CN113198516A - Iron-nitrogen co-doped biochar catalyst, and preparation method and application thereof - Google Patents
Iron-nitrogen co-doped biochar catalyst, and preparation method and application thereof Download PDFInfo
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- CN113198516A CN113198516A CN202110562158.8A CN202110562158A CN113198516A CN 113198516 A CN113198516 A CN 113198516A CN 202110562158 A CN202110562158 A CN 202110562158A CN 113198516 A CN113198516 A CN 113198516A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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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- C02F1/722—Oxidation by peroxides
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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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- 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
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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
- C02F2305/00—Use of specific compounds during water treatment
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- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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Abstract
The invention discloses an iron-nitrogen co-doped biochar catalyst, and a preparation method and application thereof. The method is used for solving the problems that the removal effect of the existing catalyst on antibiotic pollutants which are difficult to degrade in sewage is poor, and the purification quality of advanced wastewater treatment is influenced. The iron-nitrogen co-doped biochar catalyst is used for removing antibiotic pollutants which are difficult to degrade in tail water of municipal sewage treatment plants. The iron-nitrogen co-doped biochar catalyst comprises the following components: the iron-nitrogen co-doped biochar catalyst is prepared from corn straws, an iron source, a nitrogen source and a reducing agent in proportion. Wherein the weight ratio of the iron source, the nitrogen source and the reducing agent is 5.56: 3: 2.5. the iron-nitrogen co-doped biochar catalyst obtained by the invention has the characteristics of high efficiency, stability, reusability, wide applicability and economy, can realize conversion and utilization of biomass resources, and provides a new method for antibiotic wastewater treatment and even deep treatment of industrial wastewater.
Description
Technical Field
The invention relates to the technical field of advanced sewage treatment, in particular to an iron-nitrogen co-doped biochar catalyst, a preparation method of the iron-nitrogen co-doped biochar catalyst and application of the iron-nitrogen co-doped biochar catalyst.
Background
Research data show that during the period from 2000 to 2015, the total consumption of antibiotics worldwide increases from 21.1 to 348 billion DDDs (defined daily dose), and that about 61.5% of the antibiotics in the human body will keep the parent structure unchanged and directly enter the pipe network through excretion, and then enter the sewage treatment plant for purification. Although the antibiotics in the liquid phase can be effectively removed after the wastewater has been subjected to extensive and intensive treatment in a wastewater treatment plant, the antibiotics may still accumulate in the biosolids, which leads to an increased risk of the spread of antibiotic resistance genes in the aquatic environment. Particularly in rural areas, the wastewater and livestock manure are discharged directly into rivers without being treated due to lack of original capital and laggard behind sewage treatment technology. Therefore, the search for an efficient, low-cost and simple-process method for degrading antibiotics is an urgent requirement for solving antibiotic pollution.
In recent years, the advanced oxidation process based on sulfate radicals has attracted much attention because of its advantages of high oxidation-reduction potential, high selectivity for organic substances, good adaptability to pH change, and longer half-life. Therefore, the development of the efficient, stable and recyclable heterogeneous catalyst is an urgent need for the wide application of persulfate advanced oxidation technology for treating antibiotic wastewater. When the lower catalyst is used for wastewater treatment, the problem that the removal effect of antibiotic pollutants which are difficult to degrade in the wastewater is poor and the purification quality of the wastewater advanced treatment is influenced exists
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an iron-nitrogen co-doped biochar catalyst, a preparation method and application thereof, and aims to solve the problems that the existing catalyst has poor removal effect on antibiotic pollutants which are difficult to degrade in sewage and influences the purification quality of advanced wastewater treatment.
The invention is realized by adopting the following technical scheme:
the iron-nitrogen co-doped biochar catalyst is used for removing antibiotic pollutants which are difficult to degrade in tail water of a municipal sewage treatment plant and is characterized by comprising the following components: preparing the iron-nitrogen co-doped biochar catalyst from corn straws, an iron source, a nitrogen source and a reducing agent in proportion;
wherein the weight ratio of the iron source, the nitrogen source and the reducing agent is 5.56: 3: 2.5.
as a further improvement of the scheme, the iron source adopts FeSO4·7H2O; the nitrogen source adopts urea; the reducing agent adopts ascorbic acid.
A preparation method of an iron-nitrogen co-doped biochar catalyst is applied to preparation of the iron-nitrogen co-doped biochar catalyst and comprises the following steps:
s1, providing corn stalks, an iron source, a nitrogen source and a reducing agent;
the iron source adopts FeSO4·7H2O; the nitrogen source adopts urea; the reducing agent adopts ascorbic acid;
s2, preparing the corn straws into powder for later use;
s3, dissolving the iron source, the nitrogen source and the reducing agent in deionized water to obtain a mixed solution marked as solution A;
s4, adding the corn straws which are made into powder into the solution A, and marking the mixed material as a mixture B;
s5, calcining the mixture B to obtain a reactant marked as a mixture C;
s6, drying the mixture C, wherein the dried product is marked as a material D;
s7, washing the material D, and marking the washed object as a material E;
s8, drying the material E to obtain a dried substance marked as a material F;
s9, calcining the material F, and marking the calcined product as a material G;
s10, washing the material G, and marking the washing product as a material H;
and S11, drying the material H to constant weight to obtain the iron-nitrogen co-doped biochar.
As a further improvement of the scheme, the process of preparing the corn straws into powder is carried out in a plant crusher; the specification of the screen is 80 meshes.
As a further improvement of the above scheme, the solution A is 5.56g of FeSO4·7H2O, 3.00g of urea and 2.50g of ascorbic acid were dissolved in 100mL of deionized water to prepare a mixed solution.
As a further improvement of the above scheme, the calcination treatment process is carried out in a muffle furnace; the operating temperature of the muffle furnace is 180 ℃, and the reaction time is 10 hours; and (3) putting the mixture C in a vacuum drying oven, and drying at 50 ℃ for 12 h.
As a further improvement of the above scheme, the material F is placed in a tube furnace, heated at a rate of 10 ℃/min and calcined at 600 ℃ for 2 h.
An application of an iron-nitrogen co-doped biochar catalyst in the efficient removal of antibiotics in water.
As a further improvement of the above solution, the operation of the application is as follows:
providing persulfate and the iron-nitrogen co-doped biochar catalyst, wherein the iron-nitrogen co-doped biochar catalyst is prepared by adopting a preparation method of the iron-nitrogen co-doped biochar catalyst;
putting the iron-nitrogen co-doped biochar catalyst into wastewater containing antibiotics;
throwing persulfate into the wastewater;
after reacting for a period of time, separating out the iron-nitrogen co-doped biochar catalyst, and repeatedly using for more than five times.
As a further improvement of the scheme, the adding standard of the iron-nitrogen co-doped biochar catalyst is 0.1 g/L; the adding standard of the persulfate is 10 mmol/L.
The iron-nitrogen co-doped biochar catalyst, the preparation method and the application thereof provided by the invention have the following beneficial effects: the iron-nitrogen co-doped biochar catalyst is solid and loaded with iron oxide and rich nitrogen functional groups, and can efficiently activate persulfate to generate strong-oxidizing hydroxyl free radicals, sulfate free radicals and singlet oxygen, so that antibiotic pollutants in water are continuously degraded. The iron-nitrogen co-doped biochar catalyst has the characteristics of high efficiency, stability, reusability and wide applicability, can realize conversion and utilization of biomass resources, and provides a new method for antibiotic wastewater treatment and even advanced treatment of industrial wastewater.
In conclusion, the iron-nitrogen co-doped biochar catalyst obtained by the invention has the characteristics of high efficiency, stability, reusability, wide applicability and economy, can realize conversion and utilization of biomass resources, and provides a new method for antibiotic wastewater treatment and even deep treatment of industrial wastewater.
Drawings
Fig. 1 is a scanning electron microscope image of an iron-nitrogen co-doped biochar catalyst provided in example 1.
Fig. 2 is a flowchart of a preparation method of an iron-nitrogen co-doped biochar catalyst, which is proposed in example 2, and is used for preparing the iron-nitrogen co-doped biochar catalyst in fig. 1.
Fig. 3 is a flowchart of an application of the iron-nitrogen co-doped biochar catalyst in the efficient removal of antibiotics in water, which is provided in example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
When the lower catalyst is used, the problem that the removal effect of antibiotic pollutants which are difficult to degrade in sewage is poor and the purification quality of advanced wastewater treatment is influenced exists. Therefore, the present inventors provide the following embodiments to solve the above problems.
Example 1
Referring to fig. 1, the present embodiment discloses an iron-nitrogen co-doped biochar catalyst, which is used for removing refractory antibiotic pollutants in the tail water of a municipal sewage treatment plant. The iron-nitrogen co-doped biochar catalyst comprises the following components: the iron-nitrogen co-doped biochar catalyst is prepared from corn straws, an iron source, a nitrogen source and a reducing agent in proportion. Wherein the weight ratio of the iron source, the nitrogen source and the reducing agent is 5.56: 3: 2.5.
in this example, FeSO was used as the iron source4·7H2The examples of the O and nitrogen sources are urea and the reducing agent is ascorbic acid, but in other examples, the iron source, the nitrogen source and the reducing agent can be replaced according to actual conditions.
Fig. 1 is a scanning electron microscope image of the iron-nitrogen co-doped biochar catalyst in the embodiment. From the figure, it can be analyzed that the iron-nitrogen co-doped biochar catalyst is solid, and is loaded with iron oxide and abundant nitrogen functional groups, and can efficiently activate persulfate to generate strong oxidizing hydroxyl free radicals, sulfate free radicals and singlet oxygen, thereby continuously degrading antibiotic pollutants in water. The iron-nitrogen co-doped biochar catalyst is applied to the purification treatment of sewage and belongs to the class of heterogeneous catalysts.
Compared with the existing sewage treatment catalyst, the iron-nitrogen co-doped biochar catalyst provided by the embodiment has the following advantages: the iron-nitrogen co-doped biochar catalyst has the characteristics of high efficiency, stability, reusability, wide applicability and economy, can realize the conversion and utilization of biomass resources, and provides a new method for antibiotic wastewater treatment and even advanced treatment of industrial wastewater.
Example 2
Referring to fig. 2, this embodiment discloses a preparation method of an iron-nitrogen co-doped biochar catalyst, which is applied to prepare the iron-nitrogen co-doped biochar catalyst described in embodiment 1, and the preparation method includes the following steps:
s1, providing corn stalks, an iron source, a nitrogen source and a reducing agent;
the iron source adopts FeSO4·7H2O; the nitrogen source adopts urea; the reducing agent adopts ascorbic acid.
S2, preparing the corn straws into powder for later use;
washing corn straws with deionized water, drying to constant weight, making the dried corn straws into powder, making the corn straws into powder in a plant crusher, and sieving the powder with a sieve with the specification of 80 meshes to obtain the corn straw powder.
S3, dissolving the iron source, the nitrogen source and the reducing agent in deionized water to obtain a mixed solution marked as solution A;
the solution A was 5.56g FeSO4·7H2O, 3.00g of urea and 2.50g of ascorbic acid were dissolved in 100mL of deionized water to prepare a mixed solution.
S4, adding the corn straws which are made into powder into the solution A, and marking the mixed material as a mixture B;
and adding the corn straw powder into the mixed solution A, and mixing under an ultrasonic condition to obtain a mixture B.
S5, calcining the mixture B to obtain a reactant marked as a mixture C;
and placing the mixture B in a reaction kettle, placing the mixture B together with the reaction kettle I in a muffle furnace with the operating temperature set to 180 ℃ for calcination treatment for 10 hours to obtain a mixture C.
S6, drying the mixture C, wherein the dried product is marked as a material D;
and (5) placing the mixture C in a vacuum drying oven, and drying at 50 ℃ for 12h to obtain a material D.
S7, washing the material D, and marking the washed object as a material E;
and repeatedly washing the material D with deionized water until the material D is neutral to obtain a material E.
S8, drying the material E to obtain a dried substance marked as a material F;
and (3) putting the material E in a vacuum drying oven, and drying for 24h at the temperature of 60 ℃ to obtain a material F.
S9, calcining the material F, and marking the calcined product as a material G;
and (3) placing the material F in a tube furnace, raising the temperature at the speed of 10 ℃/min, and calcining for 2h at the temperature of 600 ℃ to obtain a material G.
S10, washing the material G, and marking the washing product as a material H;
and repeatedly washing the material G by using ethanol and deionized water to obtain a material H.
S11, drying the material H to constant weight to obtain iron-nitrogen co-doped biochar;
and (3) placing the material H in a forced air drying oven at 50 ℃ for drying treatment to constant weight to obtain the iron-nitrogen co-doped biochar.
In the preparation method provided in this embodiment, the corn stalk raw material is converted into the iron-nitrogen co-doped biochar catalyst by adopting a direct pyrolysis carbonization method, and the iron-nitrogen co-doped biochar catalyst is specifically described in embodiment 1, and therefore, details are not described in this embodiment again.
Example 3
Referring to fig. 3, the embodiment discloses an application of an iron-nitrogen co-doped biochar catalyst in efficiently removing antibiotics in water. The operation of the application is as follows:
providing persulfate and the iron-nitrogen co-doped biochar catalyst as described in example 1, wherein the iron-nitrogen co-doped biochar catalyst is prepared by adopting the preparation method of the iron-nitrogen co-doped biochar catalyst as described in example 2.
Putting the iron-nitrogen co-doped biochar catalyst into wastewater containing (norfloxacin) antibiotics;
the adding standard of the iron-nitrogen co-doped biochar catalyst is 0.1 g/L.
Throwing persulfate into the wastewater;
the addition standard of the persulfate is 10 mmol/L.
After reacting for a period of time, separating out the iron-nitrogen co-doped biochar catalyst, and repeatedly using for more than five times;
the iron-nitrogen co-doped biochar catalyst and persulfate are added into wastewater, and the iron-nitrogen co-doped biochar catalyst efficiently activates persulfate to generate strong-oxidizing hydroxyl free radicals, sulfate free radicals and singlet oxygen, so that antibiotics in water are continuously degraded.
This example illustrates the removal of norfloxacin from wastewater by using an iron-nitrogen co-doped biochar catalyst. And the following results are obtained through testing: the iron-nitrogen co-doped biochar catalyst can degrade 96% of norfloxacin within 20min, can still reach 70% of removal rate after 5 times of recycling, and simultaneously has mineralization rate of 50%. The test result proves that the iron-nitrogen co-doped biochar material has the advantages of high efficiency, stability, reusability, wide applicability and economy.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The iron-nitrogen co-doped biochar catalyst is used for removing antibiotic pollutants which are difficult to degrade in tail water of a municipal sewage treatment plant and is characterized by comprising the following components: preparing the iron-nitrogen co-doped biochar catalyst from corn straws, an iron source, a nitrogen source and a reducing agent in proportion;
wherein the weight ratio of the iron source, the nitrogen source and the reducing agent is 5.56: 3: 2.5.
2. the iron-nitrogen co-doped biochar catalyst as claimed in claim 1, wherein the iron source is FeSO4·7H2O; the nitrogen source adopts urea; the reducing agent adopts ascorbic acid.
3. A preparation method of an iron-nitrogen co-doped biochar catalyst, which is applied to the preparation of the iron-nitrogen co-doped biochar catalyst as claimed in any one of claims 1 to 2, and is characterized by comprising the following steps:
s1, providing corn stalks, an iron source, a nitrogen source and a reducing agent;
the iron source adopts FeSO4·7H2O; the nitrogen source adopts urea; the reducing agent adopts ascorbic acid;
s2, preparing the corn straws into powder for later use;
s3, dissolving the iron source, the nitrogen source and the reducing agent in deionized water to obtain a mixed solution marked as solution A;
s4, adding the corn straws which are made into powder into the solution A, and marking the mixed material as a mixture B;
s5, calcining the mixture B to obtain a reactant marked as a mixture C;
s6, drying the mixture C, wherein the dried product is marked as a material D;
s7, washing the material D, and marking the washed object as a material E;
s8, drying the material E to obtain a dried substance marked as a material F;
s9, calcining the material F, and marking the calcined product as a material G;
s10, washing the material G, and marking the washing product as a material H;
and S11, drying the material H to constant weight to obtain the iron-nitrogen co-doped biochar.
4. The preparation method of the iron and nitrogen co-doped biochar catalyst as claimed in claim 3, wherein the process of preparing the corn stalks into powder is carried out in a plant crusher; the specification of the screen is 80 meshes.
5. The preparation method of the iron-nitrogen co-doped biochar catalyst as claimed in claim 3, wherein the solution A is 5.56g of FeSO4·7H2O, 3.00g of urea and 2.50g of ascorbic acid were dissolved in 100mL of deionized water to prepare a mixed solution.
6. The preparation method of the iron and nitrogen co-doped biochar catalyst as claimed in claim 3, wherein the calcination treatment process is carried out in a muffle furnace; the operating temperature of the muffle furnace is 180 ℃, and the reaction time is 10 hours; and (3) putting the mixture C in a vacuum drying oven, and drying at 50 ℃ for 12 h.
7. The preparation method of the iron and nitrogen co-doped biochar catalyst as claimed in claim 3, wherein the material F is placed in a tubular furnace, heated at a rate of 10 ℃/min and calcined at 600 ℃ for 2 h.
8. An application of an iron-nitrogen co-doped biochar catalyst in the efficient removal of antibiotics in water.
9. The application of the iron-nitrogen co-doped biochar catalyst in the high-efficiency removal of antibiotics in water according to claim 8 is characterized by operating as follows:
providing persulfate and the iron-nitrogen co-doped biochar catalyst as claimed in any one of claims 1 to 2, wherein the iron-nitrogen co-doped biochar catalyst is prepared by adopting the preparation method of the iron-nitrogen co-doped biochar catalyst as claimed in any one of claims 3 to 7;
putting the iron-nitrogen co-doped biochar catalyst into wastewater containing antibiotics;
throwing persulfate into the wastewater;
after reacting for a period of time, separating out the iron-nitrogen co-doped biochar catalyst, and repeatedly using for more than five times.
10. The application of the iron-nitrogen co-doped biochar catalyst in the efficient removal of antibiotics in water according to claim 9, wherein the addition standard of the iron-nitrogen co-doped biochar catalyst is 0.1 g/L; the adding standard of the persulfate is 10 mmol/L.
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CN113813984A (en) * | 2021-10-21 | 2021-12-21 | 东北农业大学 | Preparation method and application of N/Fe co-doped nanotube catalytic material |
CN114146723A (en) * | 2021-12-20 | 2022-03-08 | 山东大学 | Iron-nitrogen co-doped nano carbon composite catalyst, preparation method and application |
CN114307964A (en) * | 2022-01-17 | 2022-04-12 | 合肥学院 | Method for preparing iron-nitrogen-doped biochar functional material based on waste paper box and application |
CN114516672A (en) * | 2022-03-03 | 2022-05-20 | 苏州同达澄澈环境科技有限公司 | Method for removing organic pollutants and heavy metals in water by using iron-nitrogen co-doped biochar activated calcium peroxide |
CN114671510A (en) * | 2022-04-12 | 2022-06-28 | 湖南大学 | Method for degrading antibiotics by activating persulfate through Fe-N self-doped algae-based carbon catalyst |
CN114749154A (en) * | 2022-04-22 | 2022-07-15 | 西南科技大学 | Preparation method of nitrogen-rich porous carbon-based composite functional material |
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CN115254159A (en) * | 2022-08-24 | 2022-11-01 | 北京市生态环境保护科学研究院 | Synthetic method of citric acid modified iron-phosphorus co-doped biochar |
CN115646525A (en) * | 2022-09-22 | 2023-01-31 | 华南理工大学 | Iron-nitrogen co-doped biochar, preparation method thereof and application thereof in wastewater treatment |
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CN115738998A (en) * | 2022-11-25 | 2023-03-07 | 师大(清远)环境修复科技有限公司 | Nitrogen-doped magnetic biochar as well as preparation method and application thereof |
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CN115779855A (en) * | 2022-10-24 | 2023-03-14 | 广州大学 | Preparation method of hot-process iron-nitrogen co-doped magnetic carbon material |
CN115920937A (en) * | 2022-11-02 | 2023-04-07 | 南华大学 | Preparation method of iron-nitrogen co-doped biomass carbon material catalyst |
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CN115770604A (en) * | 2022-11-15 | 2023-03-10 | 江南大学 | Fe-N@C catalyst prepared from blue algae in Taihu lake and preparation method and application thereof |
CN115738998A (en) * | 2022-11-25 | 2023-03-07 | 师大(清远)环境修复科技有限公司 | Nitrogen-doped magnetic biochar as well as preparation method and application thereof |
CN115722227A (en) * | 2022-12-28 | 2023-03-03 | 国科大杭州高等研究院 | Iron slag-doped wine-making sludge biochar material and preparation method and application thereof |
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