CN111389343A - Lanthanum-based loaded magnetic nano adsorption phosphorus removal material and synthesis method thereof - Google Patents
Lanthanum-based loaded magnetic nano adsorption phosphorus removal material and synthesis method thereof Download PDFInfo
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Abstract
The invention discloses a lanthanum-based loaded magnetic nano adsorption dephosphorization material and a synthesis method thereof, wherein the preparation method comprises the following steps: step 1: sequentially adding ferroferric oxide, a chelating agent and lanthanum salt into deionized water, and sequentially stirring and uniformly mixing, wherein the molar ratio of the ferroferric oxide to the lanthanum salt is 1:6-5: 1; step 2: and (3) putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, and reacting at the temperature of 120-200 ℃ for 8-12h to obtain the prepared phosphorus adsorbing and removing material. The magnetic lanthanum-based phosphorus removal adsorbent prepared by the method has the advantages of excellent phosphorus removal effect, wide pH application range, strong phosphate radical specific adsorption capacity and easiness in recycling and reutilization.
Description
Technical Field
The invention belongs to the field of inorganic nano/micron materials, and particularly relates to a lanthanum-based loaded magnetic nano adsorption dephosphorization material and a synthesis method thereof.
Background
The problem of eutrophication of water bodies has been one of the biggest environmental problems facing the world, and this problem has resulted in the following consequences: 1. the dissolved oxygen in the water body is consumed, so that the water quality is deteriorated; 2. reducing the diversity of organisms. Because the blue algae forms an absolute dominant population, the deterioration of the water body environment is aggravated, and the survival and the propagation of other algae, plankton and aquatic animals are greatly influenced; 3. generating peculiar smell; 4. when the water source of the water works blooms, a large amount of algae can cause the treatment capacity of the treatment plant to be reduced, the water body can have musty and rotten taste, and even the algae toxins can directly influence the life safety of residents, so that the drinking water safety is influenced; 5. destroying the water landscape. The current subject research considers that the eutrophic element phosphorus is the most direct cause of water eutrophication, especially in fresh water, so that phosphorus control is very important for inhibiting water eutrophication.
In the prior art, the phosphorus removal method of sewage comprises a chemical precipitation method, an electrolysis method, a microbiological method, a hydrobiological method, an adsorption method, a soil treatment method, a membrane technology treatment method and the like. The adsorption method has the advantages of large capacity, low energy consumption, low pollution, quick removal, recyclability and the like, and is widely applied to the aspect of dephosphorization. The adsorption material is the core of the adsorption process, and how to construct a high-performance adsorption material structure is the key point of global attention at present. Among various phosphorus removal adsorbing materials, the lanthanum-containing adsorbing material has excellent phosphorus removal performance due to the high phosphate radical binding capacity of the lanthanum-containing adsorbing material.
When a lanthanum-based material is used as a phosphorus removal adsorption material, two problems need to be solved at present: 1. how to improve the utilization rate of metal lanthanum in the material to the maximum extent and enable the metal lanthanum to exert the maximum phosphate radical adsorption performance; 2. how to recover and reuse metal lanthanum.
Disclosure of Invention
Aiming at the problems, the invention provides a lanthanum-based loaded magnetic nano adsorption phosphorus removal material and a synthesis method thereof.
The technical purpose is achieved, the technical effect is achieved, and the invention is realized through the following technical scheme:
the invention provides a synthesis method of a lanthanum-based loaded magnetic nano adsorption phosphorus removal material, which comprises the following steps:
step 1: sequentially adding ferroferric oxide, a chelating agent and a lanthanum salt into deionized water, and sequentially stirring and uniformly mixing, wherein the molar ratio of the ferroferric oxide to the lanthanum salt is 1:6-5: 1;
step 2: and (3) putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, and reacting at the temperature of 120-200 ℃ for 8-12h to obtain the prepared phosphorus adsorbing and removing material.
As a further improvement of the invention, the particle size of the selected ferroferric oxide is 5-50 nm.
As a further improvement of the invention, the molar ratio of the ferroferric oxide to the lanthanum salt is 1:1-4:1
As a further improvement of the invention, the reaction temperature in the second step is 180-200 ℃.
As a further improvement of the invention, the reaction time in the second step is 10-12 h.
As a further improvement of the invention, the lanthanum salt is selected from lanthanum chloride or lanthanum nitrate.
As a further improvement of the invention, the chelating agent is selected from any one or more of sodium citrate, anhydrous sodium acetate and sodium ethylene diamine tetracetate.
In addition, the invention also provides a lanthanum-based loaded magnetic nano adsorption dephosphorization material prepared by adopting the method.
The invention has the beneficial effects that:
(1) the invention provides a simple and efficient preparation method of a phosphorus removal adsorbent, and the magnetic lanthanum-based phosphorus removal adsorbent prepared by the method has the advantages of complete crystal structure, small size and uniform distribution.
(2) The method has the advantages of simple experimental conditions, easy operation, no special equipment requirements, good reproducibility and large-scale preparation and commercialization realization.
(3) The magnetic lanthanum-based phosphorus removal adsorbent prepared by the invention has the advantages of excellent phosphorus removal effect, wide pH application range, strong phosphate radical specific adsorption capacity and easiness in recycling and reutilization.
Drawings
FIG. 1 is a macroscopic view of the magnetic lanthanum-based phosphorus removal adsorbent material obtained in example 1 of the present invention;
fig. 2 is a Scanning Electron Microscope (SEM) image of the magnetic lanthanum-based phosphorus removal adsorbing material obtained in example 1 of the present invention;
fig. 3 is a Scanning Electron Microscope (SEM) image of the magnetic lanthanum-based phosphorus removal adsorbing material obtained in example 2 of the present invention;
fig. 4 is a Scanning Electron Microscope (SEM) image of the magnetic lanthanum-based phosphorus removal adsorbing material obtained in example 3 of the present invention;
fig. 5 is a Scanning Electron Microscope (SEM) image of the magnetic lanthanum-based phosphorus removal adsorbing material obtained in example 4 of the present invention;
fig. 6 is a Scanning Electron Microscope (SEM) image of the magnetic lanthanum-based phosphorus removal adsorbing material obtained in example 5 of the present invention;
FIG. 7 is an X-ray powder diffraction pattern (XRD) of the magnetic lanthanum-based phosphorus removal adsorbent obtained in examples 1 to 5 of the present invention;
FIG. 8 is an X-ray powder diffraction pattern (XRD) of magnetic ferroferric oxide used in the present invention;
FIG. 9 is a graph of the change in adsorption performance of a lanthanum-based magnetic material under the influence of pH;
FIG. 10 is a graph of the change in adsorption performance of a lanthanum-based magnetic material under the influence of different coexisting ions;
FIG. 11 is a graph showing the magnetic effect of the adsorbed material;
fig. 12 is a cycle diagram of adsorption and desorption of a material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
Preparation of ferroferric oxide
The method specifically comprises the following steps of firstly putting deionized water in a vacuum device for 0.5 hour to remove oxygen in the water, then dissolving 13.51g of 100mmol FeCl3 & 6H2O and 6.95g of 50mmol FeSO4 & 7H2O in 150m L oxygen-removed deionized water, transferring the deionized water into a three-neck flask, heating the deionized water to 60 ℃ under the protection of nitrogen, dropwise adding 52m L4 mol/L NaOH solution into the three-neck flask within 30 minutes, simultaneously mechanically stirring at 400rpm to increase the pH of the solution to 9-10, mechanically stirring at 500rpm for reaction for 1 hour, carrying out magnetic separation on a final product, washing the final product with ethanol and water for 2 times respectively, freeze-drying the product by a freeze dryer, and storing the product in a vacuum drying box for later use, wherein the particle size distribution of the ferroferric oxide prepared by the method is 5-50 nm.
Preparation of adsorption phosphorus removal material
Example 1
Weighing 5mmol of ferroferric oxide, adding the ferroferric oxide into 80ml of pure water, and carrying out ultrasonic treatment for 15 min; then 6.0g of sodium citrate is added and mechanically stirred for 30 min; then 20mmol of lanthanum chloride is added and mechanically stirred for 30min, 1000 r/min; and then sealed in a teflon lined stainless steel autoclave. Heating at 180 deg.C for 12h, and cooling to room temperature. And washing the product after magnetic separation with pure water and ethanol for a plurality of times, and carrying out vacuum freeze drying to obtain the magnetic lanthanum-based phosphorus removal adsorbing material.
Example 2
Weighing 5mmol of ferroferric oxide, adding the ferroferric oxide into 80ml of ethanol, and carrying out ultrasonic treatment for 15 min; then 6.0g of sodium ethylene diamine tetracetate is added and mechanically stirred for 30 min; then adding 5mmol lanthanum chloride, and mechanically stirring for 60min at a speed of 500 r/min; and then sealed in a teflon lined stainless steel autoclave. Heating at 200 deg.C for 10h, and cooling to room temperature. And washing the product after filtering and separating for a plurality of times by pure water and ethanol, and carrying out vacuum freeze drying to obtain the magnetic lanthanum-based phosphorus removal adsorbing material.
Example 3
Weighing 5mmol of ferroferric oxide, adding the ferroferric oxide into 80ml of water, and carrying out ultrasonic treatment for 15 min; then 6.0g of sodium citrate is added and mechanically stirred for 30 min; then adding 1mmol lanthanum chloride, mechanically stirring for 10min, 2000 r/min; and then sealed in a teflon lined stainless steel autoclave. Heating at 180 deg.C for 8h, and cooling to room temperature. Washing the product after gravity settling for a plurality of times by pure water and ethanol, and carrying out vacuum freeze drying to obtain the magnetic lanthanum-based dephosphorization adsorbing material.
Example 4:
weighing 5mmol of ferroferric oxide, adding the ferroferric oxide into 80ml of water, and carrying out ultrasonic treatment for 15 min; then 6.0g of anhydrous sodium acetate is added and mechanically stirred for 30 min; then 30mmol of lanthanum nitrate is added and mechanically stirred for 60min, 1000 r/min; and then sealed in a teflon lined stainless steel autoclave. Heating at 200 deg.C for 12h, and cooling to room temperature. Washing the product after centrifugal separation with pure water and ethanol for several times, heating to 80 ℃ in vacuum, and drying to obtain the magnetic lanthanum-based phosphorus removal adsorbing material.
Example 5:
weighing 5mmol of ferroferric oxide, adding the ferroferric oxide into 80ml of ethylene glycol, and carrying out ultrasonic treatment for 15 min; then 6.0g of sodium citrate and sodium ethylene diamine tetracetate are added and mechanically stirred for 30 min; then 30mmol of lanthanum chloride is added and mechanically stirred for 120min, 2000 r/min; and then sealed in a teflon lined stainless steel autoclave. Heating at 200 deg.C for 10h, and cooling to room temperature. Washing the product after centrifugal separation and magnetic separation with pure water and ethanol for several times, and performing vacuum freeze drying to obtain the magnetic lanthanum-based phosphorus removal adsorbing material.
Performance testing
Various results characterizations were performed for the materials in the various examples. FIG. 1 shows a photomicrograph of a sample of example 1. It can be seen that the prepared magnetic lanthanum-based phosphorus removal adsorbing material is uniform powder. In the corresponding SEM image, the material structure is a simpler spherical structure, and the structure is complete and has better uniformity. As can be seen from the SEM images of fig. 2 to 6, the magnetic lanthanum-based phosphorus removal adsorption material prepared in examples 1 to 5 generally has a small size, which is about 50nm, and increases the specific surface area of the material, which is helpful for improving the adsorption performance of the material. As can be seen from the XRD pattern of fig. 7, the materials in the above examples all have diffraction peaks corresponding to the form of lanthanum and magnetite. Comparing the XRD characteristic peak diagram of pure ferroferric oxide in FIG. 8, it can be determined that the purity of the ferroferric oxide components contained in the materials prepared in examples 1-5 is high. Compared with other examples, the morphology and diffraction peaks of examples 1 and 2 show that sodium citrate complexes the lanthanum iron compound better and the adsorption effect is better.
In fig. 9, under the conditions that the adding amount is 0.1 g/L and the initial phosphate concentration is 2mg P/L, 10 groups of different environments with pH values of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 and the like are set and certain conditions are performed to perform adsorption experiments, the change of the adsorption amount is detected, the material is less influenced by the pH, the material can have a good adsorption effect under an acid-base environment with pH of 4-11, the adsorption amount can reach about 19.7mg/g, the adsorption requirement can be met under a neutral condition, and the adsorption performance of the material cannot be damaged by the acidity and alkalinity in a general actual water body.
In fig. 10, a certain amount of common ions are added into a phosphate solution to simulate actual wastewater, and three concentration levels are set, namely 10 mg/L, 50 mg/L and 100 mg/L. under the influence of different coexisting ions, an adsorption experiment is carried out under the conditions that the adding amount is 0.1 g/L, the initial phosphate concentration is 2mg P/L and the pH is 7 +/-0.2, the change of the coexisting ion concentration between 10 and 100 mg/L is 5 to 50 times of the initial phosphate concentration used in the experiment, but the adsorption amount is still above 19.6mg/g, and is not changed too much, and the addition of ions at different concentration levels does not influence the adsorption effect of the material, so that the influence of the coexisting ions on the adsorption performance of the material is obviously negligible.
Fig. 11 can be seen from a macroscopic magnetic test that the material exhibits significant superparamagnetism, which means that the material can be separated by magnetization in the presence of a magnetic field, and can be well dispersed in a solution in the absence of a magnetic field, which is beneficial to recycling and can greatly improve the practical application capability of the material.
In the figure 12, a material with the addition amount of 0.5 g/L is used for carrying out 20 times of adsorption and desorption cycle experiments on phosphate radical in water, wherein the adsorption conditions are that the material reacts at 25 ℃ and 150rpm for 3 hours, and the desorption conditions are that the material reacts at 40 ℃ and 150rpm for 3 hours, tests show that the adsorption amount of the material after the first 12 times of regeneration is more than 90% of the first adsorption amount, and the adsorption amount of the material after the regeneration 12 times is more than 80% of the first adsorption amount.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A synthetic method of a lanthanum-based loaded magnetic nano adsorption dephosphorization material is characterized by comprising the following steps:
step 1: sequentially adding ferroferric oxide, a chelating agent and a lanthanum salt into deionized water, and sequentially stirring and uniformly mixing, wherein the molar ratio of the ferroferric oxide to the lanthanum salt is 1:6-5: 1;
step 2: and (3) putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, and reacting at the temperature of 120-200 ℃ for 8-12h to obtain the prepared phosphorus adsorbing and removing material.
2. The method of synthesis according to claim 1, characterized in that: the grain size of the selected ferroferric oxide is 5-50 nm.
3. The method of synthesis according to claim 1, characterized in that: the molar ratio of the ferroferric oxide to the lanthanum salt is 1:1-4: 1.
4. The method of synthesis according to claim 1, characterized in that: the reaction temperature in the second step is 180-200 ℃.
5. The method of synthesis according to claim 1, characterized in that: the reaction time in the second step is 10-12 h.
6. The method of synthesis according to claim 1, characterized in that: the lanthanum salt is selected from lanthanum chloride or lanthanum nitrate.
7. The method of synthesis according to claim 1, characterized in that: the chelating agent is selected from any one or more of sodium citrate, anhydrous sodium acetate and sodium ethylene diamine tetracetate.
8. The lanthanum-based supported magnetic nano adsorption phosphorus removal material prepared by the synthesis method of any one of claims 1 to 7.
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Cited By (6)
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| CN112427006A (en) * | 2020-11-12 | 2021-03-02 | 复旦大学 | Algae control application of magnetic lanthanum-based material |
| CN112675804A (en) * | 2020-12-02 | 2021-04-20 | 哈尔滨工业大学 | Hydrated cerium carbonate phosphorus removal adsorbent and preparation method and application thereof |
| CN113145063A (en) * | 2020-12-01 | 2021-07-23 | 北京师范大学珠海校区 | Magnetic lanthanum-loaded attapulgite clay phosphorus removal adsorbent and preparation and application methods thereof |
| CN115318300A (en) * | 2022-08-19 | 2022-11-11 | 深圳市深水水务咨询有限公司 | Preparation method of magnetic biochar with catalytic and specific phosphorus adsorption performances |
| CN115920828A (en) * | 2023-01-05 | 2023-04-07 | 中国科学院生态环境研究中心 | Magnetic lanthanum-based adsorbent, preparation method thereof and method for enriching phosphorus in water body |
| CN117339545A (en) * | 2023-12-04 | 2024-01-05 | 中国农业大学 | Lanthanum-containing magnetic nano material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112427006A (en) * | 2020-11-12 | 2021-03-02 | 复旦大学 | Algae control application of magnetic lanthanum-based material |
| CN113145063A (en) * | 2020-12-01 | 2021-07-23 | 北京师范大学珠海校区 | Magnetic lanthanum-loaded attapulgite clay phosphorus removal adsorbent and preparation and application methods thereof |
| CN112675804A (en) * | 2020-12-02 | 2021-04-20 | 哈尔滨工业大学 | Hydrated cerium carbonate phosphorus removal adsorbent and preparation method and application thereof |
| CN115318300A (en) * | 2022-08-19 | 2022-11-11 | 深圳市深水水务咨询有限公司 | Preparation method of magnetic biochar with catalytic and specific phosphorus adsorption performances |
| CN115920828A (en) * | 2023-01-05 | 2023-04-07 | 中国科学院生态环境研究中心 | Magnetic lanthanum-based adsorbent, preparation method thereof and method for enriching phosphorus in water body |
| CN117339545A (en) * | 2023-12-04 | 2024-01-05 | 中国农业大学 | Lanthanum-containing magnetic nano material and preparation method and application thereof |
| CN117339545B (en) * | 2023-12-04 | 2024-03-26 | 中国农业大学 | Lanthanum-containing magnetic nano material and preparation method and application thereof |
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