CN114797811A - MoS applied to tetracycline removal in water 2 Preparation method of hydrothermal activated sludge biochar - Google Patents
MoS applied to tetracycline removal in water 2 Preparation method of hydrothermal activated sludge biochar Download PDFInfo
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- CN114797811A CN114797811A CN202210405474.9A CN202210405474A CN114797811A CN 114797811 A CN114797811 A CN 114797811A CN 202210405474 A CN202210405474 A CN 202210405474A CN 114797811 A CN114797811 A CN 114797811A
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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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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
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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
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Abstract
The invention discloses a MoS for removing tetracycline in water 2 A preparation method of hydrothermal activated sludge biochar specifically comprises the step of placing Sludge Biochar (SBC) prepared by tubular furnace pyrolysis in a reactor containing sodium molybdate (NaMoO) 4 ·2H 2 O), thioacetamide (CH) 3 CSNH 2 ) And polyethylene glycol (PEG10000) solution in a reaction kettle, and performing hydrothermal activation to prepare MoS 2 Hydrothermal activated sludge biochar (MoS) 2 -SBC). The biochar prepared by the method has excellent physicochemical properties, and can realize high tetracycline content in waterThe maximum adsorption capacity of the tetracycline can reach 461.40mg/g when the reaction temperature is 35 ℃.
Description
Technical Field
The invention relates to the technical field of biochar preparation and water treatment, in particular to MoS applied to tetracycline removal in water 2 Hydrothermal activated sludge organismsA method for preparing charcoal.
Background
The tetracycline has good treatment effect on diseases of human bodies and animals and poultry as an antibiotic medicament. After the tetracycline enters into organisms, except that 10% -20% of the tetracycline can be absorbed by human or animals, the rest tetracycline is finally discharged into the water environment in the mode of excrement and urine. Tetracycline has a long half-life, and tetracycline entering the environment is not easily degraded and accumulated continuously, so that the propagation of drug-resistant bacteria and antibiotic resistance genes can be caused, and finally, the safety of an ecological system and the health of human beings are directly or indirectly threatened. Therefore, it is important to find a suitable method for removing tetracycline.
At present, the removal method of the tetracycline antibiotic-containing wastewater mainly comprises an advanced oxidation method, an electrochemical degradation method, an adsorption method, a microbial degradation method and the like. Advanced oxidation processes and electrochemical degradation have limited the large-scale application of such processes due to their high energy consumption, stringent and complex operating conditions and the production of toxic intermediates. The long period required for microbial degradation may result in drug resistance genes, which is not favorable for large-scale application. The adsorption is a removal method with great potential for pollutants in the environment due to the characteristics of simplicity, high efficiency, economy, sustainability and the like. Biochar is a carbon-rich material formed by thermochemical reaction of agricultural or industrial waste under oxygen-limited conditions, and has a certain surface area, porosity and functional groups. Sludge is the main solid waste generated by sewage plants, and is a complex heterogeneous body consisting of organic matters, dead bacterial cells, inorganic salts and the like. In recent years, with the advancement of urbanization, the number of domestic sewage treatment plants is increased sharply, and researches show that the annual output of sludge in China is 3000 ten thousand tons, and the annual output of sludge is increased year by year at the increasing rate of 8-10% per year, so that the treatment of sludge becomes a serious environmental problem. Researches show that organic compounds, pathogenic microorganisms and potential toxic elements in the sludge have risks of polluting the environment and threatening human dangers, and the current sludge treatment modes mainly include landfill and incineration, which can cause underground water and atmospheric pollution and are not consistent with sustainable developmentAnd (4) a exhibition principle. The high organic matter content of the municipal sludge makes the municipal sludge have the potential to become a good raw material for preparing the biochar, and the resource utilization of the biochar can be realized. Research shows that the sludge biochar has certain adsorption capacity on organic matters (norfloxacin, imidacloprid and the like) and inorganic matters (nickel and the like) in water, but the practical and large-scale application of the sludge biochar is limited by the limited adsorption capacity. The hydrothermal activation method is completed by placing the biochar and the active agent in a closed environment under the conditions of autogenous pressure and certain temperature, and can better ensure the activation effect of the active agent on the biochar. Based on molybdenum disulfide (MoS) 2 ) And the invention is used for modifying the sludge biochar without being combined with the activation of the sludge biochar. In addition, after the modified sludge biochar adsorbs tetracycline, how to realize efficient regeneration has important research value and significance for realizing the sustainable removal of the tetracycline in water.
Disclosure of Invention
Based on the defects of the prior art, the technical problem solved by the invention is to provide the MoS with good treatment effect and applied to removing tetracycline in water 2 Preparation method of hydrothermal activated sludge biochar, MoS applied to tetracycline removal in water 2 The preparation method of the hydrothermal activated sludge biochar can effectively and reasonably utilize waste gas containing chemical components and reach the standard of safe discharge.
In order to solve the technical problems, the invention provides mos for removing tetracycline in water 2 The preparation method of the hydrothermal activated sludge biochar comprises the following steps:
(1) preparing sludge biochar: cleaning municipal sludge with ultrapure water, drying to constant weight, pyrolyzing, grinding and sieving to obtain sludge biochar SBC;
(2)MoS 2 preparing the hydrothermal activated sludge biochar: placing the sludge biochar SBC obtained in the step (1) into a reactor containing sodium molybdate (NaMoO) 4 ·2H 2 O), thioacetamide (CH) 3 CSNH 2 ) And polyethylene glycol (PEG10000) solution in a reaction kettle, performing hydrothermal activation, washing with ultrapure water, drying, grinding and sieving to obtain MoS 2 Water heating activityModified sludge biochar MoS 2 -SBC。
As the optimization of the technical scheme, the MoS applied to removing tetracycline in water provided by the invention 2 The preparation method of the hydrothermal activated sludge biochar further comprises part or all of the following technical characteristics:
as an improvement of the technical scheme, in the step (1), the drying temperature is 70-105 ℃; the pyrolysis condition is that the nitrogen flow rate is 0.3-0.6L/min, the heating rate is 5-20 ℃/min, and the pyrolysis is continued for 60-120min at the temperature of 400-; grinding, and sieving with 60-200 mesh sieve.
As an improvement of the technical scheme, in the step (2), the sodium molybdate (NaMoO) 4 ·2H 2 O), thioacetamide (CH) 3 CSNH 2 ) SBC, ultrapure water and polyethylene glycol (PEG10000) in the following proportions: 2.3-6.9 g: 4.6-13.8 g: 1-3 g: 40-80 mL: 0.0176g-1.762 g; wherein the concentration of polyethylene glycol (PEG10000) is 0.1-0.5 mol/L; the hydrothermal activation conditions are as follows: the temperature of the air drying box is 160-220 ℃, and the activation time is 720-1440 min; drying at 70-105 deg.C, grinding, and sieving with 60-200 mesh sieve.
Mos applied to removing tetracycline in water 2 Hydrothermally activated sludge biochar, said mos 2 The hydrothermal activated sludge biochar is prepared by any method.
As the optimization of the technical scheme, the MoS applied to removing tetracycline in water provided by the invention 2 The hydrothermal activated sludge biochar further comprises part or all of the following technical characteristics:
as an improvement of the above solution, said mos 2 Hydrothermal activated sludge biochar MoS 2 The removal rate of tetracycline with the concentration of 20mg/L reaches more than 90% when the SBC dose is 0.2 g/L; at a concentration of 200mg/L and a reaction temperature of 35 ℃ in mos 2 Hydrothermal activated sludge biochar MoS 2 The maximum adsorption capacity of SBC to tetracycline can reach 461.40 mg/g; the MoS 2 Hydrothermal activated sludge biochar MoS 2 Maintenance of MoS by NaOH regeneration treatment of SBC 2 SBC reaches more than 83% of initial use in subsequent cycle use。
Preferably, the regeneration treatment process of the NaOH is to reach the adsorption equilibrium of MoS 2 SBC is subjected to filtration separation and regeneration treatment with absolute ethanol and 0.1mol/L NaOH for 20 min.
Mos for use in removal of tetracycline from water as described in any of the above 2 Application of hydrothermal activated sludge biochar, namely SBC and MoS 2 Hydrothermal activated sludge biochar MoS 2 Adding SBC as an adsorbent into an aqueous solution containing tetracycline, and filtering after the adsorption process reaches equilibrium to obtain a solution after tetracycline removal.
As the optimization of the technical scheme, the mos applied to removing tetracycline in water provided by the invention 2 The application of the hydrothermal activated sludge biochar further comprises part or all of the following technical characteristics:
as an improvement of the technical scheme, the concentration of the tetracycline in the tetracycline-containing solution is 20-200mg/L, pH and is 3-11; the dosage of the adsorbent is 0.1-0.3 g/L.
As an improvement of the technical scheme, the temperature in the adsorption process is controlled to be 15-35 ℃.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: provides the utilization of MoS 2 The method for efficiently removing tetracycline in water by using the hydrothermal activated sludge biochar as the adsorbent can effectively reduce environmental pollution caused by tetracycline and realize resource utilization of municipal sludge.
(1) MoS of the invention 2 SBC has a strong tetracycline removal capacity and a MoS dose of 0.2g/L 2 The SBC has a tetracycline removal rate of more than 90% at a concentration of 20 mg/L. At a concentration of 200mg/L and a reaction temperature of 35 ℃, MoS 2 The maximum adsorption capacity of SBC to tetracycline can reach 461.40 mg/g.
(2) Compared with other technologies (photocatalysis, advanced oxidation, microbial degradation and the like), the MoS adopted by the invention 2 The method for removing tetracycline in water by using the hydrothermal activated sludge biochar as the adsorbent has the advantages of low cost, simple operation, environmental protection and large-scale applicationThe application prospect.
(3) MoS prepared by the invention 2 The hydrothermal activated sludge biochar can realize the resource utilization of municipal sludge, can efficiently remove tetracycline in water, and has low use cost.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the contents of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below.
FIG. 1(a) is a MoS dose of 0.2g/L 2 SBC removal of 20mg/L tetracycline at 0-1440 min;
FIG. 1(b) shows MoS 2 -the relationship between the concentration of tetracycline, the reaction temperature and its adsorption capacity when SBC is used as adsorbent;
FIG. 2(a) shows MoS 2 SBC adsorption capacity for 20mg/L tetracycline as a function of solution pH;
FIG. 2(b) shows the concentration of NaCl at 1-100mmol/L vs. MoS 2 -effect of SBC adsorption capacity to tetracycline at 20 mg/L;
FIG. 2(c) shows CaCl at a concentration of 1-100mmol/L 2 To MoS 2 The effect of the ability of SBC to adsorb tetracycline at a concentration of 20 mg/L;
FIG. 2(d) shows the concentration of humic acid to MoS of 1-10mg/L 2 -effect of SBC adsorption capacity to tetracycline at 20 mg/L;
FIG. 3(a) shows MoS 2 The ability of SBC to regenerate tetracycline.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention.
Example one: the municipal sludge is dried in an oven at 105 ℃ to constant weight and then transferred into a high temperature tube furnace (N) 2 The flow rate is 0.5L/min, the heating rate is 10 ℃/min) and the sludge is pyrolyzed for 120min at the temperature of 600 ℃, and the sludge is ground and sieved by a 100-mesh sieve to obtain the sludge biochar SBC. SBC (1.0 g by mass) was transferred to ultrapure water having a volume of 60mL and dissolved therein 2.3g of sodium molybdate (NaMoO) 4 ·2H 2 O), 4.6g thioacetamide (CH) 3 CSNH 2 ) And 0.1mol/L polyethylene glycol (PEG10000) in a reaction kettle, performing hydrothermal activation at 180 ℃ for 1440min, drying in a 70 ℃ oven to constant weight, grinding and sieving with a 100-mesh sieve to obtain MoS 2 Hydrothermal activated sludge biochar MoS 2 -SBC。
Example two: 0.2g/L of MoS 2 SBC was added to a tetracycline solution of 100mL volume and 20mg/L concentration, and adsorption experiments were performed in a constant temperature shaking chamber (160rpm) at 25 deg.C, samples were taken at a set time (0-1440min), and the residual concentration of tetracycline was measured at λ -360 nm using an ultraviolet spectrophotometer to calculate its tetracycline removal rate at different times.
As shown in FIG. 1(a), MoS 2 SBC can realize the quick and efficient removal of tetracycline, and the removal rate of tetracycline at 1440min can reach 90.12%.
Example three: the MoS dosage is 0.2g/L 2 SBC was added to tetracycline solutions of 100mL volume and 20, 40, 80, 100, 120, 160 and 200mg/L concentration, respectively, and then placed in constant temperature shaking chambers (160rpm/min) at 15 deg.C, 25 deg.C and 35 deg.C, respectively, and the residual concentration of tetracycline was measured at λ 360nm using an ultraviolet spectrophotometer at the time of reaction equilibrium.
As shown in FIG. 1(b), MoS 2 The adsorption capacity of SBC for tetracycline increases with increasing tetracycline concentration and reaction temperature. The maximum adsorption capacity of the tetracycline adsorbent at 35 ℃ can reach 461.40 mg/g.
Example four: the MoS dosage is 0.2g/L 2 SBC was added to a tetracycline solution of 20mg/L and pH 3, 5, 7, 9, 11 (pH adjusted with 0.1mol/L HCl/NaOH) in a volume of 100mL, and placed in a 25 ℃ incubator (160rpm)Performing an adsorption experiment, measuring the residual concentration of tetracycline at the position of lambda being 360nm by using an ultraviolet spectrophotometer when the adsorption is balanced, and exploring MoS under different pH conditions 2 Adsorption capacity of SBC for tetracycline.
As is clear from FIG. 2(a), MoS was observed when the pH of the solution was 5 2 SBC has the greatest adsorption capacity for tetracycline (94.28 mg/g). When the pH of the solution is>5 hour, MoS 2 The adsorption capacity of SBC to tetracycline is significantly inhibited.
Example five: the MoS dosage is 0.2g/L 2 SBC was added in a volume of 100mL, a concentration of 20mg/L and a concentration of NaCl (1-100mmol/L) and CaCl, respectively 2 Placing (1-100mmol/L) and humic acid (1-10mg/L) in tetracycline solution, placing in a constant temperature shaking box (160rpm) at 25 deg.C for adsorption experiment, measuring tetracycline residual concentration at lambda of 360nm with ultraviolet spectrophotometer when adsorption is balanced, and evaluating MoS by coexisting inorganic ions and organic matters 2 The effect of the ability of SBCs to adsorb tetracycline.
As is clear from FIGS. 2(b) to 2(d), NaCl and CaCl 2 To MoS 2 The inhibition of the tetracycline adsorption capacity of SBC increases with increasing concentration, with essentially negligible inhibition of NaCl and with CaCl 2 The inhibition effect of the compound is obviously stronger than that of NaCl. Humic acid to MoS 2 The ability of SBCs to adsorb tetracycline has little effect.
Example six: the MoS dosage is 0.2g/L 2 SBC was added to a tetracycline solution of 800mL volume and 20mg/L concentration, and the adsorption experiment was performed in a 25 ℃ constant temperature shaking chamber (160rpm), and at the time of reaction equilibrium, the absorbance of residual tetracycline was measured at λ 360nm using an ultraviolet spectrophotometer. To the above MoS achieving adsorption equilibrium 2 SBC was subjected to filtration separation, regeneration treatment with absolute ethanol and NaOH (0.1mol/L) for 20min, treatment of the control with ultrapure water and repetition of 3 times, and MoS was measured 2 The regenerative adsorption capacity of SBC.
FIG. 3(a) shows that the NaOH treatment can maintain MoS as compared with the ultrapure water and absolute ethanol treatment 2 SBC continues to have a stable adsorption capacity in subsequent cycling (up to 83% or more of initial use).
The raw materials listed in the invention, the upper and lower limits and interval values of the raw materials of the invention, and the upper and lower limits and interval values of the process parameters (such as temperature, time and the like) can all realize the invention, and the examples are not listed.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (9)
1. MoS applied to removing tetracycline in water 2 The preparation method of the hydrothermal activated sludge biochar is characterized by comprising the following steps:
(1) preparing sludge biochar: cleaning municipal sludge with ultrapure water, drying to constant weight, pyrolyzing, grinding and sieving to obtain sludge biochar SBC;
(2)MoS 2 preparing the hydrothermal activated sludge biochar: placing the sludge biochar SBC obtained in the step (1) into a reactor containing sodium molybdate (NaMoO) 4 ·2H 2 O), thioacetamide (CH) 3 CSNH 2 ) And polyethylene glycol (PEG10000) solution in a reaction kettle, performing hydrothermal activation, washing with ultrapure water, drying, grinding and sieving to obtain MoS 2 Sludge biochar MoS for hydrothermal activation 2 -SBC。
2. MoS for tetracycline removal in water application according to claim 1 2 The preparation method of the hydrothermal activated sludge biochar is characterized by comprising the following steps: in the step (1), the drying temperature is 70-105 ℃; the pyrolysis condition is that the nitrogen flow rate is 0.3-0.6L/min, the heating rate is 5-20 ℃/min, and the pyrolysis is continued for 60-120min at the temperature of 400-; grinding, and sieving with 60-200 mesh sieve.
3. MoS for tetracycline removal in water application according to claim 1 2 The preparation method of the hydrothermal activated sludge biochar is characterized by comprising the following steps: in the step (2)Sodium molybdate (NaMoO) 4 ·2H 2 O), thioacetamide (CH) 3 CSNH 2 ) SBC, ultrapure water and polyethylene glycol (PEG10000) in the following proportions: 2.3-6.9 g: 4.6-13.8 g: 1-3 g: 40-80 mL: 0.0176g-1.762 g; wherein the concentration of polyethylene glycol (PEG10000) is 0.1-0.5 mol/L; the hydrothermal activation conditions are as follows: the temperature of the air drying box is 160-220 ℃, and the activation time is 720-1440 min; drying at 70-105 deg.C, grinding, and sieving with 60-200 mesh sieve.
4. MoS applied to removing tetracycline in water 2 The hydrothermal activated sludge biochar is characterized in that: said mos 2 The hydrothermal activated sludge biochar is prepared by the method as claimed in any one of claims 1-3.
5. MoS for tetracycline removal in water application according to claim 4 2 The hydrothermal activated sludge biochar is characterized in that: said mos 2 Hydrothermal activated sludge biochar MoS 2 The removal rate of tetracycline with the concentration of 20mg/L reaches more than 90% when the SBC dose is 0.2 g/L; at a concentration of 200mg/L and a reaction temperature of 35 ℃ in mos 2 Hydrothermal activated sludge biochar MoS 2 The maximum adsorption capacity of SBC to tetracycline can reach 461.40 mg/g; os is the 2 Hydrothermal activated sludge biochar MoS 2 Maintenance of MoS by NaOH regeneration treatment of SBC 2 SBC reaches more than 83% of the initial use in subsequent cycle use.
6. MoS for tetracycline removal in water according to claim 5 2 The hydrothermal activated sludge biochar is characterized in that: the regeneration treatment process of the NaOH comprises the step of absorbing and balancing MoS 2 SBC is subjected to filtration separation and regeneration treatment with absolute ethanol and 0.1mol/L NaOH for 20 min.
7. MoS for use in the removal of tetracycline from water according to any one of claims 1-6 2 The application of the hydrothermal activated sludge biochar is characterized by comprising the following steps: the sludge biochar SBC and MoS 2 Hydrothermal activated sludge biochar MoS 2 Adding SBC as an adsorbent into an aqueous solution containing tetracycline, and filtering after the adsorption process reaches equilibrium to obtain a solution after tetracycline removal.
8. The MoS of claim 7, wherein 2 The application of the hydrothermal activated sludge biochar in removing tetracycline in water is characterized in that: the concentration of the tetracycline in the tetracycline-containing solution is 20-200mg/L, pH and is 3-11; the dosage of the adsorbent is 0.1-0.3 g/L.
9. The MoS of claim 7, wherein 2 The application of the hydrothermal activated sludge biochar in removing tetracycline in water is characterized in that: the temperature in the adsorption process is controlled to be 15-35 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603810A (en) * | 2018-12-28 | 2019-04-12 | 湖南大学 | Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and its preparation method and application |
| CN112169755A (en) * | 2020-09-24 | 2021-01-05 | 武汉理工大学 | Preparation method of hydrothermally synthesized zinc chloride activated magnetic sludge biochar applied to tetracycline removal in water |
| AU2020103432A4 (en) * | 2020-01-22 | 2021-01-28 | Qingdao Agricultural University | Method for adsorbing oxytetracycline with cufeo2/bc composite magnetic material |
| CN114160098A (en) * | 2021-12-07 | 2022-03-11 | 武汉理工大学 | Preparation method of alkali/double-metal salt water heat activated sludge biochar applied to removal of norfloxacin in water |
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- 2022-04-18 CN CN202210405474.9A patent/CN114797811A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603810A (en) * | 2018-12-28 | 2019-04-12 | 湖南大学 | Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and its preparation method and application |
| AU2020103432A4 (en) * | 2020-01-22 | 2021-01-28 | Qingdao Agricultural University | Method for adsorbing oxytetracycline with cufeo2/bc composite magnetic material |
| CN112169755A (en) * | 2020-09-24 | 2021-01-05 | 武汉理工大学 | Preparation method of hydrothermally synthesized zinc chloride activated magnetic sludge biochar applied to tetracycline removal in water |
| CN114160098A (en) * | 2021-12-07 | 2022-03-11 | 武汉理工大学 | Preparation method of alkali/double-metal salt water heat activated sludge biochar applied to removal of norfloxacin in water |
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