CN113480073A - Method for removing pollutants in water by using periodate - Google Patents
Method for removing pollutants in water by using periodate Download PDFInfo
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- CN113480073A CN113480073A CN202110842293.8A CN202110842293A CN113480073A CN 113480073 A CN113480073 A CN 113480073A CN 202110842293 A CN202110842293 A CN 202110842293A CN 113480073 A CN113480073 A CN 113480073A
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- 238000000034 method Methods 0.000 title claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 16
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 16
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 55
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims description 64
- 239000010865 sewage Substances 0.000 claims description 49
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 238000002156 mixing Methods 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 11
- 230000008859 change Effects 0.000 claims description 10
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 10
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 10
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 10
- 239000000356 contaminant Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 5
- 229940072172 tetracycline antibiotic Drugs 0.000 claims description 4
- 229940123317 Sulfonamide antibiotic Drugs 0.000 claims description 3
- 239000003242 anti bacterial agent Substances 0.000 claims description 3
- 229940088710 antibiotic agent Drugs 0.000 claims description 3
- MLIWQXBKMZNZNF-KUHOPJCQSA-N (2e)-2,6-bis[(4-azidophenyl)methylidene]-4-methylcyclohexan-1-one Chemical compound O=C1\C(=C\C=2C=CC(=CC=2)N=[N+]=[N-])CC(C)CC1=CC1=CC=C(N=[N+]=[N-])C=C1 MLIWQXBKMZNZNF-KUHOPJCQSA-N 0.000 claims description 2
- 229940124307 fluoroquinolone Drugs 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000003213 activating effect Effects 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract description 2
- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 description 60
- 229960004989 tetracycline hydrochloride Drugs 0.000 description 60
- 230000015556 catabolic process Effects 0.000 description 35
- 238000006731 degradation reaction Methods 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 20
- 238000001914 filtration Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 238000005070 sampling Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000013543 active substance Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000010840 domestic wastewater Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940011871 estrogen Drugs 0.000 description 1
- 239000000262 estrogen Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003306 quinoline derived antiinfective agent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
-
- 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
- C02F1/008—Control or steering systems not provided for elsewhere in subclass C02F
-
- 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
-
- 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
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
一种利用高碘酸盐去除水中污染物的方法，它涉及一种去除水中有机污染物的方法。本发明的目的是要解决单一使用高碘酸盐降解有机污染物去除率不高，同时常规的基于高碘酸盐的高级氧化方法的活化方式容易造成二次污染及对工艺操作者容易造成身体损害的问题。方法：在60～80℃的环境温度下，通过热激活高碘酸盐来去除水中有机污染物的方法能有效去除有机污染物，有机污染物去除率高达90％以上。本发明适用于去除水中的有机污染物。
A method for removing pollutants in water by using periodate, which relates to a method for removing organic pollutants in water. The purpose of the present invention is to solve the problem that the removal rate of organic pollutants degraded by single use of periodate is not high, and the activation mode of the conventional advanced oxidation method based on periodate is easy to cause secondary pollution and easily cause physical damage to process operators. damage problem. Methods: The method of removing organic pollutants in water by thermally activating periodate at an ambient temperature of 60-80 °C can effectively remove organic pollutants, and the removal rate of organic pollutants is as high as 90%. The present invention is suitable for removing organic pollutants in water.
Description
Technical Field
The invention relates to a method for removing organic pollutants in water.
Background
In recent years, with the rapid development of the pharmaceutical and chemical industries, a large amount of domestic and industrial wastewater containing high-concentration drugs and organic pollutants of personal care products is discharged into water environment after being treated by a conventional sewage plant. However, conventional wastewater treatment processes have difficulty in efficiently removing organic contaminants from pharmaceutical and personal care products in wastewater, which in turn leads to a gradual increase in the types and concentrations of residual organic contaminants in the aqueous environment. The residual pollutants in the water environment comprise various antibiotics, environmental estrogens, pesticides and other residual compounds, the half-life period of the pollutants in the water environment is long, the pollutants are slowly biodegraded, and the pollutants have potential hazards of acute carcinogenesis, teratogenesis and mutagenesis at a certain concentration. Therefore, a method capable of efficiently removing various residual organic pollutants in the water body is widely concerned.
Periodate alone is not effective in removing organic contaminants. In recent years, periodate-based advanced oxidation methods for removing organic pollutants in water have been reported in large numbers, and periodate-based advanced oxidation methods can efficiently remove refractory organic matters in water. However, the conventional periodate-based advanced oxidation methods all require the addition of chemical agents such as manganese ions or iron ions which are easy to cause secondary pollution, and external ultraviolet or ultrasonic exogenous energy which is easy to cause physical damage to process operators.
Disclosure of Invention
The invention aims to solve the problems that the removal rate of organic pollutants degraded by using periodate is low, and the conventional activation method based on the periodate is easy to cause secondary pollution and damage to the bodies of process operators, and provides a method for removing pollutants in water by using periodate.
A method for removing pollutants in water by using periodate is completed according to the following steps:
firstly, heating sewage containing organic pollutants to enable the temperature of the sewage to be higher than room temperature and maintain the temperature to obtain high-temperature sewage;
and secondly, adding periodate into the high-temperature sewage, and carrying out mixing reaction through a mixing device to obtain water with organic pollutants removed.
The principle and the advantages of the invention are as follows:
the principle of degrading organic pollutants of the invention is as follows:
periodate thermal activation produces active species degrading pollutants:
active substances + Organic polutants → intermedia → CO2+H2O (4)
The periodate can rapidly generate active substances with strong oxidizing property under the action of heat energy, thereby realizing the efficient degradation of organic matters; the result shows that the system can not only quickly oxidize and remove the tetracycline antibiotic organic pollutants in the water body, but also quickly remove one or two organic pollutants of the tetracycline antibiotic, the fluoroquinolone antibiotic and the sulfonamide antibiotic;
the method has the advantages of simple process, convenient operation, low cost, high efficiency and no secondary pollution, can provide theoretical support for the advanced treatment of water, and has higher practical value in practical application;
and thirdly, when the degradation time is 60min, the degradation rate of the system disclosed by the invention to organic pollutants is up to more than 90%.
Fourthly, the removal rate of the organic pollutants in the invention can reach 100%.
The invention is suitable for removing organic pollutants in sewage.
Drawings
FIG. 1 is a graph showing degradation curves of tetracycline hydrochloride in a 30 ℃ ambient temperature system containing sodium periodate, in a 30 ℃ ambient temperature system and in a 80 ℃ ambient temperature system containing sodium periodate, where "□" is a degradation curve of tetracycline hydrochloride in comparative example 1 in a 30 ℃ ambient temperature system containing sodium periodate, ". O" is a degradation curve of tetracycline hydrochloride in comparative example 2 in an ambient temperature system at 30 ℃ and "Δ" is a degradation curve of tetracycline hydrochloride in example 1 in an ambient temperature system at 80 ℃ containing sodium periodate;
FIG. 2 is a graph showing the effect of tetracycline hydrochloride removal in different systems, wherein "□" is the degradation curve of tetracycline hydrochloride in example 3 at an ambient temperature of 60 ℃ with sodium periodate, ". O" is the degradation curve of tetracycline hydrochloride in example 2 at an ambient temperature of 70 ℃ with sodium periodate, ". DELTA" is the degradation curve of tetracycline hydrochloride in example 1 at an ambient temperature of 80 ℃ with sodium periodate,
in comparative example 5, the degradation curve of tetracycline hydrochloride at an ambient temperature of 60 deg.C, ". diamond" is the degradation curve of tetracycline hydrochloride at an ambient temperature of 70 deg.C in comparative example 4,
the degradation curve of tetracycline hydrochloride in comparative example 3 at an ambient temperature of 80 ℃ is shown.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
The first embodiment is as follows: the method for removing pollutants in water by using periodate is completed according to the following steps:
firstly, heating sewage containing organic pollutants to enable the temperature of the sewage to be higher than room temperature and maintain the temperature to obtain high-temperature sewage;
and secondly, adding periodate into the high-temperature sewage, and carrying out mixing reaction through a mixing device to obtain water with organic pollutants removed.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the concentration of the sewage containing the organic pollutants in the step one is 5-50 mu mol/L, wherein the organic pollutants are one or a mixture of several of tetracycline antibiotics, fluoroquinolone antibiotics or sulfonamide antibiotics. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the method for maintaining the temperature in the first step is one or a combination of a water bath, an oil bath and an air bath. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the temperature of the high-temperature sewage in the first step is 60-80 ℃. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the periodate in the second step is potassium periodate or sodium periodate. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the volume ratio of the periodate substance in the step two to the high-temperature sewage is (100 mu mol-1000 mu mol): 1L. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the mixing device in the step two is one or a combination of a plurality of methods of mechanical stirring, magnetic stirring and a shaking table; the mixing speed of the mixing reaction is 20 r/min-100 r/min. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the time of the mixing reaction in the second step is 60 min. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: filtering 200 mu L of water for removing organic pollutants by using a filter head with the aperture of 0.22 mu m, and adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to terminate the reaction to obtain a sample to be detected; and (3) adopting high performance liquid chromatography for determination, determining the concentration of the organic pollutants through a standard curve, and calculating the removal rate of the organic pollutants under different reaction time and reaction conditions through concentration change before and after reaction. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: the removal rate of the organic pollutants is more than 90%. The other steps are the same as those in the first to ninth embodiments.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Example 1: the degradation experiment of tetracycline hydrochloride in an environment temperature system of 80 ℃ containing sodium periodate is completed according to the following steps:
firstly, heating sewage containing tetracycline hydrochloride to enable the temperature of the sewage to be 80 ℃;
the concentration of the tetracycline hydrochloride in the tetracycline hydrochloride-containing sewage in the step one is 50 mu mol/L;
adding sodium periodate into sewage at the temperature of 80 ℃, reacting by using a magnetic stirring device at the stirring speed of 30r/min, sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes respectively, filtering 200 mu L of sewage by using a filter head with the pore diameter of 0.22 mu m, and adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to terminate the reaction to obtain a sample to be detected; measuring by high performance liquid chromatography, measuring the concentration of organic pollutants by a standard curve, and calculating the removal rate of the organic pollutants at different reaction times according to the concentration change before and after the reaction, wherein the figure is shown in figure 1;
the volume ratio of the sodium periodate substance in the step two to the sewage with the temperature of 80 ℃ is 500 mu mol: 1L.
Comparative example 1: the degradation experiment of tetracycline hydrochloride in a 30 ℃ environment temperature system containing sodium periodate is completed according to the following steps:
firstly, heating sewage containing tetracycline hydrochloride to ensure that the temperature of the sewage is 30 ℃;
the concentration of the tetracycline hydrochloride in the tetracycline hydrochloride-containing sewage in the step one is 50 mu mol/L;
adding sodium periodate into sewage with the temperature of 30 ℃, then using a magnetic stirring device to react under the condition of stirring speed of 30r/min, respectively sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes, filtering 200 mu L of sewage by using a filter head with the pore diameter of 0.22 mu m, and then adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to stop the reaction to obtain a sample to be detected; measuring by high performance liquid chromatography, measuring the concentration of organic pollutants by a standard curve, and calculating the removal rate of the organic pollutants at different reaction times according to the concentration change before and after the reaction, wherein the figure is shown in figure 1;
the volume ratio of the sodium periodate substance in the step two to the sewage with the temperature of 30 ℃ is 500 mu mol: 1L.
Comparative example 2: the degradation experiment of tetracycline hydrochloride in an environment temperature system of 30 ℃ is completed according to the following steps:
reacting sewage containing tetracycline hydrochloride at 30 ℃ and at a stirring speed of 30r/min, sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes respectively, filtering 200 mu L of sewage by using a filter head with the aperture of 0.22 mu m, and adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to terminate the reaction to obtain a sample to be detected; the determination is carried out by adopting high performance liquid chromatography, the concentration of the organic pollutants is determined by a standard curve, and the removal rate of the organic pollutants under different reaction time is calculated by the concentration change before and after the reaction, which is shown in figure 1.
FIG. 1 is a graph showing degradation curves of tetracycline hydrochloride in a 30 ℃ ambient temperature system containing sodium periodate, in a 30 ℃ ambient temperature system and in a 80 ℃ ambient temperature system containing sodium periodate, where "□" is a degradation curve of tetracycline hydrochloride in comparative example 1 in a 30 ℃ ambient temperature system containing sodium periodate, ". O" is a degradation curve of tetracycline hydrochloride in comparative example 2 in an ambient temperature system at 30 ℃ and "Δ" is a degradation curve of tetracycline hydrochloride in example 1 in an ambient temperature system at 80 ℃ containing sodium periodate;
as can be seen from FIG. 1, in the case of the sodium periodate-containing system of example 1 at a room temperature of 80 ℃, tetracycline hydrochloride was degraded by 90% within 60 minutes, and the pseudo-first order reaction kinetic constant was 0.036min-1. In contrast, the degradation rates of tetracycline hydrochloride in the system at room temperature of 30 ℃ containing sodium periodate of comparative example 1 and the system at room temperature of 30 ℃ of comparative example 2 were 9% and 0%, respectively. Therefore, the method for removing the organic pollutants in the water by thermally activating the sodium periodate can effectively remove the organic pollutants.
Example 2: the degradation experiment of tetracycline hydrochloride in a 70 ℃ environment temperature system containing sodium periodate is completed according to the following steps:
firstly, heating sewage containing tetracycline hydrochloride to enable the temperature of the sewage to be 70 ℃;
the concentration of the tetracycline hydrochloride in the tetracycline hydrochloride-containing sewage in the step one is 50 mu mol/L;
adding sodium periodate into sewage at the temperature of 70 ℃, then using a magnetic stirring device to react at the stirring speed of 30r/min, respectively sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes, filtering 200 mu L of sewage by using a filter head with the pore diameter of 0.22 mu m, and then adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to stop the reaction to obtain a sample to be detected; and (3) measuring by adopting high performance liquid chromatography, measuring the concentration of the organic pollutants by using a standard curve, and calculating the removal rate of the organic pollutants at different reaction times according to the concentration change before and after the reaction.
Example 3: the degradation experiment of tetracycline hydrochloride in an ambient temperature system of 60 ℃ containing sodium periodate is completed according to the following steps:
firstly, heating sewage containing tetracycline hydrochloride to enable the temperature of the sewage to be 60 ℃;
the concentration of the tetracycline hydrochloride in the tetracycline hydrochloride-containing sewage in the step one is 50 mu mol/L;
adding sodium periodate into sewage at the temperature of 60 ℃, then using a magnetic stirring device to react at the stirring speed of 30r/min, respectively sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes, filtering 200 mu L of sewage by using a filter head with the pore diameter of 0.22 mu m, and then adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to stop the reaction to obtain a sample to be detected; and (3) measuring by adopting high performance liquid chromatography, measuring the concentration of the organic pollutants by using a standard curve, and calculating the removal rate of the organic pollutants at different reaction times according to the concentration change before and after the reaction.
Comparative example 3: the degradation experiment of tetracycline hydrochloride in an environment temperature system of 80 ℃ is completed according to the following steps:
reacting sewage containing tetracycline hydrochloride at 80 ℃ and at a stirring speed of 30r/min, sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes respectively, filtering 200 mu L of sewage by using a filter head with the aperture of 0.22 mu m, and adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to terminate the reaction to obtain a sample to be detected; and (3) measuring by adopting high performance liquid chromatography, measuring the concentration of the organic pollutants by using a standard curve, and calculating the removal rate of the organic pollutants at different reaction times according to the concentration change before and after the reaction.
Comparative example 4: the degradation experiment of tetracycline hydrochloride in an environment temperature system of 70 ℃ is completed according to the following steps:
reacting sewage containing tetracycline hydrochloride at 70 ℃ and at a stirring speed of 30r/min, sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes respectively, filtering 200 mu L of sewage by using a filter head with the aperture of 0.22 mu m, and adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to terminate the reaction to obtain a sample to be detected; and (3) measuring by adopting high performance liquid chromatography, measuring the concentration of the organic pollutants by using a standard curve, and calculating the removal rate of the organic pollutants at different reaction times according to the concentration change before and after the reaction.
Comparative example 5: the degradation experiment of tetracycline hydrochloride in an ambient temperature system of 60 ℃ is completed according to the following steps:
reacting sewage containing tetracycline hydrochloride at 60 ℃ and at a stirring speed of 30r/min, sampling at time points of 0, 2, 5, 10, 15, 20, 30, 45 and 60 minutes respectively, filtering 200 mu L of sewage by using a filter head with the aperture of 0.22 mu m, and adding 20 mu L of sodium thiosulfate with the concentration of 0.5mol/L to terminate the reaction to obtain a sample to be detected; and (3) measuring by adopting high performance liquid chromatography, measuring the concentration of the organic pollutants by using a standard curve, and calculating the removal rate of the organic pollutants at different reaction times according to the concentration change before and after the reaction.
FIG. 2 is a graph showing the effect of tetracycline hydrochloride removal in different systems, wherein "□" is the degradation curve of tetracycline hydrochloride in example 3 at an ambient temperature of 60 ℃ with sodium periodate, ". O" is the degradation curve of tetracycline hydrochloride in example 2 at an ambient temperature of 70 ℃ with sodium periodate, ". DELTA" is the degradation curve of tetracycline hydrochloride in example 1 at an ambient temperature of 80 ℃ with sodium periodate,
in comparative example 5, the degradation curve of tetracycline hydrochloride at an ambient temperature of 60 deg.C, ". diamond" is the degradation curve of tetracycline hydrochloride at an ambient temperature of 70 deg.C in comparative example 4,
the degradation curve of tetracycline hydrochloride in comparative example 3 at an ambient temperature of 80 ℃ is shown;
as can be seen from FIG. 2, in the case of tetracycline hydrochloride in the system of example 1 at an ambient temperature of 80 ℃ containing sodium periodate, the tetracycline hydrochloride achieved 90% degradation in 60 minutes with a pseudo-first order reaction kinetic constant of 0.036min-1(ii) a In the system of tetracycline hydrochloride in the embodiment 2 at the environmental temperature of 70 ℃ containing sodium periodate, the tetracycline hydrochloride can realize 80 percent degradation within 60 minutes, and the first-order reaction kinetic constant is 0.026min-1(ii) a In the system of tetracycline hydrochloride in the embodiment 3 at the ambient temperature of 60 ℃ containing sodium periodate, the tetracycline hydrochloride can realize 64 percent degradation within 60 minutes, and the pseudo-first-order reaction kinetic constant is 0.016min-1(ii) a While the tetracycline hydrochloride in comparative example 3 isIn a system at the ambient temperature of 80 ℃, 21 percent of tetracycline hydrochloride is degraded within 60 minutes, and the quasi-first-order reaction kinetic constant is 0.004min-1(ii) a In contrast, in the system of the tetracycline hydrochloride in the comparative example 4 at the ambient temperature of 70 ℃, the tetracycline hydrochloride can be degraded by 7% within 60 minutes, and the first-order reaction kinetic constant is 0.001min-1(ii) a In contrast, in the system of the tetracycline hydrochloride in the comparative example 5 at the ambient temperature of 60 ℃, the tetracycline hydrochloride can be degraded by 8% within 60 minutes, and the first-order reaction kinetic constant is 0.001min-1。
It can be seen that the method for removing organic pollutants in water by thermally activating periodate can effectively remove the organic pollutants at the ambient temperature of 60-80 ℃, the removal rate of the organic pollutants is up to more than 90%, and the removal rate is far greater than that of a system at the ambient temperature of 30 ℃.
Claims (10)
1. A method for removing pollutants in water by using periodate is characterized by comprising the following steps:
firstly, heating sewage containing organic pollutants to enable the temperature of the sewage to be higher than room temperature and maintain the temperature to obtain high-temperature sewage;
and secondly, adding periodate into the high-temperature sewage, and carrying out mixing reaction through a mixing device to obtain water with organic pollutants removed.
2. The method for removing pollutants in water by using periodate as claimed in claim 1, wherein the concentration of the sewage containing organic pollutants in the step one is 5 μmol/L to 50 μmol/L, wherein the organic pollutants are one or a mixture of several of tetracycline antibiotics, fluoroquinolone antibiotics or sulfonamide antibiotics.
3. The method for removing pollutants from water by using periodate as claimed in claim 1, wherein the temperature is maintained in the first step by one or more of water bath, oil bath and air bath.
4. The method for removing contaminants from water using periodate according to claim 1, wherein the temperature of the high temperature wastewater in the first step is 60 ℃ to 80 ℃.
5. The method of claim 1, wherein the periodate used in step two is potassium periodate or sodium periodate.
6. The method for removing pollutants from water by using periodate as claimed in claim 1, wherein the volume ratio of the periodate in the second step to the high-temperature sewage is (100 μmol-1000 μmol): 1L.
7. The method for removing contaminants from water with periodate according to claim 1, wherein the mixing device in step two is one or a combination of mechanical stirring, magnetic stirring and shaking table; the mixing speed of the mixing reaction is 20 r/min-100 r/min.
8. The method for removing contaminants from water with periodate according to claim 1, wherein the mixing reaction time in step two is 60 min.
9. The method for removing pollutants in water by using periodate as claimed in claim 1, wherein in the second step, 200 μ L of water for removing organic pollutants is filtered by using a filter head with the pore diameter of 0.22 μm, and 20 μ L of sodium thiosulfate with the concentration of 0.5mol/L is added to terminate the reaction, so as to obtain a sample to be detected; and (3) adopting high performance liquid chromatography for determination, determining the concentration of the organic pollutants through a standard curve, and calculating the removal rate of the organic pollutants under different reaction time and reaction conditions through concentration change before and after reaction.
10. The method of claim 9, wherein the removal rate of the organic contaminants is greater than 90%.
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