CN114590882A - Method for removing algae in water by activating persulfate during preparation of ferrate - Google Patents
Method for removing algae in water by activating persulfate during preparation of ferrate Download PDFInfo
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- CN114590882A CN114590882A CN202210202620.8A CN202210202620A CN114590882A CN 114590882 A CN114590882 A CN 114590882A CN 202210202620 A CN202210202620 A CN 202210202620A CN 114590882 A CN114590882 A CN 114590882A
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- ferrate
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a method for removing algae in water by preparing ferrate activated persulfate, which comprises the following steps: preparing materials for electrolytic reaction; carrying out electrolytic reaction to form electrolyte; measuring the concentration of a generating substance in the electrolyte; removing impurities in the electrolyte; adding a potassium hydroxide solution into the electrolyte with impurities removed to form a second solution; carrying out suction filtration on the second solution; dehydrating the filtered crystal; carrying out vacuum drying treatment; and preserving the prepared crystals. The method for removing algae in water by using the ferrate activated persulfate has the advantages that only a small amount of ferrate and persulfate is needed, the dosage of the medicament is small compared with other chemical methods, the degradation cost is reduced, compared with the traditional physical mechanical separation method, the method for removing algae is convenient and quick, the consumption of manpower and electricity is reduced, and the cost for removing algae is greatly saved.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a method for removing algae in water by activating persulfate during ferrate preparation.
Background
With the rapid development of industry and agriculture in China, a large amount of nitrogen and phosphorus flow into a water body, so that the water body is eutrophicated, algae outbreak is caused, the transparency of the water body is reduced, the water quality is turbid, the sensory effect is poor, dissolved oxygen in the water body can be reduced, other organisms in the water are dead due to oxygen deficiency, the ecological balance of the water body is damaged, and the safety of the water environment is greatly threatened. Therefore, the development of technology for algae removal is imminent.
In recent years, a physical algae removal method is not favored because of overhigh removal cost, a biological algae removal method is not widely used because of insufficient research, and a chemical algae removal method is convenient to operate, has low cost, does not influence the biological diversity in the original water body, and is widely applied to practical engineering. Wherein, the persulfate and the ferrate both have stronger oxidability, and are more algaecides used at present.
Persulfates (PS) are a type of peroxides with strong oxidizing properties, mainly comprising Peroxymonosulfate (PMS) and Peroxydisulfate (PDS), and are often used in the field of sewage treatment. Relevant studies have shown that when PS is activated, sulfate radicals with strong oxidizing properties are generated (· SO 4-); several studies have shown that SO 4-has a higher redox potential (E0 ═ 2.5-3.1V) than hydroxyl radicals (E0 ═ 1.8-2.7V), SO 4-is more effective in removing contaminants; SO 4-has a long half-life and high reactivity over a wide pH range, and therefore can be used in complex water for the removal of refractory organics.
Ferrate is a powdery flaky crystal with dark red luster and a tetrahedral configuration, and researches show that the oxidation-reduction potential of ferrate under acidic and alkaline conditions is respectively 2.2V (E0) and 0.72V (E0), so that the ferrate has strong oxidizability in all pH ranges, and multiple researches show that the reduction product Fe3+ of the ferrate forms Fe (OH)3 in a water body, so that the ferrate can play a good role in adsorption, flocculation and sedimentation on suspended matters in the water body, and the water transparency is improved; the strong oxidizing property of the ferrate can destroy the cell structure and the substances in the cells of bacteria, so that the synthesis of protein and nucleic acid is hindered and inhibited, the growth and the propagation of thalli are hindered, and the sterilization effect is achieved, and when the mass concentration of the ferrate in a water sample is 5-6 mg/L, the sterilization efficiency can reach 99.95% -99.99%; ferrate can remove algae from water by oxidative flocculation.
The activation of PS can be done in several ways: transition metal ion (such as Fe2+, Co2+, and the like) activation, Ultraviolet (UV) activation, thermal activation and the like, wherein although the thermal activation is simple and convenient, the activation efficiency is not high, and the treatment time is long; the ultraviolet activation is only suitable for removing algae in small water bodies; the PS is activated by the ferrate, so that the algae removal effects of the PS and the ferrate can be coupled, the algae removal efficiency is greatly improved, and the method is convenient to operate, low in cost, wide in application range and wide in application prospect.
Disclosure of Invention
The invention aims to solve the problems and designs a method for removing algae in water by using ferrate activated persulfate.
The technical scheme of the invention is that the method for removing algae in water by using ferrate activated persulfate comprises the following steps:
the method comprises the following steps: preparing materials for electrolytic reaction;
step two: carrying out electrolytic reaction to form electrolyte;
step three: measuring the concentration of a generating substance in the electrolyte;
step four: removing impurities in the electrolyte;
step five: adding a potassium hydroxide solution into the electrolyte with impurities removed to form a second solution;
step six: carrying out suction filtration on the second solution;
step seven: dehydrating the filtered crystal;
step eight: carrying out vacuum drying treatment;
step nine: and preserving the prepared crystals.
In the second step, sponge iron is added into a 1mM potassium hydroxide solution for electrolysis for 4 hours, the electrolysis reaction is controlled by a self-made electrolytic cell with a SiO4 ceramic diaphragm and a periodic reversing device, the current density is controlled to be 40-50 mA/cm3, and the current is controlled to be 10-15A.
As a further description of the technical scheme, after electrolysis, when the anode solution gradually becomes purple, ferrate is generated in the electrolyte, in the third step, a fixed volume of sodium ferrate solution is taken out every half hour to measure the concentration, in the fourth step, when the concentration of the sodium ferrate is more than 0.1mM, the sodium ferrate solution is taken out and placed in a refrigerator to be cooled for 1 hour, and then a G4 sand core funnel is used for suction filtration to remove impurities.
As a further description of the technical scheme, in the fifth step, the filtrate is placed in a beaker, the beaker is placed in an ice-water bath, a refrigerated 14mM potassium hydroxide solution is slowly dropped and fully stirred, the volume of the potassium hydroxide solution is 1/2 of the volume of the sodium ferrate solution, a second solution is formed in the process, then the second solution is stirred and placed in a refrigerator freezing layer for 40-60 min after being stirred, and in the sixth step, the stirred second solution is subjected to suction filtration to obtain crystals.
And as further description of the technical scheme, in the seventh step, cyclohexane dehydration and isopropanol dealkalization are adopted for the obtained crystals, and in the eighth step, the dealkalized potassium ferrate crystals are dried in a vacuum drying oven at 40 ℃ for 4 hours.
And as further description of the technical scheme, in the ninth step, the prepared crystals are placed in a brown reagent bottle and stored in a dryer at normal temperature, the prepared ferrate is added into the algae-containing wastewater to be treated, persulfate is added into the algae-containing wastewater to be treated and is continuously stirred, and the algae in the water body can be efficiently removed after a period of time.
As a further description of the present technical solution, the Persulfate (PS) is a peroxymonosulfate or peroxydisulfate, including sodium, potassium and ammonium salts.
As further description of the technical scheme, the adding amount of the ferrate is 0.1-0.5 g/L, the adding amount of the persulfate is 0.2-1.0 g/L, the stirring speed is 100-200 r/min, and the stirring time is 10-30 min.
As further description of the technical scheme, the pH in the sewage system does not need to be adjusted, and the reaction can be carried out under the condition of the pH of 3-11.
The method for removing algae in water by using the ferrate activated persulfate, disclosed by the invention, has the beneficial effects that 1, only a small amount of ferrate and persulfate is needed, the dosage of the agent is small compared with other chemical methods, and the degradation cost is reduced.
2. Compared with the traditional physical mechanical separation method, the method for removing the algae in the water by using the ferrate activated persulfate, which is disclosed by the invention, is convenient and quick, reduces the consumption of manpower and electricity, and greatly saves the cost for removing the algae.
3. Compared with the traditional chemical method for removing algae, the method for removing algae in water by using the ferrate activated persulfate can perform reaction in a wider range of pH, the pH in a sewage system does not need to be adjusted, and the reaction can be performed under the condition of the pH of 3-11.
4. Compared with a single oxidation repair technology, the method for removing algae in water by preparing ferrate activated persulfate has the advantages that the reaction speed is higher, the action effect is better, the application range is wider, the synergistic effect of ferrate and persulfate is mainly embodied in that ferrate is a chemical substance with oxidation and activation functions, PS is activated to generate SO4 with strong oxidation property to remove algae, the ferrate and PS also have the function of removing algae, the degradation speed of algae is greatly accelerated by coupling of the ferrate and the SO4, the reaction time is shortened, and the algae in the water body is efficiently removed.
Detailed Description
Firstly, the design of the invention is designed originally, along with the rapid development of the industry and agriculture in China, a large amount of nitrogen and phosphorus flow into the water body, so that the water body is eutrophicated, algae outbreak is caused, the transparency of the water body is reduced, the water quality is turbid, the sensory effect is deteriorated, dissolved oxygen in the water body can be reduced, other organisms in the water body die due to oxygen deficiency, the ecological balance of the water body is damaged, and the safety of the water environment is greatly threatened, therefore, the technical development for removing the algae is urgent, and therefore, the invention designs a method for removing the algae in the water by using the ferrate activated persulfate.
As will be described in more detail below, a method for producing ferrate-activated persulfate salts for removing algae from water includes the steps of:
the method comprises the following steps: preparing materials for electrolytic reaction; in the first step, sponge iron is prepared as a material for electrolytic reaction, iron in the sponge iron is used as an anode material, and carbon in the sponge iron is used as a cathode material.
Step two: carrying out electrolytic reaction to form electrolyte; and in the second step, adding the sponge iron into 1mM potassium hydroxide solution for electrolysis for 4 hours, wherein the electrolysis reaction is controlled by a self-made electrolytic cell with a SiO4 ceramic diaphragm and a periodic reversing device, the current density is controlled to be 40-50 mA/cm3, and the current is controlled to be 10-15A.
Step three: measuring the concentration of a generating substance in the electrolyte; after electrolysis, when the anode solution gradually turns purple, ferrate is generated in the electrolyte, and in the third step, a fixed volume of sodium ferrate solution is taken out every half hour for measuring the concentration.
Step four: removing impurities in the electrolyte; in the fourth step, when the concentration of the sodium ferrate is more than 0.1mM, the sodium ferrate is taken out and placed in a refrigerator for cooling for 1 hour, and then impurities are removed by suction filtration through a G4 sand core funnel.
Step five: adding a potassium hydroxide solution into the electrolyte with impurities removed to form a second solution; and in the fifth step, the filtrate is placed in a beaker, the beaker is placed in an ice water bath, a refrigerated 14mM potassium hydroxide solution is slowly dripped and fully stirred, the volume of the potassium hydroxide solution is 1/2 of the volume of the sodium ferrate solution, a second solution is formed in the process, then the second solution is stirred, and the second solution is placed in a freezing layer of a refrigerator for 40-60 min after being stirred.
Step six: carrying out suction filtration on the second solution; and in the sixth step, carrying out suction filtration on the stirred second solution to obtain crystals.
Step seven: dehydrating the filtered crystal; in the seventh step, cyclohexane dehydration and isopropanol dealkalization are carried out on the obtained crystals.
Step eight: carrying out vacuum drying treatment; and in the step eight, drying the potassium ferrate crystal subjected to dealkalization for 4 hours at 40 ℃ in a vacuum drying oven.
Step nine: and (4) storing the prepared crystals, wherein in the step nine, the prepared crystals are placed in a brown reagent bottle and are stored in a dryer at normal temperature.
Adding the prepared ferrate into the algae-containing wastewater to be treated, adding persulfate into the algae-containing wastewater to be treated, continuously stirring, and efficiently removing algae in a water body after a period of time, wherein the Persulfate (PS) is peroxymonosulfate or peroxydisulfate and comprises sodium salt, potassium salt and ammonium salt, the adding amount of the ferrate is 0.1-0.5 g/L, the adding amount of the persulfate is 0.2-1.0 g/L, the stirring speed is 100-200 r/min, the stirring time is 10-30 min, the pH in a sewage system does not need to be adjusted, and the reaction can be carried out under the pH condition of 3-11.
The following will be described with reference to examples:
example 1:
the method is characterized in that a self-made electrolytic cell with a SiO4 ceramic diaphragm and a periodic reversing device are adopted for electrolytic control, sponge iron is used as anode and cathode materials, a 1mM sodium hydroxide solution is used as an electrolyte, the current density is controlled to be 45mA/cm3, the current is controlled to be 15A, the electrolytic time is 4 hours, and a fixed volume of sodium ferrate solution is taken out every half an hour, and the concentration of the sodium ferrate solution is measured by adopting a chromate titration method.
When the concentration of the sodium ferrate is more than 0.1mM, taking out the sodium ferrate, placing the sodium ferrate in a refrigerator, cooling for one hour, then carrying out suction filtration by using a G4 sand core funnel to remove impurities, placing the filtrate in a beaker, placing the beaker in an ice water bath, slowly dropwise adding refrigerated 14mM potassium hydroxide solution, fully stirring, dropwise adding 1/2 with the volume of the sodium ferrate, fully stirring, and placing the solution in a refrigerator freezing layer for 50 minutes. Then taking out the solution for suction filtration again, dehydrating the obtained crystal by using cyclohexane, and dealkalizing by using isopropanol.
Drying the dealkalized potassium ferrate crystal in a vacuum drying oven at 40 ℃ for 4h, placing the prepared crystal in a brown reagent bottle, and storing the crystal in a dryer at normal temperature.
Taking microcystis aeruginosa as a research object, taking 100ml of algae-containing wastewater into a beaker, adjusting the initial pH value to 6 by using phosphoric acid and sodium hydroxide, adding 0.02g of prepared ferrate and 0.04g of prepared PS into the beaker, and continuously stirring for 30min to realize that the removal rate of algae reaches more than 95%.
Example 2:
the method is characterized in that a self-made electrolytic cell with a SiO4 ceramic diaphragm and a periodic reversing device are adopted for electrolytic control, sponge iron is used as anode and cathode materials, a 1mM sodium hydroxide solution is used as an electrolyte, the current density is controlled to be 45mA/cm3, the current is controlled to be 15A, the electrolytic time is 4 hours, and a fixed volume of sodium ferrate solution is taken out every half an hour, and the concentration of the sodium ferrate solution is measured by adopting a chromate titration method.
When the concentration of the sodium ferrate is more than 0.1mM, taking out the sodium ferrate, placing the sodium ferrate in a refrigerator, cooling for one hour, then carrying out suction filtration by using a G4 sand core funnel to remove impurities, placing the filtrate in a beaker, placing the beaker in an ice water bath, slowly dropwise adding refrigerated 14mM potassium hydroxide solution, fully stirring, dropwise adding 1/2 with the volume of the sodium ferrate, fully stirring, and placing the solution in a refrigerator freezing layer for 50 minutes. Then taking out the solution for suction filtration again, dehydrating the obtained crystal by using cyclohexane, and dealkalizing by using isopropanol. Drying the dealkalized potassium ferrate crystal in a vacuum drying oven at 40 ℃ for 4h, placing the prepared crystal in a brown reagent bottle, and storing the crystal in a dryer at normal temperature.
Taking microcystis aeruginosa as a research object, taking 100ml of algae-containing wastewater into a beaker, adjusting the initial pH value to 9 by using phosphoric acid and sodium hydroxide, adding 0.02g of prepared ferrate and 0.04g of prepared PS into the beaker, and continuously stirring for 30min to realize that the removal rate of algae reaches over 90 percent.
Example 3:
the electrolysis control is carried out by adopting a self-made electrolytic cell with a SiO4 ceramic diaphragm and a periodic reversing device, sponge iron is used as anode and cathode materials, 1mM sodium hydroxide solution is used as electrolyte, the current density is controlled to be 45mA/cm3, the current is controlled to be 15A, the electrolysis time is 4 hours, a fixed volume of sodium ferrate solution is taken out every half an hour, and the concentration of the sodium ferrate solution is measured by adopting a chromate titration method.
When the concentration of the sodium ferrate is more than 0.1mM, taking out the sodium ferrate, placing the sodium ferrate in a refrigerator, cooling for one hour, then carrying out suction filtration by using a G4 sand core funnel to remove impurities, placing the filtrate in a beaker, placing the beaker in an ice water bath, slowly dropwise adding refrigerated 14mM potassium hydroxide solution, fully stirring, dropwise adding 1/2 with the volume of the sodium ferrate, fully stirring, and placing the solution in a refrigerator freezing layer for 50 minutes. Then taking out the solution for suction filtration again, dehydrating the obtained crystal by using cyclohexane, and dealkalizing by using isopropanol. Drying the dealkalized potassium ferrate crystal for 4 hours at 40 ℃ in a vacuum drying oven. The prepared crystal is placed in a brown reagent bottle and is stored in a dryer at normal temperature.
Taking microcystis aeruginosa as a research object, taking 100ml of algae-containing wastewater into a beaker, adjusting the initial pH value to 6 by using phosphoric acid and sodium hydroxide, adding 0.01g of prepared ferrate and 0.02g of prepared PS into the beaker, and continuously stirring for 20min to realize that the removal rate of algae reaches more than 85 percent.
Therefore, the method for preparing ferrate activated persulfate to remove algae in water, which is used by the invention, only needs a small amount of ferrate and persulfate, and compared with other chemical methods, the dosage of the agent is small, so that the degradation cost is reduced.
2. Compared with the traditional physical mechanical separation method, the method for removing the algae in the water by using the ferrate activated persulfate, which is disclosed by the invention, is convenient and quick, reduces the consumption of manpower and electricity, and greatly saves the cost for removing the algae.
3. Compared with the traditional chemical method for removing algae, the method for removing algae in water by using the ferrate activated persulfate can perform reaction in a wider range of pH, the pH in a sewage system does not need to be adjusted, and the reaction can be performed under the condition of the pH of 3-11.
4. Compared with a single oxidation repair technology, the method for removing algae in water by preparing ferrate activated persulfate has the advantages that the reaction speed is higher, the action effect is better, the application range is wider, the synergistic effect of ferrate and persulfate is mainly embodied in that ferrate is a chemical substance with oxidation and activation functions, PS is activated to generate SO4 with strong oxidation property to remove algae, the ferrate and PS also have the function of removing algae, the degradation speed of algae is greatly accelerated by coupling of the ferrate and the SO4, the reaction time is shortened, and the algae in the water body is efficiently removed.
The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.
Claims (9)
1. A method for preparing ferrate activated persulfate to remove algae in water is characterized by comprising the following steps:
the method comprises the following steps: preparing materials for electrolytic reaction;
step two: carrying out electrolytic reaction to form electrolyte;
step three: measuring the concentration of a generating substance in the electrolyte;
step four: removing impurities in the electrolyte;
step five: adding a potassium hydroxide solution into the electrolyte with impurities removed to form a second solution;
step six: carrying out suction filtration on the second solution;
step seven: dehydrating the filtered crystal;
step eight: carrying out vacuum drying treatment;
step nine: and preserving the prepared crystals.
2. The method for removing algae in water by using ferrate-activated persulfate as claimed in claim 1, wherein in the first step, sponge iron is prepared as a material for electrolysis, iron in the sponge iron is used as an anode material, carbon in the sponge iron is used as a cathode material, and in the second step, the sponge iron is added into 1mM potassium hydroxide solution for electrolysis for 4 hours, and the electrolysis is carried out by using a self-made SiO-containing solution4The electrolytic bath of the ceramic diaphragm and the periodic reversing device are subjected to electrolytic control, the current density is controlled to be 40-50 mA/cm3, and the current is controlled to be 10-15A.
3. The method for removing algae in water by using ferrate-activated persulfate as claimed in claim 2, wherein ferrate is generated in the electrolyte when the anode solution gradually turns purple after electrolysis, and wherein in the third step, a fixed volume of sodium ferrate solution is taken out every half hour to measure the concentration, and in the fourth step, when the concentration of sodium ferrate is more than 0.1mM, the solution is taken out and placed in a refrigerator to be cooled for 1 hour, and then impurities are removed by suction filtration through a G4 sand core funnel.
4. The method for preparing ferrate-activated persulfate salts to remove algae from water according to claim 3, wherein in the fifth step, the filtrate is placed in a beaker, the beaker is placed in an ice-water bath, a refrigerated 14mM potassium hydroxide solution is slowly added dropwise and fully stirred, the volume of the potassium hydroxide solution is 1/2 of that of the sodium ferrate solution, the second solution is formed in the fifth step, then the second solution is stirred and placed in a freezing layer of a refrigerator for 40-60 min, and in the sixth step, the stirred second solution is subjected to suction filtration to obtain crystals.
5. The method for preparing ferrate-activated persulfate salts to remove algae from water as claimed in claim 4, wherein in the seventh step, cyclohexane dehydration and isopropanol dealkalization are performed on the obtained crystals, and in the eighth step, the dealkalized potassium ferrate crystals are dried in a vacuum drying oven at 40 ℃ for 4 hours.
6. The method for removing algae in water by preparing ferrate-activated persulfate according to claim 5, wherein in the ninth step, the prepared crystals are placed in a brown reagent bottle and stored in a dryer at normal temperature, the prepared ferrate is added into the algae-containing wastewater to be treated, the persulfate is added into the algae-containing wastewater to be treated and is continuously stirred, and the algae in the water body can be efficiently removed after a period of time.
7. The method of claim 6, wherein the Persulfate (PS) is peroxymonosulfate or peroxydisulfate, including sodium, potassium and ammonium salts.
8. The method for preparing ferrate-activated persulfate salts to remove algae from water according to claim 7, wherein the ferrate is added in an amount of 0.1-0.5 g/L, the persulfate salt is added in an amount of 0.2-1.0 g/L, the stirring speed is 100-200 r/min, and the stirring time is 10-30 min.
9. The method for removing algae in water by using ferrate-activated persulfate as claimed in claim 8, wherein the pH in the sewage system is not required to be adjusted, and the reaction can be carried out under the condition of pH of 3-11.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115155587A (en) * | 2022-08-03 | 2022-10-11 | 北京师范大学 | Iron-aluminum mud-based magnetic catalyst, preparation method and algae removal method |
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| CN101713078A (en) * | 2009-09-22 | 2010-05-26 | 上海市政工程设计研究总院 | Device and method for preparing potassium ferrate through electrolysis |
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| CN101713078A (en) * | 2009-09-22 | 2010-05-26 | 上海市政工程设计研究总院 | Device and method for preparing potassium ferrate through electrolysis |
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