CN109534477B - Method for degrading lincomycin - Google Patents
Method for degrading lincomycin Download PDFInfo
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- CN109534477B CN109534477B CN201811456473.7A CN201811456473A CN109534477B CN 109534477 B CN109534477 B CN 109534477B CN 201811456473 A CN201811456473 A CN 201811456473A CN 109534477 B CN109534477 B CN 109534477B
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention discloses a method for degrading lincomycin, which comprises the following steps of (1) preparing hydrochloric acid solution of lincomycin; (2) mixing iron powder, hydrogen peroxide and hydrochloric acid solution of lincomycin to obtain mixed solution; (3) adding antioxidant into the mixed solution, and placing on a constant temperature oscillation box for oscillation. The invention has the beneficial effects that: the method for degrading lincomycin is simple, convenient to operate, low in cost, wide in application range and suitable for large-scale popularization and application. In addition, the method also provides a new idea for the degradation work of other antibiotics and organic matters. Hydroxyl free radicals generated by the reaction of a Fenton-like reaction system consisting of divalent iron ions and hydrogen peroxide attack lincomycin to degrade the lincomycin, and the low-price and simple operation performance of the lincomycin are applied to the removal of the antibiotic-containing wastewater.
Description
Technical Field
The invention relates to the technical field of lincomycin degradation, in particular to a lincomycin degradation method.
Background
Lincomycin, a typical contaminant of PPCPs, is very effective in killing gram-positive bacteria and is therefore widely used in human and animal medicine, mainly for respiratory infections, osteomyelitis, joint and soft tissue infections, biliary tract infections and septicaemia caused by staphylococci, streptococci, streptococcus pneumoniae. The residue of lincomycin brings adverse effect to a aquatic ecosystem, causes the generation of various drug-resistant bacteria, and poses potential threat to human health in the modes of drinking water, food chain and the like. High concentrations of lincomycin are mainly caused by the large amount of waste streams from animal farms flowing into rivers and lakes. In china, lincomycin is used in the third of all antibiotics. The safety problem of animal-derived foods caused by lincomycin is concerned by people, the limit of lincomycin in animal-derived foods is strictly regulated in European Union and China, and the maximum residual quantity of lincomycin is 1 microgram/kg. Lincomycin molecules are mainly composed of three functional groups, namely a pyranose ring, an amido group and a pyrrolidine ring, and are difficult to be effectively degraded by a conventional wastewater treatment method due to complex structures. Therefore, the method for degrading the lincomycin is of great significance.
At present, the degradation method of lincomycin mainly comprises a physical method, a biological method, an advanced oxidation technology and the like. The physical method is mainly to treat the lincomycin solution by using methods of instant high energy release such as gamma-radiation, electron beam radiation, dielectric barrier discharge and the like, thereby destroying the molecular structure of the lincomycin solution and achieving the purpose of degradation. However, the physical method has high requirements for equipment, and the problems of cost and operation difficulty cause that the physical method is difficult to popularize and apply. The biological method is a method for effectively degrading lincomycin by culturing microorganisms or bacteria with a specific degradation effect on the lincomycin, and is also the most studied method at present. However, since the biological method has problems such as a long reaction period and an excessively large floor space, it is difficult to effectively use the method. The advanced oxidation technology mainly comprises technologies such as a photocatalytic oxidation method, an ozone catalytic oxidation method and the like, has obvious degradation effect on lincomycin, however, the cost is still too high, and certain requirements are made on operation.
Disclosure of Invention
The invention aims to provide a method for degrading lincomycin, which aims to overcome the defects of difficult operation and high cost of the existing lincomycin degradation technology.
To this end, the present invention provides a method for the degradation of lincomycin, said method comprising the steps of:
(1) preparing hydrochloric acid solution of lincomycin;
(2) mixing a Fenton-like reaction system consisting of iron powder and hydrogen peroxide with a hydrochloric acid solution of lincomycin to obtain a mixed solution;
(3) adding antioxidant into the mixed solution, and placing on a constant temperature oscillation box for oscillation.
Preferably, in the step (1), the prepared hydrochloric acid solution of lincomycin has a concentration of 10-30mg/L and a pH value of 5-7.
Preferably, in the step (2), the iron powder is micron-sized reduced iron powder, and the adding amount of the iron powder is 0.1-2 g/L.
Preferably, in the step (2), the adding amount of the hydrogen peroxide is 0.1 mM-10M.
Preferably, in the step (3), the antioxidant is at least one of polyphenols, flavonoids, hydroxylamine and the like.
Preferably, in the step (3), the antioxidant is added in an amount of 0.001mM-1 mM.
Preferably, in the step (3), the oscillation speed is 150-400 rpm.
Preferably, in the step (3), the reaction temperature is oscillated at 20 to 80 ℃.
Preferably, in the step (3), the reaction time is 60-180min under oscillation.
Compared with the prior art, the invention has the advantages and positive effects that: the invention provides a method for degrading lincomycin, which comprises the following steps: (1) preparing hydrochloric acid solution of lincomycin; (2) mixing iron powder, hydrogen peroxide and hydrochloric acid solution of lincomycin to obtain mixed solution; (3) adding antioxidant into the mixed solution, and placing on a constant temperature oscillation box for oscillation. The invention has the beneficial effects that: the method for degrading lincomycin is simple, convenient to operate, low in cost, wide in application range and suitable for large-scale popularization and application. In addition, the method also provides a new idea for the degradation work of other antibiotics and organic matters. Hydroxyl free radicals generated by the reaction of a Fenton-like reaction system consisting of divalent iron ions and hydrogen peroxide attack lincomycin to degrade the lincomycin, and the low-price and simple operation performance of the lincomycin are applied to the removal of the antibiotic-containing wastewater.
Other features and advantages of the present invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
Drawings
FIG. 1 is a graph comparing the degradation effect of different Fenton-like reaction systems of example 1 on lincomycin;
FIG. 2 is a graph comparing the degradation effect of different Fenton-like reaction systems of example 2 on lincomycin;
FIG. 3 is a graph comparing the degradation effect of different Fenton-like reaction systems of example 3 on lincomycin;
FIG. 4 is a graph comparing the degradation effect of different amounts of tea polyphenols on lincomycin in example 4;
FIG. 5 is a graph comparing the degradation effect of different reaction systems of example 5 on lincomycin.
Detailed Description
The following detailed description of specific embodiments of the present invention is provided to illustrate and explain the present invention and to be understood not to limit the present invention.
The invention provides a method for degrading lincomycin, which comprises the following steps:
(1) preparing hydrochloric acid solution of lincomycin;
(2) mixing a Fenton-like reaction system consisting of iron powder and hydrogen peroxide with a hydrochloric acid solution of lincomycin,
obtaining a mixed solution; (3) adding antioxidant into the mixed solution, and placing on a constant temperature oscillation box for oscillation.
In the step (1), the prepared hydrochloric acid solution of the lincomycin has the concentration of 10-30mg/L and the pH value of 5-7.
In the step (2), the iron powder is micron-sized reduced iron powder, and the adding amount of the iron powder is 0.1-2 g/L.
In the step (2), the adding amount of the hydrogen peroxide is 0.1 mM-10M.
In the step (3), the antioxidant is at least one of polyphenols, flavonoids, hydroxylamine and the like.
In the step (3), the addition amount of the antioxidant is 0.001mM-1 mM.
In the step (3), the oscillation speed is 150-400 rpm.
In the step (3), the reaction temperature is oscillated to 20-80 ℃.
In the step (3), the oscillation reaction time is 60-180 min.
Example 1
The method for degrading lincomycin comprises the following steps:
(1) preparing 100mL of hydrochloric acid solution of lincomycin with the concentration of 20mg/L, and determining that the initial pH value is 5.8;
(2) adding a Fenton-like reaction system consisting of 0.1g of reduced iron powder and 1mL of hydrogen peroxide with the concentration of 10M into a prepared hydrochloric acid solution of lincomycin to obtain a mixed solution;
(3) adding four 1mL antioxidants with the concentration of 10mM into the mixed solution obtained in the step (2) respectively, placing the mixed solution on a constant-temperature oscillator for reaction, and setting the rotation speed to be 200rpm and the temperature to be 25 ℃.
A comparative Fenton-like reaction system S1 was set, and the comparative Fenton-like reaction system contained only 0.1g of reduced iron powder. The four antioxidants are hydroxylamine, catechin, tea polyphenol and glucose respectively, and the corresponding four fenton-like reaction systems are S2, S3, S4 and S5 respectively. And (3) oscillating for 2 hours, sampling and testing at 0.5h, 1.0h, 1.5h and 2.0h respectively, measuring the concentration of the residual lincomycin by using a high performance liquid chromatograph, and calculating the removal rate eta by taking the average value Ce of the concentration.
η=(C0-Ce)/C0
FIG. 1 is a graph comparing the degradation effect of different Fenton-like reaction systems of this example on lincomycin, and it can be seen from FIG. 1,
after the antioxidant is added, the degradation efficiency of the lincomycin is greatly improved. After 2 hours of reaction, the degradation rate of lincomycin of the comparative Fenton reaction system S1 is about 35%, the degradation rate of the comparative Fenton reaction system S2 added with hydroxylamine reaches 63%, and the lincomycin of the comparative Fenton reaction system S4 added with tea polyphenol is almost completely removed even after 1 hour of reaction, which is probably because a large amount of OH contained in hydroxylamine and tea polyphenol promotes the occurrence of Fenton effect on the surface of iron powder. The promotion effect of the comparative fenton-like reaction system S3 and the comparative fenton-like reaction system S5 is not obvious, and is similar to the effect of the comparative fenton-like reaction system S1, which may be related to the molecular structures of catechin and glucose.
Example 2
The method for degrading lincomycin comprises the following steps:
(1) preparing 100mL of hydrochloric acid solution of lincomycin with the concentration of 20mg/L, and determining that the initial pH value is 5.8;
(2) adding a Fenton-like reaction system consisting of 0.1M hydrogen peroxide and 0.2mL, 0.5mL, 1.0mL, 1.5mL, 2.0mL and 3.0mL of 0.1M reduced iron powder and the volumes of hydrogen peroxide to a prepared hydrochloric acid solution of lincomycin to obtain a mixed solution;
(3) adding 1mL of 10mM tea polyphenol solution into the mixed solution obtained in the step (2), and placing the mixed solution on a constant-temperature oscillator for reaction, wherein the set rotating speed is 200rpm, and the temperature is 25 ℃.
The Fenton-like reaction systems consisting of 0.2mL, 0.5mL, 1.0mL, 1.5mL, 2.0mL and 3.0mL of hydrogen peroxide are respectively T1, T2, T3, T4, T5 and T6; and (3) oscillating for reaction for 2 hours, sampling at 0.5h, 1.0h, 1.5h and 2.0h respectively, measuring the concentration of the residual lincomycin by using a high performance liquid chromatograph, and calculating the removal rate by taking the average value of the concentrations.
Fig. 2 is a comparison graph of the degradation effect of the different fenton-like reaction systems of the embodiment on lincomycin, and it can be seen from fig. 2 that the degradation effect of lincomycin is better when the amount of hydrogen peroxide is larger, which is probably because OH is the main effect in the degradation process, and the more hydrogen peroxide is, the more ■ OH is generated, which promotes the degradation reaction.
Example 3
The method for degrading lincomycin comprises the following steps:
(1) preparing 100mL of hydrochloric acid solution of lincomycin with the concentration of 20mg/L, and determining that the initial pH value is 5.8;
(2) adding 1.0mL of hydrogen peroxide with the concentration of 10M and a Fenton-like reaction system consisting of 0.01g, 0.02g, 0.05g, 0.1g, 0.2g and 0.3g of reduced iron powder by mass into a prepared lincomycin solution to obtain a mixed solution;
(3) adding 1mL of 10mM tea polyphenol solution into the mixed solution obtained in the step (2), and placing the mixed solution on a constant-temperature oscillator for reaction, wherein the set rotating speed is 200rpm, and the temperature is 25 ℃.
The Fenton-like reaction systems consisting of 0.01g, 0.02g, 0.05g, 0.1g, 0.2g and 0.3g of reduced iron powder are respectively W1, W2, W3, W4, W5 and W6; performing oscillation reaction for 80min, sampling at 20min, 40min, 60min and 80min respectively, determining the concentration of the rest lincomycin by high performance liquid chromatograph, and calculating the removal rate by taking the average value.
FIG. 3 is a comparison graph of the degradation effect of different Fenton-like reaction systems of this example on lincomycin, and it can be seen from FIG. 3 that when the amount of added iron powder is greater than or equal to 0.05g, the degradation rate of 1h can reach 90% or more; but with the increase of the adding amount of the iron powder, the influence on the degradation rate of the lincomycin is not greatly different, and the degradation rate is even lower than that of 0.1g and 0.2g when the adding amount reaches 0.3 g; this is probably because the iron powder is easily agglomerated and a large amount of iron powder causes agglomeration, which hinders the progress of the reaction.
Example 4
The method for degrading lincomycin comprises the following steps:
(1) preparing 100mL of hydrochloric acid solution of lincomycin with the concentration of 20mg/L, and determining that the initial pH value is 5.8;
(2) adding a Fenton-like reaction system consisting of 0.05g of reduced iron powder and 1mL of 0.1M hydrogen peroxide into a prepared hydrochloric acid solution of lincomycin to obtain a mixed solution;
(3) adding 1mL of tea polyphenol solution (TP) with the concentration of 0.1mM, 1.0mM, 5.0mM and 10mM into the mixed solution obtained in the step (2), and arranging a comparative reaction system which does not contain the tea polyphenol solution (TP); placing the mixture on a constant-temperature oscillator for reaction, setting the rotating speed to be 200rpm and the temperature to be 25 ℃. Performing oscillation reaction for 120min, sampling at 15min, 30min, 45min, 60min, 90min and 120min respectively, determining the concentration of the rest lincomycin by high performance liquid chromatograph, and calculating the removal rate by taking the average value.
FIG. 4 is a graph comparing the degradation effect of different amounts of tea polyphenols on lincomycin in example 4, and it can be seen from FIG. 4 that the degradation rate of the reaction system is significantly improved after the tea polyphenols are added. After reacting for 2 hours, the reaction system without TP solution had a residual lincomycin concentration of about 11mg/L, while the reaction systems with TP solution concentrations of 1mM, 5mM and 10mM had almost no lincomycin residue, and thus was considered to be a high-performance group. The degradation effect of the TP solution is obviously lower than that of the high-efficiency group when the concentration of the TP solution is 100mM, and the residual concentration of the lincomycin reaches about 8 mg/L. This is probably due to the limited solubility of tea polyphenols, and the presence of small amount of incompletely dissolved tea polyphenol particles in 100mM TP solution, which adsorbed ■ OH during the reaction, and competed with the contaminants, thus affecting the degradation of the contaminants.
Example 5
The method for degrading lincomycin comprises the following steps:
(1) preparing 100mL of hydrochloric acid solution of lincomycin with the concentration of 20mg/L, and determining that the initial pH value is 5.8;
(2) respectively adding 0.05g of reduced iron powder Fe, H2O2, a tea polyphenol solution (TP), Fe + H2O2, Fe + TP, H2O2+ TP and Fe + H2O2+ TP into a prepared hydrochloric acid solution of lincomycin to obtain a mixed solution; fe 0.05g, H2O2 solution 1mL, 0.1M concentration, tea polyphenols solution (TP) 1mL, 10mM concentration;
(3) placing the mixed solution obtained in the step (2) on a constant-temperature oscillator for reaction, wherein the set rotating speed is 200rpm, and the temperature is 25 ℃. Performing oscillation reaction for 120min, sampling at 15min, 30min, 45min, 60min, 90min and 120min respectively, determining the concentration of the rest lincomycin by high performance liquid chromatograph, and calculating the removal rate by taking the average value.
FIG. 5 is a graph comparing the degradation effects of different reaction systems of example 5 on lincomycin, and it can be seen from FIG. 5 that among seven processes of Fe, H2O2, TP, Fe + H2O2, Fe + TP, H2O2+ TP and Fe + H2O2+ TP, the two processes of Fe + H2O2 and Fe + H2O2+ TP show advantages over the other processes. The advantage of the Fe + H2O2 process proves that the Fenton-like reaction plays a certain role in the degradation reaction of lincomycin. It can be seen that the Fe + H2O2+ TP process has a very significant advantage over other processes, and the pollutants are basically removed, which indicates that the TP plays an important role in the process of degrading lincomycin by fenton-like reaction.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (4)
1. A method for degrading lincomycin, comprising the steps of:
(1) preparing hydrochloric acid solution of lincomycin;
(2) mixing a Fenton-like reaction system consisting of iron powder and hydrogen peroxide with a hydrochloric acid solution of lincomycin to obtain a mixed solution;
(3) adding tea polyphenols into the mixed solution, and oscillating in a constant temperature oscillation box with the addition amount of tea polyphenols of 0.001mM-1 mM;
in the step (1), the prepared hydrochloric acid solution of the lincomycin has the concentration of 10-30mg/L and the pH value of 5-7;
in the step (2), the iron powder is micron-sized reduced iron powder, and the adding amount of the iron powder is 0.1-2 g/L;
in the step (2), the adding amount of the hydrogen peroxide is 1mM-100 mM.
2. The method for degrading lincomycin according to claim 1,
in the step (3), the oscillation speed is 150-400 rpm.
3. The method for degrading lincomycin according to claim 1,
in the step (3), the reaction temperature is oscillated to be 20-80 ℃.
4. The method for degrading lincomycin according to claim 1,
in the step (3), the oscillation reaction time is 60-180 min.
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