CN112973645A - Rotating magnetic field enhanced sodium alginate/MXene/CoFeO gel, preparation method and application in high-efficiency pollutant enrichment - Google Patents
Rotating magnetic field enhanced sodium alginate/MXene/CoFeO gel, preparation method and application in high-efficiency pollutant enrichment Download PDFInfo
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Abstract
The invention provides a rotating magnetic field enhanced sodium alginate/MXene/CoFeO gel, a preparation method and an application of high-efficiency enriched pollutants, wherein the preparation method comprises the following steps: MXene forms MXene aqueous solution in the aqueous solution; adding sodium alginate into MXene aqueous solution to obtain a first mixed solution; adding CoFeO and NaHCO into the first mixed solution3L-cysteine to obtain a second mixed solution; dropping the organic gel balls into a calcium chloride solution through a peristaltic pump to obtain organic gel balls; the sodium alginate/MXene/CoFeO organic gel ball has excellent adsorption performance and the characteristic that sodium alginate is easy to form gel, not only the adsorption effect is enhanced, but also the solid-liquid separation process is simplified; the method further improves the adsorption and mechanical properties of the organic gel spheres by doping the two-dimensional material MXene. The applied rotating magnetic field can greatly improve the speed of fast adsorption and show the enhanced adsorption capacity of ciprofloxacin adsorption selectivity.
Description
Technical Field
The invention belongs to the technical field of synthesis of environmental materials, and particularly relates to a sodium alginate/MXene/CoFeO gel, a preparation method thereof and application of an external rotating magnetic field to excite an internal magnetic field of an organogel and enhance the adsorption performance of the organogel.
Background
Sodium alginate is a natural polysaccharide, has low cost and high hydrophilicity, and is widely researched due to excellent characteristics such as stability, biocompatibility and the like. Alginate composite gel has become a hot material for solving the problems of dye and heavy metal in water. On the other hand, however, alginate has low porosity and the adsorption effect needs to be improved. Due to the characteristics of high specific surface area and the like, the graphene and the derivative material thereof have excellent adsorption performance on pollutants in water. However, the powdered graphene is also difficult to separate, and is liable to cause secondary pollution after adsorption.
Disclosure of Invention
Aiming at the defects in the prior art, the primary object of the invention is to provide a sodium alginate/MXene/CoFeO organogel, and the adsorption performance is enhanced by applying a rotating magnetic field.
The second purpose of the invention is to provide a preparation method of the sodium alginate/MXene/CoFeO organogel.
The third purpose of the invention is to provide the application of the sodium alginate/MXene/CoFeO organogel.
In order to achieve the above purpose, the solution of the invention is as follows:
a preparation method of sodium alginate/MXene/CoFeO organic gel spheres comprises the following steps:
(1) MXene forms MXene aqueous solution in the aqueous solution;
(2) adding sodium alginate into MXene aqueous solution to obtain a first mixed solution;
(3) adding CoFeO and NaHCO into the first mixed solution3L-cysteine to obtain a second mixed solution;
(4) adding divalent calcium chloride metal salt into the aqueous solution to obtain a third mixed solution;
(5) dripping the second mixed solution into the third mixed solution to obtain sodium alginate/MXene/CoFeO organic gel spheres;
preferably, in the step (1), the concentration of MXene in the MXene aqueous solution is 4 mg/mL.
Preferably, in step (2), the concentration of sodium alginate is 20 mg/mL.
Preferably, in step (3), CoFeO is added at a concentration of 4mg/mL, NaHCO3 at a concentration of 4mg/mL, and L-cysteine at a concentration of 4 mg/mL.
Preferably, in the step (4), the concentration of the divalent metal salt ion in the divalent metal salt, which is Ca2+, is 10 mg/mL.
Preferably, in step (5), the heating temperature is 90 ℃ and the heating time is 3 h.
A sodium alginate/MXene/CoFeO gel ball is prepared by the above preparation method.
The sodium alginate/MXene/CoFeO gel ball is used as an adsorbent.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the invention adopts sodium alginate to form gel, not only has better biocompatibility, but also has excellent gelling performance and good mechanical performance of the gel, and provides convenience for effective separation and recovery of the adsorbent.
Secondly, the Mxene has excellent electrochemical performance, and a large number of functional groups and active sites are arranged on the surface of the Mxene. The combination of Mxene and sodium alginate improves the adsorption performance of sodium alginate and also improves the mechanical strength of organogel
Thirdly, the absorption of the sodium alginate/MXene/CoFeO organogel is assisted by an external rotating magnetic field, the absorption rate of the organogel on pollutants can be effectively improved, and the absorption comparison experiment on ciprofloxacin and copper ions shows that the absorption capacity of ciprofloxacin can be selectively and independently improved under the action of the external magnetic field.
Fourthly, the preparation method of the invention has simple equipment, simple and easy process and continuous operation, thereby being suitable for large-scale production.
In conclusion, the sodium alginate/MXene/CoFeO gel spheres of the invention are organic gels formed by combining sodium alginate with MXene, and the materials have a large number of functional groups and can provide rich adsorption sites in the adsorption process. The magnetic field is combined with the adsorbent, the advantages of the magnetic field and the adsorbent are complementary, the enrichment rate of the adsorbent to pollutants can be greatly improved under the external rotating magnetic field, the problem that the organic gel has the defect of slow adsorption rate is solved, the adsorption effect is enhanced, and the new characteristic of selectively enhancing is shown.
Drawings
FIG. 1 is a schematic diagram of the adsorption kinetic effect of sodium alginate/MXene/CoFeO gel spheres on environmental-friendly Samsung under the condition of magnetization and no magnetization;
FIG. 2 is a schematic diagram showing the adsorption kinetics effect of sodium alginate/MXene/CoFeO gel spheres on copper ions under the condition of magnetization and no magnetization;
FIG. 3 is a schematic diagram showing the comparison of the compressive stress-Strain curves of the sodium alginate/MXene/CoFeO gel spheres and the sodium alginate/CoFeO gel spheres of the present invention (the abscissa represents Strain and the ordinate represents compressive stress);
FIG. 4 is a schematic diagram of the characterization result of scanning electron microscope of sodium alginate/MXene/CoFeO gel spheres of the invention.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
the preparation method of the sodium alginate/MXene/CoFeO gel ball of the embodiment comprises the following steps:
(1) weighing 400mg of MXene to dissolve in a neutral aqueous solution, transferring into a 250mL volumetric flask, and stirring and ultrasonically treating for 200min to form a uniform MXene aqueous solution, wherein the concentration of MXene is 4 mg/mL;
(2) adding 2g of sodium alginate into MXene aqueous solution, and uniformly dispersing for 4 hours by mechanical stirring to obtain first mixed solution;
(3) 400mgCoFeO is added into the first mixed solution, and the concentration of 400mgNaHCO3 is 400 mgL-cysteine;
(4) weighing 4g of calcium chloride in a neutral aqueous solution, and stirring in an ultrasonic machine for 1.5min to obtain a third mixed solution, wherein the concentration of the calcium chloride in the third mixed solution is 10 mg/mL;
(5) dropwise adding the second mixed solution into the third mixed solution by using a peristaltic pump to obtain a sodium alginate/MXene/CoFeO organic solution, and standing for 7 hours;
(6) heating the sodium alginate/MXene/CoFeO organic solution in a water bath kettle (the temperature is 90 ℃ and the time is 3 hours) to obtain sodium alginate/MXene/CoFeO gel spheres, and washing the gel spheres with distilled water to remove residual impurities.
< experiment >
The following experiments were carried out with the products of the above examples, respectively.
< experiment 1>
The purpose of the experiment is to explore the influence of sodium alginate/MXene/CoFeO gel spheres on the adsorption performance of different pollutants under the magnetic and non-magnetic conditions.
As shown in fig. 1, fig. 2, adsorption rates of contaminants on SA/MX/COF magnetic beads were estimated by fitting adsorption data to pseudo-Primary (PF) and pseudo-secondary (PS) kinetic models. The analysis results are shown in FIG. 1. Clearly, the PS kinetic model matches the adsorption kinetic data of CIP better, indicating that the heat of adsorption decreases linearly with increasing adsorption, the intermolecular interaction between adsorbate and adsorbent. By regression analysis of the model, the rate constants were 0.0013g/mg/h and 0.00083g/mg/h, respectively, with and without a rotating magnetic field. Clearly, the CIP adsorption rate increased significantly by about 359.76% in the presence of a rotating magnetic field. Furthermore, the theoretical saturated adsorption capacity of CIP with and without the application of a rotating magnetic field was 290.91 and 234.24mg/g, respectively. The adsorption kinetics data of copper ions are also applied to the PS model, Cu in the presence and absence of a rotating magnetic field2+The theoretical saturated adsorption amounts of (1) and (7) respectively are 100.58 and 96.85mg/g, which shows that the rotating magnetic field is applied to Cu2+The effect of adsorption capacity is almost nil. The rotating magnetic field mainly affects Cu2+The adsorption rate of k2 increased significantly by 371%.
< experiment 2>
The purpose of the experiment is to explore the influence of the mechanical properties of the sodium alginate/MXene/CoFeO gel spheres.
FIG. 3 is the compressive stress-strain curves of sodium alginate/MXene/CoFeO gel spheres and sodium alginate/CoFeO gel spheres. To test the mechanical properties of the gels, the materials were made into small cylinders with a radius of 50 mm (+ -0.1 mm) and a height of 100 mm. From the compressive stress-strain curve of FIG. 3, it is shown that the SA/MX/CFO hydrogel performs very well, with a breaking stress of 1.64MPa at 73.4% strain, while the SA/CFO hydrogel is 1.27 MPa at 32.73% strain. The elastic moduli of the SA/MX/CFO and SA/CFO composite hydrogels were 2.23 and 3.88 MPa.
< experiment 3>
The purpose of the experiment is to research SEM topography of sodium alginate/MXene/CoFeO gel spheres under different resolutions.
As can be seen from fig. 3, the SEM image shows that the surface of the functional composite exhibits phase separation and non-uniformity, and the surface has a non-porous structure. The layered structure of MXene and the bulk crystal of CoFeO can be clearly distinguished from each other. Figure 3 shows a typical MXene structure of the flake, which demonstrates that MXene and CoFeO have been well mixed into the material.
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 (9)
1. A preparation method of sodium alginate/MXene/CoFeO gel balls is characterized in that: which comprises the following steps:
(1) MXene forms MXene aqueous solution in the aqueous solution;
(2) adding sodium alginate into MXene aqueous solution to obtain first mixed solution;
(3) adding CoFeO and NaHCO into the first mixed solution3L-cysteine to obtain a second mixed solution;
(4) adding divalent calcium chloride metal salt into the aqueous solution to obtain a third mixed solution;
(5) and dripping the second mixed solution into the third mixed solution to obtain the sodium alginate/MXene/CoFeO organic gel spheres.
2. The method for preparing sodium alginate/MXene/CoFeO organic gel spheres as claimed in claim 1, wherein: in the step (1), the concentration of MXene in the MXene aqueous solution is 4 mg/mL.
3. The method for preparing sodium alginate/MXene/CoFeO organic gel spheres as claimed in claim 1, wherein: in the step (2), the concentration of the sodium alginate is 20 mg/mL.
4. The method for preparing sodium alginate/MXene/CoFeO organic gel spheres as claimed in claim 1, wherein: in step (3), the concentration of CoFeO added is 4mg/mL, the concentration of NaHCO3 is 4mg/mL, and the concentration of L-cysteine is 4 mg/mL.
5. The method for preparing sodium alginate/MXene/CoFeO organic gel spheres as claimed in claim 1, wherein: in the step (4), the divalent metal salt ion in the divalent metal salt is Ca2+The concentration of (2) is 100 g/mL.
6. The method for preparing sodium alginate/MXene/CoFeO organic gel spheres as claimed in claim 1, wherein: in the step (5), the heating temperature is 90 ℃, and the heating time is 3 h.
7. A sodium alginate/MXene/CoFeO organic gel sphere obtained by the preparation method of any one of claims 1 to 6.
8. Use of the sodium alginate/MXene/CoFeO organic gel beads according to claim 7 as adsorbent.
9. A condition for adsorption according to claim 8, wherein the magnetic field configuration using the externally applied rotating magnetic field is a magnetic field strength of 200mT and a rotation speed of 400 r/min.
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Cited By (3)
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| CN114887591A (en) * | 2022-04-14 | 2022-08-12 | 同济大学 | Method for simply recovering gold from MXene/GO/NbFeB hydrogel by one-step method and application |
| CN117443354A (en) * | 2023-11-29 | 2024-01-26 | 山东大学 | Preparation method of salicylaldoxime grafted MXene/sodium alginate composite gel electrode adsorbent with high adsorption selectivity |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114487083A (en) * | 2022-01-19 | 2022-05-13 | 中国地质大学（北京） | Magnetic hydroxyl nano material Fe3O4@ COFs and application thereof in sulfanilamide mass spectrometry detection field |
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| CN114887591A (en) * | 2022-04-14 | 2022-08-12 | 同济大学 | Method for simply recovering gold from MXene/GO/NbFeB hydrogel by one-step method and application |
| CN114887591B (en) * | 2022-04-14 | 2024-01-12 | 同济大学 | Method for simply recovering gold through MXene/GO/NbFeB hydrogel by one-step method and application |
| CN117443354A (en) * | 2023-11-29 | 2024-01-26 | 山东大学 | Preparation method of salicylaldoxime grafted MXene/sodium alginate composite gel electrode adsorbent with high adsorption selectivity |
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