CN112194332A - Bioleaching sludge recycling method based on biochar pyrolysis - Google Patents

Bioleaching sludge recycling method based on biochar pyrolysis Download PDF

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Publication number
CN112194332A
CN112194332A CN202011151719.7A CN202011151719A CN112194332A CN 112194332 A CN112194332 A CN 112194332A CN 202011151719 A CN202011151719 A CN 202011151719A CN 112194332 A CN112194332 A CN 112194332A
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sludge
biochar
bioleaching
pyrolysis
drying
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奥琪勒
赵林
汪伶俐
王啸
于丽丽
吕文龙
廖漓文
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Sinomine Rock And Mineral Analysis (tianjin) Co ltd
Tianjin University
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Sinomine Rock And Mineral Analysis (tianjin) Co ltd
Tianjin University
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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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/06—Sludge reduction, e.g. by lysis
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention discloses a bioleaching sludge recycling method based on biochar pyrolysis, which comprises the following steps: adding an energy substrate FeSO4 & 7H2O into the sludge, performing shake culture at 25-30 ℃ and 180rpm until the pH value of the sludge is reduced and stabilized to 2.0-3.0, adding the bacterial liquid serving as an inoculum into a 9K liquid culture medium, and repeating the process for 3-5 times to obtain enriched bacterial liquid. The bioleaching dried sludge and the rice straw are crushed and sieved to be mixed in proportion, and then the mixture is put into a muffle furnace, the temperature rise rate is set to be 15 ℃/min, the final temperature is 500 ℃, and the mixture stays for 2 hours. The modified sludge-based biochar is obtained by operations of water washing, filtering, freeze-drying, drying and the like after modification by HNO 3. Adjusting the solid content of the sludge to be 4-8%, and adding 5-10g/L of prepared modified sludge-based biochar to perform bioleaching reaction. The invention realizes resource utilization of the sludge and the agricultural wastes, efficiently removes heavy metals in the sludge at lower economic cost and time cost, and reduces the loss of nutrient substances such as total nitrogen, total phosphorus and the like.

Description

Bioleaching sludge recycling method based on biochar pyrolysis
Technical Field
The invention relates to the technical field of solid waste resource utilization, in particular to a bioleaching sludge resource method based on biochar pyrolysis.
Background
The growing population, the continuous expansion of urbanization and the improvement of living standard worldwide are continuously causing large-scale environmental pollution. Government's heavily subsidized policies and abundant energy supplies naturally also contribute to the habit of wasting and inattenting protection, thereby consuming large amounts of materials and energy, producing large amounts of waste pollutants, including sewage sludge. The sludge is rich in plant nutrients such as organic matters, nitrogen, phosphorus, potassium and the like, is beneficial to the growth and development of plants, and can change the physical and chemical properties and biological characteristics of soil. The types and the concentrations of heavy metals in the sludge are different due to different sources and different proportions of domestic wastewater and industrial wastewater, wherein the heavy metals such as Cd, Cr, Cu, Hg, Ni, Pb, Zn and the like have higher contents. Due to the ubiquitous heavy metal in the sludge and the harm to the human health, if the sludge is directly used for improving the soil without being treated, the content of the heavy metal in the soil exceeds the standard, and the growth quality of plants is reduced. Therefore, it is necessary to study heavy metals commonly found in sludge.
At present, various technologies for passivating heavy metals in sludge have been researched, including chemical precipitation, filtration, ion exchange, electrochemical treatment, activated carbon adsorption, membrane technology and the like, but all the technologies have the problems of high treatment cost, difficult operation, difficult application in practice and the like. Bioleaching is mainly used for dissolving heavy metals in sludge into a liquid phase to remove the heavy metals in the sludge through the direct or indirect action of specific microorganisms in the nature. Compared with physical and chemical processes, the bioleaching is environment-friendly, can create good conditions for subsequent resource utilization, and is a new sludge treatment technology with great engineering application value
The sludge generally contains 30-50% of organic matters, so that the sludge can be carbonized through pyrolysis to prepare biochar which is used as an adsorption material. The biological carbon prepared by pyrolyzing the sludge can realize the reduction and the harmlessness of the sludge and can recycle biological oil and biogas with utilization value. Therefore, the preparation of the biochar by pyrolyzing the sludge has obvious economic and environmental benefits, and becomes one of the research hotspots for resource utilization of the sludge in recent years. However, due to the low carbon content and high ash content of the sludge, the biochar prepared by the independent pyrolysis of the sludge has poor performance, agricultural and forestry wastes such as straws, wood chips and the like mainly comprise cellulose, hemicellulose and lignin, the carbon content is high, the ash content is low, the biochar is an excellent material for preparing the biochar, and the prepared biochar has developed pores, large specific surface area and strong adsorption capacity. The straw, the wood chips and the like are added in the sludge pyrolysis process, so that the thermal conversion of the sludge can be promoted, and the biochar performance of the sludge can be improved. The biochar has redox characteristics and can reversibly store and release electrons, so that the biochar has the capability of transferring electrons, and is a potential electron shuttle material.
The sludge is a complex buffer system, the higher the concentration of the sludge is, the better the pH buffer performance is, so the pH reduction speed in the bioleaching process is limited, and the leaching effect of heavy metals in the sludge is influenced. According to the invention, the solid concentration with larger sludge buffering capacity is selected, and the leached dried sludge and the agricultural wastes are subjected to co-pyrolysis to obtain the biochar so as to promote the electron transfer rate in the reaction process.
Disclosure of Invention
The invention aims to provide a bioleaching sludge recycling method based on biochar pyrolysis.
A bioleaching sludge recycling method based on biochar pyrolysis comprises the following specific steps:
(1) the concentrated/dewatered sludge of sewage treatment plant is taken, and the solid content is adjusted to 2-6%.
(2) Adding 10-30g/L energy substrate FeSO into the sludge obtained in the step (1)4·7H2And O, performing shake culture at the temperature of 25-30 ℃ and under the condition of 180rpm until the pH value of the sludge is reduced and stabilized to 2.0-3.0, and obtaining the domesticated sludge.
(3) And (3) inoculating 5-15% of the domesticated sludge mixed liquor in the step (2) into a sterilized 9K liquid culture medium, and repeating the process for 3-5 times to obtain enriched bacterial liquid.
(4) And (3) adding 5-15% of the enriched bacterial liquid obtained in the step (3) into the sludge obtained in the step (1), and performing bioleaching under the same reaction condition as the step (2). And after the reaction is finished, centrifuging a proper amount of sludge, removing supernatant, and freeze-drying the precipitate to obtain dried sludge through a 100-mesh standard sieve.
(5) And (3) taking rice straws, drying, crushing and sieving, mixing with the dried sludge obtained in the step (4) according to the proportion of 20-60%, filling the mixture in a ceramic crucible, putting the mixture in a muffle furnace, setting the heating rate to be 10-20 ℃/min and the final temperature to be 500 ℃, and staying for 2 hours after reaching the final pyrolysis temperature.
(6) Adding 5-10% (m/V) 65% HNO into the burnt sludge-based biochar3Heating and stirring for modification, then pouring into a beaker, adding ultrapure water, carrying out magnetic stirring cleaning and filtering, and repeating the steps for a plurality of times until the pH value of the filtrate is unchanged and is nearly neutral. And (3) drying the cleaned sludge-based biochar in a freeze dryer until the water content is lower than 10%, taking out the dried sludge-based biochar, drying the dried sludge-based biochar in a drying oven at 105 ℃ to remove residual water, crushing the dried sludge-based biochar, and screening the crushed sludge-based biochar through a 100-mesh standard screen to obtain the modified sludge-based biochar.
(7) Adjusting the solid content of the sludge to be 4-8%, adding 5-10g/L of prepared modified sludge-based biochar, and carrying out bioleaching reaction under the same conditions as the step (4).
The prepared modified activated carbon can be used as an electronic shuttle in the heavy metal reaction process of bioleaching sludge to accelerate the leaching rate of heavy metals.
Compared with the prior art, the invention has the beneficial effects that:
(1) the sludge and the agricultural wastes after bioleaching are adopted as raw materials of the biochar, and a solution is provided for recycling the sludge and the wastes.
(2) The invention realizes the harmlessness and reclamation of the sludge, and efficiently removes the heavy metals in the sludge at lower economic cost and time cost.
(3) The heavy metals in the sludge are effectively removed through bioleaching treatment, the removal rate of Zn, Ni, Cd and the like reaches 77-95%, and the concentration of the heavy metals is reduced to be below the limit value of A-grade sludge products specified in the pollutant control standard GB4284-2018 in agricultural sludge.
(4) Compared with a control group which is not added, the addition of the modified sludge-based biochar can reduce total phosphorus, and the loss amount of the total phosphorus is 13.0 percent and 10.4 percent.
Drawings
Fig. 1 is a technical route diagram of the present invention.
FIG. 2 is a graph showing the removal rate of 3 heavy metals in sludge in the bioleaching process according to the embodiment of the invention.
Fig. 3 is a bar graph of total nitrogen and total phosphorus changes during bioleaching according to the embodiment of the invention.
Detailed Description
(1) Basic information of sludge
In the implementation, mechanically dewatered sludge of a certain sludge treatment plant in Tianjin is selected as bioleaching sludge, and the basic characteristics of the sludge are shown in Table 1.
Figure BDA0002741815070000031
(2) Preparation of bacterial liquid
Sludge domestication: adjusting the solid content of the sludge in the step (1) to 2% by using ultrapure water, adding 300mL of sludge mixed solution into a 500mL beaker, and adding 20g/L of FeSO4·7H2And O, performing shake culture at 28 ℃ and 180rpm for 7 days until the pH value of the sludge is reduced and stabilized to about 2.5 or the ORP value is increased and stabilized to about 500 mV.
Enrichment culture: and (3) inoculating the acclimatized sludge mixed solution into a sterilized 9K liquid culture medium according to the inoculation proportion (volume ratio) of 10%, and performing shake culture at the temperature of 28 ℃ at 180r/min for several days until the ORP value rises stably to about 500 mV. Repeating the steps for 3 times again to finally obtain fourth generation bacterial liquid, wherein the fourth generation bacterial liquid takes thiobacillus ferrooxidans as dominant bacteria.
The sterilized 9K culture medium is formed by mixing A liquid and B liquid. A liquid component: (NH)4)2SO4，3g/L；KCl0.1g/L；K2HPO4，0.5g/L；MgSO4.7H2O，0.5g/L；Ca(NO3)20.01 g/L; 800mL of ultrapure water. Through (1+3) H2SO4Adjusting pH of the liquid A to 2.0-2.2, and sterilizing at 121 deg.C for 20min in autoclave. B, liquid component: FeSO4·7H2O, 44.72 g/L; 200mL of ultrapure water. Through (1+3) H2SO4Adjusting pH of liquid B to 2.0-2.2, sterilizing with 0.22 μm filter membrane, and mixing with liquid A.
(3) Preparation of sludge-based biochar
Adjusting the solid content of the sludge in the step (1) to 4% by using ultrapure water, putting 180mL of the sludge into a 250mL conical flask, adding 20mL of fourth generation enrichment culture bacterial liquid according to the inoculation proportion of 10%, and adding FeSO with the concentration of 20g/L4·7H2And O. And measuring the change of pH (a pen test pH meter, a lightning magnet E-301-F) and oxidation-reduction potential ORP (a pen test ORP meter, a lightning magnet 501) in the leaching reaction group every 24h until the pH value is stabilized to about 2.5, and the ORP value stabilized to about 500mV is considered as the end of the reaction.
And (3) centrifuging the sludge subjected to bioleaching treatment for 30min at the rotating speed of 4200rpm in a 500mL polytetrafluoroethylene bottle, discarding the supernatant, drying the centrifuged precipitate in a freeze dryer, grinding the dried precipitate by using an agate mortar and sieving the dried precipitate by using a 100-mesh standard sieve.
Rice straw is dried until the water content is lower than 10%, crushed and sieved by a 100-mesh standard sieve. Mixing the dried bioleaching sludge and the rice straws according to the mass ratio of 1:1, filling the mixture in a ceramic crucible, wrapping the ceramic crucible by three layers of tin foil paper, putting the ceramic crucible into a muffle furnace, setting the temperature rise rate to be 15 ℃/min and the final temperature to be 500 ℃, standing for 2 hours after the final pyrolysis temperature is reached, then turning off a power supply, and taking out the mixture after the temperature is reduced to the room temperature.
Weighing the fired sludge-based biochar in a 1000mL beaker, adding 5% (m/V) 65% HNO3The modification was carried out by stirring at 90 ℃ for 5 h.
And pouring the modified sludge-based biochar into a 1000mL beaker, adding 600mL of ultrapure water, magnetically stirring and cleaning at the rotating speed of 300rpm for 3h, filtering, and repeating the step for a plurality of times until the pH value of the filtrate is unchanged and is nearly neutral. And (3) putting the cleaned sludge-based biochar into a freeze dryer for drying until the water content is lower than 10%, taking out the biochar, putting the biochar into a drying oven for drying at 105 ℃ to remove residual water, crushing and sieving by a 100-mesh standard sieve.
(4) Modified sludge-based biochar-mediated bioleaching of sludge
Adjusting the solid content of the sludge in the step (1) to 4% by using ultrapure water, putting 180mL of the sludge into a 250mL conical flask, adding 20mL of fourth generation enrichment culture bacterial liquid according to the inoculation proportion of 10%, adding 20g/L FeSO4 & 7H2O and 5g/L modified sludge-based organisms, taking the treatment without addition as a control, repeating the experiments in each group for 3 times, and taking the average value as the experiment result. Sealing the conical bottle by using a sterile air-permeable sealing film, placing the conical bottle in a constant-temperature shaking table at 28 ℃ at 180r/min for shake culture, measuring the change of pH and oxidation-reduction potential ORP in a leaching reaction group every 24h until the pH value is stabilized to about 2.5, and determining that the reaction is finished when the ORP value is stabilized to about 500mV, and adopting 6mL of sludge mixed liquor for measuring the content of heavy metals (Zn, Ni and Cd) in the leaching solution, and 4mL of sludge mixed liquor for measuring the capillary water absorption time (CST) of the sludge. During the sludge culture, the water lost due to evaporation every day is supplemented by a weighing method.
(5) Heavy metal, total nitrogen and total phosphorus determination results:
the collected 6mL sludge mixed solution was put into a 50mL centrifuge tube, centrifuged at 4200rpm for 30min, and the supernatant was passed through 0.45 μm and then applied to ICP-OES (Thermo Scientific) using inductively coupled plasma emission spectrometerTMiCAPTM7200) And measuring Zn, Ni and Cd. The removal rates of heavy metals in each group were measured as shown in FIG. 2. The leaching of the control group is stable on the 10 th day, and the adding of the modified sludge-based biochar treatment group can greatly improve the reaction in the early stage of the reactionAt this rate, the stabilization could be achieved earlier on day 8.
The sludge solid total nitrogen is measured by alkaline potassium persulfate digestion ultraviolet spectrophotometry, and the total phosphorus is measured by molybdenum-antimony anti-spectrophotometry after sodium hydroxide is melted. Through determination, compared with a control group which is not added, the total phosphorus can be reduced by 13.0 percent and 10.4 percent by adding the modified sludge-based biochar.

Claims (4)

1. A bioleaching sludge recycling method based on biochar pyrolysis is characterized by comprising the following specific steps:
(1) adjusting the solid content of the sludge to 2-6%, and adding 10-30g/L of energy substrate FeSO4·7H2Performing shake culture at 25-30 ℃ until the pH value of the sludge is reduced and stabilized to 2.0-3.0 to obtain domesticated sludge;
(2) inoculating 5% -15% of the domesticated sludge mixed liquor in the step (1) into a sterilized 9K liquid culture medium, and repeating the process for 3-5 times to obtain enriched bacterial liquid;
(3) preparing modified sludge-based biochar, namely crushing and sieving bioleaching dried sludge and rice straw, mixing the crushed and sieved sludge and the rice straw according to a ratio of 20-60%, putting the mixture into a muffle furnace, setting a temperature rise rate of 15 ℃/min and a final temperature of 500 ℃, and staying for 2 hours; by HNO3And after modification, washing, filtering, freeze-drying and drying to obtain the modified sludge-based biochar.
2. The bioleaching sludge recycling method based on biochar pyrolysis as claimed in claim 1, characterized in that HNO is added3The mass fraction is 65%, the solid-to-liquid ratio is 5% -10%, the heating and stirring are carried out for 2-6h, the pH of the filtrate is stabilized after the modification through multiple times of water washing, and the filtrate is subjected to freeze drying and then passes through a 100-mesh standard sieve to obtain the modified sludge-based biochar.
3. The method for recycling bioleaching sludge based on biochar pyrolysis as claimed in claim 1, wherein the solid content of the sludge is adjusted to 4% -8%, 5-10g/L of modified sludge-based biochar and 10-30g/L of energy substrate FeSO are added4·7H2Inoculating 10-20% of the inoculation ratio to the bacterial liquid, and oscillating for 4-16 days at 25-30 ℃ and 180rpm to finish the bioleaching reaction.
4. The method for recycling bioleaching sludge based on biochar pyrolysis as claimed in claim 1, wherein the prepared modified sludge-based biochar can be used as an electron shuttle in the reaction process to accelerate the leaching rate of heavy metals.
CN202011151719.7A 2020-10-26 2020-10-26 Bioleaching sludge recycling method based on biochar pyrolysis Pending CN112194332A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
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US20160230193A1 (en) * 2015-02-06 2016-08-11 Anaergia Inc. Solid waste treatment with conversion to gas and anaerobic digestion
CN108905965A (en) * 2018-07-04 2018-11-30 桂林理工大学 The method that sludge bioleaching-pyrolysis Combined Treatment prepares heavy metal absorbent

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Application publication date: 20210108