CN108905965A - The method that sludge bioleaching-pyrolysis Combined Treatment prepares heavy metal absorbent - Google Patents
The method that sludge bioleaching-pyrolysis Combined Treatment prepares heavy metal absorbent Download PDFInfo
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- CN108905965A CN108905965A CN201810721696.5A CN201810721696A CN108905965A CN 108905965 A CN108905965 A CN 108905965A CN 201810721696 A CN201810721696 A CN 201810721696A CN 108905965 A CN108905965 A CN 108905965A
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- sludge
- heavy metal
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- bioleaching
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Classifications
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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
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
-
- 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
-
- 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
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses the methods that a kind of sludge bioleaching-pyrolysis Combined Treatment prepares heavy metal absorbent.（1）Using thickened sludge as bacterium source, FeSO is added4·7H2O is as energy substrate, and culture to pH is 2.0 ~ 3.0, then is added to using bacterium solution as inoculum thickened sludge culture 3 ~ 5 times, as bioleaching inoculation liquid；（2）Thickened sludge is adjusted to solid content 2% ~ 6%, above-mentioned inoculum is added, adds FeSO4·7H2O is handled 3 ~ 7 days, is separated by solid-liquid separation and dry to moisture content 10% hereinafter, being drip leaching dewatered sludge；（3）Gained sludge is crushed to 0.3 mm, the smashed organic waste of addition, is warming up to 300 ~ 700oC, isothermal pyrolysis 0.5 ~ 3 hour.The present invention is at low cost, material is from a wealth of sources, and gained composite sludge base charcoal heavy-metal residual is low, the high and heavy metal ion adsorbed capacity of iodine sorption value is high.
Description
Technical field
The present invention relates to solid waste waste resource utilization technology fields, with municipal sludge are main more particularly to one kind
Raw material, the preparation method that heavy metal absorbent is obtained using bioleaching-pyrolysis joint processing technology.
Background technique
With Chinese society rapid development of economy, the surplus sludge volume that municipal sewage treatment process generates increases severely year by year.
It is shown according to State Statistics Bureau, by 2016 bottoms, national the planned city, county add up to build up sewage treatment plant to be more than 3500, day
Sewage load is up to 1.5 billion cubic meters.5 tons of dewatered sludge (moisture content 80%) estimations are generated according to every 10,000 tons of sewage of processing,
2016 produce about 30,000,000 tons of primary sludge per year.According to national " ten, water " requirement, China's municipal sewage amount also be will be further increased, according to
Bottom China dewatered sludge yield will be increased to 5000~60,000,000 tons to 2020 for estimation.And current also a large amount of sludge is not
It is thrown aside by harmless treatment, huge environmental risk is caused to Soil Surrounding and water body environment, it would be highly desirable to carry out innoxious
It is disposed with recycling treatment.
The specific resistance to filtration technology path of mainstream mainly includes at present：It is deeply dehydrating sludge+desiccation+sanitary landfills, good
Aerobe fermentation+land use, anaerobic digestion+land use, anhydration and incineration+lime-ash landfill (or building materials utilization) etc..Due to China
It is often mixed into a certain proportion of industrial wastewater in municipal sewage, causes heavy metal concentration in part of contaminated water factory sludge relatively
Height is either utilized using land use, building materials or landfill all has potential environmental risk.Bioleaching is with sulfide or Asia
Molysite be energy substrate, the acidic environment generated during aoxidize above process substrate using thiobacillus ferrooxidans, make adsorb or
It is deposited in the heavy metal dissolution on sludge zoogloea surface, eliminates the heavy metal environmental risk of the subsequent disposition of sludge.In addition, above-mentioned
In treatment process, the dewatering of sludge significantly improves, and therefore, bioleaching pretreatment just becomes specific resistance to filtration mistake
One of important process selection in journey.
It is pyrolyzed one of the common processing method of organic solid castoff.It is under the conditions of certain temperature, organic solid waste is such as dynamic
Object excrement, timber, stalk, activated sludge etc. are placed in anoxic or anoxybiotic environment, carry out high temperature pyrolysis processing, biology can be obtained
Charcoal, pyrolysis oil and pyrolysis gas etc..Wherein, being pyrolyzed resulting charcoal has many advantages, such as that preparation cost is low, adsorption capacity is big, can be wide
The general removal of heavy metal ions in sewage and contaminated soil.Municipal sludge can also be after drying and other treatment, and directly preparation is biological
Charcoal, but products obtained therefrom has the shortcomings that heavy-metal residual is high, specific surface area is low and content of ashes is high.Therefore, it is necessary to municipal administration
Sludge is pre-processed, and is reduced its environmental risk and is improved charcoal pore structure, to become environmental-friendly absorption
Material.
For municipal sludge, currently used main preprocess method is to add other substances, passes through dilution or immobilization
Heavy metal in effect degradation sludge.As Patent No. 201310445872.4 report in use organic-inorganic antidote, drop
Heavy metal and activity in low sludge carbon compound add as number of patent application is used as the report of 201610363037.X using palygorskite
Add agent, reduces the activity of heavy metal in prepared charcoal.In contrast, directly pre-processing removal sludge by bioleaching
Heavy metal can thoroughly eliminate heavy metal hidden danger present in sludge base charcoal.Currently, there has been no use bioleaching-pyrolysis
Prepare the patent report of charcoal.In other literature, with the presence of report similar with process of the present invention, such as using pure bacterium to dirt
Mud carries out bioleaching and is modified and further prepares charcoal.But in the specific implementation process with it, there is significant by the present invention
Difference is in particular in：(1) present invention carries out bioleaching processing using resulting mixed bacterial is tamed, and the technology of can be improved is answered
With range and reduce the toxigenic capacity of strain；(2) present invention improves preparation gained sludge organism charcoal using agricultural wastes as auxiliary material
Specific surface area and heavy metal adsorption capacity.
Summary of the invention
To use mixed bacterium for drip leaching inoculum, organic waste be auxiliary material, bioleaching-the object of the present invention is to provide a kind of
It is pyrolyzed Combined Treatment municipal sludge, the method for preparing composite sludge base charcoal.
The specific steps are：
(1) 4~10g energy substrate FeSO is added into the municipal fresh sludge after 1000mL gravity concentration4·7H2O,
180r/min shaken cultivation under 25~28 DEG C of constant temperatures obtains sludge bacterium solution until sludge pH is down to setting value 2.0~3.0.
(2) sludge bacterium solution obtained by 50~200mL step (1) is taken to be added in 1000mL fresh sludge, 4~10g's of addition
FeSO4·7H2O, the 180r/min shaken cultivation under 25~28 DEG C of constant temperatures, until sludge pH be down to setting value 2.0~
3.0, it repeats the above steps 3~5 times, obtains seed sludge bacterium solution.
(3) the municipal fresh sludge moisture content after adjusting gravity concentration is 2%~6%.
(4) seed sludge bacterium solution obtained by addition 50~300mL step (2) in the sludge obtained by 1000mL step (3), then plus
Enter 4~10g energy substrate FeSO4·7H2O, temperature is 25~28 DEG C and handles 3~7 days, is then centrifuged for handling, discards supernatant liquid,
It is put into drying in freeze drier, until moisture percentage in sewage sludge is lower than 10%, dewatered sludge is soaked in as drip.
(5) by drip leaching dewatered sludge obtained by step (4), partial size is crushed to lower than 0.3mm, it is low that 100~500mL partial size is added
It is put into porcelain boat in the organic waste mixing that the pulverization process of 0.5mm is crossed, porcelain boat is put into and is passed through N2Flow is 300mL/min
Vacuum drying oven sample feeding pipe in be pyrolyzed, pyrolysis temperature program is with the rate of 10~20 DEG C/min to be warming up to 300~700
DEG C, the duration is 0.5~3 hour, and the solid product that pyrolysis terminates to obtain is composite sludge base charcoal.
The organic waste is one of rice straw, sawdust and wheat straw.
Prepared composite sludge base charcoal can apply to as heavy metal absorbent to containing heavy metal containing sewage and a huge sum of money
Belong to contaminated soil to be handled.
The present invention has significant beneficial effect：
1, carry out charcoal preparation as principle using sludge and agricultural wastes after drip leaching, at the same solve agricultural wastes with
The problem of two aspects of sludge treatment explores new approach for the resource utilization of municipal sludge.
2, the acidizing effect of used mixed bacterium bioleaching processing sludge is preferable, and sludge leaching system can be made at 3~5 days
PH is inside dropped to 3.5 or less.
3, bioleaching processing effectively removes remaining heavy metal in sludge, goes to wherein Pb, Zn, Cu, Ni, Cd and Cr
Except rate reaches 61%~90%, six heavy metal species concentration drop in sludge《Pollutant catabolic gene standard in agricultural sludge
GB4284-2018》Below defined A grades of sludge product limit value.
4, bioleaching processing and auxiliary material addition effectively improve the absorption property of sludge base charcoal.Its iodine sorption value is more not
The charcoal that the charcoal of drip leaching processing improves 116%~239%, is relatively not added with auxiliary material improves 15%~80%.
5, the adsorption capacity of composite sludge base charcoal heavy metal ion with higher, to Pb under the conditions of 25 DEG C2+、Cd2+
Adsorption capacity be 30.68,19.82mg/g, have and be applied to containing heavy metal-polluted water process and heavy-metal contaminated soil reparation
Potentiality.
Detailed description of the invention
Fig. 1 is Technology Roadmap of the invention.
Fig. 2 is that the present invention is embodiment sludge bioleaching process pH and ORP tense variation diagram；Wherein：a-pH；b-ORP.
Fig. 3 is that the present invention is 6 heavy metal species removal rate tense variation diagrams in sludge during embodiment bioleaching,
In：a-Cd；b-Cr；c-Cu；d-Ni；e-Pb；f-Zn.
Fig. 4 is the stereoscan photograph that the present invention is embodiment sludge base charcoal：A does not drip leaching processing sludge base biology
Charcoal；B, drip leaching processing gained sludge base charcoal.
Fig. 5 is the iodine sorption value and yield that the present invention is embodiment composite sludge base charcoal.
Fig. 6 be the present invention be after embodiment bioleaching sludge base charcoal to the adsorption isotherm of heavy metal ion,
In：a-Pb2+；b-Cd2+。
Specific embodiment
Embodiment：
(1) Guangxi sludge of sewage treatment plant concentration basin fresh sludge is taken, it is fresh that 500mL is added into 1000mL serum bottle
Sludge adds the FeSO of 5g4·7H2O is substrate, at 25 DEG C, 180r/min shaken cultivation, until sludge pH decline is stablized
To 2.0, sludge bacterium solution is obtained.
(2) it takes sludge bacterium solution obtained by 50mL step (1) to be added in 500mL fresh sludge, adds the FeSO of 5g4·7H2O,
At 25 DEG C, 180r/min shaken cultivation, until pH stable repeats the above steps 5 times to 2.0, obtains seed sludge bacterium solution；With
Inoculation times increase, and culture bacterium solution to the time for stablizing growth period shorten to 5 days gradually every time.
(3) fresh sludge for taking Guangxi sludge of sewage treatment plant concentration basin is adjusted to sludge solid content to 2.2%；It will
The above-mentioned fresh sludge of 300mL is put into 1000mL conical flask, and seed sludge bacterium solution obtained by 30mL step (2) is added, is separately added into
4, the FeSO of 6,8,10g4·7H2O, not add FeSO4·7H2The processing of O does 3 repetitions as control, every group of test,
It is averaged as experimental result.Two layers of gauze of conical flask used are sealed, 160r/min is placed in, shakes in 26 DEG C of constant-temperature tables
Culture is swung, measures pH (written examination pH meter, model C T-6123) and oxidation-reduction potential ORP (written examination ORP in leaching reaction group daily
Meter, model SX630) variation, until pH stable is to 2.0, ORP value stabilization, which is considered as reaction in 500mV or so, to be terminated.During culture
The moisture lost daily by evaporation is supplemented using weighing method.
(4) it takes using the FeSO for adding 6g4·7H2O carries out above-mentioned bioleaching treated sludge, and drying and dehydrating is gone forward side by side
Row pulverizes and sieves, and adds the rice straw after pulverizing and sieving as auxiliary material, carries out pyrolysis processing, the sludge after bioleaching is set
In centrifuge tube, 4000r/min is centrifuged after ten minutes, discards supernatant liquid, and excess sludge is put into freeze drier and is dried to containing
Water rate is taken out after being lower than 10%, grinds and sieves with 100 mesh sieve；Take rice straw dry to moisture content 10% hereinafter, crushing and crossing 100
Mesh.Take sieving after sludge and rice straw, wherein the percent by volume of rice straw be 10%, 20%, 30%, 40%,
50%, it takes well-mixed material 6.0g to be put into porcelain boat, porcelain boat is put into the sample feeding pipe of GWL-1200 DEG C of tube type vacuum furnace
It is pyrolyzed.Before heating, N is passed through into closed tube type vacuum furnace2Protective atmosphere (N2Flow 300mL/min), with 15 DEG C/min
Heating rate be warming up to 500 DEG C, calcining at constant temperature 2 hours.It is ground after product is cooling, and mixes concussion with the HCl of 1mol/L
10 minutes, adsorbent is then washed repeatedly with distilled water, until the pH of the aqueous solution after cleaning, close to neutrality, products therefrom is multiple
Close sludge base charcoal product.To be not added with the processing of stalk as control.
(5) characterization and heavy metal adsorption of composite sludge base charcoal：Choosing rice straw addition percent by volume is
It is tested under the conditions of 20%, the surface topography of scanning electron microscope is respectively adopted；Using iodine sorption value characterization charcoal to organic matter
Adsorption capacity, using adsorption capacity characterization charcoal to the adsorption capacity of heavy metal ion.The measurement of activated carbon-iodine adsorptive value
Using national Specification《The measurement (GB/T12496.8-1999) of wood activated charcoal test method iodine sorption value》.It weighs
Sludge base charcoal is put in the plastic centrifuge tube of 100mL after 0.1g bioleaching, at 25 DEG C, 35 DEG C, 45 DEG C, is separately added into
50mL concentration be 2,5,10,20,30,40,50,60,80,100,120,150,200,300,400,500mg/L contain Pb2+、Cd2 +Solution, adjusting pH value of solution is 5, carries out adsorption test in 200r/min constant temperature water bath shaking table, it is small that the reaction time is set as 24
When.After the completion of adsorption reaction, centrifuge tube is placed in the centrifuge high speed that revolving speed is 4000r/min and is centrifuged 5 minutes, syringe is used
Then Aspirate supernatant passes through 0.45 μm of filter membrane, sampling measures residue Pb with ICP-AES2+、Cd2+Content, calculate its absorption
It measures and adsorption capacity is obtained using Langmuir equation model, be shown in Table 1.
Table 1：Composite sludge base charcoal is to heavy metal ion Pb2+And Cd2+Adsorption capacity
Claims (2)
1. a kind of preparation method of composite sludge base charcoal, it is characterised in that the specific steps are：
（1）4 ~ 10 g energy substrate FeSO47H2O are added into the municipal fresh sludge after 1000mL gravity concentration, 25 ~
28 o180 r/min shaken cultivation under C constant temperature obtains sludge bacterium solution until sludge pH is down to setting value 2.0 ~ 3.0；
(2) 50 ~ 200 mL steps are taken（1）Gained sludge bacterium solution is added in 1000 mL fresh sludges, 4 ~ 10 g's of addition
FeSO4·7H2O, 25 ~ 28o180 r/min shaken cultivation under C constant temperature, until sludge pH be down to setting value 2.0 ~
3.0, it repeats the above steps 3 ~ 5 times, obtains seed sludge bacterium solution；
（3）Municipal fresh sludge moisture content after adjusting gravity concentration is 2% ~ 6%；
（4）In 1000mL step（3）50 ~ 300 mL steps are added in gained sludge（2）Gained seed sludge bacterium solution, add 4 ~
10 g energy substrate FeSO47H2O, temperature are 25 ~ 28oC is handled 3 ~ 7 days, is then centrifuged for handling, is discarded supernatant liquid, is put into
Dry in freeze drier, until moisture percentage in sewage sludge is lower than 10%, dewatered sludge is soaked in as drip；
（5）By step（4）Gained drip leaching dewatered sludge is crushed to partial size lower than 0.3 mm, 100 ~ 500mL partial size is added and is lower than
The organic waste mixing that the pulverization process of 0.5 mm is crossed is put into porcelain boat, and porcelain boat is put into and is passed through N2Flow is 300 mL/min
Vacuum drying oven sample feeding pipe in be pyrolyzed, pyrolysis temperature program be with 10 ~ 20oThe rate of C/min is warming up to 300 ~ 700oC,
Duration is 0.5 ~ 3 hour, and the solid product that pyrolysis terminates to obtain is composite sludge base charcoal；
The organic waste is one of rice straw, sawdust and wheat straw.
2. the application of the composite sludge base charcoal of preparation method preparation according to claim 1, it is characterised in that described multiple
Closing sludge base charcoal can apply to handle as heavy metal absorbent containing heavy metal containing sewage and heavy-metal contaminated soil.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204058A (en) * | 2019-07-05 | 2019-09-06 | 陈贞辉 | A kind of sewage treatment chemical reagent that can remove heavy metal |
| CN111410183A (en) * | 2020-03-05 | 2020-07-14 | 华南农业大学 | Sludge biochar and preparation method and application thereof |
| CN112194332A (en) * | 2020-10-26 | 2021-01-08 | 天津大学 | Bioleaching sludge recycling method based on biochar pyrolysis |
| CN112374713A (en) * | 2020-10-30 | 2021-02-19 | 桂林理工大学 | Method for conditioning sludge by two-phase folded plate flow bioleaching reactor |
| CN113636896A (en) * | 2021-08-20 | 2021-11-12 | 华电西藏能源有限公司大古水电分公司 | Method for promoting sandy aggregate dewatered sludge to be in soil by using wood processing excess material and biochar thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112374713A (en) * | 2020-10-30 | 2021-02-19 | 桂林理工大学 | Method for conditioning sludge by two-phase folded plate flow bioleaching reactor |
| CN112374713B (en) * | 2020-10-30 | 2023-09-01 | 桂林理工大学 | Method for conditioning sludge by two-phase folded plate flow bioleaching reactor |
| CN113636896A (en) * | 2021-08-20 | 2021-11-12 | 华电西藏能源有限公司大古水电分公司 | Method for promoting sandy aggregate dewatered sludge to be in soil by using wood processing excess material and biochar thereof |
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Application publication date: 20181130 |