CN111744454A - Preparation method of composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite - Google Patents
Preparation method of composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite Download PDFInfo
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- CN111744454A CN111744454A CN202010667667.2A CN202010667667A CN111744454A CN 111744454 A CN111744454 A CN 111744454A CN 202010667667 A CN202010667667 A CN 202010667667A CN 111744454 A CN111744454 A CN 111744454A
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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
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a preparation method of a composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite, and relates to a preparation method of a composite phosphorus removal adsorbent. The invention aims to solve the technical problems that the existing phosphorus removal adsorbent has more preparation processes, small adsorption capacity, difficult recycling of powdery adsorbent, high treatment cost and easy secondary sludge generation. The method comprises the following steps: dissolving montmorillonite in strong acid solution, and stirring uniformly; repeatedly washing acid-modified montmorillonite with deionized water to neutrality, and performing suction filtration; drying the filter cake to obtain modified montmorillonite; weighing a certain amount of lanthanum nitrate and glycine according to a molar ratio, adding a small amount of deionized water into a beaker, and uniformly stirring; adding a certain amount of modified montmorillonite, adding a small amount of deionized water, and continuously stirring to uniformly mix; transferring the mixture into a drying oven and drying. And transferring the precursor into a muffle furnace, and calcining. And cooling to room temperature, and uniformly grinding to obtain the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite which can be used in the field of phosphorus-containing wastewater treatment.
Description
Technical Field
The invention relates to a preparation method of a composite dephosphorizing adsorbent.
Background
Phosphorus is an indispensable key nutrient element for the growth of aquatic plants, but excessive phosphorus can cause eutrophication of water bodies and is a main cause of water body pollution, lake eutrophication and red tide in gulf, so the key to solve the problems is to remove excessive PO in the water bodies4 3-. How to improve the dephosphorization efficiency becomes a hotspot and a difficulty of research at present.
Different phosphorus removal technologies should be adopted for different wastewater sources. Commonly used water phosphorus removal techniques include chemical, biological, membrane separation, ion exchange, and adsorption. The adsorption dephosphorization technology has the characteristics of small occupied area, low energy consumption, low cost, high efficiency and the like, and can adsorb PO with a larger concentration range4 3-And the adsorbent can be recovered by desorption treatment, contributing to the realization of the reuse of resources. Therefore, the adsorption method is widely used for pretreatment of wastewater, advanced treatment, and emergency treatment.
The rare earth element lanthanum is an environment-friendly, non-toxic and harmless substance, and has strong binding force to soluble phosphate. Lanthanum can be reacted with PO4 3-Form stable and water insoluble LaPO at a molar ratio of 1:14And the lanthanum-containing adsorbent has the advantages of high adsorption capacity, reproducibility and the like, and is often used as a phosphorus removal adsorbent. However, the powdery adsorbent can sink to the bottom of the water body in the dephosphorization process and is difficult to recycle, which greatly increases the treatment cost of the phosphorus-containing wastewater and is easy to cause sludge pollution.
Montmorillonite is a universal material, and has the characteristics of good ion exchange property, strong adsorption capacity, economy, large storage capacity, no pollution and the like, so that montmorillonite is widely applied to the field of adsorption. The montmorillonite can be peeled and dispersed into thin single crystal under the action of interlayer and solvent, thereby improving the adsorption capacity and the adsorption effect. However, the adsorption capacity of montmorillonite is still small, and the treatment of wastewater containing high-concentration phosphorus cannot be satisfied.
In order to solve the problems, the invention provides La2O2CO3Loading on modified montmorillonite to form La2O2CO3The @ Mt composite adsorbent effectively improves the dephosphorization efficiency and the powder utilization rate.
Disclosure of Invention
The invention aims to solve the problem that the existing phosphorus removal adsorbent is PO4 3-The removal rate is low, and provides a phosphorus removal composite adsorbent La2O2CO3A method for the preparation of @ Mt.
The preparation method of the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite comprises the following steps:
s1: preparation of modified montmorillonite: dissolving montmorillonite in a strong acid solution, and stirring for 1-3 h; repeatedly washing acid-modified montmorillonite with deionized water to neutrality, and performing suction filtration; transferring the filter cake to an oven, and drying at 100-120 ℃ for 5-7 h to obtain modified montmorillonite;
s2: preparing a precursor: weighing a certain amount of lanthanum nitrate and glycine in a beaker, adding a small amount of deionized water, and uniformly stirring; adding a certain amount of modified montmorillonite, adding a small amount of deionized water, heating to 65 ℃ under magnetic stirring, and stirring at the speed of 200-500r/min for 30 min; transferring the mixture to an oven, and drying the mixture for 10 to 12 hours at the temperature of between 120 and 180 ℃ to obtain a precursor;
s3: preparing a composite adsorbent: transferring the precursor into a muffle furnace, and calcining; cooling to room temperature, and grinding uniformly to obtain the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite marked as La2O2CO3@ Mt adsorbent.
Preferably, in step S1, the acid is sulfuric acid or nitric acid, and the pH is 1;
preferably, in step S1, the solid-to-liquid ratio of montmorillonite to acid having a pH of 1 is 1 (9 to 11);
preferably, in step S2, the molar ratio n (lanthanum nitrate) n (glycine) is 1: 2;
preferably, in the step S2, the mass ratio of the lanthanum nitrate to the modified montmorillonite is (0.3-0.6): 1;
preferably, in the step S3, the calcination temperature in the muffle furnace is 440 to 460 ℃, and the calcination time is 2 to 3 hours.
La of the invention2O2CO3The @ Mt adsorbent is prepared by the glycine-nitrate method, by calcining La2O2CO3Is tightly loaded on the surface of the montmorillonite, and is easy to recycle. La2O2CO3The @ Mt adsorbent greatly increases the specific surface area and enhances the adsorption effect on PO4 3-The adsorption capacity of the phosphorus removal agent improves the phosphorus removal efficiency.
La prepared by the invention2O2CO3@ Mt adsorbent Pair PO4 3-Carrying out adsorption of PO4 3-The removal rate of the phosphorus-containing wastewater reaches 98.1-99.5 percent, and the phosphorus-containing wastewater can be used in the field of phosphorus-containing wastewater treatment.
Drawings
FIG. 1 shows modified montmorillonite and La of example 12O2CO3X-ray diffraction patterns of @ Mt;
FIG. 2 is a scanning electron micrograph of the modified montmorillonite in example 1;
FIG. 3 is an enlarged scanning electron micrograph of the modified montmorillonite in example 1;
FIG. 4 shows La in example 12O2CO3Scanning electron micrographs of @ Mt;
FIG. 5 shows La in example 12O2CO3Scanning electron microscope photographs magnified by @ Mt;
FIG. 6 shows La of example 22O2CO3@ Mt vs. PO4 3-A graph of the removal rate of (d) as a function of adsorption time;
FIG. 7 shows La of example 32O2CO3@ Mt vs. PO4 3-The removal rate of (d) is plotted as a function of pH;
FIG. 8 shows La in example 42O2CO3@ Mt vs. PO4 3-A graph of the removal rate of (a) as a function of substrate concentration;
FIG. 9 shows La in example 52O2CO3@ Mt vs. PO4 3-The removal rate of (a) is plotted as a function of the amount of adsorbent added.
Detailed Description
The following examples are used to demonstrate the beneficial effects of the present invention.
Example 1: the preparation method of the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite of the embodiment comprises the following steps:
s1: and (3) placing 10g of montmorillonite into 100mL of sulfuric acid solution with the pH value of 1, stirring for 2h at normal temperature by using a constant-temperature magnetic stirrer, after the reaction is finished, performing suction filtration and washing on the modified montmorillonite to be neutral, placing the modified montmorillonite into a drying oven, drying for 6h at the temperature of 110 ℃, and grinding to obtain the modified montmorillonite (Mt) for the experiment.
S2: weighing a certain amount of lanthanum nitrate and glycine in a beaker according to a molar ratio n (lanthanum nitrate) to n (glycine) of 1:2, adding a small amount of deionized water, and magnetically stirring for 30 min; according to the mass ratio of the lanthanum nitrate to the modified montmorillonite of 0.5:1, adding a certain amount of the modified montmorillonite, continuing to stir by magnetic force to uniformly mix the materials, transferring the materials to a drying oven at 180 ℃ to dry for 12 hours, and grinding the materials to obtain a precursor;
s3: calcining the precursor in a muffle furnace at 450 ℃ for 2h, cooling and grinding to obtain the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite, namely the phosphorus removal composite adsorbent La2O2CO3@Mt。
Modified montmorillonite and La obtained in example 12O2CO3The XRD spectrum of @ Mt is shown in figure 1. As can be seen from FIG. 1, the XRD diffraction peak of the modified montmorillonite takes the shape of a steamed bun peak, indicating that montmorillonite exists in an amorphous state. La2O2CO3XRD pattern of @ MtA series of sharp diffraction peaks appear, which indicates that the calcined sample is completely crystallized, and the comparison with the standard card PDF #20-0452 shows that the generated substance is CaAl2Si2O8·H2O, which is the main component of montmorillonite. Further, diffraction peaks at 11.080 °, 22.266 °, 25.831 °, 30.368 ° and 44.420 ° correspond to La, respectively2O2CO3(PDF #84-1963) for (002), (004), (101), (103) and (110) crystal planes, indicating La2O2CO3Has been successfully loaded on the surface of montmorillonite, and shows that La2O2CO3@ Mt was successfully prepared.
In the SEM photograph of the modified montmorillonite in step S1 of this example 1, as shown in FIGS. 2 and 3, it can be seen that the particle size of the modified montmorillonite is about 70 μm, the surface is uneven, some regions are smooth, and a large number of particles having a size of about 1 μm are distributed in some other regions. La obtained in the third step2O2CO3The scanning electron micrographs of @ Mt are shown in FIGS. 4 and 5, and it is known from XRD analysis that the internal structure of montmorillonite is destroyed by high-temperature calcination, and the amorphous state is transformed into the crystalline state, which results in large changes in the particle size and morphology of the material, and the original morphology is changed into fragments with uneven shapes and holes, and the particle sizes are different, and the size of the larger fragments is 30 μm.
Example 2:
la obtained in step S32O2CO3@ Mt adsorption performance test, the procedure is as follows: weighing 50mg of La2O2CO3@ Mt, addition of 50mg/L PO4 3-In solution, at room temperature to PO4 3-Adsorbing the solution, representing the removal effect by using a removal rate R, and calculating according to the following formula:
R(％)＝(c0-c)/c0×100％
wherein, c0Represents PO before adsorption4 3-C represents PO after adsorption4 3-The concentration of (c). As a result, as shown in FIG. 6, La was observed in FIG. 62O2CO3@ Mt vs. PO4 3-The adsorption is balanced for about 120 minutes, and the removal rate can reach 98.1 to 99.5 percent.
Example 3:
adding 50mg/L KH with HCl or NaOH2PO4Adjusting the pH value of the solution to 1-7, and then adding 50mg/LLa2O2CO3@ Mt the adsorption experiment was carried out using the same procedure as in example 2.
As shown in FIG. 7, it can be seen from FIG. 7 that the pH of the solution is in the range of 1 to 7, as compared with La2O2CO3Less influence of the adsorption effect of @ Mt, La2O2CO3@ Mt vs. PO4 3-The removal rate of (A) is kept above 98%.
Example 4:
weighing 50mg of La2O2CO3@ Mt added to PO at 50mg/L, 100mg/L, 150mg/L, 200mg/L and 250mg/L, respectively4 3-The adsorption experiments were carried out in solution, the procedure being the same as in example 2.
The results are shown in FIG. 8, and it can be seen from FIG. 8 that PO increases with the substrate concentration4 3-The removal rate of (2) is in a descending trend, and when the concentration of the substrate is 50 mg/L-250 mg/L, the removal rate is reduced from 98.63 percent to 93.88 percent.
Example 5:
12.5mg, 25mg, 50mg, 75mg, 100mg, 125mg and 150mg La were weighed out2O2CO3@ Mt, adding 50mg/L PO separately4 3-The adsorption experiments were carried out in solution, the procedure being the same as in example 2.
The result is shown in FIG. 9, and it can be seen from FIG. 9 that La is used2O2CO3When the dosage of the @ Mt adsorbent is 0.25g/L, the removal rate is 94.26%, when the dosage of the adsorbent is increased to 1.0g/L, the removal rate reaches 99.50%, the dosage of the adsorbent is continuously increased to 3.0g/L, and the adsorbent is used for PO4 3-The removal rate of (a) is substantially unchanged.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A preparation method of a composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite is characterized by comprising the following steps:
s1: preparation of modified montmorillonite: dissolving montmorillonite in a strong acid solution, and stirring for 1-3 h; repeatedly washing acid-modified montmorillonite with deionized water to neutrality, and performing suction filtration; transferring the filter cake to an oven, and drying at 100-120 ℃ for 5-7 h to obtain modified montmorillonite;
s2: preparing a precursor: weighing a certain amount of lanthanum nitrate and glycine in a beaker, adding a small amount of deionized water, and uniformly stirring; adding a certain amount of modified montmorillonite, adding a small amount of deionized water, heating to 65 ℃ under magnetic stirring, and stirring at the speed of 200-500r/min for 30 min; transferring the mixture to an oven to be dried for 10-12 h at the temperature of 120-180 ℃;
s3: preparing a composite adsorbent: transferring the precursor into a muffle furnace for calcining; cooling to room temperature, and grinding uniformly to obtain the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite marked as La2O2CO3@ Mt adsorbent.
2. The method for preparing the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite according to claim 1, wherein in step S1, the acid is sulfuric acid or nitric acid, and the pH is 1.
3. The preparation method of the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite according to claim 1, characterized in that in step S1, the solid-liquid mass ratio of montmorillonite to acid with pH of 1 is 1 (9-11).
4. The composite phosphorus removal adsorbent La as claimed in claim 12O2CO3The preparation method of @ Mt is characterized in that in step S2, the molar ratio of lanthanum nitrate to glycine is 1: 2.
5. The preparation method of the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite according to claim 1, characterized in that in step S2, the mass ratio of lanthanum nitrate to montmorillonite is (0.3-0.6): 1.
6. The preparation method of the composite phosphorus removal adsorbent lanthanum oxycarbonate loaded montmorillonite according to claim 1, characterized in that in step S3, the calcination temperature in a muffle furnace is 440-460 ℃, and the calcination time is 2-3 h.
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Cited By (3)
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| CN114100561A (en) * | 2021-12-01 | 2022-03-01 | 中国科学院生态环境研究中心 | Metal modified La2O2CO3Adsorbent and preparation method and application thereof |
| CN114849642A (en) * | 2022-04-22 | 2022-08-05 | 重庆三峡学院 | Preparation method and application of Ping-pong chrysanthemum-shaped lanthanum carbonate oxide adsorbent |
| CN115518620A (en) * | 2022-09-15 | 2022-12-27 | 西南交通大学 | Starch and lanthanum modified montmorillonite material and preparation and application methods thereof |
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