CN112960724A - Method for removing veterinary antibiotics by active materials - Google Patents
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- CN112960724A CN112960724A CN202110155775.6A CN202110155775A CN112960724A CN 112960724 A CN112960724 A CN 112960724A CN 202110155775 A CN202110155775 A CN 202110155775A CN 112960724 A CN112960724 A CN 112960724A
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
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- Environmental & Geological Engineering (AREA)
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
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Abstract
The invention belongs to the technical field of antibiotic removal. The invention provides a method for removing antibiotics for livestock by using active materials, which comprises the following steps: filling a porous material and quartz sand into a stainless steel column; sequentially introducing a background solution 1 and a background solution 2 into the stainless steel column from bottom to top; injecting the solution to be treated containing the veterinary antibiotics into a stainless steel column; the porous material is zero-valent iron filings, calcined magnesite, straw biochar or limestone; the particle size of the zero-valent iron chips is 0.45-0.85 mm, the particle size of the calcined magnesite is 0.45-0.85 mm, the particle size of the straw biochar is less than or equal to 2mm, and the particle size of the limestone is 1.0-1.7 mm. The invention has the highest retention rate of 91.85 percent on sulfamethoxazole and 95.01 percent on erythromycin.
Description
Technical Field
The invention relates to the technical field of antibiotic removal, in particular to a method for removing antibiotics for livestock by using an active material.
Background
In recent years, the pollution problem caused by the antibiotics for animals in the environment is increasingly serious, and the detection rate of the antibiotics for animals in the environments such as breeding wastewater, sewage treatment plants, farmland soil and the like is very high and even reaches more than 90%. On one hand, the abuse phenomenon of veterinary antibiotics in a farm is serious, so that the utilization rate of the bred livestock and poultry is low, and about 30-90% of the antibiotics are excreted; on the other hand, because of the lack of treatment facilities in small farms, which occupy a large proportion of the breeding industry, the breeding wastewater or manure is directly applied as fertilizer into the soil. The harm of the antibiotic for animals to the ecological environment is mainly three points: firstly, the growth activity of microorganisms is inhibited to enable the microorganisms to generate resistance genes or drug-resistant super bacteria, secondly, the bioavailability of veterinary antibiotics in animals and plants is high, the antibiotics can be continuously enriched in the animals and plants to influence the normal development and growth of the animals and plants, thirdly, the antibiotics can be continuously accumulated and transmitted in a food chain, so that the antibiotics are gradually accumulated in human bodies to cause pathological changes, and unpredictable influence is generated on an ecosystem and human health.
At present, chemical, physical and biological methods used by sewage treatment plants, such as coagulating sedimentation, membrane separation, activated sludge method and the like, are mainly used for treating high-concentration domestic sewage and industrial wastewater, so that trace veterinary antibiotics in the wastewater are difficult to effectively remove, and even the concentration of the veterinary antibiotics in some treated wastewater is higher than that of the veterinary antibiotics at a water inlet end. And other research methods with high removal rate are changed by various experimental conditions, so that the practical application value is low and the price is high. Therefore, the research and development of the method for removing the antibiotic for the livestock in the environment with high removal rate, low cost and simple used equipment have important significance and value.
Disclosure of Invention
The invention aims to provide a method for removing antibiotics from livestock by using active materials, aiming at overcoming the defects of the prior art. The removal method is simple and easy to implement, and has high removal efficiency on the antibiotics for livestock. The maximum rejection rate of the zero-valent iron chips and the quartz sand with the volume ratio of 1:3 to the sulfamethoxazole can reach 91.85 percent; the maximum retention rate of the corn straw biochar and the quartz sand with the volume ratio of 1:2.5 to the erythromycin can reach 95.01%.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for removing antibiotics for livestock by using active materials, which comprises the following steps:
1) filling a porous material and quartz sand into a stainless steel column;
2) sequentially introducing a background solution 1 and a background solution 2 into the stainless steel column from bottom to top;
3) injecting the solution to be treated containing the veterinary antibiotics into a stainless steel column;
step 1) the porous material is zero-valent iron chips, calcined magnesite, straw biochar or limestone; the particle size of the zero-valent iron chips is 0.45-0.85 mm, the particle size of the calcined magnesite is 0.45-0.85 mm, the particle size of the straw biochar is less than or equal to 2mm, and the particle size of the limestone is 1.0-1.7 mm.
Preferably, the stainless steel column is cylindrical, the inner diameter of the stainless steel column is 0.7-1.3 cm, and the height of the stainless steel column is 4-7 cm; the filling mode is dry filling.
Preferably, the volume ratio of the porous material to the quartz sand in the step 1) is 1: 2-4.
Preferably, the background solution 1 in the step 2) is a NaCl solution, and the concentration of the NaCl solution is 8-12 mmol/L; the introduction time of the background solution 1 is 2-3 h.
Preferably, the background solution 2 in the step 2) contains trace Br-The NaCl solution of (2); in background solution 2, Br-The concentration of the NaCl solution is 550-650 mg/L, and the concentration of the NaCl solution is 8-12 mmol/L; the introduction time of the background solution 2 is 2-3 h.
Preferably, when the porous material is zero-valent iron filings, the flow rates of the background solution 1 and the background solution 2 are both 3-3.5 mL/h; when the porous material is calcined magnesite, the flow rates of the background solution 1 and the background solution 2 are both 3.3-4 mL/h; when the porous material is straw biochar, the flow rates of the background solution 1 and the background solution 2 are both 3.2-3.9 mL/h; when the porous material is limestone, the flow rates of the background solution 1 and the background solution 2 are both 2.3-3 mL/h.
Preferably, the injection position in the step 3) is the lower end of a stainless steel column; the contact time of the solution to be treated containing the veterinary antibiotics and the porous material in the stainless steel column is 0.3-0.8 h.
Preferably, in the solution to be treated containing the veterinary antibiotic in the step 3), the solvent is water, and the concentration of the veterinary antibiotic is 80-120 μ g/L.
Preferably, the veterinary antibiotic in the step 3) is sulfamethoxazole, tilmicosin, tylosin, erythromycin, ciprofloxacin, enrofloxacin or norfloxacin.
The invention has the beneficial effects that:
the removal method is simple and easy to implement, and has high removal efficiency on the antibiotics for livestock. The maximum rejection rate of the zero-valent iron chips and the quartz sand with the volume ratio of 1:3 to the sulfamethoxazole can reach 91.85 percent; the maximum retention rate of the corn straw biochar and the quartz sand with the volume ratio of 1:2.5 to the erythromycin can reach 95.01%.
Detailed Description
The invention provides a method for removing antibiotics for livestock by using active materials, which comprises the following steps:
1) filling a porous material and quartz sand into a stainless steel column;
2) sequentially introducing a background solution 1 and a background solution 2 into the stainless steel column from bottom to top;
3) injecting the solution to be treated containing the veterinary antibiotics into a stainless steel column;
step 1) the porous material is zero-valent iron chips, calcined magnesite, straw biochar or limestone; the particle size of the zero-valent iron chips is 0.45-0.85 mm, the particle size of the calcined magnesite is 0.45-0.85 mm, the particle size of the straw biochar is less than or equal to 2mm, and the particle size of the limestone is 1.0-1.7 mm.
The particle size of the zero-valent iron chips is preferably 0.5-0.8 mm, and more preferably 0.6-0.7 mm; the zero-valent iron scraps are preferably industrial waste; the particle size of the calcined magnesite is preferably 0.5-0.8 mm, more preferably 0.6-0.7 mm, and the calcined magnesite is preferably a mining byproduct; the grain size of the straw biochar is preferably less than or equal to 1mm, and the straw biochar is preferably corn straw biochar; the particle size of the limestone is preferably 1.2-1.6 mm, and more preferably 1.3-1.5 mm; the limestone is preferably natural minerals; the zero-valent iron chips, the calcined magnesite, the straw biochar or the limestone are directly used without chemical treatment.
The stainless steel column is preferably cylindrical, and the inner diameter of the stainless steel column is preferably 0.7-1.3 cm, more preferably 0.9-1.1 cm, and even more preferably 1.0 cm; the height of the stainless steel column is preferably 4-7 cm, more preferably 5-6.5 cm, and further preferably 5.28-6 cm.
The filling mode in the step 1) is preferably dry filling; the filling is preferably performed by a funnel; in the filling process, preferably knocking the column body every time when 0.8-1.2 cm of the stainless steel column is filled, so that the porous materials in the stainless steel column are uniformly and compactly distributed; further preferably 1 cm.
According to the invention, the stainless steel column is preferably arranged in the area through which the wastewater flows in the farm, and the solution to be treated containing the veterinary antibiotics and four low-cost industrial and agricultural materials (limestone, calcined magnesite, straw biochar and scrap iron) filled in the stainless steel column are subjected to adsorption, degradation and other reactions, so that the pollution of the veterinary antibiotics in the environment is reduced.
The volume ratio of the porous material and the quartz sand in the step 1) is preferably 1: 2-4, and more preferably 1:3.
Preferably, in the step 2) of the invention, the stainless steel column is vertically fixed and then sequentially injected with the background solution 1 and the background solution 2; the background solution 1 is preferably a NaCl solution, and the concentration of the NaCl solution is preferably 8-12 mmol/L, more preferably 9-11 mmol/L, and more preferably 10 mmol/L; the background solution 1 is preferably a degassed solution; the introduction time of the background solution 1 is preferably 2-3 h, and more preferably 2.5 h.
The purpose of the invention for passing background solution 1 is to stabilize the stainless steel column system and achieve the required hydraulic and chemical equilibrium.
The background solution 2 in step 2) of the invention preferably contains trace Br-Of NaCl solution(ii) a In background solution 2, Br-The concentration of (b) is preferably 550-650 mg/L, more preferably 570-620 mg/L, and even more preferably 590-600 mg/L; the concentration of the NaCl solution is preferably 8-12 mmol/L, and more preferably 9-10 mmol/L; the background solution 2 is preferably a degassed solution; the introduction time of the background solution 2 is preferably 2-3 h, and more preferably 2.5 h.
According to the invention, the background solution 2 flowing out of the stainless steel column is preferably collected every 7-8 min, and the further preference is 7.5 min; the purpose of collecting background solution 2 was to study Br-The penetration curve in the stainless steel column was examined for the contact time of the background solution 2 with the porous material in the stainless steel column and whether the system was stable.
According to the invention, the background solution 1 and the background solution 2 are preferably pumped into the stainless steel column body by adopting a peristaltic pump.
When the porous material is zero-valent iron chips, the flow rates of the background solution 1 and the background solution 2 are preferably 3-3.5 mL/h, and more preferably 3.15-3.3 mL/h; when the porous material is calcined magnesite, the flow rates of the background solution 1 and the background solution 2 are preferably 3.3-4 mL/h, more preferably 3.5-3.8 mL/h, and even more preferably 3.6-3.7 mL/h; when the porous material is straw biochar, the flow rates of the background solution 1 and the background solution 2 are preferably 3.2-3.9 mL/h, more preferably 3.3-3.7 mL/h, and even more preferably 3.52-3.6 mL/h; when the porous material is limestone, the flow rates of the background solution 1 and the background solution 2 are preferably 2.3-3 mL/h, more preferably 2.5-2.8 mL/h, and even more preferably 2.58-2.7 mL/h.
The position of the injection in the step 3) of the invention is preferably the lower end of a stainless steel column; the contact time of the solution to be treated containing the veterinary antibiotics and the porous material in the stainless steel column is preferably 0.3-0.8 h, and further preferably 0.5-0.7 h.
In the solution to be treated containing the veterinary antibiotics in the step 3), the solvent is preferably water, and the concentration of each veterinary antibiotic is preferably 80-120 mug/L, more preferably 90-110 mug/L, and even more preferably 100 mug/L; the solution to be treated of the veterinary antibiotic preferably contains sodium chloride; in the solution to be treated of the sodium chloride-containing veterinary antibiotic, the ion concentration is preferably 8-12 mmol/L, and more preferably 9-10 mmol/L; according to the invention, after the solution to be treated containing the veterinary antibiotics is injected into the stainless steel column, the effluent is preferably collected at the outlet of the stainless steel column; the collection interval time is preferably 0.3-0.8 h, and further preferably 0.5-0.6 h; the collection is preferably a fraction collector.
The veterinary antibiotic in the step 3) is preferably sulfamethoxazole, tilmicosin, tylosin, erythromycin, ciprofloxacin, enrofloxacin or norfloxacin; the concentration of each veterinary antibiotic is preferably 90-110 mu g/L, and more preferably 100 mu g/L.
After the injection of the solution to be treated containing the veterinary antibiotics is finished, the column is preferably washed by NaCl solution and NaCl solution containing 20 wt% of ethanol in sequence; the concentration of the NaCl solution is preferably 8-12 mmol/L, and more preferably 9-10 mmol/L.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Zero-valent iron pieces (particle size of 0.6mm) and quartz sand in a volume ratio of 1:3 were filled into a cylindrical stainless steel column (inner diameter of 1cm, height of 5.28cm) by a funnel by a dry method. After uniform and compact filling, vertically fixing a stainless steel column, and injecting 10mmol/L degassed NaCl solution from the lower end of the stainless steel column to the top by a peristaltic pump, wherein the flow rate of the NaCl solution is 3.15mL/min, and the introduction time is 2.5 h; then introducing degassed tracer Br from bottom to top-NaCl solution (Br)-The concentration of (1) was 600mg/L, the concentration of the NaCl solution was 10mmol/L), the flow rate was 3.15mL/min, and the flow-in time was 2.5 h. And then injecting a wastewater solution containing veterinary antibiotics (the concentration of each veterinary antibiotic is 100 mug/L) into the stainless steel column from the lower end of the stainless steel column, wherein the contact time of the aqueous solution containing veterinary antibiotics with zero-valent scrap iron and quartz sand is 0.5 h. And automatically collecting the treated water solution containing the veterinary antibiotics at the outlet of the stainless steel column by using a fraction collector every 0.5 h.
Example 1 within 50h of the PRB plant operation, zero-valent iron filings and silica sand in a volume ratio of 1:3 can effectively remove six veterinary antibiotics in wastewater: sulfamethoxazole, tilmicosin, tylosin, ciprofloxacin, enrofloxacin and norfloxacin. Wherein the highest retention rate of sulfamethoxazole can reach 91.85%. Cumulative retention and cumulative retention of six veterinary antibiotics within 50h of PRB plant operation are shown in table 1.
TABLE 1 cumulative retention and cumulative retention of zero-valent iron filings and quartz sand to veterinary antibiotics
Example 2
Corn stalk biochar (particle size of 1.5mm) and quartz sand in a volume ratio of 1:2.5 were filled into a cylindrical stainless steel column (inner diameter of 1cm, height of 5.28cm) by a funnel by a dry method. After uniform and compact filling, vertically fixing a stainless steel column, and injecting 9mmol/L degassed NaCl solution from the lower end of the stainless steel column to the top by adopting a peristaltic pump, wherein the flow rate of the NaCl solution is 3.52mL/min, and the introduction time is 2.5 h; then introducing degassed tracer Br from bottom to top-NaCl solution (Br)-The concentration of (3) was 570mg/L, the concentration of the NaCl solution was 9mmol/L), the flow rate was 3.52mL/min, and the flow-in time was 3 hours. And injecting a wastewater solution containing veterinary antibiotics (the concentration of each veterinary antibiotic is 100 mug/L) into the stainless steel column from the lower end of the stainless steel column, wherein the contact time of the aqueous solution containing veterinary antibiotics with the corn stalk biochar and the quartz sand is 0.5 h. And automatically collecting the treated water solution containing the veterinary antibiotics at the outlet of the stainless steel column by using a fraction collector every 0.5 h.
Example 2 within 50h of PRB plant operation, corn straw biochar and quartz sand in a volume ratio of 1:2.5 can effectively remove six veterinary antibiotics in wastewater: tilmicosin, tylosin, erythromycin, ciprofloxacin, enrofloxacin and norfloxacin. Wherein, the retention rate of the erythromycin can reach 95.01 percent at most. Cumulative retention and cumulative retention of six veterinary antibiotics within 50h of PRB plant operation are shown in table 2.
TABLE 2 retention rate and retention amount of corn stalk biochar and quartz sand for veterinary antibiotics
Example 3
Limestone (particle size 1.4mm) and quartz sand in a volume ratio of 1:3.5 were filled into a cylindrical stainless steel column (inner diameter 1cm, height 5.28cm) by dry method using a funnel. After uniform and compact filling, vertically fixing a stainless steel column, and injecting 11mmol/L degassed NaCl solution from the lower end of the stainless steel column to the top by a peristaltic pump, wherein the flow rate of the NaCl solution is 2.58mL/min, and the introduction time is 2 h; then introducing degassed tracer Br from bottom to top-NaCl solution (Br)-The concentration of (1) was 620mg/L, the concentration of the NaCl solution was 11mmol/L), the flow rate was 2.58mL/min, and the flow-in time was 2.5 h. And then injecting a wastewater solution containing veterinary antibiotics (the concentration of each veterinary antibiotic is 100 mug/L) into the stainless steel column from the lower end of the stainless steel column, wherein the contact time of the aqueous solution containing veterinary antibiotics with limestone and quartz sand is 0.5 h. And automatically collecting the treated water solution containing the veterinary antibiotics at the outlet of the stainless steel column by using a fraction collector every 0.5 h.
Example 3 within 50h of PRB plant operation, limestone and quartz sand in a 1:3.5 volume ratio were able to effectively remove three veterinary antibiotics in wastewater: tilmicosin, tylosin and ciprofloxacin. Cumulative retention and cumulative retention of three veterinary antibiotics within 50h of PRB plant operation are shown in table 3.
TABLE 3 cumulative percent retention and cumulative percent retention of limestone and silica sand to veterinary antibiotics
| Antibiotic | Ciprofloxacin | Tylosin | Tilmicosin |
| Retention (%) | 61.05 | 57.94 | 48.45 |
| Cut-off (mg/kg) | 7.72 | 7.32 | 6.12 |
Comparative example 1
The porous materials of this comparative example were all quartz sand without addition of zero-valent iron pieces, and the other conditions were the same as in example 1.
Cumulative retention and cumulative retention of seven veterinary antibiotics within 50h of PRB plant operation with silica sand are shown in table 4.
TABLE 4 cumulative retention and cumulative retention of quartz sand to veterinary antibiotics
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for removing antibiotics from animals by using active materials, which is characterized by comprising the following steps:
1) filling a porous material and quartz sand into a stainless steel column;
2) sequentially introducing a background solution 1 and a background solution 2 into the stainless steel column from bottom to top;
3) injecting the solution to be treated containing the veterinary antibiotics into a stainless steel column;
step 1) the porous material is zero-valent iron chips, calcined magnesite, straw biochar or limestone; the particle size of the zero-valent iron chips is 0.45-0.85 mm, the particle size of the calcined magnesite is 0.45-0.85 mm, the particle size of the straw biochar is less than or equal to 2mm, and the particle size of the limestone is 1.0-1.7 mm.
2. The removal method according to claim 1, wherein the stainless steel column is cylindrical in shape, has an inner diameter of 0.7 to 1.3cm and a height of 4 to 7 cm; the filling mode is dry filling.
3. The removing method according to claim 1 or 2, wherein the volume ratio of the porous material and the quartz sand in the step 1) is 1: 2-4.
4. The removing method according to claim 3, wherein the background solution 1 in the step 2) is a NaCl solution, and the concentration of the NaCl solution is 8-12 mmol/L; the introduction time of the background solution 1 is 2-3 h.
5. The removal method according to claim 4, wherein the background solution 2 in the step 2) contains trace Br-The NaCl solution of (2); in background solution 2, Br-The concentration of the NaCl solution is 550-650 mg/L, and the concentration of the NaCl solution is 8-12 mmol/L; the introduction time of the background solution 2 is 2-3 h.
6. The removing method according to claim 5, wherein when the porous material is zero-valent iron pieces, the flow rates of the background solution 1 and the background solution 2 are both 3-3.5 mL/h; when the porous material is calcined magnesite, the flow rates of the background solution 1 and the background solution 2 are both 3.3-4 mL/h; when the porous material is straw biochar, the flow rates of the background solution 1 and the background solution 2 are both 3.2-3.9 mL/h; when the porous material is limestone, the flow rates of the background solution 1 and the background solution 2 are both 2.3-3 mL/h.
7. The removal method according to claim 5 or 6, wherein the injection position of step 3) is the lower end of a stainless steel column; the contact time of the solution to be treated containing the veterinary antibiotics and the porous material in the stainless steel column is 0.3-0.8 h.
8. The removal method according to claim 7, wherein the solution to be treated containing the veterinary antibiotic in the step 3) is water, and the concentration of the veterinary antibiotic is 80-120 μ g/L.
9. The removal method according to claim 8, wherein the veterinary antibiotic of step 3) is sulfamethoxazole, tilmicosin, tylosin, erythromycin, ciprofloxacin, enrofloxacin or norfloxacin.
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