CN113457618A - Lanthanum-doped ordered mesoporous molecular sieve for environmental remediation and preparation method and application thereof - Google Patents
Lanthanum-doped ordered mesoporous molecular sieve for environmental remediation and preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention relates to a lanthanum-doped ordered mesoporous molecular sieve for environmental remediation and a preparation method and application thereof, wherein the preparation method of the molecular sieve comprises the following steps: soaking a ZSM-5 molecular sieve in an alkaline solution; immersing a ZSM-5 molecular sieve in deionized water, oscillating, washing and drying; carrying out oscillation reaction on a ZSM-5 molecular sieve and a lanthanum salt solution by adopting an ion exchange method; adding urea into the solution, reacting again, stably loading lanthanide compounds on a ZSM-5 molecular sieve by adopting a hydrothermal synthesis method, and then washing and drying to obtain the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation. The lanthanum-doped ordered mesoporous molecular sieve has high stability, physical strength and excellent environmental tolerance, and can simultaneously exert the advantages of good adsorption efficiency of lanthanide compounds, good stability of the molecular sieve, high mechanical strength and excellent corrosion resistance.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a lanthanum-doped ordered mesoporous molecular sieve for environmental remediation and a preparation method and application thereof.
Background
In 2008, David et al (Schinder D.W., et al. P Natl Acad Sci Usa.2008,105(32): 11254-11258) analyzed the water quality monitoring data of lakes for 37 years, and found that phosphorus elements, particularly phosphate, are a key factor causing eutrophication of water bodies. Phosphate is an essential nutrient substance of algae, when the content of the phosphate in water is too high, a large number of aquatic plants such as algae and other bacteria microorganisms rapidly propagate to cause the reduction of water transparency and the reduction of dissolved oxygen, so that aquatic animals such as fishes and the like are anoxic and die in a large number, the propagation of anaerobic bacteria in the water is increased, toxic substances are generated, and an aquatic ecosystem is seriously damaged. The eutrophication phenomenon mainly occurs in fresh water bodies, the water quality deterioration can possibly cause the influence on the water supply of residents, even threatens the drinking water safety if the water quality deterioration is serious, and at present, the occurrence of the eutrophication phenomenon further aggravates the severe situation of water supply shortage and obviously influences normal social production and resident life. By combining the reasons, how to purify the phosphorus-containing wastewater efficiently, the economic and effective technical means is adopted to restore the phosphorus-polluted water body, thereby avoiding the eutrophication phenomenon and having very important practical significance on ecological protection, economic development and social progress.
The most common method for treating phosphorus-containing wastewater and repairing phosphorus-polluted water is an adsorption method, and the selection of an adsorbent is a very critical factor. The rare earth element lanthanum is an element with abundant content in nature, and most lanthanum compounds have no pollution to the environment. Many studies have demonstrated that lanthanum compounds, including lanthanum carbonate, lanthanum hydroxide, lanthanum oxide, etc., have strong binding capacity for phosphates. In addition, the lanthanide compounds often show higher adsorption rate, adsorption selectivity and adsorption capacity in adsorption, and are important environmental remediation agents for remedying phosphorus-polluted water and avoiding eutrophication. Most of polluted water bodies in actual environments are in an acidic condition, so that the structures of a plurality of environment restoration agents are unstable, and lanthanide compounds can play a role stably in the acidic environment and show higher treatment efficiency in the treatment of phosphorus-containing wastewater. In addition, most importantly, the lanthanide compounds are less harmful to human bodies, and lanthanum carbonate is also commonly used in medicine for treating hyperphosphatemia, so that the safety is higher in the using process. Although lanthanide compounds have proven to have good potential for environmental remediation applications, their development is limited by problems associated with complex fabrication processes, high cost, and difficulty in scale-up. Although the lanthanide compound has a high specific surface area and a suitable porous structure, the nano-scale lanthanide compound has an excessively small particle size, and is often agglomerated during use, so that the porosity is often difficult to be fully utilized. Meanwhile, the smaller particle size also causes the adsorbent to be difficult to recover after use, an additional separation step is required, the operation difficulty and the cost are increased, and the loss of the lanthanide compound is inevitable.
In order to solve the problems, scholars uniformly load the lanthanide compounds on different carriers, avoid agglomeration, increase the contact efficiency of the adsorbent and pollutants in water, and simultaneously are easy to separate, thereby improving the recovery efficiency and reducing the loss of the lanthanide compounds. The molecular sieve has uniform pore channel distribution, larger specific surface area, good mechanical strength and chemical stability and abundant active center sites, and is an excellent carrier material. He et al (He Y., et al. appl Surf Sci.2017,426) prepared a novel porous lanthanum composite molecular sieve La-Z adsorbent by hydrothermal synthesis, and found that the La-Z surface is positively charged, so that phosphate can be adsorbed by electrostatic attraction and ligand exchange reaction. Researchers further apply the obtained adsorbent to the actual polluted water treatment of an environmental system, and ideal results are obtained. Huang et al (Huang W., et al, Micropor Mesopor Mat.2015,217:225-232) prepared a novel lanthanum-supported flower-like silica (FMS-La) and applied it for phosphate adsorption. The narrow inner pore canal and the open outer pore canal of the flower-shaped mesoporous silica enable the inner surface and the outer surface of the flower-shaped mesoporous silica to be used for adsorbing pollutants. Although the flower-like silica has good adsorption performance, the preparation process is complicated and the application is limited.
How to prepare an environmental remediation adsorption material with high stability, physical strength and excellent environmental tolerance is a problem to be solved. In order to solve the problems, the lanthanide compound is uniformly dispersed and loaded on the molecular sieve carrier by adopting a hydrothermal synthesis method, so that the advantages of good adsorption efficiency of the lanthanide compound and good stability, strong mechanical strength and excellent corrosion resistance of the molecular sieve can be simultaneously played, and the treatment efficiency of the environment repairing agent is improved.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the defects of the existing adsorbing material for treating phosphorus in water, the invention provides a lanthanum-doped ordered mesoporous molecular sieve for environmental remediation, and a preparation method and application thereof.
The technical scheme is as follows: a preparation method of lanthanum-doped ordered mesoporous molecular sieve for environmental remediation comprises the following preparation steps:
(1) soaking a ZSM-5 molecular sieve in an alkaline solution for 12-36 h;
(2) immersing the ZSM-5 molecular sieve soaked in the alkaline solution in the step (1) in deionized water, oscillating and washing at the temperature of 50-100 ℃ and the oscillation rate of 150-250 rpm, and drying at the temperature of-30-50 ℃ for 8-24 h;
(3) carrying out oscillation reaction on the ZSM-5 molecular sieve dried in the step (2) and a lanthanum salt solution for 12-36 h at the temperature of 50-100 ℃ and the rotating speed of 150-200 rpm by adopting an ion exchange method;
(4) and (4) adding urea into the solution oscillated in the step (3), reacting for 8-24 h again, stably loading lanthanide compounds on a ZSM-5 molecular sieve by adopting a hydrothermal synthesis method, washing, and drying at-30-50 ℃ to obtain the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation.
The ZSM-5 molecular sieve in the step (1) has the aperture of 0.5nm and the silica-alumina ratio of 50-70 spheres, and the alkaline solution is NaOH solution, KOH solution or Ca (OH) with the concentration of 2-3 mol/L2And (3) solution.
The preparation method of the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation is characterized by comprising the following steps: the lanthanum salt solution in the step (3) is La (NO) with the concentration of 0.1-0.3 mol/L3)3And (3) solution.
The lanthanum-doped ordered mesoporous molecular sieve for environmental remediation, which is prepared by the preparation method, is provided.
An application of the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation in removing phosphate in water.
The application method of the lanthanum-doped ordered mesoporous molecular sieve in removing phosphate in water comprises the following steps: and (3) putting the lanthanum-doped ordered mesoporous molecular sieve into a polluted water body, purifying the water body in a multi-gradient pool, and recovering and recycling the lanthanum-doped ordered mesoporous molecular sieve after adsorbing for a period of time.
Has the advantages that: the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation, the preparation method and the application thereof provided by the invention have the following beneficial effects:
1. according to the preparation method, the lanthanide compound is uniformly dispersed and loaded on the molecular sieve carrier by adopting a hydrothermal synthesis method, so that the good adsorption efficiency of the lanthanide compound can be exerted, and the treatment efficiency of the environment repairing agent is improved;
2. the invention loads the lanthanide compound on the molecular sieve carrier with good stability, high mechanical strength and excellent corrosion resistance, can reduce the difficulty of the separation process after use, is beneficial to reducing the operation cost, improves the recovery efficiency while increasing the adsorption performance, reduces the loss of the lanthanide compound,
3. according to the material disclosed by the invention, the lanthanide compound is combined on the molecular sieve, so that the utilization of the surface of an inner hole is improved, and the adsorption efficiency of pollutants is improved;
4. the lanthanum-doped ordered mesoporous molecular sieve is a renewable material, has high adsorption efficiency after regeneration, is simple in regeneration process and easy to operate, greatly saves time cost, prolongs the service life of a repairing agent, and improves economic benefits.
Detailed Description
Example 1
A preparation method of lanthanum-doped ordered mesoporous molecular sieve for environmental remediation comprises the following steps:
(1) preparation of 2.5mol/L sodium hydroxide solution: weighing 50g of sodium hydroxide solid, dissolving in 500mL of water, and stirring in a fume hood with a glass rod until the solid is completely dissolved;
(2) preparation of 0.2mol/L lanthanum nitrate solution: weighing 17.32g of lanthanum nitrate hexahydrate solid, dissolving in 200mL of water, and reserving for later use;
(3) preparing the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation:
1) weighing 1g of ZSM-5 molecular sieve, completely immersing in 2.5mol/L sodium hydroxide solution, and standing for 24 h;
2) taking out the ZSM-5 molecular sieve immersed in the sodium hydroxide solution, immersing the molecular sieve in deionized water, placing the molecular sieve in a shaking table, oscillating the molecular sieve for 10min at the temperature of 80 ℃ and the rotating speed of 200rpm, sucking water by using filter paper, repeating the steps for three times, and after washing, placing the molecular sieve in a freeze dryer and drying the molecular sieve for 12h at the temperature of-20 ℃;
3) placing the dried ZSM-5 molecular sieve in 200mL of 0.2mol/L lanthanum nitrate solution, placing the solution in a constant temperature shaking table, and oscillating for 24 hours at the temperature of 80 ℃ and the rotating speed of 165 rpm;
4) adding 192g of urea into the solution after the oscillation is finished, putting the solution into a constant-temperature shaking table again, and reacting for 12 hours at the temperature of 80 ℃ and the rotating speed of 165 rpm;
5) and taking out the molecular sieve after the reaction is finished, immersing the molecular sieve in deionized water, placing the molecular sieve in a shaking table, oscillating the molecular sieve for 10min at the rotating speed of 200rpm, sucking water by using filter paper, repeating the operation for three times, and placing the molecular sieve in a freeze dryer to dry the molecular sieve for 12h at the temperature of minus 20 ℃ after the washing is finished, thus obtaining the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation.
The performance test of the lanthanum-doped ordered mesoporous molecular sieve of the embodiment comprises the following steps:
the lanthanum-doped ordered mesoporous molecular sieve prepared in the example is placed in 200mL of 200mg/L phosphate solution for adsorption for 8 hours, the initial pH of the phosphate is 5.52, the adsorption reaction is carried out in a constant-temperature shaking table at 80 ℃ and 200rpm, and the pH of the remaining solution after the reaction is finished is 6.54.
Example 2
A preparation method of lanthanum-doped ordered mesoporous molecular sieve for environmental remediation comprises the following steps:
(1) preparation of 2.5mol/L sodium hydroxide solution: weighing 50g of sodium hydroxide solid, dissolving in 500mL of water, and stirring in a fume hood with a glass rod until the solid is completely dissolved;
(2) preparation of 0.2mol/L lanthanum nitrate solution: weighing 43.3g of lanthanum nitrate hexahydrate solid, dissolving in 500mL of water, and reserving for later use;
(3) preparing the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation:
1) weighing 1g of ZSM-5 molecular sieve, completely immersing in 2.5mol/L sodium hydroxide solution, and standing for 24 h;
2) taking out the ZSM-5 molecular sieve immersed in the sodium hydroxide solution, immersing the molecular sieve in deionized water, placing the molecular sieve in a shaking table, oscillating the molecular sieve for 10min at the temperature of 80 ℃ and the rotating speed of 200rpm, sucking water by using filter paper, repeating the steps for three times, and after washing, placing the molecular sieve in a freeze dryer and drying the molecular sieve for 12h at the temperature of-20 ℃;
3) placing the dried ZSM-5 molecular sieve in 200mL of 0.2mol/L lanthanum nitrate solution, placing the solution in a constant temperature shaking table, and oscillating the solution for 24 hours at the temperature of 80 ℃ and the rotating speed of 165 rpm;
4) adding 192g of urea into the solution after the oscillation is finished, putting the solution into a constant-temperature shaking table again, and reacting for 12 hours at the temperature of 80 ℃ and the rotating speed of 165 rpm;
5) and taking out the molecular sieve after the reaction is finished, immersing the molecular sieve in deionized water, placing the molecular sieve in a shaking table, oscillating the molecular sieve for 10min at the rotating speed of 200rpm, sucking water by using filter paper, repeating the operation for three times, and placing the molecular sieve in a freeze dryer to dry the molecular sieve for 12h at the temperature of minus 20 ℃ after the washing is finished, thus obtaining the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation.
The performance test of the lanthanum-doped ordered mesoporous molecular sieve of the embodiment comprises the following steps:
firstly, the lanthanum-doped ordered mesoporous molecular sieve prepared in the example is subjected to a pH effect experiment. Lanthanum-doped ordered mesoporous molecular sieve with the same mass is added into phosphate solution with the same concentration and content, the initial pH is adjusted to be different, phosphate adsorption experiments are carried out, and the reaction time is the same. The lanthanum-doped ordered mesoporous molecular sieve prepared in the embodiment has good adsorption performance under an acidic condition.
Example 3
A preparation method of lanthanum-doped ordered mesoporous molecular sieve for environmental remediation comprises the following steps:
(1) preparation of 2.5mol/L sodium hydroxide solution: weighing 50g of sodium hydroxide solid, dissolving in 500mL of water, and stirring in a fume hood with a glass rod until the solid is completely dissolved;
(2) preparation of 0.1mol/L lanthanum nitrate solution: weighing 8.66g of lanthanum nitrate hexahydrate solid, dissolving in 200mL of water, and reserving for later use;
(3) preparing a lanthanum-doped ordered mesoporous molecular sieve:
1) weighing 0.5g of ZSM-5 molecular sieve, completely immersing in 2.5mol/L sodium hydroxide solution, and standing for 24 h;
2) taking out the ZSM-5 molecular sieve immersed in the sodium hydroxide solution, immersing the molecular sieve in deionized water, placing the molecular sieve in a shaking table, oscillating the molecular sieve for 10min at the temperature of 80 ℃ and the rotating speed of 200rpm, sucking water by using filter paper, repeating the steps for three times, and after washing, placing the molecular sieve in a freeze dryer and drying the molecular sieve for 12h at the temperature of-20 ℃;
3) placing the dried ZSM-5 molecular sieve in 200mL of 0.2mol/L lanthanum nitrate solution, placing the solution in a constant temperature shaking table, and oscillating for 24 hours at the temperature of 80 ℃ and the rotating speed of 165 rpm;
4) adding 96.096g of urea into the solution after the oscillation is finished, placing the solution in a constant temperature shaking table again, and reacting for 12 hours at the temperature of 80 ℃ and the rotating speed of 165 rpm;
5) and taking out the molecular sieve after the reaction is finished, immersing the molecular sieve in deionized water, placing the molecular sieve in a shaking table, oscillating the molecular sieve for 10min at the rotating speed of 200rpm, sucking water by using filter paper, repeating the operation for three times, and placing the molecular sieve in a freeze dryer to dry the molecular sieve for 12h at the temperature of minus 20 ℃ after the washing is finished, thus obtaining the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation.
The performance test of the lanthanum-doped ordered mesoporous molecular sieve of the embodiment comprises the following steps:
the lanthanum-doped ordered mesoporous molecular sieve prepared in the embodiment is placed in 200mL and 100mg/L phosphate solution at the concentration of 3g/L for adsorption for 8 hours, the initial pH is controlled to be 5.52, the adsorption reaction is carried out in a constant-temperature shaking table at 30 ℃ and 200rpm, and the removal rate of phosphorus can reach more than 99% after the reaction is finished.
While the embodiments of the present invention have been described in detail, those skilled in the art will recognize that the embodiments of the present invention can be practiced without departing from the spirit and scope of the claims.
Claims (6)
1. A preparation method of lanthanum-doped ordered mesoporous molecular sieve for environmental remediation is characterized by comprising the following preparation steps:
(1) soaking a ZSM-5 molecular sieve in an alkaline solution for 12-36 h;
(2) immersing the ZSM-5 molecular sieve soaked in the alkaline solution in the step (1) in deionized water, oscillating and washing at the temperature of 50-100 ℃ and the oscillation rate of 150-250 rpm, and drying at the temperature of-30-50 ℃ for 8-24 hours;
(3) carrying out oscillation reaction on the ZSM-5 molecular sieve dried in the step (2) and a lanthanum salt solution for 12-36 h at the temperature of 50-100 ℃ and the rotating speed of 150-200 rpm by adopting an ion exchange method;
(4) and (3) adding urea into the solution oscillated in the step (3), reacting for 8-24 h again, stably loading a lanthanide compound on a ZSM-5 molecular sieve by adopting a hydrothermal synthesis method, washing, and drying at-30-50 ℃ to obtain the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation.
2. The method for preparing the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation according to claim 1, wherein the lanthanum-doped ordered mesoporous molecular sieve comprises the following steps: the ZSM-5 molecular sieve in the step (1) has the aperture of 0.5nm and the silicon-aluminum ratio of 50-70 spheres, and the alkaline solution is NaOH solution, KOH solution or Ca (OH) with the concentration of 2-3 mol/L2And (3) solution.
3. The method for preparing the lanthanum-doped ordered mesoporous molecular sieve for environmental remediation according to claim 1, wherein the lanthanum-doped ordered mesoporous molecular sieve comprises the following steps: the lanthanum salt solution in the step (3) is La (NO) with the concentration of 0.1-0.3 mol/L3)3And (3) solution.
4. An environment-repairing lanthanum-doped ordered mesoporous molecular sieve prepared by the preparation method of any one of claims 1 to 3.
5. Use of the lanthanum doped ordered mesoporous molecular sieve for environmental remediation according to claim 4 for removing phosphate from water.
6. The use of the lanthanum doped ordered mesoporous molecular sieve for environmental remediation according to claim 5, wherein the method of use is as follows: and (3) putting the lanthanum-doped ordered mesoporous molecular sieve into a polluted water body, purifying the water body in a multi-gradient pool, and recovering and recycling the lanthanum-doped ordered mesoporous molecular sieve after adsorbing for a period of time.
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| CN116328824A (en) * | 2023-03-28 | 2023-06-27 | 上海翊嘉生物科技有限公司 | Cerium oxide cluster nano-enzyme anchored by defective molecular sieve, and preparation method and application thereof |
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| YI YANG ET AL.: ""Construction of a novel lanthanum carbonate-grafted ZSM-5 zeolite for effective highly selective phosphate removal from wastewater"", 《MICROPOROUS AND MESOPOROUS MATERIALS》 * |
| 林建伟等: ""氢氧化镧-天然沸石复合材料对水中低浓度磷酸盐的吸附作用"", 《环境科学》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114713185A (en) * | 2022-04-22 | 2022-07-08 | 重庆三峡学院 | Preparation method and application of spherical lanthanum carbonate loaded zeolite phosphate adsorbent |
| CN116328824A (en) * | 2023-03-28 | 2023-06-27 | 上海翊嘉生物科技有限公司 | Cerium oxide cluster nano-enzyme anchored by defective molecular sieve, and preparation method and application thereof |
| CN116328824B (en) * | 2023-03-28 | 2023-10-13 | 上海翊嘉生物科技有限公司 | Cerium oxide cluster nano-enzyme anchored by defective molecular sieve, and preparation method and application thereof |
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