CN107583673B - Modified anion resin material and preparation method and application thereof - Google Patents
Modified anion resin material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a modified anion resin material and a preparation method and application thereof, wherein the preparation method comprises the following steps: washing the strong base type anion resin material, and drying to obtain a dry strong base type anion resin material; mixing hydrochloric acid solution of ferric chloride and hydrochloric acid solution of zirconium oxychloride to obtain mixed solution, and then adding the dried strong-base anion resin material into the mixed solution to obtain the modified anion resin material after treatment. The modified anion resin material can be applied as a phosphorus removal adsorbent. According to the invention, the iron oxide and the zirconium oxide are respectively and successfully loaded on the strong alkali type anion resin material, so that the modified anion resin material not only retains the respective phosphorus adsorption performance of the iron oxide and the zirconium oxide, but also provides a good mechanical strength and an excellent hydraulic performance fixing environment for the iron oxide and the zirconium oxide, and further exerts the excellent phosphorus adsorption effect of the iron oxide and the zirconium oxide.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a modified anion resin material, and a preparation method and application thereof.
Background
In recent years, with the development of industry and the continuous enhancement of human activities, a large amount of phosphorus-rich industrial wastewater and domestic sewage are discharged into water bodies, so that the phenomenon of water body eutrophication in China is increasingly serious, and the sustainable development of society is restricted. Therefore, an economic and effective sewage dephosphorization method is actively sought, which is beneficial to improving water quality and reducing pollution.
At present, the sewage dephosphorization method is mainly divided into a biological method, a chemical precipitation method and an adsorption method. Wherein, the biological dephosphorization process is complex, the effluent quality stability is poor, and the problem of difficulty in treatment of excess sludge exists; most of the phosphorus removal agents used in the chemical precipitation method are aluminum salt, ferric salt, ferrous salt and other process products, so that the cost is high, and the generated sludge amount is large. In contrast, the adsorption method utilizes certain porous or large-specific-surface-area substances, realizes phosphorus removal mainly through the effects of phosphorus on the surface precipitation, ion exchange or adsorption and the like of the adsorbent, and has the advantages of simple process, convenient and easy operation, wide application and the like.
A large number of adsorbents are developed for removing phosphorus in water, and among them, metal oxide adsorbents such as iron oxide, zirconium oxide and aluminum oxide are paid attention by researchers because they can form coordination compounds with phosphorus ions and have good adsorption selectivity. However, these metal oxides in the normal state are limited in size to be difficult to be directly applied to adsorption systems such as fixed beds. The patent "preparation method of iron oxide modified quartz sand filter material for removing arsenic and phosphorus by adsorption" (publication No. CN104815611A) discloses that the quartz sand is used as a carrier, and iron oxide particles are loaded on the surface of the quartz sand by a filtration and purification method, so that the modified quartz sand filter material capable of synchronously removing arsenic and phosphorus is prepared.
However, most of the conventional adsorbents have the disadvantages of small adsorption capacity and poor adsorption performance. Iron oxides and zirconium oxides have been shown to have excellent adsorption properties and high adsorption capacity for phosphorus ions. However, the preparation method of the resin-based composite adsorbent at present mainly comprises the steps of exchanging metal oxides to the pore passages and the surface of a resin carrier in a complex ion mode, and then precipitating metal compounds by using alkali liquor. And both the iron and zirconium metal elements have positive charges, so that the iron and zirconium metal elements are difficult to perform ion exchange with anion resin, and a preparation method for loading two oxides is not reported. Therefore, how to simultaneously and effectively load the iron oxide and the zirconium oxide on the anion resin to prepare the phosphorus removal adsorbent still remains a technical problem to be solved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention mainly aims to provide a preparation method of a modified anionic resin material.
The second purpose of the invention is to obtain modified anion resin material by the preparation method.
The third purpose of the invention is to provide the application of the modified anion resin material.
In order to achieve the above purpose, the solution of the invention is as follows:
a preparation method of a modified anion resin material comprises the following steps:
(1) washing the strong base type anion resin material, and drying to obtain a dry strong base type anion resin material;
(2) hydrochloric acid solution (FeCl) of ferric chloride3+ HCl) and hydrochloric acid solution of zirconium oxychloride (ZrOCl2·8H2O + HCl) to obtain a first mixed solution, then adding the dried strong base type anion resin material obtained in the step (1) into the first mixed solution, and stirring at 25 +/-5 ℃ to facilitate impregnation;
(3) adding a sodium hydroxide (NaOH) solution into the reaction system in the step (2), adjusting the pH value of the reaction system to 7-8, and stirring at 25 +/-5 ℃ to obtain a second mixed solution;
(4) and (4) centrifuging the second mixed solution obtained in the step (3), and drying to constant weight to obtain the modified anion resin material.
Wherein the strong base type anion resin material contains quaternary ammonium salt functional groups.
Preferably, in the step (1), the drying temperature is 50-70 ℃, and the drying time is 12-24 h.
Preferably, in the step (2), the concentration of the hydrochloric acid solution of ferric chloride is 0.1-0.5 mol/L.
Preferably, in the step (2), the concentration of the hydrochloric acid solution of zirconium oxychloride is 0.1 to 0.5 mol/L.
Preferably, in the step (2), the rotation speed of stirring is 300-400 rpm, and the time of immersion is 2-3 h.
Preferably, in the step (3), the concentration of the sodium hydroxide solution is 0.5-1.0 mol/L.
Preferably, in the step (4), the rotation speed of the centrifugation is 3000-4000 rpm, and the time of the centrifugation is 10-20 min.
Preferably, in the step (4), the drying temperature is 50-70 ℃, and the drying time is 12-24 h.
A modified anion resin material prepared by the preparation method.
The modified anion resin material is applied as a phosphorus removal adsorbent.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the invention takes strong base type anion resin material as a carrier, and iron oxide and zirconium oxide are respectively loaded on the surface of the carrier to form a composite adsorbent with three active sites for adsorbing and removing phosphorus in water, wherein quaternary ammonium salt functional groups in the strong base type anion resin material adsorb and remove phosphorus through electrostatic action, and the iron oxide and the zirconium oxide respectively generate surface complex reaction with the phosphorus in the water through hydroxyl active sites on the surface to form a coordination complex, thereby removing the phosphorus.
Secondly, the modified anion resin material prepared by the invention combines the Donnan film effect (namely enhanced diffusion and enrichment concentration effect) of the carrier charged group and the adsorption effect of iron oxide and zirconium oxide on phosphorus, so that the modified anion resin material has the characteristics of large adsorption capacity, good adsorption performance and the like; in addition, the preparation process is simple, so that the application cost in practical engineering is reduced, and the method can be used for large-scale production, so that the method has a good application prospect, is widely applied to water pollution remediation engineering, and can be further applied to black and odorous water and eutrophic water to improve the water quality.
In conclusion, the iron oxide and the zirconium oxide are respectively and successfully loaded on the strong alkali type anion resin material, so that the modified anion resin material prepared by the invention not only keeps the respective phosphorus adsorption performance of the iron oxide and the zirconium oxide, but also provides a fixed environment with good mechanical strength and excellent hydraulic performance, and further exerts the excellent phosphorus adsorption effect of the iron oxide and the zirconium oxide.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a modified anionic resin material of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) image of an unmodified anionic resin material of the present invention.
FIG. 3 is a graph showing the effect of the modified anionic resin material of the present invention on phosphorus removal at different pH values.
FIG. 4 is a graph showing the effect of modified anionic resin materials of different amounts of adsorbents in the present invention on phosphorus removal.
FIG. 5 is a graph showing the effect of the modified anion resin material of the present invention on removing phosphorus in phosphorus-containing wastewater with different coexisting anions.
Detailed Description
The invention provides a modified anion resin material and a preparation method and application thereof.
< preparation method of modified anionic resin Material >
A preparation method of a modified anion resin material comprises the following steps:
(1) washing the strong alkali type anion resin material with deionized water for 5-6 times, and drying to obtain a dry strong alkali type anion resin material;
(2) hydrochloric acid solution (FeCl) of ferric chloride3+ HCl) andhydrochloric acid solution of zirconium oxychloride (ZrOCl)2·8H2O + HCl) to obtain a first mixed solution, then adding the dried strong base type anion resin material obtained in the step (1) into the first mixed solution, and stirring at 25 +/-5 ℃ to facilitate impregnation;
(3) adding a sodium hydroxide (NaOH) solution into the reaction system in the step (2) at a speed of 5 drops per second, adjusting the pH value of the reaction system to 7-8, and stirring at 25 +/-5 ℃ to obtain a second mixed solution;
(4) and (4) centrifuging the second mixed solution obtained in the step (3), and drying to constant weight to obtain the modified anion resin material.
Wherein the strong base type anion resin material contains quaternary ammonium salt functional groups. The strong base anion resin material is IRA402 (type) strong base anion exchange resin, and is purchased from Shanghai Aladdin Biotechnology, Inc.
The adsorption principle of the modified anion resin material of the invention is as follows: the strong base type anion resin material is used as a carrier, and because iron in an iron chloride solution and zirconium in a zirconium oxychloride solution are both positively charged and then are respectively loaded on the surface and pore channels of the strong base type anion resin material through ion exchange, a composite adsorbent with three active sites is formed on the carrier and is further used for adsorbing and removing phosphorus in a water body, wherein quaternary ammonium salt functional groups in the strong base type anion resin material adsorb and remove phosphorus through electrostatic action, and iron oxide and zirconium oxide respectively perform surface complexation reaction with phosphorus in the water body through hydroxyl active sites on the surface to form a coordination complex, so that the phosphorus is removed.
In the step (1), the drying temperature can be 50-70 ℃, preferably 50 ℃; the drying time can be 12-24 h, and is preferably 12 h.
In the step (2), the concentration of the hydrochloric acid solution of ferric chloride can be 0.1-0.5 mol/L, and is preferably 0.1 mol/L; the concentration of the hydrochloric acid solution of zirconium oxychloride can be from 0.1 to 0.5mol/L, preferably 0.1 mol/L.
In the step (2), the rotation speed of stirring can be 300-400 rpm, preferably 300 rpm; the time for impregnation may be 2-3 h, preferably 2 h.
In step (3), the concentration of the sodium hydroxide solution may be 0.5 to 1.0mol/L, preferably 0.5 mol/L.
The purpose of adding the sodium hydroxide solution is: so that the surfaces of the iron oxide and the zirconium oxide respectively generate hydroxyl active sites, thereby forming the iron hydroxide and the zirconium hydroxide.
In step (4), the rotation speed of centrifugation may be 3000-4000 rpm, preferably 3000 rpm; the time for centrifugation may be 10-20 min, preferably 10 min.
In the step (4), the drying temperature can be 50-70 ℃, preferably 50 ℃; the drying time can be 12-24 h, and is preferably 12 h.
< modified anionic resin Material >
A modified anion resin material prepared by the preparation method.
< use of modified anionic resin Material >
The modified anion resin material is applied as a phosphorus removal adsorbent.
The invention will be further described with reference to examples of embodiments shown in the drawings.
Example 1:
the preparation method of the modified anionic resin material of the embodiment comprises the following steps:
(1) washing the strong base type anion resin material (containing quaternary ammonium salt functional group) for 6 times by using deionized water, and drying to obtain a dry strong base type anion resin material, wherein the drying temperature is 50 ℃, and the drying time is 12 hours;
(2) 0.1mol/L hydrochloric acid solution (FeCl) of ferric chloride3+ HCl) and 0.1mol/L hydrochloric acid solution of zirconium oxychloride (ZrOCl)2·8H2O + HCl) to obtain a first mixed solution, then adding the dried strong base type anion resin material obtained in the step (1) into the first mixed solution, and stirring at 25 ℃ to facilitate impregnation, wherein the stirring speed is 300rpm, and the impregnation time is 2 hours;
(3) adding 0.5mol/L sodium hydroxide (NaOH) solution into the reaction system in the step (2) at the speed of 5 drops per second, adjusting the pH value of the reaction system to 7, and stirring at 25 ℃ to obtain a second mixed solution;
(4) centrifuging the second mixed solution obtained in the step (3), wherein the rotating speed of the centrifugation is 3000rpm, and the time of the centrifugation is 10 min; and drying to obtain the modified anion resin material, wherein the drying temperature is 50 ℃, and the drying time is 12 h.
Wherein, in the step (1), the drying temperature is within 50-70 ℃ and the drying time is within 12-24 h.
In the step (2), the concentration of the hydrochloric acid solution of ferric chloride is within 0.1-0.5 mol/L, and the concentration of the hydrochloric acid solution of zirconium oxychloride is within 0.1-0.5 mol/L.
In the step (2), the rotation speed of stirring is within 300-400 rpm, and the soaking time is within 2-3 h.
In step (3), the concentration of the sodium hydroxide solution is within 0.5 to 1.0 mol/L.
In the step (4), the rotating speed of the centrifugation is within 3000-4000 rpm, and the time of the centrifugation is within 10-20 min.
In the step (4), the drying temperature is within 50-70 ℃ and the drying time is within 12-24 h.
Example 2:
the preparation method of the modified anionic resin material of the embodiment comprises the following steps:
(1) washing the strong base type anion resin material (containing quaternary ammonium salt functional group) for 6 times by using deionized water, and drying to obtain a dry strong base type anion resin material, wherein the drying temperature is 70 ℃, and the drying time is 24 hours;
(2) 0.5mol/L hydrochloric acid solution (FeCl) of ferric chloride3+ HCl) and 0.5mol/L hydrochloric acid solution of zirconium oxychloride (ZrOCl)2·8H2O + HCl) to obtain a first mixed solution, then adding the dried strong base type anion resin material obtained in the step (1) into the first mixed solution, and stirring at 25 ℃ to facilitate impregnation, wherein the stirring speed is 400rpm, and the impregnation time is 3 hours;
(3) adding 1.0mol/L sodium hydroxide (NaOH) solution into the reaction system in the step (2) at the speed of 5 drops per second, adjusting the pH value of the reaction system to 7, and stirring at 25 ℃ to obtain a second mixed solution;
(4) centrifuging the second mixed solution obtained in the step (3), wherein the rotation speed of the centrifugation is 4000rpm, and the time of the centrifugation is 20 min; and drying to obtain the modified anion resin material, wherein the drying temperature is 70 ℃, and the drying time is 24 h.
Example 3:
the preparation method of the modified anionic resin material of the embodiment comprises the following steps:
(1) washing the strong base type anion resin material (containing quaternary ammonium salt functional group) for 6 times by using deionized water, and drying to obtain a dry strong base type anion resin material, wherein the drying temperature is 60 ℃, and the drying time is 20 hours;
(2) 0.3mol/L hydrochloric acid solution (FeCl) of ferric chloride3+ HCl) and 0.2mol/L hydrochloric acid solution of zirconium oxychloride (ZrOCl)2·8H2O + HCl) to obtain a first mixed solution, then adding the dried strong base type anion resin material obtained in the step (1) into the first mixed solution, and stirring at 25 ℃ to facilitate impregnation, wherein the stirring speed is 350rpm, and the impregnation time is 2 hours;
(3) adding 0.8mol/L sodium hydroxide (NaOH) solution into the reaction system in the step (2) at the speed of 5 drops per second, adjusting the pH value of the reaction system to 8, and stirring at 25 ℃ to obtain a second mixed solution;
(4) centrifuging the second mixed solution obtained in the step (3), wherein the rotation speed of the centrifugation is 3500rpm, and the centrifugation time is 15 min; and drying to obtain the modified anion resin material, wherein the drying temperature is 60 ℃, and the drying time is 20 h.
< experiment >
The following experiments were conducted with the modified anionic resin materials of the above examples as products, respectively.
< experiment 1>
This experiment was to verify that the modified anionic resin material has successfully loaded iron oxide and zirconium oxide compared to the unmodified anionic resin material.
The experimental process is as follows: the modified anion resin material (experimental group) and the unmodified anion resin material (control group) were subjected to a scanning electron microscope experiment, respectively.
As can be seen from fig. 1 and 2, the surfaces of the anionic resin materials of the experimental group were rough compared to those of the anionic resin materials of the control group, and a number of irregular granular crystals were attached, thus illustrating that the surfaces of the anionic resin materials of the experimental group were successfully loaded with iron oxide and zirconium oxide.
< experiment 2>
The experiment is to verify that the modified anion resin material has good phosphorus removal effect under different pH values.
The experimental process is as follows: 0.1g of the modified anion resin material was placed in a glass bottle (volume: 250ml) containing 100ml of phosphorus-containing simulated sewage (phosphorus concentration: 5mg/L, initial pH: 3. + -. 0.05 to 11. + -. 0.05), and after stirring at 25 ℃ for 12 hours at 200rpm, the concentration of residual phosphorus in the supernatant in the glass bottle was measured and the phosphorus removal rate was calculated.
As can be seen from FIG. 3, under the conditions of different pH values, the removal rate of phosphorus is between 57.1 and 97.3%, and when the pH value is between 4 and 11, the removal rate of phosphorus is not affected basically and is maintained above 90%, so that the method has a wide use space.
< experiment 3>
The experiment is to verify that the modified anion resin materials with different adsorbents have good removal effect on phosphorus.
The experimental process is as follows: 0.0100g, 0.0125g, 0.0250g, 0.0500g, 0.0750g, 0.1000g, 0.1250g and 0.2500g of the modified anionic resin material were put in a glass bottle (volume 250ml) containing phosphorus-containing simulated sewage (concentration of phosphorus 5mg/L, initial pH 7) and stirred at 25 ℃ at 200rpm for 12 hours, and then the concentration of residual phosphorus in the supernatant in the glass bottle was measured and the removal rate of phosphorus was calculated.
As can be seen from FIG. 4, the removal rate of phosphorus is between 46.3-98.8% and can reach more than 90% generally under the modified anion resin materials with different amounts of the adsorbent.
< experiment 4>
The experiment is to verify that the modified anion resin material does not cause obvious reduction influence on the removal of phosphorus in phosphorus-containing sewage with different coexisting anions.
The experimental process is as follows: first, Cl containing coexisting anions is prepared‐、NO3 ‐、SO4 2‐、HCO3 ‐The phosphorus-containing simulated sewage has the phosphorus concentration of 5mg/L, and the concentration ratio of the phosphorus to the anions is respectively 5:1, 1:1 and 1:5, wherein the anions comprise Cl-and NO3 ‐、SO4 2‐、HCO3 ‐The concentration ratio of phosphorus to anions is 5:1 and is expressed as P (Cl)‐、NO3 ‐、SO4 2‐、HCO3 ‐) The concentration ratio of (A) to (B) is 5:1, namely C (P) to C (Cl)‐)＝5:1，C(P):C(NO3 ‐)＝5:1，C(P):C(SO4 2‐)＝5:1，C(P):C(HCO3 ‐) The same is true for the concentration ratio of phosphorus to anion of 1:1, 1:5, 5: 5.
Next, 0.1g of the modified anion resin material was placed in a glass bottle (volume: 250ml) containing 100ml of phosphorus-containing simulated sewage (initial pH 7), and after stirring at 25 ℃ for 12 hours at 200rpm, the concentration of residual phosphorus in the supernatant in the glass bottle was measured, and the phosphorus removal rate was calculated.
As can be seen from FIG. 5, the removal rates of phosphorus in the phosphorus-containing wastewater containing different coexisting anions of the modified anion resin material were all 95% or more, thus demonstrating that the presence of different coexisting anions in the phosphorus-containing wastewater does not significantly reduce the phosphorus removal rate.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (10)
1. A preparation method of a modified anion resin material is characterized by comprising the following steps: which comprises the following steps:
(1) washing the strong base type anion resin material, and drying to obtain a dry strong base type anion resin material;
(2) mixing a hydrochloric acid solution of ferric chloride and a hydrochloric acid solution of zirconium oxychloride to obtain a first mixed solution, adding the dried strong base type anion resin material obtained in the step (1) into the first mixed solution, and stirring at 25 +/-5 ℃ to facilitate impregnation;
(3) adjusting the pH value of the reaction system in the step (2) to 7-8, and stirring at 25 +/-5 ℃ to obtain a second mixed solution;
(4) centrifuging the second mixed solution obtained in the step (3), and drying to obtain the modified anion resin material;
the strong base type anionic resin material contains quaternary ammonium salt functional groups.
2. The method of claim 1, wherein: in the step (1), the drying temperature is 50-70 ℃, and the drying time is 12-24 h.
3. The method of claim 1, wherein: in the step (2), the concentration of the hydrochloric acid solution of the ferric chloride is 0.1-0.5 mol/L.
4. The method of claim 1, wherein: in the step (2), the concentration of the hydrochloric acid solution of zirconium oxychloride is 0.1-0.5 mol/L.
5. The method of claim 1, wherein: in the step (2), the rotation speed of the stirring is 300-400 rpm, and the dipping time is 2-3 h.
6. The method of claim 1, wherein: in the step (3), the adjusted solution is sodium hydroxide solution, and the concentration of the sodium hydroxide solution is 0.5-1.0 mol/L.
7. The method of claim 1, wherein: in the step (4), the rotation speed of the centrifugation is 3000-4000 rpm, and the time of the centrifugation is 10-20 min.
8. The method of claim 1, wherein: in the step (4), the drying temperature is 50-70 ℃, and the drying time is 12-24 h.
9. A modified anionic resinous material characterized by: which is prepared by the preparation method as described in any one of claims 1 to 8.
10. Use of the modified anionic resin material as claimed in claim 9 as a phosphorus removal adsorbent.
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| CN108404880A (en) * | 2018-05-28 | 2018-08-17 | 苏州佑君环境科技有限公司 | A kind of preparation method of inorganic dephosphorization adsorbent |
| CN109250838A (en) * | 2018-09-25 | 2019-01-22 | 芜湖沃泰环保科技有限公司 | Pretreated purifier and process for purifying water are carried out using flue gas |
| CN109502681B (en) * | 2018-11-28 | 2021-10-26 | 北京工业大学 | Method for recovering phosphate in town sewage by resin loaded with hydrous zirconia |
| CN110523395B (en) * | 2019-09-06 | 2021-10-29 | 南京师范大学 | MOF-loaded resin composite adsorbent and preparation method and application thereof |
| CN110681344B (en) * | 2019-10-10 | 2022-04-22 | 南京大学 | Zirconium series nano hybrid material and application method thereof |
| CN111729649B (en) * | 2020-06-23 | 2022-03-18 | 南京大学 | High-selectivity anion adsorbent and preparation method and application thereof |
| CN112079414A (en) * | 2020-09-15 | 2020-12-15 | 昆明理工大学 | Method for treating arsenic in arsenic-containing solution by using strong base anion resin loaded with cobalt |
| CN114797801B (en) * | 2022-06-06 | 2022-11-29 | 哈尔滨工业大学 | Sewage landscape recycling advanced treatment magnetic resin containing two types of quaternary ammonium sites for synchronously removing nitrogen and phosphorus and preparation method thereof |
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