CN116354487A - Double-coating persulfate slow-release material and preparation method and application thereof - Google Patents
Double-coating persulfate slow-release material and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/722—Oxidation by peroxides
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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Abstract
The invention discloses a double-coated persulfate slow-release material, and a preparation method and application thereof, and relates to the technical field of groundwater pollution remediation. The double-coated persulfate slow-release material consists of an inner layer material and an outer layer material, wherein the inner layer material is prepared by uniformly melting and stirring persulfate, silica sand and polycaprolactone, and the outer layer material is prepared by uniformly melting and stirring silica sand and polycaprolactone. The invention also comprises a preparation method and application of the slow-release material. The invention changes the slow release effect of the persulfate slow release material by changing the proportion of the inner layer material and the outer layer material and the thickness of the outer layer material; meanwhile, the iron-nitrogen co-doped biochar is prepared to activate persulfate, so that the persulfate slowly released by the slow-release material is activated, the removal effect of antibiotics in groundwater is enhanced, and the problems that the oxidation environment cannot be maintained for a long time, the utilization rate is low, the production cost is high and the like in the prior art are effectively solved.
Description
Technical Field
The invention relates to the technical field of groundwater pollution remediation, in particular to a double-coated persulfate slow-release material and a preparation method and application thereof.
Background
The method is a large country for producing and using antibiotics, and waste water generated in the production process of the antibiotics is difficult to treat after entering the environment, and can destroy ecological balance and even threaten the health and safety of human bodies. Therefore, it is important to find an efficient and economical method for removing antibiotics in groundwater environments.
The conventional groundwater remediation technology at present comprises an in-situ remediation technology and an ex-situ remediation technology, wherein the ex-situ remediation technology takes a long time and has high treatment cost, and the in-situ remediation technology becomes a common method for remediating groundwater pollutants. In-situ chemical oxidation is one of the main treatment modes for treating the organic pollution of the underground water, and common oxidants include persulfates, potassium permanganate and Fenton reagents.
The persulfate has strong oxidizing property and water solubility, when the persulfate reagent is directly added into the underground water, the persulfate reagent can react with the reducing substances in the environment, the oxidizing environment can not be maintained for a long time, the utilization rate of the oxidant is low, and the production cost is increased. Therefore, the sustained and slow release of persulfate in groundwater is realized, and the improvement of the pollutant removal efficiency is important.
At present, a method for degrading antibiotics by combining a persulfate catalyst and a double-coated slow-release material by using modified biochar has not been reported, and has important significance for realizing the synchronous execution of persulfate slow release and activation and improving the treatment efficiency of antibiotics.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a double-coated persulfate slow-release material, a preparation method and application thereof, wherein the slow-release effect of the persulfate slow-release material is changed by changing the proportion of inner and outer materials and the thickness of the outer materials; meanwhile, the persulfate released slowly by the slow-release material is activated by the iron-nitrogen co-doped biochar, so that the removal effect of antibiotics in groundwater is enhanced, and the problems that the oxidation environment cannot be maintained for a long time, the utilization rate is low, the production cost is high and the like in the prior art are effectively solved.
The technical scheme for solving the technical problems is as follows: the double-coating persulfate slow-release material is prepared by uniformly melting and stirring persulfate, silica sand and polycaprolactone according to the mass ratio of 1/3-1/2:1:1/3-1, and an outer layer material prepared by uniformly melting and stirring silica sand and polycaprolactone according to the mass ratio of 1-6:1.
Further, the mass ratio of persulfate to silica sand to polycaprolactone is 1/3:1:1/2.
Further, the mass ratio of silica sand to polycaprolactone is 5:1.
Further, the double-coated persulfate slow-release material is a cube with a side length of 1.3-2 cm.
The preparation method of the double-coated persulfate slow-release material comprises the following steps of:
(1) Mixing persulfate, silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring, and pouring the mixture into a mold after the polycaprolactone is completely melted to obtain an inner layer material;
(2) Mixing silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring conditions, and uniformly mixing to obtain a mixed material;
(3) And (3) placing the inner layer material obtained in the step (1) in the middle of a die, uniformly wrapping and shaping the mixed material obtained in the step (2) to obtain the double-coated persulfate slow-release material.
Further, in the step (1), the side length of the inner layer material is 1-1.3cm.
Further, the biochar is iron-nitrogen co-doped biochar.
Further, the iron-nitrogen co-doped biochar is prepared by the following method: dissolving ferrous sulfate heptahydrate, urea and ascorbic acid in deionized water, adding lotus leaf powder, mixing and reacting completely, centrifuging, freeze-drying in vacuum, and sintering in a tube furnace at 900 deg.C for 2 hr to obtain Fe-N co-doped biochar.
Further, the mass-volume ratio of the lotus leaf powder, the ferrous sulfate heptahydrate, the urea, the ascorbic acid and the deionized water is 3g to 5.56g to 3g to 2.5g to 100mL.
The double-coated persulfate slow-release material is applied to repairing groundwater antibiotic pollution.
The prepared double-coated persulfate slow-release material is placed in 100mL of sulfamethoxazole solution with the initial concentration of 10mg/L and 10mg/L ciprofloxacin solution to react for 8 hours at room temperature (20+/-1 ℃), or placed in 200mL of ultrapure water to slowly release and sample for 14-21d at fixed time to determine the residual concentration of antibiotics or the accumulated and released concentration of persulfate in the solution, and the material is found to be capable of stably releasing persulfate for a long time and has good degradation capability on groundwater polluted by sulfamethoxazole and ciprofloxacin.
The invention has the following beneficial effects:
1. the invention changes the slow release effect of the persulfate slow release material by changing the proportion of the inner layer material and the outer layer material and the thickness of the outer layer material; meanwhile, the persulfate released slowly by the slow-release material is activated by the iron-nitrogen co-doped biochar, so that the removal effect of antibiotics in groundwater is enhanced, and the problems that the oxidation environment cannot be maintained for a long time, the utilization rate is low, the production cost is high and the like in the prior art are effectively solved.
2. The invention selects nontoxic, harmless and biodegradable polycaprolactone as the binder of the slow release material to prepare the environment-friendly persulfate slow release material, the slow release material combines the in-situ oxidation technology and the slow release technology, and the persulfate slow release material and the iron-nitrogen co-doped biochar are combined to jointly degrade antibiotics. The biochar has rich pore structure and surface functional groups, so that organic pollutants can be effectively catalytically degraded. Compared with the original biochar and the biochar modified by using simple transition metal and hetero atoms, the iron-nitrogen co-doped biochar has larger specific surface area and can catalyze persulfate more efficiently. Therefore, the iron-nitrogen co-doped biochar is used as a persulfate catalyst, and has important significance for improving the treatment efficiency of antibiotics.
3. The persulfate slow-release material is prepared by adopting a double-coating structure, and the permeability of the inner layer and the outer layer is regulated and controlled by changing the proportion of the silica sand and the PCL, so that the release speed of the persulfate is controlled. Therefore, the double-coated slow release material overcomes the defect that the single-layer slow release material is too fast in early release rate and insufficient in later release rate, prolongs the acting time of the slow release agent, and improves the utilization rate of persulfate. The higher the silica sand ratio in the material is, the better the permeability is, and the higher the PCL ratio is, the better the material formability is.
4. The inner layer and the whole of the double-coating persulfate slow-release material are both of cube structures. The cube is better to transport and store than the sphere and the cylinder, and the specific surface area is larger and the contact area between the sustained release agent and the environment is larger under the condition of the same volume. Therefore, under the condition of using the same amount of materials, the release efficiency of the oxidant is higher, and the production cost is reduced.
Drawings
FIG. 1 is a graph showing the release profile of the double coated persulfate slow release material obtained in example 1;
FIG. 2 is a graph showing the release profile of the double coated persulfate slow release material obtained in example 2;
FIG. 3 is a graph showing the release profile of the double coated persulfate slow release material obtained in example 3.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
A double-coated persulfate slow-release material comprises a cube with a side length of 1.5cm, an inner layer material and an outer layer material, wherein the inner layer material is prepared by uniformly melting and stirring persulfate, silica sand and polycaprolactone according to a mass ratio of 1/3:1:1/2, and the outer layer material is prepared by uniformly melting and stirring silica sand and polycaprolactone according to a mass ratio of 3:1.
The preparation method of the double-coated persulfate slow-release material comprises the following steps of:
(1) Mixing persulfate, silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring, and pouring the mixture into a mold after the polycaprolactone is completely melted to obtain an inner layer material with the side length of 1 cm;
(2) Mixing silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring, and melting and uniformly mixing to obtain a mixed material;
(3) And (3) placing the inner layer material obtained in the step (1) in the middle of a die, uniformly wrapping and shaping the mixed material obtained in the step (2) to obtain the double-coated persulfate slow-release material.
The obtained double-coated persulfate slow-release material is placed in 200mL of ultrapure water, and is slowly released for 21d at room temperature (20+/-1 ℃) and sampled at intervals of 24 hours each time, the concentration of persulfate in the solution is measured, the release rate of the persulfate reaches 35.52% after 21d, the release rate of the persulfate is stable in the whole release period, and the release rate is about 5.88mg/d, and the release curve chart is shown in figure 1.
Example 2
A double-coated persulfate slow-release material comprises a cube with a side length of 1.5cm, an inner layer material and an outer layer material, wherein the inner layer material is prepared by uniformly melting and stirring persulfate, silica sand and polycaprolactone according to a mass ratio of 1/3:1:1/2, and the outer layer material is prepared by uniformly melting and stirring silica sand and polycaprolactone according to a mass ratio of 6:1.
The preparation method of the double-coated persulfate slow-release material comprises the following steps of:
(1) Mixing persulfate, silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring, and pouring the mixture into a mold after the polycaprolactone is completely melted to obtain an inner layer material with the side length of 1 cm;
(2) Mixing silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring conditions, and uniformly mixing to obtain a mixed material;
(3) And (3) placing the inner layer material obtained in the step (1) in the middle of a die, uniformly wrapping and shaping the mixed material obtained in the step (2) to obtain the double-coated persulfate slow-release material.
The obtained double-coated persulfate slow-release material is put into 200mL of ultrapure water, and is slowly released for 7d at room temperature (20+/-1 ℃) and sampled at intervals of 24 hours each time, the concentration of persulfate in the solution is measured, the release rate of persulfate reaches 44.42% after 7d, the release rate of persulfate is stable after 48 hours, the release rate is about 11.854mg/d, and the release curve chart is shown in figure 2.
Example 3
The double-coated persulfate slow-release material comprises a cube with a side length of 2cm, an inner layer material and an outer layer material, wherein the inner layer material is prepared by uniformly melting and stirring persulfate, silica sand and polycaprolactone according to a mass ratio of 1/3:1:1/2, and the outer layer material is prepared by uniformly melting and stirring silica sand and polycaprolactone according to a mass ratio of 3:1.
The preparation method of the double-coated persulfate slow-release material comprises the following steps of:
(1) Mixing persulfate, silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring, and pouring the mixture into a mold after the polycaprolactone is completely melted to obtain an inner layer material with the side length of 1.3 cm;
(2) Mixing silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring conditions, and uniformly mixing to obtain a mixed material;
(3) And (3) placing the inner layer material obtained in the step (1) in the middle of a die, uniformly wrapping and shaping the mixed material obtained in the step (2) to obtain the double-coated persulfate slow-release material.
The obtained double-coated persulfate slow-release material is put into 200mL of ultrapure water, and is slowly released for 21d at room temperature (20+/-1 ℃) and sampled at intervals of 24h each time, the concentration of persulfate in the solution is measured, the release rate of the persulfate reaches 2.364% after 21d, the release rate of the persulfate is stable in the whole release period, the release rate is about 4.213mg/d, and the release curve is shown in figure 3.
Example 4
A double-coated persulfate slow-release material comprises a cube with a side length of 1.5cm, an inner layer material and an outer layer material, wherein the inner layer material is prepared by uniformly melting and stirring persulfate, silica sand and polycaprolactone according to a mass ratio of 1/3:1:1/2, and the outer layer material is prepared by uniformly melting and stirring silica sand and polycaprolactone according to a mass ratio of 4:1.
The preparation method of the double-coated persulfate slow-release material comprises the following steps of:
(1) Mixing persulfate, silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring, and pouring the mixture into a mold after the polycaprolactone is completely melted to obtain an inner layer material with the side length of 1 cm;
(2) Mixing silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring conditions, and uniformly mixing to obtain a mixed material;
(3) And (3) placing the inner layer material obtained in the step (1) in the middle of a die, uniformly wrapping and shaping the mixed material obtained in the step (2) to obtain the double-coated persulfate slow-release material.
The prepared double-coated slow release material is respectively placed into 100mL of 10mg/L sulfamethoxazole solution and 10mg/L ciprofloxacin solution, 0.03g of biochar is added, the mixture is kept away from light and is subjected to standing reaction for 8 hours at room temperature (20+/-1 ℃), sampling is carried out at fixed time, and the residual concentration of sulfamethoxazole and ciprofloxacin in the solution is measured. Meanwhile, the experiment designs a control group experiment without adding biochar.
Wherein the biochar is iron-nitrogen co-doped biochar; the iron-nitrogen co-doped biochar is prepared by the following method: dissolving ferrous sulfate heptahydrate, urea and ascorbic acid in deionized water, adding lotus leaf powder, mixing and reacting completely, centrifuging, freeze-drying in vacuum, and sintering in a tube furnace at 900 deg.C for 2 hr to obtain Fe-N co-doped biochar. The mass volume ratio of the lotus leaf powder, the ferrous sulfate heptahydrate, the urea, the ascorbic acid and the deionized water is 3g to 5.56g to 3g to 2.5g to 100mL.
After 8h of reaction, the removal rate of 10mg/L ciprofloxacin under the condition of charcoal catalysis is 34.5 percent, and the removal rate of 10mg/L sulfamethoxazole is 18.1 percent. In contrast, the control experiment without charcoal had a removal rate of 10mg/L ciprofloxacin of 3.7% and a removal rate of 10mg/L sulfamethoxazole of 3.3% after 24 hours of reaction.
The result shows that the prepared double-coated persulfate slow-release agent can effectively degrade sulfamethoxazole and ciprofloxacin in underground water under the catalysis condition of iron-nitrogen co-doped biochar.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The double-coating persulfate slow-release material is characterized by comprising an inner layer material and an outer layer material, wherein the inner layer material is prepared by uniformly melting and stirring persulfate, silica sand and polycaprolactone according to the mass ratio of 1/3-1/2:1:1/3-1, and the outer layer material is prepared by uniformly melting and stirring silica sand and polycaprolactone according to the mass ratio of 1-6:1.
2. The double-coated persulfate slow-release material according to claim 1, wherein the mass ratio of the persulfate to the silica sand to the polycaprolactone is 1/3:1:1/2.
3. The double-coated persulfate slow-release material according to claim 1, wherein the mass ratio of silica sand to polycaprolactone is 5:1.
4. The double-coated persulfate slow-release material according to claim 1, wherein the whole double-coated persulfate slow-release material is a cube with a side length of 1.3-2 cm.
5. The method for preparing the double-coated persulfate slow-release material according to any one of claims 1 to 4, comprising the steps of:
(1) Mixing persulfate, silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring, and pouring the mixture into a mold after the polycaprolactone is completely melted to obtain an inner layer material;
(2) Mixing silica sand and polycaprolactone, heating to 70 ℃ under constant-temperature magnetic stirring conditions, and uniformly mixing to obtain a mixed material;
(3) And (3) placing the inner layer material obtained in the step (1) in the middle of a die, uniformly wrapping and shaping the mixed material obtained in the step (2) to obtain the double-coated persulfate slow-release material.
6. The method for preparing a double-coated persulfate slow-release material according to claim 5, wherein in the step (1), the side length of the inner layer material is 1-1.3cm.
7. Use of the double-coated persulfate slow-release material and biochar according to any one of claims 1 to 4 for repairing groundwater antibiotic pollution.
8. The use according to claim 7, wherein the biochar is an iron-nitrogen co-doped biochar.
9. The use according to claim 7, wherein the iron-nitrogen co-doped biochar is prepared by: dissolving ferrous sulfate heptahydrate, urea and ascorbic acid in deionized water, adding lotus leaf powder, mixing and reacting completely, centrifuging, freeze-drying in vacuum, and sintering in a tube furnace at 900 deg.C for 2 hr to obtain Fe-N co-doped biochar.
10. The use according to claim 7, wherein the mass to volume ratio of lotus leaf powder, ferrous sulfate heptahydrate, urea, ascorbic acid and deionized water is 3g to 5.56g to 3g to 2.5g to 100ml.
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