CN110550736A - Method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using iron-carbon microelectrolysis coupling anaerobic acid production fermentation process - Google Patents
Method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using iron-carbon microelectrolysis coupling anaerobic acid production fermentation process Download PDFInfo
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
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Abstract
the invention relates to a coupling iron-carbon micro-electrolysis and anaerobic acid-production fermentation process, which is characterized in that two technologies are arranged in the same reaction system, mutual promotion and common play can effectively shorten the treatment process, save space and time, and effectively treat high-concentration fluoroquinolone antibiotic wastewater, wherein the iron-carbon micro-electrolysis utilizes a micro-galvanic cell to react to generate substances with reducing action such as [ H ], H 2 and Fe 2+, can degrade macromolecular organic pollutants in water, reduce the biotoxicity of wastewater and improve the biodegradability of wastewater, and can also remove part of antibiotics through the coprecipitation action of ferrous iron and ferric hydroxide.
Description
Technical Field
The invention relates to the field of sewage treatment, in particular to application of an iron-carbon micro-electrolysis coupling anaerobic acid-producing fermentation process to pretreatment of high-concentration fluoroquinolone antibiotic wastewater.
Background
Fluoroquinolone antibiotics are artificially synthesized antibacterial drugs, especially ciprofloxacin, and are widely used for preventing and treating human diseases, livestock and poultry and aquaculture industry due to the characteristics of strong broad-spectrum antibacterial capability, good curative effect and the like. With the increasing demand of antibiotics, fluoroquinolone antibiotics are synthesized in a large scale, the medicaments can generate a large amount of intermediate products in the production process, and the wastewater contains high-concentration antibiotic residues, has the characteristics of poor biodegradability, complex components, high toxicity and the like, and is regarded as high-concentration refractory organic wastewater. However, the conventional treatment technology is difficult to directly and effectively treat the high-concentration fluoroquinolone antibiotic wastewater, so that the serious impact on a biological treatment unit is easily caused, and even the subsequent biochemical process is possibly collapsed, and the stable operation is difficult. Therefore, the research of the pretreatment process for the high-concentration fluoroquinolone antibiotic wastewater has important practical significance.
At present, the treatment methods of high-concentration fluoroquinolone antibiotics, particularly ciprofloxacin, for resisting wastewater mainly comprise a physical adsorption method, a chemical oxidation method and a biological treatment method. In the physical adsorption method, for example, the diatomite is used for treating the ciprofloxacin wastewater, the transfer of the ciprofloxacin can only be realized, and the ciprofloxacin cannot be removed, so that secondary pollution is easily caused if the adsorbate is improperly treated. Chemical oxidation methods such as photo-Fenton technology can destroy the chemical structure of fluoroquinolone antibiotics and reduce the toxicity of wastewater, but have the defects of difficult process control, low operation cost, high maintenance cost and the like. Although the biological treatment method is widely used as a mature and economical antibiotic treatment method, the fluoroquinolone antibiotics have a very strong inhibitory effect on microorganisms, and the advantages of the biological treatment method cannot be achieved due to the fact that the biological treatment method is used alone.
Disclosure of Invention
The invention aims to solve the problem that the conventional treatment technology in the field of pharmaceutical wastewater of fluoroquinolone antibiotics is difficult to directly and effectively treat the high-concentration fluoroquinolone antibiotic wastewater, and provides a method for removing the high-concentration fluoroquinolone antibiotic wastewater, especially ciprofloxacin antibiotic wastewater and partial COD (chemical oxygen demand) with simple and convenient operation, economy and high efficiency and achieving a better pretreatment effect.
In order to solve the problem, the invention provides an iron-carbon micro-electrolysis coupling anaerobic acid-producing fermentation process for pretreating high-concentration fluoroquinolone antibiotic wastewater, which comprises the following steps:
1. Acclimating anaerobic activated sludge (pH is 7.0 ~ 8.0.0) and carbon-rich nutrient substrate (COD content is 5000 ~ 8000 mg/L) at a volume ratio of 10:1 ~ 15: 1;
2. Introducing high-purity nitrogen to ensure that the reaction system is in an anaerobic state, wherein the reaction temperature is 37 +/-1 ℃, and the reaction time is 10 ~ 12 hours;
3. Discharging supernatant after natural precipitation, and reserving sludge at the lower layer, namely the sludge at the anaerobic acidogenic stage (the pH is 4.0 ~ 5.5.5);
4. Mixing sludge in an anaerobic acid production stage with high-concentration fluoroquinolone antibiotic wastewater for anaerobic fermentation, wherein the volume ratio of the wastewater to the sludge is 15:1 ~ 20: 1;
5. adding zero-valent nano iron and granular activated carbon (namely an iron-carbon mixture), wherein the mass ratio of the zero-valent nano iron to the granular activated carbon is 1:1, and the mass ratio of the iron-carbon mixture to the volatile solid of the sludge in the anaerobic acid production stage is 1:1 ~ 1.5.5: 1;
6. introducing high-purity nitrogen to ensure that the reaction system is in an anaerobic state, wherein the reaction temperature is 37 +/-1 ℃ and the reaction time is 6 ~ 8 hours.
7. After the reaction is finished, standing and settling, and obtaining supernatant which is effluent after the high-concentration fluoroquinolone antibiotic wastewater is pretreated.
The invention is mainly characterized in that:
1. the method comprises the steps of coupling iron-carbon microelectrolysis (zero-valent nano iron and granular activated carbon) with an anaerobic acid-producing fermentation process, utilizing iron-carbon contact to generate microcurrent and redox effect thereof, anaerobic activated sludge adsorption effect, anaerobic microorganism degradation effect and the like, pretreating high-concentration fluoroquinolone antibiotic wastewater, greatly reducing the concentration of fluoroquinolone antibiotics in effluent, and laying a foundation for subsequent treatment of pretreated effluent.
2. the optimum pH value of the iron-carbon micro-electrolysis reaction is acidic, and the invention utilizes the characteristics of the acid-producing fermentation process stage and replaces the acidifying reagent with the sludge (the pH value is 4.0 ~ 5.5.5) in the hydrolysis acidification stage to provide an acidic environment.
the invention relates to a coupling iron-carbon micro-electrolysis and anaerobic acid-production fermentation process, which is characterized in that two technologies are arranged in the same reaction system, mutual promotion and common play can effectively shorten the treatment process, save space and time, and effectively treat high-concentration fluoroquinolone antibiotic wastewater, wherein the iron-carbon micro-electrolysis utilizes a micro-galvanic cell to react to generate substances with reducing action such as [ H ], H 2 and Fe 2+, can degrade macromolecular organic pollutants in water, reduce the biotoxicity of wastewater and improve the biodegradability of wastewater, and can also remove part of antibiotics through the coprecipitation action of ferrous iron and ferric hydroxide.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
the anaerobic activated sludge in the embodiment is taken from an upflow anaerobic sludge bed reactor of a citric acid plant, a carbon-rich nutrient substrate takes glucose as a carbon source (COD is 5000-8000 mg/L), ammonium chloride and potassium dihydrogen phosphate are taken as a nitrogen source and a phosphorus source, 1mL/L of trace element solution and vitamin solution are added, wherein the ratio of the trace element solution to the phosphorus-rich nutrient substrate is C: N: P =200:5:1, and 1mL/L of the trace element solution and the vitamin solution are added, the trace element solution (g/L) is H 3 BO 3, 0.05, ZnCl 2, 0.05, CuCl 2.2H 2 O, 0.038, MnCl 2.4H 2 O, 0.05, (NH 4) 6 Mo 7 O 24.4H 2 O, 0.05, AlCl 3, 0.05, CoCl 2.6H 2 O, 0.05, NiCl 2. 2 O, 0.090.092, Na 2. 3.9H 9O, 0.1, vitamin B, vitamin B, niacin, vitamin B, and vitamin B.
Example 1
In the embodiment, the COD of the carbon-rich nutrient substrate is 5000 mg/L, the antibiotic wastewater is taken from a laboratory for self-water distribution, and the concentration of the ciprofloxacin is 100 mg/L. The method for treating the anaerobic sludge by adopting the iron-carbon micro-electrolysis coupling comprises the following specific steps:
(1) Putting anaerobic activated sludge into an anaerobic bottle, adding a carbon-rich nutrient substrate and sludge, mixing and domesticating, wherein the volume ratio of the anaerobic activated sludge to the carbon-rich nutrient substrate is 1:10, introducing nitrogen into the anaerobic bottle for 15 minutes to remove oxygen, sealing, and domesticating at 37 +/-1 ℃ for 12 hours.
(2) Removing supernatant, mixing the lower layer sludge with the ciprofloxacin antibiotic wastewater in a volume ratio of 1:20, and adding zero-valent nano iron and granular activated carbon (the iron-carbon ratio is 1: 1) with the mass ratio of the volatile solids of the lower layer sludge being 1: 1. And introducing nitrogen into the anaerobic bottle for 15 minutes to remove oxygen, sealing, and performing anaerobic acidogenic fermentation for 8 hours at the temperature of 37 +/-1 ℃ and the speed of 120 r/min.
when the water inlet and the water outlet are measured, the ciprofloxacin removal rate reaches 96 percent, the COD removal rate reaches 28 percent, and the method has high-efficiency pretreatment capability.
Example 2
in the embodiment, the COD concentration of the carbon-rich nutrient substrate is 8000mg/L, the antibiotic wastewater is taken from the comprehensive wastewater of an antibiotic pharmaceutical factory, the concentration of ciprofloxacin is 42 mg/L, and the specific implementation steps are as follows:
(1) Putting anaerobic activated sludge into an anaerobic bottle, adding a carbon-rich nutrient substrate and sludge, mixing and acclimating, wherein the volume ratio of the sludge to the carbon-rich nutrient substrate is 1:10, introducing nitrogen into the anaerobic bottle for 15 minutes to remove oxygen, sealing, and acclimating at 37 +/-1 ℃ for 10 hours.
(2) Removing supernatant, mixing the lower layer sludge with the antibiotic wastewater in a volume ratio of 1:15, and adding zero-valent nano iron and granular activated carbon (iron-carbon ratio is 1: 1) in a mass ratio of 1:1 to the volatile solid of the sludge. Introducing nitrogen into the anaerobic reactor for 15 minutes to remove oxygen, sealing, and performing anaerobic acidogenic fermentation for 8 hours at the temperature of 37 +/-1 ℃ and the speed of 120 r/min.
When the water inlet and the water outlet are measured, the ciprofloxacin removal rate reaches 93 percent, and the COD removal rate reaches 20 percent, so the method has good removal efficiency on the high-concentration ciprofloxacin antibiotic wastewater, and can remove part of COD.
Example 3
In the embodiment, the COD of the carbon-rich nutrient substrate is 5000 mg/L, the antibiotic wastewater is taken from laboratory water distribution, and the concentration of enrofloxacin is 30 mg/L. The method for treating by adopting the iron-carbon micro-electrolysis coupling anaerobic acidogenic fermentation process comprises the following specific steps:
(1) Putting anaerobic activated sludge into an anaerobic bottle, adding a carbon-rich nutrient substrate and sludge, mixing, acclimating, wherein the volume ratio of the anaerobic activated sludge to the carbon-rich nutrient substrate is 1:15, introducing nitrogen into the anaerobic bottle for 15 minutes to remove oxygen, sealing, and acclimating at 37 +/-1 ℃ for 12 hours.
(2) Removing supernatant, mixing the lower layer sludge with the enrofloxacin antibiotic wastewater in a volume ratio of 1:15, and adding zero-valent nano iron and granular activated carbon (iron-carbon ratio is 1: 1) in a mass ratio of 1:1 to the volatile solid of the sludge. Introducing nitrogen into the anaerobic reactor for 15 minutes to remove oxygen, sealing, and performing anaerobic acidogenic fermentation for 7 hours at the temperature of 37 +/-1 ℃ and at the speed of 120 r/min.
When the water inlet and the water outlet are measured, the removal rate of enrofloxacin reaches 90 percent, and the removal rate of COD reaches 22 percent.
Claims (9)
1. A method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using an iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process comprises the following steps:
(1) The anaerobic activated sludge with normal performance index and pH of 7.0 ~ 8.0.0 is mixed with the carbon-rich nutrient substrate according to a certain proportion for domestication;
(2) Introducing high-purity nitrogen to ensure that the reaction system is in an anaerobic state;
(3) Discharging supernatant after natural precipitation, and reserving sludge at the lower layer, namely sludge at the anaerobic acid production stage with the required pH value of 4.0 ~ 5.5.5;
(4) Mixing the sludge in the anaerobic acid production stage in the step 3 with high-concentration fluoroquinolone antibiotic wastewater;
(5) Adding zero-valent nano iron and granular activated carbon into the mixture obtained in the step 4, namely an iron-carbon mixture;
(6) And (5) introducing high-purity nitrogen into the mixture in the step (5) to ensure that the reaction system is in an anaerobic state.
2. The method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process as claimed in claim 1, wherein the COD concentration of the carbon-rich nutrient substrate in the step 1 is 5000 ~ 8000mg/L and 8000 mg/L.
3. The method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process as claimed in claim 1, wherein the volume ratio of the carbon-rich nutrient substrate to the sludge in step 1 is 10:1 ~ 15: 1.
4. The method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process as claimed in claim 1, wherein the reaction temperature in step 2 is 37 +/-1 ℃, and the reaction time is 10 ~ 12 hours.
5. The method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process as claimed in claim 1, wherein the volume ratio of the wastewater to sludge in the anaerobic acidogenic stage in the step 4 is 15:1 ~ 20: 1.
6. the method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process as claimed in claim 1, wherein the mass ratio of the zero-valent nano iron to the granular activated carbon in step 5 is 1: 1.
7. The method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process as claimed in claim 1, wherein the mass ratio of the iron-carbon mixture to the volatile solids of sludge in the anaerobic acidogenic stage in the step 5 is 1:1 ~ 1.5.5: 1.
8. The method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupling anaerobic acidogenic fermentation process as claimed in claim 1, wherein the reaction temperature in step 6 is 37 +/-1 ℃, and the reaction time is 6 ~ 8 hours.
9. The method for pretreating high-concentration fluoroquinolone antibiotic wastewater by using the iron-carbon microelectrolysis coupled anaerobic acidogenic fermentation process as claimed in claim 1, wherein the fluoroquinolone antibiotic is especially referred to as ciprofloxacin.
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Cited By (6)
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| CN111592093A (en) * | 2020-05-25 | 2020-08-28 | 中国科学院城市环境研究所 | Phenolic aldehyde wastewater treatment method |
| CN111777162A (en) * | 2020-07-06 | 2020-10-16 | 苏州达道环保科技有限公司 | Method for treating wastewater by coupling iron-carbon micro-electrolysis and anaerobic organisms |
| CN111943426A (en) * | 2020-07-10 | 2020-11-17 | 同济大学 | Treatment method of high-salt-content pharmaceutical wastewater |
| CN113636733A (en) * | 2021-08-23 | 2021-11-12 | 宁波财经学院 | Ozone promotes sludge digestion device |
| CN114409057A (en) * | 2021-12-30 | 2022-04-29 | 海南大学 | Method for reducing and degrading enrofloxacin by utilizing biocathode co-metabolic system |
| CN115124209A (en) * | 2022-07-28 | 2022-09-30 | 同济大学 | Method for promoting sludge to produce methane by using antiviral drugs |
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| CN111592093A (en) * | 2020-05-25 | 2020-08-28 | 中国科学院城市环境研究所 | Phenolic aldehyde wastewater treatment method |
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| CN113636733A (en) * | 2021-08-23 | 2021-11-12 | 宁波财经学院 | Ozone promotes sludge digestion device |
| CN113636733B (en) * | 2021-08-23 | 2022-11-15 | 宁波财经学院 | Ozone promotes sludge digestion device |
| CN114409057A (en) * | 2021-12-30 | 2022-04-29 | 海南大学 | Method for reducing and degrading enrofloxacin by utilizing biocathode co-metabolic system |
| CN114409057B (en) * | 2021-12-30 | 2023-09-19 | 海南大学 | Method for reducing and degrading enrofloxacin by using biological cathode co-metabolism system |
| CN115124209A (en) * | 2022-07-28 | 2022-09-30 | 同济大学 | Method for promoting sludge to produce methane by using antiviral drugs |
| CN115124209B (en) * | 2022-07-28 | 2023-09-15 | 同济大学 | Method for promoting sludge to produce methane by using antiviral drugs |
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