CN112430338A - High-strength graphene chemically-crosslinked polyacrylamide hydrogel and preparation method thereof - Google Patents
High-strength graphene chemically-crosslinked polyacrylamide hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of hydrogel, and discloses high-strength graphene chemically-crosslinked polyacrylamide hydrogel, under the concerted catalysis of cuprous bromide and N, N, N, N, N-pentamethyldiethylenetriamine, side chain alkynyl of acrylamide hydrogel and azide groups of graphene generate efficient alkyne-azide click reaction, thereby taking the graphene as a chemical crosslinking center, covalently grafting the polyacrylamide hydrogel on the surface of the graphene, improving the interface acting force and compatibility of the graphene and the polyacrylamide hydrogel, overcoming the problems of poor dispersibility and easy occurrence of agglomeration of the graphene, taking the graphene as the chemical crosslinking center, the method has great improvement effect on the tensile strength and the elongation at break of the polyacrylamide hydrogel, so that the polyacrylamide hydrogel has higher mechanical strength and toughness.
Description
Technical Field
The invention relates to the technical field of hydrogel, in particular to high-strength graphene chemically-crosslinked polyacrylamide hydrogel and a preparation method thereof.
Background
The hydrogel is a structural gel with a three-dimensional network, has strong hydrophilicity and water absorption, can rapidly swell in water, contains a large amount of water, can be divided into natural hydrogel and synthetic hydrogel, such as chitosan hydrogel, sodium alginate hydrogel, polyacrylic acid hydrogel, polyacrylamide hydrogel and the like, and can be obtained by chemical crosslinking or physical crosslinking, and the hydrogel has high water absorption and high water retention characteristics, so that the hydrogel has important application in aspects of cosmetic masks, medical drug carriers, tissue engineering and the like.
Graphene oxide is a two-dimensional carbon nanomaterial and has the characteristics of large specific surface area, stable chemical properties, strong mechanical properties and the like, and the graphene oxide matrix and the edge contain a large number of oxygen-containing functional groups such as hydroxyl, carboxyl, epoxy and the like, so that the graphene oxide is considered to be a nano filler capable of effectively improving the comprehensive performance of polymer materials such as hydrogel and the like, has wide research and application prospects, can further introduce active groups to avoid the problems of poor agglomeration and dispersibility of the graphene oxide, can be organically combined with polymer materials such as polyurethane, epoxy resin, polyacrylamide and the like in a covalent bond grafting or non-covalent bond modification mode, overcomes the problems of agglomeration and poor dispersibility, and becomes a research focus and hot spot for carrying out surface modification on the graphene oxide.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a high-strength graphene chemically-crosslinked polyacrylamide hydrogel and a preparation method thereof, and solves the problem that the traditional acrylamide hydrogel is poor in mechanical strength and toughness.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a high strength graphene chemically cross-linked polyacrylamide hydrogel: the preparation method of the high-strength graphene chemically-crosslinked polyacrylamide hydrogel is as follows:
(1) and (2) carrying out acyl chlorination modification on graphene oxide by using thionyl chloride, placing the modified graphene oxide in a constant-temperature reactor, heating and reacting at 60-80 ℃ in the nitrogen atmosphere, carrying out reduced pressure distillation, washing and purifying to obtain the acyl chlorinated graphene.
(2) Placing 2-azido ethanol and acyl chloride graphene in a constant temperature reactor, heating at 80-110 ℃ in a nitrogen atmosphere for reaction, filtering, washing and purifying to obtain azido graphene.
(3) In a nitrogen atmosphere, adding acrylamide and propinyl acrylate into a deionized water solvent, slowly dropwise adding an initiator potassium persulfate, placing the mixture into a constant-temperature reactor, heating the mixture to 50-70 ℃ in the nitrogen atmosphere, reacting for 20-40min, adding a crosslinking agent N, N' -methylene bisacrylamide, reacting for 2-4h, then reacting for 18-36h at 25-35 ℃, filtering, washing, dialyzing and purifying to obtain the side chain alkynyl-containing acrylamide hydrogel.
(4) Adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding a catalyst and a ligand, reacting at 40-60 ℃ for 24-48h in a nitrogen atmosphere, adding deionized water to separate out a precipitate, filtering, washing, dialyzing and purifying to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
Preferably, the constant temperature reactor in step (1) includes the water bath reaction chamber, and water bath reaction chamber both sides fixedly connected with heating plate, the inside below of water bath reaction chamber are provided with the base, and the base top is provided with the bracing piece, bracing piece and adjusting screw swing joint, bracing piece fixedly connected with expanding spring, expanding spring and cardboard fixedly connected with, cardboard swing joint has the reaction bottle.
Preferably, the mass ratio of the 2-azido ethanol to the acylchlorinated graphene in the step (2) is 40-100: 10.
Preferably, the mass ratio of the acrylamide, the propinyl acrylate, the potassium persulfate and the N, N' -methylene-bisacrylamide in the step (3) is 100:1-4:0.2-0.5: 0.15-0.4.
Preferably, the catalyst in the step (4) is cuprous bromide, and the ligand is N, N, N, N, N-pentamethyldiethylenetriamine.
Preferably, the mass ratio of the side chain alkynyl-containing acrylamide hydrogel in the step (4), the azide graphene, the cuprous bromide and the N, N, N, N, N-pentamethyldiethylenetriamine is 100:0.5-2:2-4: 2.5-6.
Drawings
FIG. 1 is a schematic view of the structure of a constant temperature reactor;
figure 2 is a schematic diagram of card adjustment.
1-constant temperature reactor; 2-a water bath reaction chamber; 3-heating a sheet; 4-a base; 5-a support rod; 6-adjusting a screw rod; 7-a telescopic spring; 8-clamping plate; 9-reaction flask.
(III) advantageous technical effects
Compared with the prior art, the invention has the following chemical mechanism and beneficial technical effects:
according to the high-strength graphene chemically-crosslinked polyacrylamide hydrogel, acyl chloride groups are introduced into a graphene oxide matrix and further subjected to esterification reaction with 2-azido ethanol, so that azido groups are introduced, functional modification of graphene oxide is realized, acrylamide and propargyl acrylate containing alkynyl are copolymerized to obtain acrylamide hydrogel containing alkynyl groups on side chains, under the synergistic catalytic action of cuprous bromide and N, N, N, N, N-pentamethyldiethylenetriamine, the alkynyl groups on the side chains of the acrylamide hydrogel and the azido groups of graphene are subjected to efficient alkyne-azide click reaction, so that the graphene is used as a chemical crosslinking center, the polyacrylamide hydrogel is subjected to covalent grafting on the surface of the graphene, and the interfacial force and compatibility of the graphene and the polyacrylamide hydrogel are remarkably improved, therefore, the problems that graphene is poor in dispersity and easy to agglomerate are solved, the graphene is used as a chemical crosslinking center, the tensile strength and the elongation at break of the polyacrylamide hydrogel are greatly improved, and the polyacrylamide hydrogel has higher mechanical strength and toughness.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a preparation method of a high-strength graphene chemically-crosslinked polyacrylamide hydrogel is as follows:
(1) the method comprises the steps of carrying out acyl chlorination modification on graphene oxide by using thionyl chloride, arranging the modified graphene oxide in a constant temperature reactor, wherein the constant temperature reactor comprises a water bath reaction chamber, heating pieces are fixedly connected to two sides of the water bath reaction chamber, a base is arranged below the inner portion of the water bath reaction chamber, a supporting rod is arranged above the base, the supporting rod is movably connected with an adjusting screw rod, an expansion spring is fixedly connected with the supporting rod, the expansion spring is fixedly connected with a clamping plate, the clamping plate is movably connected with a reaction bottle, heating reaction is carried out at 60-80 ℃ under the nitrogen atmosphere, reduced pressure distillation and washing purification are carried out.
(2) Placing 2-azido ethanol and acyl chloride graphene in a mass ratio of 40-100:10 in a constant temperature reactor, heating at 80-110 ℃ in a nitrogen atmosphere for reaction, filtering, washing and purifying to obtain the azido graphene.
(3) Adding acrylamide and propynyl acrylate into a deionized water solvent in a nitrogen atmosphere, slowly dropwise adding an initiator potassium persulfate, placing the mixture into a constant-temperature reactor, heating the mixture to 50-70 ℃ in the nitrogen atmosphere, reacting for 20-40min, adding a crosslinking agent N, N '-methylene bisacrylamide, reacting for 2-4h, wherein the mass ratio of the acrylamide to the propynyl acrylate to the potassium persulfate to the N, N' -methylene bisacrylamide is 100:1-4:0.2-0.5:0.15-0.4, reacting for 18-36h at 25-35 ℃, filtering, washing, dialyzing and purifying to obtain the side chain alkynyl-containing acrylamide hydrogel.
(4) Adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding cuprous bromide serving as a catalyst and N, N, N, N, N-pentamethyldiethylenetriamine serving as a ligand in a mass ratio of 100:0.5-2:2-4:2.5-6, reacting for 24-48h at 40-60 ℃ in a nitrogen atmosphere, adding deionized water to precipitate, filtering, washing, dialyzing and purifying to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
Example 1
(1) Use thionyl chloride to carry out acyl chlorination modification to graphene oxide, arrange the isothermal reactor in, the isothermal reactor includes the water bath reaction chamber, water bath reaction chamber both sides fixedly connected with heating plate, the inside below of water bath reaction chamber is provided with the base, the base top is provided with the bracing piece, bracing piece and adjusting screw swing joint, bracing piece fixedly connected with expanding spring, expanding spring and cardboard fixedly connected with, cardboard swing joint has the reaction bottle, under nitrogen atmosphere, heating reaction under 60 ℃, reduced pressure distillation and washing purification obtain acyl chlorination graphene.
(2) Placing 2-azido ethanol and acyl chloride graphene in a mass ratio of 40:10 into a constant temperature reactor, heating at 80 ℃ in a nitrogen atmosphere for reaction, filtering, washing and purifying to obtain azido graphene.
(3) Adding acrylamide and propynyl acrylate into a deionized water solvent in a nitrogen atmosphere, slowly dropwise adding an initiator potassium persulfate, placing the mixture into a constant-temperature reactor, heating the mixture to 50 ℃ in the nitrogen atmosphere, reacting for 20min, adding a crosslinking agent N, N' -methylene bisacrylamide, reacting for 2h, reacting for 18h at 25 ℃, filtering, washing, dialyzing and purifying to obtain the side chain alkynyl-containing acrylamide hydrogel.
(4) Adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding cuprous bromide serving as a catalyst and N, N, N, N, N-pentamethyldiethylenetriamine serving as a ligand in a mass ratio of 100:0.5:2:2.5, reacting for 24 hours at 40 ℃ in a nitrogen atmosphere, adding deionized water to precipitate, filtering, washing, dialyzing and purifying to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
Example 2
(1) Use thionyl chloride to carry out acyl chlorination modification to graphene oxide, arrange the isothermal reactor in, the isothermal reactor includes the water bath reaction chamber, water bath reaction chamber both sides fixedly connected with heating plate, the inside below of water bath reaction chamber is provided with the base, the base top is provided with the bracing piece, bracing piece and adjusting screw swing joint, bracing piece fixedly connected with expanding spring, expanding spring and cardboard fixedly connected with, cardboard swing joint has the reaction bottle, under nitrogen atmosphere, heating reaction under 80 ℃, reduced pressure distillation and washing purification obtain acyl chlorination graphene.
(2) Placing 2-azido ethanol and acyl chloride graphene with the mass ratio of 65:10 in a constant temperature reactor, heating at 110 ℃ in a nitrogen atmosphere for reaction, filtering, washing and purifying to obtain azido graphene.
(3) Adding acrylamide and propynyl acrylate into a deionized water solvent in a nitrogen atmosphere, slowly dropwise adding an initiator potassium persulfate, placing the mixture into a constant-temperature reactor, heating the mixture to 60 ℃ in the nitrogen atmosphere, reacting for 40min, adding a crosslinking agent N, N' -methylene bisacrylamide, reacting for 3h, reacting for 36h at 30 ℃, filtering, washing, dialyzing and purifying to obtain the side chain alkynyl-containing acrylamide hydrogel.
(4) Adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding cuprous bromide serving as a catalyst and N, N, N, N, N-pentamethyldiethylenetriamine serving as a ligand in a mass ratio of 100:1:3:4, reacting for 36 hours at 60 ℃ in a nitrogen atmosphere, adding deionized water to precipitate, filtering, washing, dialyzing and purifying to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
Example 3
(1) Use thionyl chloride to carry out acyl chlorination modification to graphene oxide, arrange the isothermal reactor in, the isothermal reactor includes the water bath reaction chamber, water bath reaction chamber both sides fixedly connected with heating plate, the inside below of water bath reaction chamber is provided with the base, the base top is provided with the bracing piece, bracing piece and adjusting screw swing joint, bracing piece fixedly connected with expanding spring, expanding spring and cardboard fixedly connected with, cardboard swing joint has the reaction bottle, under nitrogen atmosphere, heating reaction under 80 ℃, reduced pressure distillation and washing purification obtain acyl chlorination graphene.
(2) Placing 2-azido ethanol and acyl chloride graphene in a mass ratio of 100:10 in a constant temperature reactor, heating at 110 ℃ in a nitrogen atmosphere for reaction, filtering, washing and purifying to obtain azido graphene.
(3) Adding acrylamide and propynyl acrylate into a deionized water solvent in a nitrogen atmosphere, slowly dropwise adding an initiator potassium persulfate, placing the mixture into a constant-temperature reactor, heating the mixture to 70 ℃ in the nitrogen atmosphere, reacting for 40min, adding a crosslinking agent N, N' -methylene bisacrylamide, reacting for 4h, reacting for 36h at 35 ℃, filtering, washing, dialyzing and purifying to obtain the side chain alkynyl-containing acrylamide hydrogel.
(4) Adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding cuprous bromide serving as a catalyst and N, N, N, N, N-pentamethyldiethylenetriamine serving as a ligand in a mass ratio of 100:2:4:6, reacting for 48 hours at 60 ℃ in a nitrogen atmosphere, adding deionized water to precipitate, filtering, washing, dialyzing and purifying to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
Comparative example 1
(1) Use thionyl chloride to carry out acyl chlorination modification to graphene oxide, arrange the isothermal reactor in, the isothermal reactor includes the water bath reaction chamber, water bath reaction chamber both sides fixedly connected with heating plate, the inside below of water bath reaction chamber is provided with the base, the base top is provided with the bracing piece, bracing piece and adjusting screw swing joint, bracing piece fixedly connected with expanding spring, expanding spring and cardboard fixedly connected with, cardboard swing joint has the reaction bottle, under nitrogen atmosphere, heating reaction under 80 ℃, reduced pressure distillation and washing purification obtain acyl chlorination graphene.
(2) Placing 2-azido ethanol and acyl chloride graphene in a mass ratio of 20:10 into a constant temperature reactor, heating at 110 ℃ in a nitrogen atmosphere for reaction, filtering, washing and purifying to obtain azido graphene.
(3) Adding acrylamide and propynyl acrylate into a deionized water solvent in a nitrogen atmosphere, slowly dropwise adding an initiator potassium persulfate, placing the mixture into a constant-temperature reactor, heating the mixture to 50 ℃ in the nitrogen atmosphere, reacting for 40min, adding a crosslinking agent N, N' -methylene bisacrylamide, reacting for 3h, reacting for 36h at 30 ℃, filtering, washing, dialyzing and purifying to obtain the side chain alkynyl-containing acrylamide hydrogel.
(4) Adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding cuprous bromide serving as a catalyst and N, N, N, N, N-pentamethyldiethylenetriamine serving as a ligand in a mass ratio of 100:0.2:1.5:2, reacting for 24 hours at 50 ℃ in a nitrogen atmosphere, adding deionized water to precipitate, filtering, washing, dialyzing and purifying to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
Comparative example 2
(1) Use thionyl chloride to carry out acyl chlorination modification to graphene oxide, arrange the isothermal reactor in, the isothermal reactor includes the water bath reaction chamber, water bath reaction chamber both sides fixedly connected with heating plate, the inside below of water bath reaction chamber is provided with the base, the base top is provided with the bracing piece, bracing piece and adjusting screw swing joint, bracing piece fixedly connected with expanding spring, expanding spring and cardboard fixedly connected with, cardboard swing joint has the reaction bottle, under nitrogen atmosphere, heating reaction under 70 ℃, reduced pressure distillation and washing purification obtain acyl chlorination graphene.
(2) Placing 2-azido ethanol and acyl chloride graphene with the mass ratio of 130:10 in a constant temperature reactor, heating at 100 ℃ in a nitrogen atmosphere for reaction, filtering, washing and purifying to obtain azido graphene.
(3) Adding acrylamide and propynyl acrylate into a deionized water solvent in a nitrogen atmosphere, slowly dropwise adding an initiator potassium persulfate, placing the mixture into a constant-temperature reactor, heating the mixture to 60 ℃ in the nitrogen atmosphere, reacting for 40min, adding a crosslinking agent N, N '-methylene bisacrylamide, reacting for 4h, wherein the mass ratio of the acrylamide to the propynyl acrylate to the potassium persulfate to the N, N' -methylene bisacrylamide is 100:5.5:0.65:0.6, reacting for 24h at 30 ℃, filtering, washing, dialyzing and purifying to obtain the side chain alkynyl-containing acrylamide hydrogel.
(4) Adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding cuprous bromide serving as a catalyst and N, N, N, N, N-pentamethyldiethylenetriamine serving as a ligand in a mass ratio of 100:3:5:7, reacting for 24 hours at 60 ℃ in a nitrogen atmosphere, adding deionized water to precipitate, filtering, washing, dialyzing and purifying to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
The tensile strength and the elongation at break of the high-strength graphene chemically-crosslinked polyacrylamide hydrogel are tested by using a CBW-2T microcomputer control electronic universal tester, and the test standard is GB/T1040.3-2006.
Claims (6)
1. A high-strength graphene chemically crosslinked polyacrylamide hydrogel is characterized in that: the preparation method of the high-strength graphene chemically-crosslinked polyacrylamide hydrogel is as follows:
(1) performing acyl chlorination modification on graphene oxide by using thionyl chloride, placing the modified graphene oxide in a constant-temperature reactor, and heating and reacting at 60-80 ℃ in the nitrogen atmosphere to obtain acyl chlorinated graphene;
(2) placing 2-azido ethanol and acyl chloride graphene in a constant-temperature reactor, and heating at 80-110 ℃ in a nitrogen atmosphere for reaction to obtain azido graphene;
(3) in a nitrogen atmosphere, adding acrylamide and propinyl acrylate into a deionized water solvent, slowly dropwise adding an initiator potassium persulfate, placing the mixture in a constant-temperature reactor, heating the mixture to 50-70 ℃ in the nitrogen atmosphere, reacting for 20-40min, adding a crosslinking agent N, N' -methylene bisacrylamide, reacting for 2-4h, and then reacting for 18-36h at 25-35 ℃ to obtain side chain alkynyl-containing acrylamide hydrogel;
(4) adding side chain alkynyl-containing acrylamide hydrogel and graphene azide into an N, N-dimethylformamide solvent, uniformly dispersing, adding a catalyst and a ligand, and reacting at 40-60 ℃ for 24-48h in a nitrogen atmosphere to obtain the high-strength graphene chemically-crosslinked polyacrylamide hydrogel.
2. The high-strength graphene chemically crosslinked polyacrylamide hydrogel according to claim 1, wherein: the constant temperature reactor in step (1) comprises a water bath reaction chamber, heating sheets are fixedly connected to two sides of the water bath reaction chamber, a base is arranged below the inner portion of the water bath reaction chamber, a supporting rod is arranged above the base and is movably connected with an adjusting screw rod, an expansion spring is fixedly connected with the supporting rod, the expansion spring is fixedly connected with a clamping plate, and a reaction bottle is movably connected with the clamping plate.
3. The high-strength graphene chemically crosslinked polyacrylamide hydrogel according to claim 1, wherein: the mass ratio of the 2-azido ethanol to the acylchlorinated graphene in the step (2) is 40-100: 10.
4. The high-strength graphene chemically crosslinked polyacrylamide hydrogel according to claim 1, wherein: the mass ratio of the acrylamide, the propinyl acrylate, the potassium persulfate and the N, N' -methylene bisacrylamide in the step (3) is 100:1-4:0.2-0.5: 0.15-0.4.
5. The high-strength graphene chemically crosslinked polyacrylamide hydrogel according to claim 1, wherein: and (4) cuprous bromide is used as a catalyst, and N, N, N, N-pentamethyldiethylenetriamine is used as a ligand.
6. The high-strength graphene chemically crosslinked polyacrylamide hydrogel according to claim 1, wherein: the mass ratio of the side chain alkynyl-containing acrylamide hydrogel in the step (4) to the N, N, N, N, N-pentamethyldiethylenetriamine is 100:0.5-2:2-4: 2.5-6.
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| CN116813273A (en) * | 2023-06-19 | 2023-09-29 | 湖北路城建设科技有限公司 | Slag soil type building rubbish regenerated stone plate and preparation method thereof |
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| CN116813273A (en) * | 2023-06-19 | 2023-09-29 | 湖北路城建设科技有限公司 | Slag soil type building rubbish regenerated stone plate and preparation method thereof |
| CN116813273B (en) * | 2023-06-19 | 2024-03-19 | 湖北路城建设科技有限公司 | Slag soil type building rubbish regenerated stone plate and preparation method thereof |
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Application publication date: 20210302 |