CN114768779A - Preparation method of nitrogen-doped magnetic iron sludge biochar applied to tetracycline removal in water - Google Patents
Preparation method of nitrogen-doped magnetic iron sludge biochar applied to tetracycline removal in water Download PDFInfo
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- 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
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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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
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- 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
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- C02F11/00—Treatment of sludge; Devices therefor
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a preparation method of nitrogen-doped magnetic iron sludge biochar applied to tetracycline removal in water, and specifically comprises the step of placing Sludge Biochar (SBC) prepared by tubular furnace pyrolysis in a reactor containing ferric trichloride (FeCl)3·6H2O) and urea (CH)4N2O) solution is subjected to hydrothermal activation treatment in a reaction kettle to prepare the nitrogen-doped magnetic iron sludge biochar (Fe/N-SBC). The biochar prepared by the invention has the advantages ofThe method has the advantages that the tetracycline in water can be efficiently removed due to chemical characteristics, and the maximum adsorption capacity of the tetracycline can reach 238.3mg/g at the reaction temperature of 35 ℃.
Description
Technical Field
The invention relates to the technical field of biochar preparation and water treatment, in particular to a preparation method of nitrogen-doped magnetic iron sludge biochar applied to removing tetracycline in water.
Background
Tetracycline is one of the largest-used antibiotics worldwide, produced by streptomyces or produced semi-synthetically. Tetracycline is widely used in human therapy, veterinary medicine, and the like due to its low cost, low toxicity, and oral availability. Due to low metabolism, most tetracycline is released to the environment through feces and urine, contaminating surface water, ground water, soil and even drinking water. The characteristics of high hydrophilicity and low volatility of the tetracycline enable the tetracycline to last for a long time in the environment, and the residual tetracycline can destroy the ecological balance, influence the immune system of a human body to a certain extent and reduce the immunity of the human body. Therefore, effective removal of residual tetracycline in the environment becomes a great challenge.
Common tetracycline removal techniques include: biodegradation, adsorption, membrane separation, and advanced oxidation. Biodegradation basically can only degrade a small part of degradable pollutants, has certain limitations, and retains biological activity and toxicity of intermediate products generated in the degradation process, thereby being not beneficial to wide application of the method. Membrane separation techniques and advanced oxidation techniques have limited their use due to their high energy consumption and secondary pollution problems. The adsorption method is mainly a method for accumulating substances from gas or liquid to the surface of the adsorbent through physical or chemical bonds, and the method is simple to operate, environment-friendly and efficient. Biochar is a carbon-rich solid product formed by thermochemically converting biomass at high temperature in an inert atmosphere under the condition of limited oxygen. Sludge is a semi-solid substance generated in the sewage treatment process, and comprises organic compounds, inorganic compounds, microorganisms in a dissolved or suspended state and the like. Since 2014-charge 2020, the sludge yield of sewage treatment plants in China is gradually increased year by year, and by 2020, the average daily yield of the sludge is up to 22 ten thousand tons, so that the huge amount of sludge causes certain harm to the ecological environment and the human society. Proper treatment and disposal of sludge to avoid the harm to environment are important components of sewage treatment and environmental protection. Carbonizing sludge to prepare adsorbent materialThe method is an effective method for sustainable treatment and resource utilization. On the one hand, compared with the biochar prepared by using the traditional biochar raw material, the sludge has the advantages of low price and easy obtainment. In addition, the sludge contains a large amount of harmful substances, serious pollution problems are easily caused by improper treatment, and the potential ecological risks of the sludge can be effectively reduced by preparing the sludge biochar from the sludge biochar. On the surface of research, the sludge biochar has certain adsorption capacity on organic matters (ciprofloxacin, amoxicillin and the like) and inorganic matters (chromium and the like) in water, and can achieve the aim of treating sewage with waste. 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. Researches prove that the co-doping of transition metal iron (Fe) and nitrogen (N) can effectively change the electronic structure of the carbon-based material, generate more active sites and improve the electron transfer capacity, which are beneficial to improving the adsorption capacity of the adsorbent. And FeCl3·6H2O modification is considered to be an effective method for supporting magnetism, CH4N2O is one of the most abundant compounds containing nitrogen. Based on FeCl3·6H2O and CH4N2The characteristic of O, and the invention is not combined with the activation of the sludge biochar, and the invention is used for the modification of the sludge biochar. In addition, after the modified sludge biochar adsorbs tetracycline, how to realize efficient separation and 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 invention aims to provide the nitrogen-doped magnetic iron sludge biochar capable of efficiently removing tetracycline in water, and meanwhile, the safety of an adsorbent can be ensured, and the efficient magnetic separation and regeneration of the biochar after tetracycline adsorption can be realized. The treatment technology can realize the resource utilization of the municipal sludge and can also realize the efficient and sustainable removal of the tetracycline in the water.
In order to solve the technical problem, the invention provides a preparation method of nitrogen-doped magnetic iron sludge biochar applied to removing tetracycline in water, which comprises the following steps:
(1) preparing sludge biochar: cleaning municipal sludge with ultrapure water, drying to constant weight, then pyrolyzing, grinding and sieving to obtain sludge biochar SBC;
(2) preparing nitrogen-doped magnetic iron sludge biochar: adding the SBC prepared in the step (1) into FeCl containing ferric chloride3·6H2O and Urea CH4N2And placing the O solution in a reaction kettle in a blast drying oven, performing hydrothermal activation at a certain temperature, cleaning and filtering with ultrapure water, drying, grinding and sieving to obtain the nitrogen-doped magnetic iron sludge biochar Fe/N-SBC.
As a preferred aspect of the above technical solution, the method for preparing nitrogen-doped magnetic iron sludge biochar applied to removing tetracycline from water provided by the present invention further comprises a part or all of the following technical features:
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 5-15 ℃/min, and the pyrolysis is continuously carried out 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 mass of the sludge biochar SBC and the ferric chloride FeCl are adopted3·6H2O and Urea CH4N2The volume ratio of the O solution is 2.5-10g:40-80 mL; urea CH4N2The O solution is obtained by dissolving 2.5-10g of urea in 40-80mL of water; the hydrothermal activation conditions are as follows: the temperature of the air drying box is 200-240 ℃, and the activation time is 600-900 min; drying at 70-105 deg.C, grinding, and sieving with 60-200 mesh sieve.
The nitrogen-doped magnetic iron sludge biochar is prepared by any one of the methods.
The application of nitrogen-doped magnetic iron sludge biochar in removing tetracycline in water is characterized by comprising the following steps: adding the sludge biochar SBC and the nitrogen-doped magnetic iron sludge biochar Fe/N-SBC serving as adsorbents into a tetracycline-containing aqueous solution, and filtering after the adsorption process reaches balance to obtain a solution from which tetracycline is removed and the Fe/N-SBC reaching adsorption balance.
Preferably, the application of the nitrogen-doped magnetic iron sludge biochar in removing tetracycline from water further comprises part or all of the following technical characteristics:
as an improvement of the technical proposal, the concentration of the tetracycline in the tetracycline-containing aqueous solution is 20-200mg/L, pH and is 3-11; the dosage of the adsorbent is 0.1-0.4 g/L.
As an improvement of the technical scheme, the temperature in the adsorption process is controlled to be 15-35 ℃.
The method for recycling the nitrogen-doped magnetic iron sludge biochar comprises the steps of carrying out suction filtration separation on Fe/N-SBC which reaches the adsorption balance, using 0.1mol/L NaOH solution for regeneration treatment for 20min, and repeating the steps for 3 times to obtain the continuously stable adsorption capacity of the regenerated Fe/N-SBC in the subsequent cycle use, wherein the adsorption capacity of the regenerated Fe/N-SBC is equivalent to that of the initially prepared Fe/N-SBC
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: the method for efficiently removing the tetracycline in the water by using the nitrogen-doped magnetic iron sludge biochar as the adsorbent is provided, so that the environmental pollution caused by the tetracycline can be effectively reduced, and the resource utilization of the municipal sludge can be realized. Meanwhile, the biochar prepared by the method has high safety.
(1) The Fe/N-SBC has stronger removal capacity to tetracycline, and the removal rate of the Fe/N-SBC with the dosage of 0.25g/L to the tetracycline with the concentration of 20mg/L is close to 93%. The maximum adsorption capacity of the Fe/N-SBC to the tetracycline can reach 238.3mg/g at the concentration of 200mg/L and the reaction temperature of 35 ℃.
(2) Compared with other technologies (biodegradation, membrane separation and advanced oxidation), the method for removing tetracycline in water by using the nitrogen-doped magnetic iron sludge biochar as the adsorbent has the advantages of low cost, simplicity in operation, environmental friendliness and large-scale application prospect.
(3) The nitrogen-doped magnetic iron sludge biochar prepared by the invention can realize the resource utilization of municipal sludge and the efficient removal of tetracycline in water, and has high safety and 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 content 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 with reference to 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) shows the removal rate of 20mg/L tetracycline by Fe/N-SBC at 0.25g/L at 0-1440 min;
FIG. 1(b) is a graph showing the relationship between the concentration of tetracycline and the reaction temperature and the adsorption capacity of Fe/N-SBC when used as an adsorbent;
FIG. 2(a) is a graph of the adsorption capacity of Fe/N-SBC for 20mg/L tetracycline as a function of solution pH;
FIG. 2(b) is a graph showing the effect of NaCl concentrations of 1-100mmol/L on the tetracycline adsorption capacity of 20mg/L Fe/N-SBC;
FIG. 2(c) shows CaCl at a concentration of 1-100mmol/L2Influence on the tetracycline capacity of 20mg/L of Fe/N-SBC adsorption concentration;
FIG. 2(d) is a graph showing the effect of humic acid at a concentration of 1-10mg/L on the ability of Fe/N-SBC to adsorb tetracycline at a concentration of 20 mg/L;
FIG. 3(a) shows the leaching concentrations of Fe in Fe/N-SBC at different pH;
FIG. 3(b) is a graph of the ability of the Fe/N-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: drying municipal sludge in a 70 ℃ oven to constant weight, and transferring into a high-temperature tube furnace (N)2The flow rate is 0.5L/min, the heating rate is 10 ℃/min) and the sludge is pyrolyzed for 120min at the temperature of 700 ℃, and the sludge is ground and sieved by a 100-mesh sieve to obtain the sludge biochar SBC. SBC (2.0 g by mass) was transferred to a reactor containing 40mL volume of dissolved 2.0g of FeCl3·6H2O and 2.0g CH4N2And (3) in an O reaction kettle, performing hydrothermal activation for 720min at 220 ℃, cleaning and filtering with ultrapure water, drying in a 70 ℃ oven to constant weight, grinding and sieving with a 100-mesh sieve to obtain the nitrogen-doped magnetic iron sludge biochar Fe/N-SBC.
Example two: 0.25g/L Fe/N-SBC is added into a tetracycline solution with the volume of 100mL and the concentration of 20mg/L, an adsorption experiment is carried out in a constant-temperature shaking box (160rpm) at 25 ℃, samples are taken at set time (0-1440min), the residual concentration of the tetracycline is measured at the position of lambda-360 nm by using an ultraviolet spectrophotometer, and the removal rate of the tetracycline at different time is calculated.
As can be seen from FIG. 1(a), the Fe/N-SBC can realize rapid and efficient tetracycline removal, the tetracycline removal rate is over 80% in 480min, and the tetracycline removal rate can reach 92.3% in 1140 min.
Example three: Fe/N-SBC at a dose of 0.25g/L was added to tetracycline solutions of 100mL volume and 20, 40, 60, 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, and the residual concentration of tetracycline was measured at λ 360nm using an ultraviolet spectrophotometer at the time of reaction equilibrium.
As can be seen from FIG. 1(b), the adsorption capacity of Fe/N-SBC for tetracycline increases with increasing tetracycline concentration and reaction temperature. The maximum adsorption capacity of the tetracycline adsorbent at 35 ℃ can reach 238.3 mg/g.
Example four: adding 0.25g/L Fe/N-SBC into a tetracycline solution with the volume of 100mL, the concentration of 20mg/L and the pH value of 3-11 (adjusting the pH value of the solution by using 0.1mol/L HCl/NaOH), placing the tetracycline solution in a constant-temperature shaking box (160rpm) at 25 ℃ for adsorption experiment, and measuring the residual concentration of the tetracycline at the position of 360nm by using an ultraviolet spectrophotometer and measuring the leaching concentration of Fe by using an atomic absorption spectrophotometer when the adsorption is balanced, thereby researching the adsorption capacity of the Fe/N-SBC on the tetracycline and the safety of the biochar under different pH conditions.
As can be seen from FIG. 2(a), the solution pH of 3-9 had little effect on the ability of Fe/N-SBC to adsorb tetracycline, and the adsorption capacity was maximal at a solution pH of 5 (69.74 mg/g). The adsorption capacity of Fe/N-SBC for tetracycline is significantly inhibited when the solution pH is > 9. From FIG. 3(a), it can be known that the leaching concentration of Fe in Fe/N-SBC is higher than the limit value of GB 5749-2006 only when the pH of the solution is 3, and the leaching concentration of Fe is far lower than the limit value of GB 5749-2006 under other pH conditions, which indicates that the nitrogen-doped magnetic iron sludge biochar prepared by the invention has higher safety.
Example five: adding 0.25g/L Fe/N-SBC into 100mL of Fe/N-SBC solution with concentration of 20mg/L and NaCl (1-100mmol/L) and CaCl2The tetracycline solution of (1-100mmol/L) and humic acid (1-10mg/L) is placed in a constant temperature shaking box (160rpm) at 25 ℃ for adsorption experiment, and when the adsorption is balanced, the residual concentration of tetracycline is measured at the position of lambda being 360nm by using an ultraviolet spectrophotometer, and the influence of coexisting inorganic ions and organic matters on the tetracycline adsorption capacity of Fe/N-SBC is evaluated.
As is clear from FIGS. 2(b) to 2(d), NaCl and CaCl2The inhibition effect on the tetracycline adsorption capacity of Fe/N-SBC is enhanced along with the increase of the concentration of the Fe/N-SBC, wherein the inhibition effect of NaCl is basically negligible, and CaCl is added2The inhibitory effect of (D) is stronger than that of NaCl. Humic acid also has a certain inhibiting effect on the tetracycline adsorption capacity of Fe/N-SBC.
Example six: adding Fe/N-SBC with the dose of 0.25g/L into tetracycline solution with the volume of 800mL and the concentration of 20mg/L, carrying out an adsorption experiment in a constant-temperature shaking box at 25 ℃, and measuring the absorbance of tetracycline at the position of which the lambda is 360nm by using an ultraviolet spectrophotometer when the reaction is balanced. And (3) carrying out suction filtration and separation on the Fe/N-SBC which reaches the adsorption equilibrium, carrying out regeneration treatment for 20min by using HCl (0.1mol/L) and NaOH (0.1mol/L), treating a control group by using ultrapure water, repeating the treatment for 3 times, and measuring the regeneration adsorption capacity of the Fe/N-SBC.
As can be seen from fig. 3(b), compared to the ultra-pure water and HCl treatments, the NaOH treatment can maintain the Fe/N-SBC adsorption capacity continuously stable in the subsequent cycles (substantially reaching 100% of the 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 (8)
1. A preparation method of nitrogen-doped magnetic iron sludge biochar applied to tetracycline removal in water 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) preparing nitrogen-doped magnetic iron sludge biochar: adding the SBC prepared in the step (1) into FeCl containing ferric chloride3·6H2O and Urea CH4N2And placing the reaction kettle of the O solution in a blast drying box for hydrothermal activation, cleaning and filtering with ultrapure water, drying, grinding and sieving to obtain the nitrogen-doped magnetic iron sludge biochar Fe/N-SBC.
2. The method for preparing nitrogen-doped magnetic iron sludge biochar applied to tetracycline removal in water according to claim 1, 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 5-15 ℃/min, and the pyrolysis is continuously carried out for 60-120min at the temperature of 400-; grinding, and sieving with 60-200 mesh sieve.
3. The method for preparing nitrogen-doped magnetic iron sludge biochar applied to removing tetracycline from water as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the sludge biocharQuality of SBC and FeCl3·6H2O and Urea CH4N2The volume ratio of the O solution is 2.5-10g:40-80 mL; urea CH4N2The O solution is obtained by dissolving 2.5-10g of urea in 40-80mL of water; the hydrothermal activation conditions are as follows: the temperature of the air drying box is 200-240 ℃, and the activation time is 600-900 min; drying at 70-105 deg.C, grinding, and sieving with 60-200 mesh sieve.
4. A nitrogen-doped magnetic iron sludge biochar is characterized in that: the nitrogen-doped magnetic iron sludge biochar is prepared by any one of the methods as claimed in claims 1-3.
5. The application of nitrogen-doped magnetic iron sludge biochar in removing tetracycline in water is characterized by comprising the following steps: adding the sludge biochar SBC and the nitrogen-doped magnetic iron sludge biochar Fe/N-SBC serving as adsorbents into a tetracycline-containing aqueous solution, and filtering after the adsorption process reaches balance to obtain a solution from which tetracycline is removed and the Fe/N-SBC reaching adsorption balance.
6. The use of nitrogen-doped magnetic iron sludge biochar in the removal of tetracycline from water as claimed in claim 5, wherein: 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 0.1-0.4 g/L.
7. The use of nitrogen-doped magnetic iron sludge biochar in the removal of tetracycline from water as claimed in claim 6, wherein: the temperature in the adsorption process is controlled to be 15-35 ℃.
8. A method for recycling nitrogen-doped magnetic iron sludge biochar as claimed in any one of claims 5 to 7, characterized in that: and (3) carrying out suction filtration and separation on the Fe/N-SBC which reaches the adsorption balance, regenerating the Fe/N-SBC by using a 0.1mol/L NaOH solution for 20min, and repeating for 3 times to obtain the continuously stable adsorption capacity of the regenerated Fe/N-SBC in the subsequent cycle use, wherein the adsorption capacity of the regenerated Fe/N-SBC is equivalent to that of the initially prepared Fe/N-SBC.
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| CN115321532B (en) * | 2022-08-15 | 2023-04-28 | 华南师范大学 | Nitrogen-doped iron-loaded three-dimensional self-supporting carbon material, and preparation method and application thereof |
| CN115414911A (en) * | 2022-08-18 | 2022-12-02 | 江南大学 | Fe-rich alloy x Pharmaceutical sludge biochar with N structure, preparation method and application |
| CN115414911B (en) * | 2022-08-18 | 2024-02-13 | 江南大学 | Is rich in Fe x N-structure pharmaceutical sludge biochar, preparation method and application |
| CN116139901A (en) * | 2022-11-28 | 2023-05-23 | 武汉理工大学 | Ball milling nitrogen-doped sludge biochar and preparation method and application thereof |
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