CN114702694A - Polyelectrolyte hydrogel based on zipper-unzipping effect, and preparation method and application thereof - Google Patents
Polyelectrolyte hydrogel based on zipper-unzipping effect, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses polyelectrolyte hydrogel based on a zipper-releasing effect and a preparation method and application thereof.
Description
Technical Field
The invention relates to the technical field of sustainable chemical industry, in particular to polyelectrolyte hydrogel based on zipper-releasing effect and a preparation method and application thereof.
Background
Metal ion pollution is a prominent manifestation of the water pollution problem, which not only harms the ecological environment, but also threatens the human health, and simultaneously restricts the sustainable development of economy. The method is urgent, and has urgent need of strictly monitoring the discharge of metal ion wastewater and rapidly and effectively treating metal ion pollution. At present, methods for treating metal ion wastewater mainly comprise chemical sedimentation, ion exchange, membrane treatment, adsorption capture and the like, wherein an adsorption method is widely applied to treatment of low-concentration metal ions in water bodies due to the advantages of simple operation, easy regeneration, high efficiency, low cost, biocompatibility and the like.
The hydrogel is a high molecular hydrophilic polymer which takes water as a dispersion medium, is formed by physical or chemical crosslinking and has a three-dimensional network structure, the water absorption capacity of the hydrogel can reach dozens of times or even thousands of times of the dry weight of the gel, and the hydrogel can swell in water but is insoluble in water. Wherein, the polyelectrolyte hydrogel is a kind of water-containing network polymer with positive charge and negative charge groups on the main chain of the macromolecule. In recent years, a large number of researchers have used polyelectrolyte hydrogels to adsorb and capture metal ions in solutions. As an adsorption trapping agent, the trapping efficiency is an important performance index and is another standard for measuring the adsorption cost. In order to improve the capture efficiency, related researches mainly increase the binding sites of the hydrogel and the metal ions by grafting, modifying and other methods, however, the above methods have the disadvantages of unobvious efficiency improvement, complex synthesis, higher cost and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides polyelectrolyte hydrogel based on a zipper-releasing effect and a preparation method and application thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of polyelectrolyte hydrogel based on 'unzipping' effect comprises the following steps:
step 101, dispersing 2-8 parts of polycation component chitosan in 100-200 parts of deionized water by mass, and stirring for 40-60 min at the temperature of 20-25 ℃ to obtain chitosan dispersion liquid;
102, dissolving 2-8 parts by mass of a polyanion component in 100-200 parts by mass of deionized water, and stirring at 20-25 ℃ for 40-60 min to obtain a polyanion component solution;
step 103, uniformly mixing the chitosan dispersion liquid obtained in the step 101 and the polyanion component solution obtained in the step 102, adding 0.1-0.5 part of melting agent in parts by mass, and stirring at 20-25 ℃ for 10-20 min to obtain a slurry mixed liquid;
step 104, standing the slurry mixed liquor obtained in the step 103 under a vacuum condition for 10min to 20min, pouring the mixture into a mold, exposing the mold in an acid environment, and reacting at the temperature of 20 ℃ to 25 ℃ for 20 to 26h to obtain a polyelectrolyte hydrogel precursor with the thickness of 1mm to 2 mm;
and 105, soaking the polyelectrolyte hydrogel precursor obtained in the step 104 into 200-300 parts of deionized water for 20-24h by mass, removing unreacted melting agent, and drying to obtain the polyelectrolyte hydrogel with the zipper release effect.
Further, the viscosity of the polycationic component chitosan in step 101 is 200-400 mPa.s.
Further, in step 102, the polyanion component is sodium polyacrylate with molecular weight of 2000, sodium hyaluronate with molecular weight of 1900000, or sodium alginate with molecular weight of 110000.
Further, in step 103, the melting agent is glutaraldehyde, malondialdehyde, or glyoxal.
Further, the slurry mixture is allowed to stand under vacuum in step 104, and then poured into a mold having a length × width × height of 5cm × 5cm × 3 cm.
Further, the acidic environment in step 104 is provided by formic acid or acetic acid.
The polyelectrolyte hydrogel based on the zipper-releasing effect is prepared by adopting the preparation method.
An application of polyelectrolyte hydrogel based on a 'unzipping' effect in capturing metal ions.
Further, 0.5 to 4 parts by mass of polyelectrolyte hydrogel with the zipper release effect is added into 100 parts of aqueous solution containing metal ions, and after adsorption and capture are carried out for 0.5 to 2 hours at the temperature of between 20 and 25 ℃, the polyelectrolyte hydrogel with the zipper release effect is separated.
Further, the metal ion is Cr3+、Fe3+Or Pb2+。
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, chitosan is used as a polycation component, sodium alginate, sodium polyacrylate or sodium hyaluronate is used as a polyanion component, the structure of the chitosan is very compact and is similar to a closed zipper (figure 1), and on the basis, glutaraldehyde, malondialdehyde or glyoxal is added, and micromolecular dialdehyde can perform Schiff base reaction with amino in a chitosan structure, so that two chitosan chains are crosslinked, and the originally compact zipper structure is loose. On one hand, the polyelectrolyte hydrogel with the zipper-releasing effect (figure 2) enables a large number of functional groups of carboxyl (-COOH) in the polyanion component to be exposed, and the functional groups can generate coordination with metal ions, thereby greatly improving the adsorption and capture efficiency; on the other hand, the space network structure of the 'unzipping' effect can endow the metal ion with larger specific surface area and excellent swelling performance, and can further improve the active capture capacity of the metal ion.
2. Compared with the traditional grafting, modification and other modes for improving the capture efficiency of the hydrogel material on the metal ions in the solution, the 'unzipping' strategy provided by the invention can greatly simplify the synthesis steps, is suitable for popularization, and opens up a new way for efficiently treating the metal ions in the solution.
Drawings
FIG. 1 is a schematic representation of a closed zipper structure of a polyelectrolyte hydrogel of the invention;
FIG. 2 is a schematic view of the structure of polyelectrolyte hydrogel with "unzipping" effect according to the present invention.
Detailed Description
Embodiments of the invention are described in further detail below:
a preparation method of polyelectrolyte hydrogel based on 'unzipping' effect comprises the following steps:
step 101, dispersing 2-8 parts of polycation component chitosan in 100-200 parts of deionized water by mass, and stirring for 40-60 min at 20-25 ℃ to obtain chitosan dispersion liquid; wherein the viscosity of the polycation component chitosan is 200-400 mPa.s;
102, dissolving 2-8 parts of polyanion component in 200 parts of deionized water by mass, and stirring for 40-60 min at 20-25 ℃ to obtain a polyanion component solution; the polyanion component is sodium polyacrylate with molecular weight of 2000, sodium hyaluronate with molecular weight of 1900000 or sodium alginate with molecular weight of 110000;
step 103, uniformly mixing the polycation component chitosan dispersion liquid obtained in the step 101 and the polyanion component solution obtained in the step 102, adding 0.1-0.5 part of melting agent by mass, wherein the melting agent is glutaraldehyde, malonaldehyde or glyoxal, and stirring for 10-20 min at 20-25 ℃ to obtain slurry mixed liquid;
step 104, standing the slurry mixed solution obtained in the step 103 under a vacuum condition for 10min to 20min, pouring the mixture into a mold with the length multiplied by the width multiplied by the height multiplied by 5cm multiplied by 3cm, exposing the mold in an acid environment (the acid environment is provided by formic acid or acetic acid), and reacting for 20 to 26h at the temperature of 20 ℃ to 25 ℃ to obtain a polyelectrolyte hydrogel precursor with the thickness of 1mm to 2 mm;
105, soaking the polyelectrolyte hydrogel precursor obtained in the step 104 into 200-300 parts of deionized water for 20-24 hours by mass, removing unreacted melting agent, and drying to obtain the polyelectrolyte hydrogel with zipper release effect;
the application of polyelectrolyte hydrogel based on the 'unzipping' effect in capturing metal ions comprises the following steps: adding 0.5-4 parts by mass of polyelectrolyte hydrogel with the zipper release effect into 100 parts of aqueous solution containing metal ions, adsorbing and capturing for 0.5-2 hours at the temperature of 20-25 ℃, and separating the polyelectrolyte hydrogel with the zipper release effect; the metal ion is Cr3+、Fe3+Or Pb2+。
The polyelectrolyte hydrogel with the zipper-releasing effect is prepared by using chitosan as a polycation component, sodium alginate, sodium polyacrylate or sodium hyaluronate as a polyanion component and micromolecule glutaraldehyde, malonaldehyde or glyoxal as a cross-linking agent (a melting agent); the polyelectrolyte hydrogel with the zipper release effect is used for adsorbing and capturing metal ions in a solution, and due to the introduction of a melting agent, the original compact zipper structure becomes loose, on one hand, more functional groups of carboxyl (-COOH) are exposed and can generate coordination with the metal ions, and on the other hand, the loose spatial network structure endows the polyelectrolyte hydrogel with the characteristics of larger specific surface area, excellent swelling performance and the like, so that the adsorption and capture efficiency of the metal ions can be greatly improved.
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
Step 1, preparing polyelectrolyte hydrogel with zipper release effect:
step 101, dispersing 2 parts of polycation component chitosan with the viscosity of 200mPa.s in 100 parts of deionized water by mass, and stirring for 40min at the temperature of 20 ℃ to obtain chitosan dispersion liquid;
102, dissolving 2 parts by mass of polyanion component sodium alginate in 100 parts by mass of deionized water, and stirring for 40min at the temperature of 20 ℃ to obtain a sodium alginate solution;
step 103, uniformly mixing the polycation component chitosan dispersion liquid obtained in the step 101 and the sodium alginate solution obtained in the step 102, adding 0.1 part by mass of glutaraldehyde, and stirring at 20 ℃ for 10min to obtain a slurry mixed liquid;
step 104, standing the slurry mixed liquor obtained in the step 103 for 10min under a vacuum condition, pouring the mixture into a mold, exposing the mold in an acetic acid slow-release environment, and reacting for 20h at the temperature of 20 ℃ to obtain a polyelectrolyte hydrogel precursor with the thickness of 1 mm; standing the slurry mixed solution under a vacuum condition, and pouring the slurry mixed solution into a mold, wherein the length, the width and the height of the mold are 5cm, 5cm and 3 cm;
105, soaking the polyelectrolyte hydrogel precursor obtained in the step 104 into 200 parts of deionized water for 20 hours in parts by mass, removing unreacted glutaraldehyde, and then drying to obtain the polyelectrolyte hydrogel with the zipper release effect;
step 2, high-efficiency capture of metal ions in the solution:
counting the mass parts of the components, namely the components obtained in the step 1 have the zipper-releasing effect0.5 part of polyelectrolyte hydrogel is added into 100 parts of the polyelectrolyte hydrogel containing Cr3+In an ionic water solution, adsorbing and capturing for 2 hours at the temperature of 20 ℃, and separating the polyelectrolyte hydrogel with the zipper release effect; the polyelectrolyte hydrogel with the zipper release effect is applied to Cr3+The adsorption-trapping ratio of (2) was 98%.
Example 2
Step 1, preparing polyelectrolyte hydrogel with zipper release effect:
step 101, dispersing 8 parts of polycation component chitosan with the viscosity of 300mPa.s in 200 parts of deionized water by mass, and stirring for 60min at the temperature of 25 ℃ to obtain chitosan dispersion liquid;
102, dissolving 8 parts by mass of polyanionic component sodium hyaluronate into 200 parts by mass of deionized water, and stirring for 60min at 25 ℃ to obtain a sodium hyaluronate solution;
step 103, uniformly mixing the polycation component chitosan dispersion liquid obtained in the step 101 and the sodium hyaluronate solution obtained in the step 102, adding 0.5 part by mass of glyoxal, and stirring at 25 ℃ for 20min to obtain a slurry mixed liquid;
step 104, standing the slurry mixed solution obtained in the step 103 for 20min under a vacuum condition, pouring the mixture into a mold, exposing the mold in a formic acid slow release environment, and reacting for 26h at 25 ℃ to obtain a polyelectrolyte hydrogel precursor with the thickness of 2 mm; standing the slurry mixed solution under a vacuum condition, and pouring the slurry mixed solution into a mold, wherein the length, the width and the height of the mold are 5cm, 5cm and 3 cm;
105, soaking the polyelectrolyte hydrogel precursor obtained in the step 104 in 300 parts of deionized water for 24 hours in parts by mass, removing unreacted glyoxal, and then drying to obtain the polyelectrolyte hydrogel with the zipper release effect;
step 2, efficient capture of metal ions in the solution:
adding 4 parts by mass of the polyelectrolyte hydrogel with the zipper-releasing effect obtained in the step 1 into 100 parts by mass of the polyelectrolyte hydrogel containing Fe3+Aqueous solution of ionsIn the liquid, after adsorbing and capturing for 0.5 hour at the temperature of 25 ℃, separating the polyelectrolyte hydrogel with the zipper release effect; the polyelectrolyte hydrogel with the zipper release effect is used for treating Fe3+The adsorption-trapping ratio of (2) was 99%.
Example 3
Step 1, preparing polyelectrolyte hydrogel with zipper release effect:
step 101, dispersing 4 parts of polycation component chitosan with the viscosity of 400mPa.s in 150 parts of deionized water by mass, and stirring for 50min at the temperature of 22 ℃ to obtain chitosan dispersion liquid;
102, dissolving 4 parts by mass of polyanion component sodium polyacrylate in 150 parts by mass of deionized water, and stirring for 50min at the temperature of 22 ℃ to obtain a sodium polyacrylate solution;
step 103, uniformly mixing the polycation component chitosan dispersion liquid obtained in the step 101 and the sodium polyacrylate solution obtained in the step 102, adding 0.3 part by mass of malondialdehyde, and stirring at 23 ℃ for 15min to obtain a slurry mixed liquid;
step 104, standing the slurry mixed solution obtained in the step 103 for 15min under a vacuum condition, pouring the mixture into a mold, exposing the mold in an acetic acid environment, and reacting for 24h at 23 ℃ to obtain a polyelectrolyte hydrogel precursor with the thickness of 1.5 mm; standing the slurry mixed solution under a vacuum condition, and pouring the slurry mixed solution into a mold, wherein the length, the width and the height of the mold are 5cm, 5cm and 3 cm;
105, soaking the polyelectrolyte hydrogel precursor obtained in the step 104 in 250 parts of deionized water for 22 hours in parts by mass, removing unreacted malondialdehyde, and then drying to obtain the polyelectrolyte hydrogel with the zipper release effect;
step 2, high-efficiency capture of metal ions in the solution:
adding 2 parts by mass of the polyelectrolyte hydrogel with the zipper-releasing effect obtained in the step 1 into 100 parts by mass of Pb-containing hydrogel2+Adsorbing and trapping in ionic water solution at 23 deg.C for 1 hr, and separating "Effective polyelectrolyte hydrogels; the polyelectrolyte hydrogel with the zipper release effect has the effect on Pb2+The adsorption-trapping ratio of (2) was 99%.
Finally, it should be noted that: although the present invention has been described in detail with reference to the above embodiments, those skilled in the art will appreciate that various changes, modifications and equivalents can be made in the embodiments of the invention without departing from the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of polyelectrolyte hydrogel based on 'unzipping' effect is characterized by comprising the following steps:
step 101, dispersing 2-8 parts of polycation component chitosan in 100-200 parts of deionized water by mass, and stirring for 40-60 min at the temperature of 20-25 ℃ to obtain chitosan dispersion liquid;
102, dissolving 2-8 parts of polyanion component in 200 parts of deionized water by mass, and stirring for 40-60 min at 20-25 ℃ to obtain a polyanion component solution;
step 103, uniformly mixing the chitosan dispersion liquid obtained in the step 101 and the polyanion component solution obtained in the step 102, adding 0.1-0.5 part of melting agent in parts by mass, and stirring at 20-25 ℃ for 10-20 min to obtain a slurry mixed liquid;
step 104, standing the slurry mixed liquor obtained in the step 103 under a vacuum condition for 10min to 20min, pouring the mixture into a mold, exposing the mold in an acid environment, and reacting at the temperature of 20 ℃ to 25 ℃ for 20 to 26h to obtain a polyelectrolyte hydrogel precursor with the thickness of 1mm to 2 mm;
and 105, soaking the polyelectrolyte hydrogel precursor obtained in the step 104 into 200-300 parts of deionized water for 20-24h by mass, removing unreacted melting agent, and drying to obtain the polyelectrolyte hydrogel with the zipper release effect.
2. The method as claimed in claim 1, wherein the viscosity of the chitosan polycation component in step 101 is 200-400 mpa.s.
3. The method for preparing polyelectrolyte hydrogel based on the "unzipping" effect according to claim 1, wherein said polyanion component in step 102 is sodium polyacrylate with molecular weight of 2000, sodium hyaluronate with molecular weight of 1900000 or sodium alginate with molecular weight of 110000.
4. The method of claim 1, wherein the melting agent in step 103 is glutaraldehyde, malondialdehyde, or glyoxal.
5. The method of claim 1, wherein the slurry mixture is placed under vacuum and poured into a mold, and the length, width, and height of the mold are 5cm x 3 cm.
6. The method of claim 1, wherein the acidic environment is provided by formic acid or acetic acid in step 104.
7. Polyelectrolyte hydrogel based on the unzipping effect, characterized in that it is prepared by the preparation method according to any one of claims 1-6.
8. Use of a polyelectrolyte hydrogel based on the "unzipping" effect according to claim 7 for capturing metal ions.
9. The application of the polyelectrolyte hydrogel based on the unzipping effect on the metal ion capture as claimed in claim 8, wherein 0.5-4 parts by weight of the polyelectrolyte hydrogel with the unzipping effect is added into 100 parts by weight of the aqueous solution containing metal ions, and after 0.5-2 hours of adsorption capture at 20-25 ℃, the polyelectrolyte hydrogel with the unzipping effect is separated.
10. The use of the polyelectrolyte hydrogel based on the unzipping effect in the trapping solution according to claim 9, wherein the metal ions are Cr3+、Fe3+Or Pb2+。
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