the quality of final activated carbon.Moreover, by by activation temperature, soak time etc. Key parameter is controlled in above range, enables to sludge semicoke to be activated under the active function of potassium acetate completely, and Avoid potassium acetate causes to inactivate because of heated.
(4) preparation method of the invention and adsorbent equipment are during using potassium acetate activated sludge semicoke, Bu Huizao Into secondary pollution, and it can effectively handle the heavy metal lead in waste water.And produced during active sludge carbon is prepared Fuel gas directly burn for heating, drying dewatered sludge, it is cost-effective, while reduce gas in pyrolysis and activation process again The pollution of body.
(5) preparation method of the invention is simple and easy, can not only collect the product liquid of pyrolysis sludge, reach sludge Recycling, and activated using weak base, equipment corrosion cost is reduced, improves the physico-chemical structure of active sludge carbon, is adapted to big The application scenario of scale batch production.
Brief description of the drawings
Fig. 1 is the process chart for preparing active sludge carbon method of the present invention.
Fig. 2 is the SEM figures of the active sludge carbon that potassium acetate activates in the embodiment of the present invention 1.
Fig. 3 is the FTIR figures of the active sludge carbon that potassium acetate activates in the embodiment of the present invention 1.
Fig. 4 is the adsorption curve figure of the different adsorbent heavy metals of the embodiment of the present invention 3 and 4.
Fig. 5 is the structural representation of heavy metal adsorption device of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below Conflict can is not formed each other to be mutually combined.
Preferably to explain the present invention, several specific embodiments given below：
Embodiment 1
As shown in figure 1, a kind of method that active sludge carbon is prepared using potassium acetate, it is comprised the following steps that：
Step 1, the excess sludge that will be obtained from municipal sewage plant, it is positioned in baking oven at a temperature of 105 DEG C 48h, now weight do not change, the solid particle of 120 mesh is then worn into grinder.
Step 2,10g sewage sludge solid particle is weighed, the nitrogen that 200ml/min is passed through in fixed bed is put into, using at a slow speed The method of pyrolysis, 700 DEG C, residence time 1h are warming up to from room temperature with 30 DEG C per minute of speed, then in a nitrogen atmosphere It is cooled to room temperature.
Step 3, a certain amount of potassium acetate is weighed, be ground into the solid particle of 120 mesh, then pressed with sludge semicoke (0.5-3)：1 ratio mixing, after being well mixed, is put into the nitrogen that 300ml/min is passed through in fixed bed, with 10 DEG C per minute Speed is warming up to 800 DEG C, residence time 1h, by the salt acid elution of the sludge semicoke 3mol/L after cooling, sludge semicoke Quality and the volume ratio of hydrochloric acid are 1g：10ml, the rotating speed of the gyroscope is 200 turns, Stirring 24 hours.Then spend from Sub- water cleaning is 7 up to pH value, and product is obtained into active sludge carbon in 105 DEG C of placement 36h of baking oven, drying.
Form 1 is the structural parameters of active sludge carbon in the embodiment of the present invention 1, and its parameter of pore structure is as shown in table 1.Knot Fruit shows, the potassium acetate of different proportion and the mixing of sludge semicoke, can obtain good pore structure.
Table 1
Embodiment 2
As shown in figure 1, a kind of method that active sludge carbon is prepared using potassium acetate, it is comprised the following steps that：
Step 1, the excess sludge that will be obtained from municipal sewage plant, it is positioned in baking oven at a temperature of 108 DEG C 24h, now weight do not change, the solid particle of 30 mesh is then worn into grinder.
Step 2,10g sewage sludge solid particle is weighed, the nitrogen that 200ml/min is passed through in fixed bed is put into, using at a slow speed The method of pyrolysis, 500 DEG C, residence time 3h are warming up to from room temperature with 20 DEG C per minute of speed, then in a nitrogen atmosphere It is cooled to room temperature.
Step 3, a certain amount of potassium acetate is weighed, be ground into the solid particle of 30 mesh, then press 2 with sludge semicoke： 1 ratio mixing, after being well mixed, is put into the nitrogen that 300ml/min is passed through in fixed bed, from room temperature with 20 DEG C per minute of speed Rate is warming up to 850 DEG C, residence time 2h, by the salt acid elution of the sludge semicoke 2mol/L after cooling, the matter of sludge semicoke Amount and the volume ratio of hydrochloric acid are 1g：2ml, the rotating speed of the gyroscope is 150 turns, Stirring 18 hours.Then deionization is used Water cleaning is 7 up to pH value, and product is obtained into active sludge carbon in 106 DEG C of placement 24h of baking oven, drying by product.
The pattern obtained using environmental scanning electron microscope (SEM) is as shown in Fig. 2 it can clearly be seen that abundant hole Structure；As shown in figure 3, using FTIR it is observed that activated carbon surface contains the oxygen-containing functional groups such as hydroxyl, carboxyl, aliphatic radical.
Embodiment 3
A kind of method for the solution that heavy metal lead is handled using active sludge carbon, is comprised the following steps that：
Step 1, the excess sludge that will be obtained from municipal sewage plant, it is positioned in baking oven at a temperature of 105 DEG C, Until weight does not change, the solid particle of 120-30 mesh is then worn into grinder.
Step 2,10g sewage sludge solid particle is weighed, the nitrogen that 200ml/min is passed through in fixed bed is put into, using at a slow speed The method of pyrolysis, 700 DEG C, residence time 1h are warming up to from room temperature with 10 DEG C per minute of speed, then in a nitrogen atmosphere Room temperature is cooled to, by the salt acid elution of the sludge semicoke 3mol/L after cooling, the quality of mud semicoke and the volume ratio of hydrochloric acid are 1g：2ml, the rotating speed of the gyroscope is 100 turns, Stirring 24 hours.Then with deionized water clean until pH value be 7, Product is obtained into sludge activity Jiao by product in 105 DEG C of placement 36h of baking oven, drying.
Step 3, the adsorption system reference picture 5 of use, syringe is placed on syringe pump, syringe is connected to feed tube, enters Liquid pipe is connected with adsorption tube, and the outlet of adsorption tube is connected with drain pipe, and drain pipe is ined succession sampler, and waste liquid is connected to waste liquid pool. The diameter 8mm of adsorption tube, the solution concentration of heavy metal lead is 10mg/L, and the burnt amount of sludge activity is 1.4g, is placed on adsorption tube Centre, volume flow 5ml/min.
As a result show, sludge activity Jiao's heavy metal lead has certain suction-operated, its adsorption curve such as Fig. 4 (activity It is burnt), it is 5mg/g that the burnt adsorbance of sludge activity, which is calculated,.
Embodiment 4
As shown in figure 1, a kind of method that active sludge carbon is prepared using potassium acetate, it is comprised the following steps that：
Step 1, the excess sludge that will be obtained from municipal sewage plant, it is positioned in baking oven in 106 DEG C of temperature 36h, Now weight is not changed, and the solid particle of 90 mesh is then worn into grinder.
Step 2,10g sewage sludge solid particle is weighed, the nitrogen that 200ml/min is passed through in fixed bed is put into, using at a slow speed The method of pyrolysis, 600 DEG C, residence time 2h are warming up to from room temperature with 25 DEG C per minute of speed, then in a nitrogen atmosphere It is cooled to room temperature.
Step 3, a certain amount of potassium acetate is weighed, be ground into the solid particle of 90 mesh, then press 1 with sludge semicoke: 1 mixing, after being well mixed, is put into the nitrogen that 300ml/min is passed through in fixed bed, using the method for slow pyrolysis, from room temperature with 15 DEG C per minute of speed is warming up to 700 DEG C, residence time 1.5h, by the salt pickling of the sludge semicoke 1mol/L after cooling Wash, the quality of sludge semicoke and the volume ratio of hydrochloric acid are 1g：8ml, the rotating speed of the gyroscope is 200 turns, and Stirring 12 is small When.Then cleaned with deionized water until pH value is 7, product is obtained into sludge by product in 108 DEG C of baking oven placement 24h, drying Activated carbon.
Adsorption step is the same as embodiment 1, its adsorption curve such as Fig. 4 (activated carbon), it is seen that the activated carbon tool of potassium acetate activated carbon There is preferable suction-operated, its final adsorbance is 30mg/g.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included Within protection scope of the present invention.

Claims (9)

  1. A kind of 1. method that active sludge carbon is prepared using potassium acetate, it is characterised in that mainly include the following steps that：
    S1 by dewatered sludge it is dry, crush and sieved, obtained mud granule will be sieved and carry out pyrolysis processing, then lazy Property atmosphere under cool down, collect thermal decomposition product sludge semicoke；
    S2 uniformly mixes sludge semicoke with potassium acetate powder, is then to slowly warm up to activation temperature from room temperature under an inert atmosphere Activation process is carried out, wherein, the mass ratio of the potassium acetate and sludge semicoke is (0.5~3)：1；
    Sludge semicoke is put into hydrochloric acid solution and washs and filter by S3, wherein, concentration of hydrochloric acid is 1mol/L~3mol/L, and sludge is partly Burnt quality and the volume ratio of hydrochloric acid are 1g：(2ml~10ml), cleaned and dried with deionized water after filtration, obtain sludge Activated carbon.
  2. 2. according to the method for claim 1, it is characterised in that：In the step S1, drying temperature is 105 DEG C~108 DEG C, Drying time is 24h~48h；Pyrolysis processing is heated to 500 DEG C~700 DEG C with 20 DEG C/min~30 DEG C/min heating rate, Residence time is 1h-3h.
  3. 3. method according to claim 1 or 2, it is characterised in that：The collection process of sludge semicoke in the step S1 Using circulating water.
  4. 4. according to the method for claim 3, it is characterised in that：In the step S1, used when being sieved to sludge Screen size be the mesh of 30 mesh~120；The potassium acetate grind into powder that is used in the step S2 simultaneously sieves, screen size 30 The mesh of mesh~120.
  5. 5. according to the method for claim 4, it is characterised in that：Heating rate in the step S2 is 10 DEG C/min~20 ℃/min；Activation temperature is 700 DEG C~850 DEG C, and soak time is 1h~2h.
  6. 6. according to the method for claim 5, it is characterised in that：By sludge semicoke and the mixed liquor of hydrochloric acid in the step S3 It is placed on gyroscope and carries out carrying out washing treatment, the rotating speed of the gyroscope is 100 turns~200 turns, and rotational time is 12h~24h.
  7. 7. according to the method for claim 6, it is characterised in that：Drying temperature in the step S3 is 105 DEG C~108 DEG C, the time is 24h~36h.
  8. 8. the heavy metal lead in removing waste water is applied to according to the active sludge carbon of any one of claim 1~7 preparation.
  9. A kind of 9. heavy metal adsorption device, it is characterised in that it includes syringe pump, adsorption tube and sampler, the syringe pump with It is connected between adsorption tube by feed tube, is connected between the other end and sampler of the adsorption tube by drain pipe, it is described to take The other end of sample device is provided with pipeline and waste liquid is obtained from waste liquid pool, is placed in the adsorption tube just like described in claim 1-7 The waste liquid that is extracted as adsorbent, the sampler from waste liquid pool of obtained active sludge carbon for preparing of method, through adsorbing Heavy metal is removed after active sludge carbon absorption in pipe, is finally entered in syringe pump.
CN201710832065.6A 2017-09-15 2017-09-15 A kind of method and device that active sludge carbon is prepared using potassium acetate Pending CN107473222A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116459791A (en) * 2023-04-26 2023-07-21 福建省鑫森炭业股份有限公司 Filter material based on honeycomb activated carbon and preparation method and application thereof

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CN104817379A (en) * 2015-04-20 2015-08-05 广东大众农业科技股份有限公司 Bamboo biomass charcoal based composite fertilizer and preparation method thereof
CN205556152U (en) * 2016-04-29 2016-09-07 福建中烟工业有限责任公司 A waste liquid heavy metal adsorption device for inductively coupled plasma mass spectrograph
CN105967894A (en) * 2016-06-16 2016-09-28 广东大众农业科技股份有限公司 Efficient environment-friendly nitrogen fertilizer based on biomass charcoal and production process thereof
CN106433713A (en) * 2016-11-01 2017-02-22 新疆大学 Sludge pyrolysis method adopting biomass adding
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

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Publication number Priority date Publication date Assignee Title
CN104386685A (en) * 2014-10-22 2015-03-04 北京化工大学 Method for preparing nitrogen-doped active carbon from nitrogen-enriched biomass raw material
CN104817379A (en) * 2015-04-20 2015-08-05 广东大众农业科技股份有限公司 Bamboo biomass charcoal based composite fertilizer and preparation method thereof
CN205556152U (en) * 2016-04-29 2016-09-07 福建中烟工业有限责任公司 A waste liquid heavy metal adsorption device for inductively coupled plasma mass spectrograph
CN105967894A (en) * 2016-06-16 2016-09-28 广东大众农业科技股份有限公司 Efficient environment-friendly nitrogen fertilizer based on biomass charcoal and production process thereof
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* Cited by examiner, † Cited by third party
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CN116459791A (en) * 2023-04-26 2023-07-21 福建省鑫森炭业股份有限公司 Filter material based on honeycomb activated carbon and preparation method and application thereof

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Application publication date: 20171215