CN114702975A - Preparation method and application of two-step sulfur-doped sludge biochar - Google Patents
Preparation method and application of two-step sulfur-doped sludge biochar Download PDFInfo
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- 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
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- 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
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- 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
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/02—Multi-step carbonising or coking processes
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- 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
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
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- 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
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
- C10B57/10—Drying
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- 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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- 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 discloses a preparation method and application of two-step sulfur-doped biochar, wherein the preparation process comprises the following steps: the method comprises the steps of adopting excess sludge as a raw material, drying and crushing the excess sludge, uniformly mixing the dried excess sludge with sulfur, firstly using a high-temperature high-pressure reaction kettle to perform hydrothermal carbonization in an oven, then placing the oven in a tubular furnace, and performing N-type carbonization2Pyrolyzing in the atmosphere, taking out, crushing and sieving to obtain the sulfur-doped sludge biochar. The sulfur-doped sludge biochar prepared by the invention has a higher specific surface area and a rich pore structure, can activate persulfate PMS to generate environment-persistent free radicals (EPFRs) to efficiently degrade antibiotics in water, realizes resource utilization of excess sludge, is simple in preparation process, is green and environment-friendly, and is suitable for removing antibiotics in water treatment.
Description
Technical Field
The invention belongs to the technical field of resource utilization of excess sludge and removal of antibiotics in water, and particularly relates to a two-step sulfur-doped sludge biochar preparation method and application.
Background
Most antibiotics are discharged into sewage, and after the antibiotics enter a water body, the growth of aquatic plants is influenced, so that chronic poisoning of aquatic organisms is caused. When entering the human body through the food chain, the human body can generate drug resistance and seriously affect various physiological functions of the human body. Therefore, there is an urgent need to develop methods for removing antibiotics from the environment.
With the gradual popularization of sewage treatment facilities in China, the sludge yield is greatly increased, and the sludge treatment problem is increasingly prominent. The sludge contains a large amount of toxic and harmful substances, but also has rich organic matters, and common sludge disposal modes such as landfill and incineration not only can cause secondary pollution, but also can waste resources. It is urgent to select a proper treatment method to realize the full treatment of the sludge and the reasonable utilization of the resource.
The biochar prepared from the sludge can achieve the purposes of reduction and harmlessness, has the advantages of large specific surface area, rich surface functional groups and the like, and is often used for removing pollutants in water. By modifying the biochar by using a heteroatom doping method, Peroxymonosulfate (PMS) can be better activated, the concentration of environment-persistent free radicals (EPFRs) is increased, and the biochar has better degradation potential. Wherein the EPFRs can activate PMS to generate multiple Reactive Oxygen Species (ROS), including SO4 •-、•OH、O2 •-And1O2. Therefore, the higher the concentration of the EPFRs, the better the activation effect of PMS, so as to generate more ROS to degrade antibiotics efficiently. The method is simple to operate, low in cost and good in effect of removing the antibiotics in the water body.
Disclosure of Invention
The invention solves the technical problem of providing a two-step sulfur-doped sludge biochar preparation method, which can be used for reducing the concentration of antibiotics in a water body while realizing resource utilization of excess sludge, and greatly solves the problem of antibiotic water pollution.
The invention adopts the following technical scheme for solving the technical problems, and the two-step preparation method of the sulfur-doped sludge biochar is characterized by comprising the following specific steps of:
step S1: sludge pretreatment and sulfur doping reagent loading
Taking the excess sludge generated by mechanical dehydration and drying in a municipal sewage treatment plant, screening out obvious impurities, placing the impurities in an oven, drying for 48-72h at 80 ℃, coarsely crushing the dried sludge by using a crusher, screening by using a 100-mesh screen, adding the excess sludge into deionized water, and then adding a sulfur-doped reagent sodium thiosulfate (Na)2S2O3) Stirring for 6-8h on a magnetic stirrer at the stirring speed of 700-;
step S2: preparation of sulfur-doped sludge biochar
Will step S1, placing the sulfur-element-loaded sludge biomass in a polytetrafluoroethylene lining, adding deionized water, placing the polytetrafluoroethylene lining in a sealed high-pressure hydrothermal reaction kettle, placing the reaction kettle in an oven, heating for 2 hours at 220 ℃, placing the reaction kettle at room temperature after the reaction is finished, taking out a sample, standing, precipitating, pouring out supernatant, drying for 4-8 hours at 80 ℃ to obtain hydrothermal carbon, placing the hydrothermal carbon in a cover-type crucible, placing the crucible in a tubular furnace for pyrolysis, and injecting N by vacuumizing repeatedly three times before pyrolysis2Method (2) discharging O in the pipe2Continuous injection of N during pyrolysis2And the gas flow rate is 25-50mL/min until the reaction is finished, the pyrolysis temperature is 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃ and 900 ℃ in sequence, the temperature rise rate is controlled to be 10 ℃/min in the process, the pyrolysis time of the corresponding temperature is 2h, and finally the obtained product is crushed by using a mortar and is screened by using a 100-mesh screen to obtain the sulfur-doped sludge biochar.
Further limiting, in the step S1, the feeding ratio of the excess sludge to the deionized water is 1g to 20mL, and the feeding mass ratio of the sulfur-doped reagent sodium thiosulfate to the excess sludge is 1:1-1: 3.
Further limiting, in the step S2, the feeding ratio of the sulfur-loaded sludge biomass to the deionized water is 1g:5 mL.
The application of the sulfur-doped sludge biochar in removing antibiotics in a water body comprises the following specific processes: adding sulfur-doped sludge biochar into a water body containing antibiotics, adding persulfate PMS, and then placing the mixture into a constant-temperature oscillator for catalytic degradation of the antibiotics at a constant temperature of 25 ℃ for oscillation time.
Further limiting, the adding amount of the sulfur-doped sludge biochar is 3g/L, and the adding amount of the persulfate PMS is 5 mmol/L.
Further defined, the antibiotic is tetracycline.
And further limiting, centrifugally separating the sulfur-doped sludge biochar through a centrifugal machine after the catalytic degradation of the antibiotics is finished, and drying the separated sulfur-doped sludge biochar in a drying oven at 80 ℃ for 2-5h to realize the regeneration and cyclic utilization of the sulfur-doped sludge biochar.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention takes the excess sludge as the raw material, has low technical cost and simple preparation method, and is economic and environment-friendly. Can realize the effective utilization of the residual sludge as resources, and has good economic benefit and environmental benefit.
2. The invention adopts a two-step (hydrothermal carbon and pyrolytic carbon) biochar preparation method, has higher specific surface area and abundant pore structures, and obviously improves the capability of degrading antibiotics.
3. After the biochar is doped with sulfur elements, active point positions on the surface of the biochar are increased, EPFRs can be promoted to be generated, ROS is activated, and the biochar has stronger catalytic degradation potential.
Drawings
FIG. 1 is an SEM image of raw sludge and prepared sulfur-doped sludge biochar, wherein (a) is raw sludge and (b) is sulfur-doped sludge biochar;
FIG. 2 is a graph showing the effect of hydrothermal + pyrolytic carbon on the degradation rate of TC before and after sulfur doping at different preparation temperatures;
fig. 3 is a graph of the effect of sulfur-doped biochar on the degradation rate of TC after five cycles.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Examples
(1) Sludge pretreatment and sulfur doping reagent loading
Taking the excess sludge generated by mechanical dehydration and drying in a municipal sewage treatment plant, screening out obvious impurities, placing the impurities in an oven, drying for 48-72h at 80 ℃, coarsely crushing the dried sludge by using a crusher, screening by using a 100-mesh screen, adding the excess sludge into deionized water, and then adding a sulfur-doped reagent sodium thiosulfate (Na)2S2O3) Stirring the mixture for 6 to 8 hours on a magnetic stirrer at the stirring speed of 700-After the precipitation, pouring out the supernatant, drying the supernatant for 8 to 12 hours at the temperature of 80 ℃, and crushing the supernatant to 100 meshes to obtain the sulfur atom loaded sludge biomass.
(2) Preparation of sulfur-doped sludge biochar
Placing the sulfur-element-loaded sludge biomass obtained in the step S1 into a polytetrafluoroethylene lining, adding deionized water, placing the polytetrafluoroethylene lining into a sealed high-pressure hydrothermal reaction kettle, placing the reaction kettle into an oven, heating for 2 hours at 220 ℃, placing the reaction kettle at room temperature after the reaction is finished, taking out a sample, standing, precipitating, pouring out supernatant, drying for 4-8 hours at 80 ℃ to obtain hydrothermal carbon, placing the hydrothermal carbon into a cover-type crucible, placing the crucible into a tubular furnace for pyrolysis, and injecting N through vacuumizing and injecting for three times before pyrolysis2Method (2) discharging O in the pipe2Continuous injection of N during pyrolysis2And the gas flow rate is 25-50mL/min until the reaction is finished, the pyrolysis temperature is 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃ and 900 ℃ in sequence, the temperature rise rate is controlled to be 10 ℃/min in the process, the pyrolysis time of the corresponding temperature is 2h, and finally the obtained product is crushed by using a mortar and is screened by using a 100-mesh screen to obtain the sulfur-doped sludge biochar.
(3) Removal of tetracycline from water
Firstly, preparing 500mg/L of tetracycline solution as stock solution in a 1000mL brown flask, adding 20mL of the stock solution into a 100mL conical flask, diluting with water to 100mL, wherein the concentration of the antibiotic is 20mg/L, then adding 0.3g of the prepared sulfur-doped sludge biochar (the addition amount is 3 g/L), then rapidly adding persulfate PMS (the addition amount is 5 mmol/L), then oscillating the mixed solution in a constant temperature oscillator at 25 ℃ for 30min, after the reaction is finished, filtering a sample through a filter membrane of 0.22 mu m, then measuring the content of the antibiotic in the supernatant of the sample by using an ultraviolet spectrophotometry method, and calculating the tetracycline removal rate to be 94.81% (figure 1).
The sulfur-doped sludge biochar recycling experiment was performed as follows: and after the degradation experiment is finished, taking out the supernatant, centrifuging for 10min at 4000rpm by using a centrifuge, taking out the sulfur-doped sludge biochar, drying in an oven at 80 ℃ for 2-5h to realize the regeneration of the sulfur-doped sludge biochar, recycling the regenerated sulfur-doped sludge biochar, and catalytically degrading tetracycline in the water body, wherein the steps are repeated for 5 times, and finally the tetracycline removal rate is 81.74% (fig. 2).
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (7)
1. A two-step preparation method of sulfur-doped sludge biochar is characterized by comprising the following specific steps:
step S1: sludge pretreatment and sulfur doping reagent loading
Taking back excess sludge generated by mechanical dehydration and drying in a municipal sewage treatment plant, screening out obvious impurities, then placing the sludge in an oven to dry for 48-72h at 80 ℃, coarsely crushing the dried sludge by using a crusher, screening the sludge by using a 100-mesh screen, adding the excess sludge raw material into deionized water, then adding a sulfur-doped reagent sodium thiosulfate, placing the mixture on a magnetic stirrer to stir for 6-8h at the stirring speed of 700-900r/min, after the reaction is finished, standing the mixture for precipitation, pouring out supernatant, drying for 8-12h at 80 ℃ and crushing the mixture to 100 meshes to obtain sulfur element-loaded sludge biomass;
step S2: preparation of sulfur-doped sludge biochar
Placing the sulfur-element-loaded sludge biomass obtained in the step S1 into a polytetrafluoroethylene lining, adding deionized water, placing the polytetrafluoroethylene lining into a sealed high-pressure hydrothermal reaction kettle, placing the reaction kettle into an oven, heating for 2 hours at 220 ℃, placing the reaction kettle at room temperature after the reaction is finished, taking out a sample, standing, precipitating, pouring out supernatant, drying for 4-8 hours at 80 ℃ to obtain hydrothermal carbon, placing the hydrothermal carbon into a cover-type crucible, placing the crucible into a tubular furnace for pyrolysis, and injecting N through vacuumizing and injecting for three times before pyrolysis2Method (2) discharging O in the pipe2Continuous injection of N during pyrolysis2The gas flow rate is 25-50mL/min until the reverseAnd after finishing pyrolysis, sequentially controlling the pyrolysis temperature to be 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃ and 900 ℃, controlling the heating rate to be 10 ℃/min in the process, controlling the pyrolysis time of the corresponding temperature to be 2h, crushing the finally obtained product by using a mortar, and screening by using a 100-mesh screen to obtain the sulfur-doped sludge biochar.
2. The two-step sulfur-doped sludge biochar preparation method according to claim 1, characterized in that: in the step S1, the feeding proportion of the excess sludge and the deionized water is 1g to 20mL, and the feeding mass ratio of the sulfur-doped reagent sodium thiosulfate to the excess sludge is 1:1-1: 3.
3. The two-step sulfur-doped sludge biochar preparation method according to claim 1, characterized in that: in the step S2, the feeding proportion of the sulfur-loaded sludge biomass to the deionized water is 1g:5 mL.
4. The application of the sulfur-doped sludge biochar prepared by the method according to any one of claims 1-3 in removing antibiotics in a water body is characterized by comprising the following specific processes: adding the sulfur-doped sludge biochar into a water body containing antibiotics, adding persulfate PMS, and then placing the mixture into a constant-temperature oscillator to carry out catalytic degradation on the antibiotics at the constant temperature of 25 ℃ for oscillation time.
5. Use according to claim 4, characterized in that: the addition amount of the sulfur-doped sludge biochar is 3g/L, and the addition amount of the persulfate PMS is 5 mmol/L.
6. Use according to claim 4, characterized in that: the antibiotic is tetracycline.
7. Use according to claim 4, characterized in that: and after the catalytic degradation of the antibiotics is finished, centrifugally separating the sulfur-doped sludge biochar by using a centrifugal machine, and drying the separated sulfur-doped sludge biochar in a drying oven at 80 ℃ for 2-5h to realize the regeneration and cyclic utilization of the sulfur-doped sludge biochar.
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| CN115520864A (en) * | 2022-09-28 | 2022-12-27 | 山西大学 | Preparation method of sulfur-nitrogen in-situ doped porous carbon material |
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| CN115520864A (en) * | 2022-09-28 | 2022-12-27 | 山西大学 | Preparation method of sulfur-nitrogen in-situ doped porous carbon material |
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