CN111470575A - Magnetic phosphorus removal agent and preparation method thereof - Google Patents
Magnetic phosphorus removal agent and preparation method thereof Download PDFInfo
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- CN111470575A CN111470575A CN202010181901.0A CN202010181901A CN111470575A CN 111470575 A CN111470575 A CN 111470575A CN 202010181901 A CN202010181901 A CN 202010181901A CN 111470575 A CN111470575 A CN 111470575A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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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
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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Abstract
The invention discloses a preparation method of a magnetic phosphorus removal agent, which comprises the following steps: (1) under inert atmosphere, dissolving ferric salt and ferrous salt in water to obtain a mixed solution, adding alkali liquor until the pH value is 8.5-10, and stirring for reaction to obtain a magnetic colloidal solution; (2) adding an inorganic coagulant or/and an organic flocculant into the magnetic colloidal solution, continuously stirring for reaction, standing, collecting a black product by using a magnet, washing the black product to be neutral, and then drying the black product in vacuum to obtain the magnetic phosphorus removal agent. According to the invention, a one-pot method is adopted, PAC and/or PAM are simultaneously added in the preparation process of the magnetic ferroferric oxide, so that magnetic ferroferric oxide particles are coated, the particles are not easy to agglomerate, the contact effect with pollutants is better, PAC and/or PAM are used for removing phosphorus in a synergistic manner, the phosphorus removal effect is better, and the magnetic particles in the magnetic phosphorus removal agent are coated, so that the effective phosphorus removal particles are not easy to leach out and fall off, and the phosphorus removal agent can be regenerated through alkali treatment and has good reutilization property.
Description
Technical Field
The invention relates to a magnetic phosphorus removal agent and a preparation method thereof, belonging to the technical field of wastewater phosphorus removal agents.
Background
In recent years, with the rapid development of economy in China, a large amount of nitrogen and phosphorus wastewater is discharged into rivers and other water body environments, so that the problem of water body eutrophication is becoming serious, wherein phosphorus is also taken as a key factor. In terms of the current form, total phosphorus is still one of the indexes which are difficult to control in town sewage treatment, and the increasingly strict effluent discharge standard cannot be met only by a biological treatment process, so that the problem of water pollution caused by excessive phosphorus worldwide is directly caused. Therefore, removal of phosphorus is already imminent.
Currently, the commonly used phosphorus removal methods are roughly classified into four methods, i.e., chemical precipitation, crystallization, biological method, and adsorption method. Although the chemical precipitation method is simple to operate and stable in dephosphorization effect, the problems that the chemical agent needs to be continuously added, the consumption of the chemical agent is high, the operation cost is high, the chemical agent cannot be recycled, a large amount of secondary sludge is generated, the treatment cost is increased and the like exist. The phosphorus removing agent commonly used at present mainly comprises iron salt, aluminum salt, polyferric oxide and polyaluminiumCoagulant, PAM flocculant, etc. For removing phosphorus from coagulant, Zhang Zhi[1]The main problems of chemical phosphorus removal found in the discussion of chemical phosphorus removal of municipal sewage are that the medicament is expensive, the operation cost is high, and the difficulty of sludge treatment and disposal is increased due to the consumption of a certain amount of medicaments and the generation of a large amount of chemical sludge; to treat chronic diarrhea[2]When the flocculating agent is used for phosphorus removal alone, the flocculating agent has weak trapping capability and poor phosphorus removal effect, and needs to be combined with ferric salt and aluminum salt for synergistic phosphorus removal. The crystallization method mainly generates struvite, is low in cost and easy to control, but is easy to block a pipeline and high in maintenance cost. The biological method has low cost, environmental protection and wide application, but has unstable treatment effect and is easily influenced by the outside. Although the adsorption method has simple process, the adsorption method has the defects of high adsorbent selectivity, limited adsorption capacity, difficult regeneration and the like, so the key point is that the adsorbent is used, currently, scholars use the characteristic that the ferroferric oxide is easy to recycle under a magnetic field to remove phosphorus, but the ferroferric oxide is easy to agglomerate in water to cause the reduction of adsorption capacity, and the ferroferric oxide needs to be modified[3]. Therefore, research and preparation of efficient and easily-regenerated phosphorus removal materials and methods are very necessary.
[1] Zhang Zhi, discussion of chemical phosphorus removal from municipal sewage, Chongqing environmental science, 2002.
[2] Xujiayu, a comparative study on the deep phosphorus removal performance of several coagulants, Guangxi light chemical industry, 2009.
[3] Picrorhiza scrophulariiflora, preparation of ferroferric oxide/polyethyleneimine nanoparticles, research on phosphorus removal performance, statement of environmental science, 2017.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of a magnetic phosphorus removal agent with small dosage, good phosphorus removal effect, easy regeneration and good reusability.
In order to achieve the technical purpose, the invention provides a preparation method of a magnetic phosphorus removal agent, which comprises the following steps:
(1) under inert atmosphere, dissolving ferric salt and ferrous salt in water to obtain a mixed solution, adding alkali liquor until the pH value is 8.5-10, and stirring for reaction to obtain a magnetic colloidal solution;
(2) adding an inorganic coagulant or/and an organic flocculant into the magnetic colloidal solution, continuously stirring for reaction, standing, collecting a black product by using a magnet, washing the black product to be neutral, and then drying the black product in vacuum to obtain the magnetic phosphorus removal agent.
Preferably, in the step (1), the molar ratio of the ferric salt to the ferrous salt is 2: 0.8-1.5, and is further preferably 2: 1, the ferric salt is one of ferric chloride, ferric sulfate and ferric nitrate, and is further preferably ferric chloride, the ferrous salt is one of ferrous chloride and ferrous sulfate, and is further preferably ferrous sulfate, and the concentration of the ferric salt in the mixed solution is 0.05-0.5 mol/L.
Preferably, in the step (1), the alkali solution added is one of ammonia water, sodium hydroxide solution and potassium hydroxide solution.
Preferably, in the step (1), the temperature of the stirring reaction is 20-60 ℃ and the time is 20-60 min.
Preferably, in the step (2), the inorganic coagulant is PAC, and the organic flocculant is anionic PAM or cationic PAM, preferably cationic PAM; the adding amount of PAC is 1-5 wt% of the magnetic colloid solution, and the adding amount of PAM is 1-5 wt% of the magnetic colloid solution.
Preferably, in the step (2), the temperature of the stirring reaction is 20-60 ℃, the time is 20-60min, and the standing time is 10-30 min.
Preferably, in the step (2), the temperature of the vacuum drying is 50-80 ℃ and the time is 6-18 h.
Preferably, in the step (2), grinding and screening are carried out after vacuum drying, and the particle size after screening is not more than 100 meshes.
Preferably, the magnetic phosphorus removal agent is used for removing phosphorus from wastewater, is placed in deionized water with the pH value adjusted to 10-14 in advance, is vibrated for 0.5-2h at normal temperature in a shaking table, is adsorbed by a magnet and is washed by deionized water until the solution is neutral, and is dried, so that the regeneration of the magnetic phosphorus removal agent can be completed.
Preferably, the drying temperature is 50-70 ℃, the drying time is 0.5-2h, and the drying can be carried out in a vacuum drying box or a forced air drying box, preferably in the vacuum drying box.
The invention also provides the magnetic phosphorus removal agent prepared by the preparation method.
The magnetic phosphorus removal agent prepared by the invention combines the advantages of chemical phosphorus removal and adsorption phosphorus removal, phosphorus removal is carried out by utilizing iron and aluminum adsorption sites and electrostatic attraction of a magnetic material, the stability of phosphorus removal effect is ensured, the magnetic phosphorus removal agent can be recycled, and the defects of large dosage of the agent in the chemical phosphorus removal, large sludge production amount, high operation cost and easy particle agglomeration in the ferroferric oxide phosphorus removal are avoided. In addition, after the magnetic ferroferric oxide is modified by PAC and/or PAM, magnetic ferroferric oxide particles are coated to form a core-shell structure, the particles are not easy to agglomerate, and the contact effect with pollutants is better; meanwhile, in order to verify that effective ions in the magnetic phosphorus removal agent are not easy to leach and fall off, the inventor conducts an ion leaching experiment on the magnetic phosphorus removal agent: respectively weighing 0.1g of magnetic phosphorus removal agent material into conical flasks filled with 100ml of distilled water, stirring and reacting for 2 hours in a shaking table at 180r/min, placing a magnet below the conical flasks, taking the supernatant of the solution for ion detection, measuring the concentration of metal ions by adopting a flame atomic absorption method, and detecting no corresponding iron ions and aluminum ions in the supernatant after the ion leaching experiment, thereby indicating that the effective ions of the magnetic phosphorus removal agent prepared by the invention are not easy to leach and fall off and ensuring the reusability of the magnetic phosphorus removal agent.
The beneficial results of the invention are as follows:
compared with single magnetic ferroferric oxide, the phosphorus removal effect is poor, PAC phosphorus removal is good, but continuous addition of medicaments is required, so that the medicament addition amount is large, and the secondary sludge amount is also large.
Drawings
FIG. 1 is SEM images of the magnetic phosphorus removal agent (b) prepared in example 3 and the magnetic ferroferric oxide (a) prepared in comparative example 1.
Detailed Description
The present invention is further illustrated by the following examples, it being understood that the examples described are only a few examples of the present invention and are not intended to limit the invention to the embodiments described. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without any inventive step, are within the scope of the present invention.
Example 1
1.3902g of FeSO4·7H2O and 2.7000g FeCl3·6H2Dissolving O in 100m L deionized water, placing the mixture in a three-neck flask, introducing nitrogen to remove air in the flask, preventing oxidation, dropwise adding a saturated ammonia water solution into the mixture solution under magnetic stirring and nitrogen protection until the pH value is 9.5, stopping dropwise adding ammonia water, fully stirring for reaction for 30min, adding 1 wt% PAC, continuously stirring for reaction for 30min, standing for 10min, collecting a black product by using a magnet, washing the black product to be neutral by using enough deionized water, drying the black product in a vacuum drying oven at 60 ℃ for 6h, grinding the dried black solid into powder by using a mortar, sieving the powder by using a 100-mesh sieve, sealing, drying and storing to obtain the magnetic phosphorus removal agent.
Example 2
1.3902g of FeSO4·7H2O and 2.7000g FeCl3·6H2Dissolving O in 100m L deionized water, placing the mixture in a three-neck flask, introducing nitrogen to remove air in the flask, preventing oxidation, dropwise adding a saturated ammonia water solution into the mixture solution under magnetic stirring and nitrogen protection until the pH value is 9.5, stopping dropwise adding ammonia water, fully stirring and reacting for 30min, then adding 1 wt% of PAM, continuing stirring and reacting for 30min, standing for 10min, collecting a black product by using a magnet, washing the black product to be neutral by using enough deionized water, drying the black product in a vacuum drying oven at 60 ℃ for 6h, grinding the dried black solid into powder by using a mortar, sieving the powder by using a 100-mesh sieve, sealing, drying and storing, thus obtaining the magnetic phosphorus removal agent.
Example 3
1.3902g of FeSO4·7H2O and 2.7000g FeCl3·6H2Dissolving O in 100m L deionized water, placing the mixture in a three-neck flask, introducing nitrogen to remove air in the flask, preventing oxidation, dropwise adding a saturated ammonia water solution into the mixture solution under magnetic stirring and nitrogen protection until the pH value is 9.5, stopping dropwise adding ammonia water, fully stirring and reacting for 30min, then sequentially adding 1 wt% PAC and 1 wt% PAM, continuing stirring and reacting for 30min, standing for 10min, collecting a black product by using a magnet, washing the black product with enough deionized water to neutrality, drying the black product in a vacuum drying oven at 60 ℃ for 6h, grinding the dried black solid into powder by using a mortar, sieving the powder by using a 100-mesh sieve, sealing, drying and storing, wherein the obtained material is the magnetic phosphorus removal agent.
Comparative example 1
1.3902g of FeSO4·7H2O and 2.7000g FeCl3·6H2Dissolving O in 100m L deionized water, placing in a three-neck flask, introducing nitrogen to remove air in the flask, preventing oxidation, dropwise adding saturated ammonia water solution into the mixture solution under magnetic stirring and nitrogen protection to pH 9.5, stopping dropwise adding ammonia water, stirring thoroughly for reaction for 30min, standing for 10min, collecting black product with magnet, washing with enough deionized water to neutrality, drying in vacuum drying oven at 60 deg.C for 6h, and dryingGrinding the color solid into powder by using a mortar, sieving by using a 100-mesh sieve, sealing, drying and storing to obtain the magnetic ferroferric oxide.
As shown in figure 1, the average particle size of the magnetic ferroferric oxide particles prepared in the comparative example 1 is about 30-50 nm (a); in the embodiment 3, the average particle size of the magnetic phosphorus removal agent generated by adding PAC and PAM is about 80-100 nm (b), and the magnetic ferroferric oxide particles are coated, so that the phosphorus removal effective particles are not easy to leach out and fall off; meanwhile, compared with magnetic ferroferric oxide, the magnetic phosphorus removal agent is more irregular, better in dispersity and more difficult to agglomerate.
Preparing a phosphorus-containing wastewater stock solution with the concentration of a phosphorus-containing solution of 50 mg/L according to national standards, diluting to obtain 10 mg/L of phosphorus-containing wastewater, putting 100m L of the phosphorus-containing wastewater into a conical flask, respectively adding 0.1g of the magnetic phosphorus removal agent prepared in examples 1-3, the magnetic ferroferric oxide, PAC and PAM prepared in comparative example 1, carrying out vibration treatment in a shaker at 20 ℃ for 2h, taking supernatant of the phosphorus-containing wastewater after vibration treatment, measuring the phosphorus-containing concentration at 700nm by using a spectrophotometry method, wherein the phosphorus removal rate is shown in Table 1,
TABLE 1 phosphorus removal rates for different samples
| Sample (I) | Example 1 | Example 2 | Example 3 | Comparative example 1 | PAC | PAM |
| Phosphorus removal rate | 92.1％ | 87.3％ | 98.3％ | 68.5％ | 93.9％ | 9.8％ |
The phosphorus removal method comprises the steps of carrying out phosphorus removal on the wastewater in examples 1-3 and comparative example 1, then respectively soaking the wastewater in deionized water with the pH value of 10-14, then oscillating the wastewater in a shaker at normal temperature for 0.5-2h, then washing the wastewater with the deionized water under the magnetic adsorption to be neutral, then drying the wastewater in a vacuum drying oven at 50-70 ℃ for 0.5-2h to finish regeneration, and then reusing the wastewater for phosphorus removal, respectively weighing 0.1g of the regenerated samples in examples 1-3 and comparative example 1, placing the regenerated samples in 100m L phosphorus-containing wastewater containing 10 mg/L, oscillating the samples in the shaker at 20 ℃ for 2h, taking supernatant of the phosphorus-containing wastewater after oscillation treatment, measuring the phosphorus-containing concentration at 700nm by using a spectrophotometry, and regenerating and using the phosphorus removal rate for 3 times, wherein the phosphorus removal rate is shown in table 2, after 3 times of regeneration and using the magnetic phosphorus removal agent, the phosphorus removal rate of the phosphorus-containing wastewater is still above 70%, the repeatability is good, and after 3 times of regeneration, the magnetic ferroferric oxide is used for 3 times, the phosphorus removal rate is only 15.4%, and the.
TABLE 2 phosphorus removal rates for different samples for reuse
| Sample (I) | Practice ofExample 1 | Example 2 | Example 3 | Comparative example 1 |
| 1 st time | 89.4％ | 84.6％ | 93.2％ | 35.2％ |
| 2 nd time | 84.5％ | 80.1％ | 88.7％ | 20.1％ |
| 3 rd time | 78.3％ | 74.8％ | 82.1％ | 15.4％ |
From the table 1 and the table 2, the magnetic phosphorus removal agent prepared by the invention has obviously improved phosphorus removal effect compared with the single magnetic ferric oxide, the sample prepared by the embodiment 3 has optimal effect, the removal rate is as high as 98.3%, the removal rate of phosphorus-containing wastewater after 3 times of regeneration can still reach 82.1%, and the repeatability is good; the removal rate of the magnetic ferroferric oxide to the phosphorus-containing wastewater is reduced from 68.5 to 15.4 percent; meanwhile, although the primary phosphorus removal effect of the single PAC can reach 93.9%, the PAC cannot be recycled in the phosphorus removal process, and the agent needs to be continuously added for many times, so that the using amount of the agent is large, the subsequent secondary sludge amount is increased, and the treatment cost of the phosphorus-containing wastewater can be increased.
Claims (10)
1. A preparation method of a magnetic phosphorus removal agent is characterized by comprising the following steps:
(1) under inert atmosphere, dissolving ferric salt and ferrous salt in water to obtain a mixed solution, adding alkali liquor until the pH value is 8.5-10, and stirring for reaction to obtain a magnetic colloidal solution;
(2) adding an inorganic coagulant or/and an organic flocculant into the magnetic colloidal solution, continuously stirring for reaction, standing, collecting a black product by using a magnet, washing the black product to be neutral, and then drying the black product in vacuum to obtain the magnetic phosphorus removal agent.
2. The preparation method of the magnetic phosphorus removing agent according to claim 1, wherein in the step (1), the molar ratio of the ferric salt to the ferrous salt is 2: 0.8-1.5, the ferric salt is one of ferric chloride, ferric sulfate and ferric nitrate, the ferrous salt is one of ferrous chloride and ferrous sulfate, and the concentration of the ferric salt in the mixed solution is 0.05-0.5 mol/L.
3. The preparation method of the magnetic phosphorus removal agent as claimed in claim 1, wherein: in the step (1), the alkali liquor is one of ammonia water, sodium hydroxide solution and potassium hydroxide solution.
4. The preparation method of the magnetic phosphorus removal agent as claimed in claim 1, wherein: in the step (1), the temperature of the stirring reaction is 20-60 ℃, and the time is 20-60 min.
5. The preparation method of the magnetic phosphorus removal agent as claimed in claim 1, wherein: in the step (2), the inorganic coagulant is PAC, and the organic flocculant is PAM; the adding amount of PAC is 1-5 wt% of the magnetic colloid solution, and the adding amount of PAM is 1-5 wt% of the magnetic colloid solution.
6. The preparation method of the magnetic phosphorus removal agent as claimed in claim 1, wherein: in the step (2), the stirring reaction is carried out at the temperature of 20-60 ℃ for 20-60min, and the standing time is 10-30 min.
7. The preparation method of the magnetic phosphorus removal agent as claimed in claim 1, wherein: in the step (2), the temperature of the vacuum drying is 50-80 ℃, and the time is 6-18 h.
8. The preparation method of the magnetic phosphorus removal agent as claimed in claim 1, wherein: in the step (2), grinding and screening are carried out after vacuum drying, and the particle size after screening is not more than 100 meshes.
9. The preparation method of the magnetic phosphorus removal agent as claimed in claim 1, wherein: the magnetic phosphorus removal agent is used for removing phosphorus from wastewater, is placed in deionized water with the pH value adjusted to 10-14 in advance, is vibrated in a shaking table at normal temperature for 0.5-2h, is adsorbed by a magnet, is washed by the deionized water to be neutral, and is dried, so that the regeneration of the magnetic phosphorus removal agent can be completed.
10. The magnetic phosphorus removal agent prepared by the preparation method of any one of claims 1 to 9.
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Cited By (4)
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| CN112619591A (en) * | 2020-12-07 | 2021-04-09 | 江门谦信化工发展有限公司 | Preparation method and application of magnetic composite adsorption material |
| CN112811706A (en) * | 2021-01-06 | 2021-05-18 | 北京国蓝环保科技有限公司 | Sewage treatment method based on heavy medium carrier |
| CN113908815A (en) * | 2021-11-15 | 2022-01-11 | 南京工业大学 | High-molecular modified adsorbent and preparation method and application thereof |
| CN115286126A (en) * | 2021-04-15 | 2022-11-04 | 国家能源投资集团有限责任公司 | Sewage treatment method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112619591A (en) * | 2020-12-07 | 2021-04-09 | 江门谦信化工发展有限公司 | Preparation method and application of magnetic composite adsorption material |
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| CN112811706A (en) * | 2021-01-06 | 2021-05-18 | 北京国蓝环保科技有限公司 | Sewage treatment method based on heavy medium carrier |
| CN115286126A (en) * | 2021-04-15 | 2022-11-04 | 国家能源投资集团有限责任公司 | Sewage treatment method |
| CN113908815A (en) * | 2021-11-15 | 2022-01-11 | 南京工业大学 | High-molecular modified adsorbent and preparation method and application thereof |
| CN113908815B (en) * | 2021-11-15 | 2022-07-26 | 南京工业大学 | High-molecular modified adsorbent and preparation method and application thereof |
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Application publication date: 20200731 |
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