CN112138624A - Quick-acting water magnetic nano phosphorus removal agent and preparation method and application thereof - Google Patents
Quick-acting water magnetic nano phosphorus removal agent and preparation method and application thereof Download PDFInfo
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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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
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
Abstract
The invention discloses a quick-acting water magnetic nano phosphorus removing agent and a preparation method and application thereof. The phosphorus removing agent comprises Fe3O4And LDH coated at Fe3O4The coating amount on the surface is 10.3 wt% -32.5 wt%. Preparation: (1) adding ferroferric oxide into a dispersing agent and carrying out ultrasonic treatment to obtain a suspension A; (2) mixing Mg (NO)3)2·6H2O and Al (NO)3)3·9H2Ultrasonically dispersing the O in water to obtain a mixed solution B; (3) adding the mixed solution B into the suspension A, adjusting the pH to 9-11, and collecting a pre-product; (4) will preAnd washing and drying the product to obtain the magnetic nano phosphorus removing agent. The application comprises the following steps: the magnetic nano phosphorus removing agent is used for removing phosphorus in the phosphorus-containing wastewater. The preparation method is simple and low in cost; the phosphorus removing agent can achieve a higher phosphorus removing effect in a short time, and can be effectively separated from a wastewater system, so that secondary pollution to a water body is avoided.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, and particularly relates to a quick-acting water magnetic nano phosphorus removal agent as well as a preparation method and application thereof.
Background
With the economic development and modernization progress of the country, various types of environmental pollution also increasingly and seriously affect our lives, and particularly, water pollution is the first threat. The problem of eutrophication of water bodies is one of the most major water pollution problems facing the world today. With the continuous development of industry and agriculture, water eutrophication becomes more and more serious, and becomes a main factor restricting the development of national economy and society in China. The related data show that phosphorus is a determinant factor for water eutrophication. The commercial chemical phosphorus removal agent on the market at present mainly comprises products such as polyaluminium chloride, polyferric sulfate, polyaluminium ferric chloride and the like, and because the contained aluminum and iron mainly exist in a polymeric state rather than an ionic state, the effect of the contained aluminum and iron with phosphorus-containing compounds in sewage is insufficient, the dosage is large, the phosphorus removal effect is poor, the phosphorus removal cost is high, and the popularization and the application of the chemical phosphorus removal technology are severely restricted.
Mg-Al layered double hydroxides (Mg-Al LDHs, hereinafter referred to as LDHs) are multifunctional two-dimensional (2D) ion layered compounds, also known as hydrotalcites, nanostructured LDHs contain positively charged metal hydroxide layers, and exchangeable anions are intercalated between the layers to maintain charge neutrality, which has attracted great interest in a number of potential applications, such as supercapacitors, catalysis, drug delivery, water treatment, and the like. Particularly, the material has the characteristics of low cost, large surface area, strong internal structure adjustability, nontoxicity and exchangeable anions, so that the material has great application potential in the field of phosphorus adsorption of water bodies. However, the defects are that LDH has long treatment time in the actual water treatment process, cannot be separated from the water body quickly and thoroughly, and is easy to cause secondary pollution to the water body.
Disclosure of Invention
The invention aims to provide a quick-acting water magnetic nano phosphorus removing agent and a preparation method and application thereof, the nano phosphorus removing agent can quickly remove phosphorus in phosphorus-containing wastewater, the removal efficiency is close to 100%, and meanwhile, the nano phosphorus removing agent can be quickly separated from a wastewater system to avoid secondary pollution to a water body.
The invention is realized by the following technical scheme:
a quick-acting water magnetic nano phosphorus removing agent is characterized in that the nano phosphorus removing agent comprises ferroferric oxide nano particles and magnesium-aluminum hydrotalcite; the magnesium-aluminum hydrotalcite is coated on the surfaces of the ferroferric oxide nanoparticles.
Further, the coating amount of the magnesium-aluminum hydrotalcite is 10.3 wt% -32.5 wt%.
A preparation method of a quick-acting water magnetic nano phosphorus removal agent is characterized by comprising the following steps:
(1) adding ferroferric oxide into a dispersing agent and carrying out ultrasonic treatment to obtain a suspension A;
(2) mixing Mg (NO)3)2·6H2O and Al (NO)3)3·9H2Ultrasonically dispersing the O in water to obtain a mixed solution B;
(3) adding the mixed solution B into the suspension A for reaction, adjusting the pH value of a reaction system to 9-11, and collecting a pre-product after the reaction;
(4) washing and drying the pre-product to obtain the magnetic nano phosphorus removal agent (Fe) with magnesium-aluminum hydrotalcite coated on the surface of the ferroferric oxide nano particles3O4@LDH)。
Further, the dispersant in the step (1) is deionized water; the mass volume ratio of the ferroferric oxide to the dispersing agent is 0.01-0.12 g/mL.
Further, it is characterized in that said Mg (NO) in the step (2)3)2·6H2O, said Al (NO)3)3·9H2The mass ratio of the O to the ferroferric oxide is 6: 3: (0.5-6); the water is deionized water; the Mg (NO)3)2·6H2The mass-volume ratio of O to the water is 0.2-0.3 g/mL.
Further, the method is characterized in that in the step (3), the mixed solution B is completely dripped into the suspension A, then the pH value of the reaction system is adjusted to 9-11 by using 2.9mol/L sodium hydroxide aqueous solution, the reaction is carried out for 0.5-2 hours at the temperature of 20-35 ℃, and the pre-product is obtained after the reaction and filtration.
Further, the method is characterized in that the pre-product is washed for 3-5 times by deionized water in the step (4); the drying is vacuum drying, and the drying temperature is 25-35 ℃.
The application of the quick-acting water magnetic nano phosphorus removal agent is characterized in that the magnetic nano phosphorus removal agent or the magnetic nano phosphorus removal agent prepared by the preparation method is used for removing phosphorus in phosphorus-containing wastewater. The magnetic nano phosphorus removing agent has the advantages that the removal rate of phosphorus in phosphorus-containing wastewater is close to 100%, the removal efficiency is high, the removal speed is high, the phosphorus in the phosphorus-containing wastewater can be rapidly removed in a short time, and meanwhile, the nano phosphorus removing agent can be rapidly separated from a wastewater system after phosphorus removal, so that secondary pollution to a water body is avoided.
Further, the process of removing phosphorus in the phosphorus-containing wastewater comprises the following steps: adding the magnetic nano phosphorus removing agent into the phosphorus-containing wastewater, carrying out oscillation reaction, and carrying out solid-liquid separation after the reaction to finish the removal of phosphorus in the phosphorus-containing wastewater.
Further, the mass-volume ratio of the magnetic nano phosphorus removal agent to the phosphorus-containing wastewater is 0.05-1.6 mg/mL; the initial concentration of phosphorus in the phosphorus-containing wastewater is 20mg/L-300 mg/L.
The invention has the beneficial effects that:
(1) the preparation method of the magnetic nano phosphorus removing agent is simple, and is convenient for industrial mass production, and the magnetic nano phosphorus removing agent prepared by the invention has high phosphorus removing efficiency in wastewater, and the magnetic nano phosphorus removing agent can achieve higher phosphorus removing effect in a short time and is expected to become a quick-acting wastewater phosphorus removing agent;
(2) ferroferric oxide (Fe) in the invention3O4) Forming composite nano particles with magnesium-aluminum hydrotalcite (LDH) by a one-step coprecipitation method, adsorbing phosphate ions in a water body by utilizing the interlayer ion exchangeability of the LDH, and introducing Fe3O4The nano particles can endow the nano phosphorus removing agent with magnetic response performance, so that the synthesized magnetic nano phosphorus removing agent (Fe)3O4@ LDH) can be effectively separated from a wastewater system under the action of an external magnetic field, so that secondary pollution to a water body is avoided;
(3) the magnetic nano phosphorus removing agent (Fe) prepared by the invention3O4@ LDH) has higher advantages in the aspects of product cost, preparation method, industrialization, phosphorus removal effect and the like, and has great application potential in the field of phosphorus-containing wastewater treatment.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a standard curve of concentration versus absorbance of a phosphate ion solution;
FIG. 2 shows the magnetic nano phosphorus removal agent (Fe) prepared in example 3 of the present invention3O4@ LDH);
FIG. 3 shows Fe in application example 1 of the present invention3O4Results of the effect of the amount of @ LDH added on the removal rate of phosphate ions are shown.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Quick-acting water magnetic nano phosphorus removal agent (Fe)3O4@ LDH), including ferroferric oxide (Fe)3O4) And magnesium aluminum hydrotalcite (LDH) coated on Fe3O4The nanoparticle surface, wherein the coating amount of LDH is 32.5 wt%. Obtaining Fe by TG analysis3O4Mass of LDH in @ LDH, then LDH/Fe3O4@ LDH, namely obtaining the coating amount of the LDH.
The magnetic nanometer phosphorus removing agent (Fe)3O4@ LDH) is prepared by the following steps:
(1) weighing 0.1g of petal-shaped ferroferric oxide nano particles, and ultrasonically dispersing the petal-shaped ferroferric oxide nano particles in 10mL of deionized water to form suspension A;
(2) 1.2g of Mg (NO) was weighed out separately3)2·6H2O and 0.6g of Al (NO)3)3·9H2Dissolving O in 5mL of deionized water by ultrasonic wave to obtain a mixed solution B;
(3) slowly dropwise adding the mixed solution B into the suspension A, simultaneously dropwise adding a NaOH solution with the concentration of 2.9mol/L to adjust the pH of the reaction system to be 10.5, stopping dropwise adding the NaOH solution, reacting at 30 ℃ for 1 hour, and performing magnetic decantation extraction after the reaction is finished to obtain a pre-product;
(4) washing the pre-product with deionized water for 5 times, and drying in a vacuum oven at 25 deg.C to obtain dried magnetic nanometer phosphorus removing agent (Fe)3O4@LDH)。
Example 2
Quick-acting water magnetic nano phosphorus removal agent (Fe)3O4@ LDH), including ferroferric oxide (Fe)3O4) And magnesium aluminum hydrotalcite (LDH) coated on Fe3O4The surface of the nanoparticles, wherein the LDH is coated in an amount of30.3wt％。
The magnetic nanometer phosphorus removing agent (Fe)3O4@ LDH) is prepared by the following steps:
(1) weighing 0.6g of petal-shaped ferroferric oxide nano particles, and ultrasonically dispersing the petal-shaped ferroferric oxide nano particles in 10mL of deionized water to form suspension A;
(2) 1.2g of Mg (NO) was weighed out separately3)2·6H2O and 0.6g of Al (NO)3)3·9H2Dissolving O in 5mL of deionized water by ultrasonic wave to obtain a mixed solution B;
(3) slowly dropwise adding the mixed solution B into the suspension A, simultaneously dropwise adding a NaOH solution with the concentration of 2.9mol/L to adjust the pH value of the reaction system to be 11, stopping dropwise adding the NaOH solution, reacting at 35 ℃ for 1 hour, and performing magnetic decantation extraction after the reaction is finished to obtain a pre-product;
(4) washing the pre-product with deionized water for 3 times, and drying in a vacuum oven at 20 deg.C to obtain dried magnetic nanometer phosphorus removing agent (Fe)3O4@LDH)。
Example 3
Quick-acting water magnetic nano phosphorus removal agent (Fe)3O4@ LDH), including ferroferric oxide (Fe)3O4) And magnesium aluminum hydrotalcite (LDH) coated on Fe3O4The nanoparticle surface, wherein the coating amount of LDH is 29.8 wt%.
The magnetic nanometer phosphorus removing agent (Fe)3O4@ LDH) is prepared by the following steps:
(1) weighing 0.8g of petal-shaped ferroferric oxide nano particles, and ultrasonically dispersing the petal-shaped ferroferric oxide nano particles in 10mL of deionized water to form suspension A;
(2) 1.2g of Mg (NO) was weighed out separately3)2·6H2O and 0.6g of Al (NO)3)3·9H2Dissolving O in 5mL of deionized water by ultrasonic wave to obtain a mixed solution B;
(3) slowly dropwise adding the mixed solution B into the suspension A, simultaneously dropwise adding a NaOH solution with the concentration of 2.9mol/L to adjust the pH of the reaction system to be 10.5, stopping dropwise adding the NaOH solution, reacting at 25 ℃ for 1 hour, and performing magnetic decantation extraction after the reaction is finished to obtain a pre-product;
(4) washing the pre-product with deionized water for 5 times, and drying in a vacuum oven at 25 deg.C to obtain dried magnetic nanometer phosphorus removing agent (Fe)3O4@LDH)。
Example 4
Quick-acting water magnetic nano phosphorus removal agent (Fe)3O4@ LDH), including ferroferric oxide (Fe)3O4) And magnesium aluminum hydrotalcite (LDH) coated on Fe3O4The nanoparticle surface, wherein the coating amount of LDH is 22.7 wt%.
The magnetic nanometer phosphorus removing agent (Fe)3O4@ LDH) is prepared by the following steps:
(1) weighing 1.2g of petal-shaped ferroferric oxide nano particles, and ultrasonically dispersing the petal-shaped ferroferric oxide nano particles in 10mL of deionized water to form suspension A;
(2) 1.2g of Mg (NO) was weighed out separately3)2·6H2O and 0.6g of Al (NO)3)3·9H2Dissolving O in 5mL of deionized water by ultrasonic wave to obtain a mixed solution B;
(3) slowly dropwise adding the mixed solution B into the suspension A, simultaneously dropwise adding a NaOH solution with the concentration of 2.9mol/L to adjust the pH of the reaction system to 10.5, stopping dropwise adding the NaOH solution, reacting at 20 ℃ for 0.5 hour, and performing magnetic decantation extraction after the reaction is finished to obtain a pre-product;
(4) washing the pre-product with deionized water for 4 times, and drying in a vacuum oven at 30 deg.C to obtain dried magnetic nanometer phosphorus removing agent (Fe)3O4@LDH)。
Example 5
Quick-acting water magnetic nano phosphorus removal agent (Fe)3O4@ LDH), including ferroferric oxide (Fe)3O4) And magnesium aluminum hydrotalcite (LDH) coated on Fe3O4The nanoparticle surface, wherein the coating amount of LDH is 23.5 wt%.
The magnetic nanometer phosphorus removing agent (Fe)3O4@ LDH) is prepared by the following steps:
(1) weighing 0.8g of petal-shaped ferroferric oxide nano particles, and ultrasonically dispersing the petal-shaped ferroferric oxide nano particles in 10mL of deionized water to form suspension A;
(2) 1.2g of Mg (NO) was weighed out separately3)2·6H2O and 0.6g of Al (NO)3)3·9H2Dissolving O in 5mL of deionized water by ultrasonic wave to obtain a mixed solution B;
(3) slowly dropwise adding the mixed solution B into the suspension A, simultaneously dropwise adding a NaOH solution with the concentration of 2.9mol/L to adjust the pH of the reaction system to 9.5, stopping dropwise adding the NaOH solution, reacting at 30 ℃ for 1 hour, and performing magnetic decantation extraction after the reaction is finished to obtain a pre-product;
(4) washing the pre-product with deionized water for 3 times, and drying in a vacuum oven at 25 deg.C to obtain dried magnetic nanometer phosphorus removing agent (Fe)3O4@LDH)。
Example 6
Quick-acting water magnetic nano phosphorus removal agent (Fe)3O4@ LDH), including ferroferric oxide (Fe)3O4) And magnesium aluminum hydrotalcite (LDH) coated on Fe3O4The nanoparticle surface, wherein the coating amount of LDH is 28.1 wt%.
The magnetic nanometer phosphorus removing agent (Fe)3O4@ LDH) is prepared by the following steps:
(1) weighing 0.8g of petal-shaped ferroferric oxide nano particles, and ultrasonically dispersing the petal-shaped ferroferric oxide nano particles in 10mL of deionized water to form suspension A;
(2) 1.2g of Mg (NO) was weighed out separately3)2·6H2O and 0.6g of Al (NO)3)3·9H2Dissolving O in 5mL of deionized water by ultrasonic wave to obtain a mixed solution B;
(3) slowly dropwise adding the mixed solution B into the suspension A, simultaneously dropwise adding a NaOH solution with the concentration of 2.9mol/L to adjust the pH of the reaction system to be 10.5, stopping dropwise adding the NaOH solution, reacting for 2 hours at 25 ℃, and performing magnetic decantation extraction after the reaction is finished to obtain a pre-product;
(4) washing the pre-product with deionized water for 5 times, and drying in a vacuum oven at 25 deg.C to obtain dried magnetic nanometer phosphorus removing agent (Fe)3O4@LDH)。
Test example 1
Magnetic properties prepared in example 3 aboveNanometer phosphorus removal agent (Fe)3O4@ LDH) was characterized by Transmission Electron Microscopy (TEM), and as shown in FIG. 2, it was revealed that the petal-like ferroferric oxide (Fe)3O4) The surfaces of the nano particles are uniformly coated with a layer of magnesium aluminum water-soluble polymer (LDH), and Fe3O4The @ LDH particles are uniform in size and good in dispersibility.
Application example 1
The magnetic nano phosphorus removal agent (Fe) prepared in the above example 3 is selected3O4@ LDH), comprising the following steps:
(1) firstly, drawing a standard curve: preparing 6 50mL glass colorimetric tubes, respectively transferring 0.0mL, 0.5mL, 1.0mL, 3.0mL, 5.0mL and 10.0mL of phosphate ion standard solution (the concentration is 20mg/L), then fixing the volume to a scale mark by using deionized water, then sequentially adding 100 mu L of ascorbic acid solution (100mg/L) and 200 mu L of molybdate solution (32.5mg/L) into the colorimetric tubes, performing timed color development for 15min, then measuring the absorbance (A) of the corresponding solution at a wavelength lambda of 700nm by using an ultraviolet spectrophotometer, drawing a standard curve by using the concentration of phosphate ions as abscissa and the absorbance as ordinate, and obtaining a standard curve equation of the phosphate ions after meridian fitting: y (a) ═ 7.9324X +0.0005, R20.9994; as shown in fig. 1, the linear relationship is good;
(2) simulating phosphorus-containing wastewater: preparing a phosphate ion solution with the initial concentration of 50mg/L to simulate phosphorus-containing wastewater; then, 6 equal parts of 100mL solution was removed from the phosphate ion solution and added into a glass bottle as phosphorus-containing wastewater, and then 0.005g, 0.015g, 0.030g, 0.060g, 0.120g, 0.160g of the magnetic nano phosphorus removal agent (Fe) prepared in example 3 was added to the 6 parts of solution respectively3O4@ LDH), ultrasonic dispersing, placing in a gas bath constant temperature oscillator at 25 ℃ and 160 r/min for oscillating for 30 min, and magnetically decanting after oscillating to obtain Fe3O4@ LDH is enriched at the bottom of a glass bottle, and after a color developing agent is added, Fe passing through a sample is measured by an ultraviolet spectrophotometer3O4@ LDH dephosphorization is carried out, and the absorbance of 6 parts of corresponding phosphate radical ion solution at the wavelength of 700nm is obtained; then comparing the absorbance with figure 1 to obtain the product Fe3O4The concentration of phosphate ion solution of each component (residual phosphate concentration) after phosphorus removal of @ LDH is determined according to the formula:
calculating Fe3O4The phosphate ion removal rate of @ LDH, wherein: c0(mg/L) and Ce(mg/L) initial concentration of phosphate ion solution and Fe3O4The residual phosphate radical concentration after the phosphorus removal of the @ LDH; the above-mentioned residual phosphate concentration and removal rate were plotted in FIG. 3.
As can be seen from FIG. 3, with the magnetic nano phosphorus removing agent Fe3O4The increase of the dosage of @ LDH sharply reduces the concentration of phosphate ions in the solution, the removal rate of the phosphate ions is increased, and Fe3O4When the amount of @ LDH added is 0.015g, the removal rate of phosphate radical ions is already up to 99.66%, then the amount added is continuously increased, the removal rate of phosphate radical ions is increased, but the increase is not obvious, and 0.160g of Fe is added3O4After @ LDH, the removal rate of phosphate ions was 99.87%, which was only increased by 0.21%. Fe prepared by the invention3O4The @ LDH nano phosphorus removal agent can achieve a high phosphorus removal effect within 30 minutes by only adding a small amount of phosphorus removal agent in water body phosphorus removal, and is expected to become a quick-acting wastewater phosphorus removal agent.
Comparative example 1
(1) 1.2g of Mg (NO) was weighed out separately3)2·6H2O and 0.6g of Al (NO)3)3·9H2Dissolving O in 5mL of deionized water by ultrasonic wave to obtain a mixed solution;
(2) dropwise adding a 2.9mol/L NaOH solution into the mixed solution, stopping dropwise adding the NaOH solution when the pH of the reaction system is adjusted to 10.5, and reacting at 25 ℃ for 1 hour to obtain a pre-product;
(3) washing the pre-product with deionized water, centrifuging, and drying in a vacuum oven at 25 deg.C to obtain dried magnesium aluminum hydrotalcite (LDH).
Application example 2
Preparing a phosphate ion solution with the initial concentration of 50mg/L to simulate phosphorus-containing wastewater and transferring 100.0mL into a glass bottle according to the conditions of application example 1, then adding 0.015g of the magnesium-aluminum hydrotalcite (LDH) prepared in the comparative example 1 into the glass bottle, placing the glass bottle in a gas bath constant temperature oscillator with the temperature of 25 ℃ and the speed of 160 r/min after ultrasonic dispersion, oscillating for 24 hours, adding a color developing agent, and then measuring the absorbance of the corresponding phosphate ion solution at the wavelength lambda of 700nm after the LDH is dephosphorized by an ultraviolet spectrophotometer; then the concentration of the corresponding solution can be obtained by comparing with the standard curve of figure 1, and the removal rate of the phosphate ions is calculated to be 95.13% according to a formula.
Comparative example 2
Referring to the conditions of application example 1, preparing a phosphate radical ion solution with an initial concentration of 50mg/L to simulate phosphorus-containing wastewater, transferring 100.0mL into a glass bottle, adding 0.015g of petal-shaped ferroferric oxide nanoparticles into the glass bottle, performing ultrasonic dispersion, placing the glass bottle in a gas bath constant temperature oscillator at 25 ℃ and 160 r/min, oscillating for 24 hours, adding a color developing agent, and measuring the absorbance of the phosphate radical ion solution corresponding to the petal-shaped ferroferric oxide nanoparticles after phosphorus removal at the wavelength lambda of 700nm by using an ultraviolet spectrophotometer; then the concentration of the corresponding solution can be obtained by comparing with the standard curve of figure 1, and the removal rate of phosphate ions is calculated to be 5.32% according to a formula.
The above-mentioned preferred embodiments of the present invention are provided for illustration only and not for the purpose of limiting the invention. Obvious variations or modifications of the present invention are within the scope of the present invention.
Claims (10)
1. A quick-acting water magnetic nano phosphorus removing agent is characterized in that the nano phosphorus removing agent comprises ferroferric oxide nano particles and magnesium-aluminum hydrotalcite; the magnesium-aluminum hydrotalcite is coated on the surfaces of the ferroferric oxide nanoparticles.
2. The quick-acting water magnetic nano phosphorus removal agent according to claim 1, wherein the coating amount of the magnesium-aluminum hydrotalcite is 10.3 wt% to 32.5 wt%.
3. The preparation method of the quick-acting water magnetic nano phosphorus removal agent according to any one of claims 1 to 2, characterized in that the method comprises the following steps:
(1) adding ferroferric oxide into a dispersing agent and carrying out ultrasonic treatment to obtain a suspension A;
(2) mixing Mg (NO)3)2·6H2O and Al (NO)3)3·9H2Ultrasonically dispersing the O in water to obtain a mixed solution B;
(3) adding the mixed solution B into the suspension A for reaction, adjusting the pH value of a reaction system to 9-11, and collecting a pre-product after the reaction;
(4) and washing and drying the pre-product to obtain the magnetic nano phosphorus removing agent.
4. The method for preparing the quick-acting water magnetic nano phosphorus removing agent according to claim 3, wherein the dispersing agent in the step (1) is deionized water; the mass volume ratio of the ferroferric oxide to the dispersing agent is 0.01-0.12 g/mL.
5. The method for preparing the quick-acting water magnetic nano phosphorus removal agent according to claim 3, wherein the Mg (NO) in the step (2)3)2·6H2O, said Al (NO)3)3·9H2The mass ratio of the O to the ferroferric oxide is 6: 3: (0.5-6); the water is deionized water; the Mg (NO)3)2·6H2The mass-volume ratio of O to the water is 0.2-0.3 g/mL.
6. The preparation method of the quick-acting water magnetic nano phosphorus removing agent as claimed in claim 3, wherein in step (3), the mixed solution B is completely dripped into the suspension A, 2.9mol/L sodium hydroxide aqueous solution is used for adjusting the pH of the reaction system to 9-11, the reaction is carried out for 0.5-2 hours at 20-35 ℃, and the pre-product is obtained after the reaction and filtration.
7. The preparation method of the quick-acting water magnetic nano phosphorus removing agent as claimed in claim 3, wherein in the step (4), the pre-product is washed 3-5 times by deionized water; the drying is vacuum drying, and the drying temperature is 25-35 ℃.
8. The application of the quick-acting water magnetic nano phosphorus removal agent is characterized in that the magnetic nano phosphorus removal agent disclosed by any one of claims 1-2 or the magnetic nano phosphorus removal agent prepared by the preparation method disclosed by any one of claims 3-7 is used for removing phosphorus in phosphorus-containing wastewater.
9. The application of the quick-acting water magnetic nano phosphorus removal agent according to claim 8, wherein the process for removing phosphorus in the phosphorus-containing wastewater comprises the following steps: adding the magnetic nano phosphorus removing agent into the phosphorus-containing wastewater, carrying out oscillation reaction, and carrying out solid-liquid separation after the reaction to finish the removal of phosphorus in the phosphorus-containing wastewater.
10. The application of the quick-acting water magnetic nano phosphorus removal agent as claimed in claim 9, wherein the mass-to-volume ratio of the magnetic nano phosphorus removal agent to the phosphorus-containing wastewater is 0.05-1.6 mg/mL; the initial concentration of phosphorus in the phosphorus-containing wastewater is 20mg/L-300 mg/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115193392A (en) * | 2022-08-01 | 2022-10-18 | 常熟理工学院 | Chloride ion adsorbent and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230805A (en) * | 2013-05-16 | 2013-08-07 | 黑龙江省科学院石油化学研究院 | Method for preparing magnetic hydrotalcite loaded nano-palladium catalyst |
| CN105854796A (en) * | 2016-04-08 | 2016-08-17 | 济南大学 | Preparation method and application of magnetic bimetallic oxide/carbon composite material |
| CN107096491A (en) * | 2017-04-20 | 2017-08-29 | 南京金泽爱控环保科技有限公司 | Dye wastewater adsorbent based on core shell structure and preparation method thereof |
| CN108889266A (en) * | 2018-07-25 | 2018-11-27 | 青海师范大学 | A kind of magnetism Mg-Al composite oxide and its preparation method and application |
| CN110876917A (en) * | 2019-11-25 | 2020-03-13 | 山东建筑大学 | Superparamagnetic response nano phosphorus adsorbent and preparation method thereof |
-
2020
- 2020-08-21 CN CN202010848489.3A patent/CN112138624A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230805A (en) * | 2013-05-16 | 2013-08-07 | 黑龙江省科学院石油化学研究院 | Method for preparing magnetic hydrotalcite loaded nano-palladium catalyst |
| CN105854796A (en) * | 2016-04-08 | 2016-08-17 | 济南大学 | Preparation method and application of magnetic bimetallic oxide/carbon composite material |
| CN107096491A (en) * | 2017-04-20 | 2017-08-29 | 南京金泽爱控环保科技有限公司 | Dye wastewater adsorbent based on core shell structure and preparation method thereof |
| CN108889266A (en) * | 2018-07-25 | 2018-11-27 | 青海师范大学 | A kind of magnetism Mg-Al composite oxide and its preparation method and application |
| CN110876917A (en) * | 2019-11-25 | 2020-03-13 | 山东建筑大学 | Superparamagnetic response nano phosphorus adsorbent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李嘉雯 等: "磁性Mg/Al-LDHs制备条件对其吸附除磷性能的影响", 《环境科学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115193392A (en) * | 2022-08-01 | 2022-10-18 | 常熟理工学院 | Chloride ion adsorbent and preparation method and application thereof |
| CN115193392B (en) * | 2022-08-01 | 2023-10-24 | 常熟理工学院 | Chloride ion adsorbent and preparation method and application thereof |
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