CN112321852A - High-strength graphene-polyacrylic acid composite conductive hydrogel and preparation method thereof - Google Patents
High-strength graphene-polyacrylic acid composite conductive hydrogel and preparation method thereof Download PDFInfo
- Publication number
- CN112321852A CN112321852A CN202011291876.8A CN202011291876A CN112321852A CN 112321852 A CN112321852 A CN 112321852A CN 202011291876 A CN202011291876 A CN 202011291876A CN 112321852 A CN112321852 A CN 112321852A
- Authority
- CN
- China
- Prior art keywords
- graphene
- hydrogel
- polyacrylic acid
- heating
- composite conductive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of hydrogel and discloses high-strength graphene-polyacrylic acid composite conductive hydrogel, wherein carboxylated graphene hydrogel and ethylenediamine are subjected to amidation reaction to obtain aminated graphene hydrogel, an oxidation-reduction initiation system is formed by active amino groups of the aminated graphene hydrogel and ammonium persulfate, a large number of active free radicals are formed on the surface of the graphene hydrogel to initiate in-situ graft polymerization of acrylic acid on the graphene hydrogel, and further Fe is used for carrying out in-situ graft polymerization on the acrylic acid3+Forming graphene-polyacrylic acid composite hydrogel, chemical covalent crosslinking of graphene grafting and Fe3+The composite hydrogel forms a dual-network interpenetrating three-dimensional structure by ion crosslinking, so that the excellent tensile strength and elongation at break of the composite hydrogel are obviously improved, and the graphene and the Fe with excellent conductivity are simultaneously used3+Highly dispersed in a composite hydrogel matrix to form a three-dimensional conductive network, and endows the hydrogel with a new function of good conductivity.
Description
Technical Field
The invention relates to the technical field of hydrogel, in particular to high-strength graphene-polyacrylic acid composite conductive hydrogel and a preparation method thereof.
Background
The acrylic acid-based hydrogel has excellent hydrophilicity and water absorbability, has a unique three-dimensional gel structure, can be prepared into an environment-responsive hydrogel composite material, and has wide application in the fields of adsorption, membrane separation, tissue engineering, drug delivery and the like, but the traditional acrylic acid hydrogel has poor mechanical strength and toughness, is easy to damage and break in the long-term use process, and seriously limits the practical application of the acrylic acid hydrogel, so that the improvement of the mechanical property of the acrylic acid hydrogel and the endowment of new functions of the acrylic acid hydrogel, such as electrical conductivity, thermal stability and the like, become research hotspots.
At present, the mechanical property of the hydrogel is improved, modes such as synthesis of topological hydrogel, novel nano composite hydrogel and hydrogel with a double-network structure can be adopted, graphene is a novel reinforcing filler, the graphene has wide application in high polymer materials, and has a strong reinforcing effect on the overall performance of the material, so that the strategy of compounding the graphene and the acrylic-based hydrogel to obtain the nano composite hydrogel with the double-network structure can be adopted, and the overall performances such as the mechanical strength and the electrical conductivity of the hydrogel are improved.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the high-strength graphene-polyacrylic acid composite conductive hydrogel and the preparation method thereof, and solves the problems of poor mechanical strength and toughness of the acrylic hydrogel.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a high-strength graphene-polyacrylic acid composite conductive hydrogel is prepared by the following steps:
(1) and dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain the graphene hydrogel.
(2) Adding a distilled water solvent and graphene hydrogel into a beaker, uniformly dispersing, adding isoamyl nitrite and 4-aminobenzoic acid, placing in a heating reactor, heating to 70-90 ℃, reacting for 12-24h, carrying out suction filtration, washing with ethanol and distilled water, and obtaining the carboxylated graphene hydrogel.
(3) Adding a toluene solvent, carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to the temperature of 100 ℃ and 120 ℃, adding ethylenediamine, reacting for 6-12h, carrying out reduced pressure distillation, and washing with ethanol and distilled water to obtain the aminated graphene hydrogel.
(4) Adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 1-3h at 0-5 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 24-48h, adding ferric nitrate, stirring at a constant speed for 12-24h, performing suction filtration, washing with ethanol and distilled water, and dialyzing to remove impurities to obtain the double-network cross-linked high-strength graphene-polyacrylic acid composite conductive hydrogel.
Preferably, the heating reaction instrument comprises a heating pipe, an oil bath pot is arranged above the heating reaction instrument, a heat preservation layer is fixedly connected to the outer side of the oil bath pot, the heat preservation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, a supporting rod is fixedly connected with the moving rod, the supporting rod is fixedly connected with a clamping plate, and a beaker is arranged between the clamping plates.
Preferably, the mass ratio of the graphene hydrogel in the step (2), isoamyl nitrite and 4-aminobenzoic acid is 10:75-120: 60-100.
Preferably, the mass ratio of the carboxylated graphene, the dicyclohexylcarbodiimide, the 4-dimethylaminopyridine and the ethylenediamine in the step (3) is 10:6-10:2-3.5: 40-80.
Preferably, the mass ratio of the aminated graphene hydrogel in the step (4), acrylic acid, ammonium persulfate and ferric nitrate is 0.2-1:100:2.5-3.5: 800-.
(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-polyacrylic acid composite conductive hydrogel, amino groups of 4-aminobenzoic acid and isoamyl nitrite are subjected to diazotization reaction to obtain a diazobenzoic acid intermediate, diazo groups are unstable and are decomposed by heating, and the diazo groups are removed to enable the diazobenzoic acid intermediate to generate carbonium ions to react with double bonds in an sp2 carbon structure in the graphene hydrogel to obtain carboxylated graphene hydrogel, so that a large number of carboxyl groups are introduced to the surface of graphene, the density and content of the carboxyl groups are far greater than those of the carboxyl groups in graphene oxide, and the carboxylated graphene prepared by the method does not contain oxygen-containing groups such as hydroxyl groups and epoxy groups, and has better conductivity than that of the graphene oxide.
According to the high-strength graphene-polyacrylic acid composite conductive hydrogel, under the activation action of dicyclohexylcarbodiimide and 4-dimethylaminopyridine, amidation reaction is carried out on carboxylated graphene hydrogel and ethylenediamine, the aminated graphene hydrogel is obtained, rich amino groups are introduced, an oxidation-reduction initiation system is formed by active amino groups and ammonium persulfate, a large number of active free radicals are formed on the surface of the graphene hydrogel, in-situ graft polymerization of acrylic acid on the graphene hydrogel is initiated, acrylic acid monomers are diffused to the surface to realize chain growth of polyacrylic acid, the polyacrylic acid is grafted in the graphene hydrogel through micelle nucleation and homogeneous phase nucleation processes, and further Fe is used for further grafting3+Forming graphene-polyacrylic acid composite hydrogel, chemical covalent crosslinking of graphene grafting and Fe3+The ion crosslinking synergistic effect of the compound hydrogel enables the compound hydrogel to form a double-network interpenetrating three-dimensional structure, thereby obviously improving the excellent tensile strength and elongation at break of the compound hydrogel, showing higher mechanical strength and toughness and simultaneously having excellent conductivity of graphene and Fe3+Highly dispersed in a composite hydrogel matrix to form a three-dimensional conductive network, and endows the hydrogel with a new function of good conductivity.
Drawings
FIG. 1 is a schematic view of a heating reactor;
fig. 2 is a schematic view of the adjustment of the travel bar structure.
1-heating the reaction instrument; 2-heating a tube; 3-oil bath pan; 4-an insulating layer; 5-adjusting the nut; 6-moving the rod; 7-a support bar; 8-clamping plate; 9-beaker.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a high-strength graphene-polyacrylic acid composite conductive hydrogel is prepared by the following steps:
(1) and dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain the graphene hydrogel.
(2) Adding distilled water solvent into a beaker, uniformly dispersing the graphene hydrogel, isoamyl nitrite and 4-aminobenzoic acid in a mass ratio of 10:75-120:60-100, and then placing the mixture into a heating reactor, wherein the heating reactor comprises a heating pipe, an oil bath pot is arranged above the heating reactor, the outer side of the oil bath pot is fixedly connected with a heat insulation layer, the inner part of the heat insulation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, the moving rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with clamping plates, the beaker is arranged between the clamping plates, heating is carried out to 70-90 ℃, reacting is carried out for 12-24 hours, and filtering, ethanol and distilled water are washed to obtain the carboxylated graphene hydrogel.
(3) Adding a toluene solvent and carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a mass ratio of 10:6-10:2-3.5:40-80 into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to 100 ℃ and 120 ℃, adding ethylenediamine, reacting for 6-12h, carrying out reduced pressure distillation, and washing with ethanol and distilled water to obtain the aminated graphene hydrogel.
(4) Adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 1-3h at 0-5 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 24-48h, and adding ferric nitrate, wherein the mass ratio of the aminated graphene hydrogel to the acrylic acid to the ammonium persulfate to the ferric nitrate is 0.2-1:100:2.5-3.5:800 and 1200, stirring for 12-24h at a constant speed, performing suction filtration, washing with ethanol and distilled water, and dialyzing to remove impurities, thereby obtaining the double-network crosslinked high-strength graphene-polyacrylic acid composite conductive hydrogel.
Example 1
(1) And dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain the graphene hydrogel.
(2) Adding a distilled water solvent, namely graphene hydrogel, isoamyl nitrite and 4-aminobenzoic acid in a mass ratio of 10:75:60 into a beaker, uniformly dispersing, and then placing the mixture into a heating reactor, wherein the heating reactor comprises a heating pipe, an oil bath pot is arranged above the heating reactor, the outer side of the oil bath pot is fixedly connected with a heat insulation layer, the inner part of the heat insulation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, the moving rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with clamping plates, the position between the clamping plates is provided with the beaker, heating is carried out to 70 ℃, reacting is carried out for 12 hours, and filtering, ethanol and distilled water are washed to.
(3) Adding a toluene solvent and carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a mass ratio of 10:6:2:40 into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to 100 ℃, adding ethylenediamine, reacting for 6 hours, carrying out reduced pressure distillation, washing with ethanol and distilled water, and obtaining the aminated graphene hydrogel.
(4) Adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 1h at 0 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 24h, and adding ferric nitrate, wherein the mass ratio of the aminated graphene hydrogel to the acrylic acid to the ammonium persulfate to the ferric nitrate is 0.2:100:2.5:800, stirring at a constant speed for 12h, performing suction filtration, washing with ethanol and distilled water, and dialyzing to remove impurities to obtain the double-network crosslinked high-strength graphene-polyacrylic acid composite conductive hydrogel.
Example 2
(1) And dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain the graphene hydrogel.
(2) Adding a distilled water solvent, graphene hydrogel, isoamyl nitrite and 4-aminobenzoic acid in a mass ratio of 10:90:70 into a beaker, uniformly dispersing, and then placing the mixture into a heating reactor, wherein the heating reactor comprises a heating pipe, an oil bath pot is arranged above the heating reactor, the outer side of the oil bath pot is fixedly connected with a heat insulation layer, the inner part of the heat insulation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, the moving rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with clamping plates, the beaker is arranged between the clamping plates, heating is carried out to 90 ℃, reacting for 18 hours, carrying out suction filtration, washing with ethanol and distilled water, and obtaining the carboxylated graphene.
(3) Adding a toluene solvent and carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a mass ratio of 10:7:2.5:50 into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to 110 ℃, adding ethylenediamine, reacting for 12 hours, carrying out reduced pressure distillation, washing with ethanol and distilled water, and obtaining the aminated graphene hydrogel.
(4) Adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 2h at 2 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 36h, and adding ferric nitrate, wherein the mass ratio of the aminated graphene hydrogel to the acrylic acid to the ammonium persulfate to the ferric nitrate is 0.4:100:2.8:900, stirring at a constant speed for 24h, carrying out suction filtration, washing with ethanol and distilled water, and dialyzing to remove impurities, thereby obtaining the double-network crosslinked high-strength graphene-polyacrylic acid composite conductive hydrogel.
Example 3
(1) And dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain the graphene hydrogel.
(2) Adding a distilled water solvent, graphene hydrogel, isoamyl nitrite and 4-aminobenzoic acid in a mass ratio of 10:105:85 into a beaker, uniformly dispersing, and then placing into a heating reactor, wherein the heating reactor comprises a heating pipe, an oil bath pot is arranged above the heating reactor, the outer side of the oil bath pot is fixedly connected with a heat insulation layer, the inner part of the heat insulation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, the moving rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with clamping plates, the beaker is arranged between the clamping plates, heating is carried out to 80 ℃, reacting for 18 hours, carrying out suction filtration, washing with ethanol and distilled water, and obtaining the carboxylated graphene hydrogel.
(3) Adding a toluene solvent and carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a mass ratio of 10:8.5:3:70 into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to 110 ℃, adding ethylenediamine, reacting for 10 hours, carrying out reduced pressure distillation, washing with ethanol and distilled water, and obtaining the aminated graphene hydrogel.
(4) Adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 2h at 2 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 36h, and adding ferric nitrate, wherein the mass ratio of the aminated graphene hydrogel to the acrylic acid to the ammonium persulfate to the ferric nitrate is 0.7:100:3.2:1100, stirring at a constant speed for 18h, performing suction filtration, washing with ethanol and distilled water, and dialyzing to remove impurities, thereby obtaining the double-network crosslinked high-strength graphene-polyacrylic acid composite conductive hydrogel.
Example 4
(1) And dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain the graphene hydrogel.
(2) Adding a distilled water solvent, graphene hydrogel, isoamyl nitrite and 4-aminobenzoic acid in a mass ratio of 10:120:100 into a beaker, uniformly dispersing, and then placing the mixture into a heating reactor, wherein the heating reactor comprises a heating pipe, an oil bath pot is arranged above the heating reactor, the outer side of the oil bath pot is fixedly connected with a heat insulation layer, the inner part of the heat insulation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, the moving rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with clamping plates, the beaker is arranged between the clamping plates, heating is carried out to 90 ℃, reacting for 24 hours, carrying out suction filtration, washing with ethanol and distilled water, and obtaining the carboxylated graphene.
(3) Adding a toluene solvent and carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a mass ratio of 10:10:3.5:80 into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to 120 ℃, adding ethylenediamine, reacting for 12 hours, carrying out reduced pressure distillation, washing with ethanol and distilled water, and obtaining the aminated graphene hydrogel.
(4) Adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 3h at 5 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 48h, and adding ferric nitrate, wherein the mass ratio of the aminated graphene hydrogel to the acrylic acid to the ammonium persulfate to the ferric nitrate is 1:100:3.5:1200, stirring at a constant speed for 24h, performing suction filtration, washing with ethanol and distilled water, and removing impurities by dialysis to obtain the double-network cross-linked high-strength graphene-polyacrylic acid composite conductive hydrogel.
Comparative example 1
(1) And dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain the graphene hydrogel.
(2) Adding a distilled water solvent, graphene hydrogel, isoamyl nitrite and 4-aminobenzoic acid in a mass ratio of 10:60:50 into a beaker, uniformly dispersing, and then placing into a heating reactor, wherein the heating reactor comprises a heating pipe, an oil bath pot is arranged above the heating reactor, the outer side of the oil bath pot is fixedly connected with a heat insulation layer, the inner part of the heat insulation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, the moving rod is fixedly connected with a supporting rod, the supporting rod is fixedly connected with clamping plates, the beaker is arranged between the clamping plates, heating is carried out to 80 ℃, reacting for 20 hours, carrying out suction filtration, washing with ethanol and distilled water, and obtaining the carboxylated graphene hydrogel.
(3) Adding a toluene solvent and carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine in a mass ratio of 10:4:1.5:30 into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to 110 ℃, adding ethylenediamine, reacting for 12 hours, carrying out reduced pressure distillation, washing with ethanol and distilled water, and obtaining the aminated graphene hydrogel.
(4) Adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 2h at 2 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 48h, and adding ferric nitrate, wherein the mass ratio of the aminated graphene hydrogel to the acrylic acid to the ammonium persulfate to the ferric nitrate is 0.08:100:2:600, stirring at a constant speed for 18h, performing suction filtration, washing with ethanol and distilled water, and removing impurities by dialysis to obtain the double-network cross-linked high-strength graphene-polyacrylic acid composite conductive hydrogel.
The tensile strength and the elongation at break of the composite conductive hydrogel are tested by using an SHK-A101 electronic universal material testing machine.
The conductivity of the composite conductive hydrogel was tested using a DDB-303A portable conductivity meter.
Claims (5)
1. A high-strength graphene-polyacrylic acid composite conductive hydrogel is characterized in that: the preparation method of the high-strength graphene-polyacrylic acid composite conductive hydrogel comprises the following steps:
(1) dispersing graphene in distilled water, and placing the graphene in a reaction kettle for hydrothermal reaction to obtain graphene hydrogel;
(2) adding a distilled water solvent and graphene hydrogel into a beaker, uniformly dispersing, adding isoamyl nitrite and 4-aminobenzoic acid, placing in a heating reactor, heating to 70-90 ℃, and reacting for 12-24h to obtain carboxylated graphene hydrogel;
(3) adding a toluene solvent, carboxylated graphene, dicyclohexylcarbodiimide and 4-dimethylaminopyridine into a beaker, uniformly dispersing, placing the mixture into a heating reactor, heating the mixture to the temperature of 100 ℃ and 120 ℃, adding ethylenediamine, and reacting for 6-12h to obtain aminated graphene hydrogel;
(4) adding a distilled water solvent and aminated graphene hydrogel into a beaker, adding acrylic acid after uniform dispersion, stirring for 1-3h at 0-5 ℃ in a nitrogen atmosphere, adding an initiator ammonium persulfate, reacting for 24-48h, adding ferric nitrate, and stirring at a constant speed for 12-24h to obtain the double-network cross-linked high-strength graphene-polyacrylic acid composite conductive hydrogel.
2. The high-strength graphene-polyacrylic acid composite conductive hydrogel according to claim 1, wherein: the heating reaction instrument comprises a heating pipe, an oil bath pot is arranged above the heating reaction instrument, a heat preservation layer is fixedly connected to the outer side of the oil bath pot, the inside of the heat preservation layer is movably connected with an adjusting nut, the adjusting nut is movably connected with a moving rod, a supporting rod is fixedly connected with the moving rod, the supporting rod is fixedly connected with a clamping plate, and a beaker is arranged between the clamping plates.
3. The high-strength graphene-polyacrylic acid composite conductive hydrogel according to claim 1, wherein: the mass ratio of the graphene hydrogel in the step (2), isoamyl nitrite and 4-aminobenzoic acid is 10:75-120: 60-100.
4. The high-strength graphene-polyacrylic acid composite conductive hydrogel according to claim 1, wherein: the mass ratio of the carboxylated graphene, the dicyclohexylcarbodiimide, the 4-dimethylaminopyridine and the ethylenediamine in the step (3) is 10:6-10:2-3.5: 40-80.
5. The high-strength graphene-polyacrylic acid composite conductive hydrogel according to claim 1, wherein: the mass ratio of the aminated graphene hydrogel in the step (4), the acrylic acid, the ammonium persulfate and the ferric nitrate is 0.2-1:100:2.5-3.5: 800-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011291876.8A CN112321852A (en) | 2020-11-18 | 2020-11-18 | High-strength graphene-polyacrylic acid composite conductive hydrogel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011291876.8A CN112321852A (en) | 2020-11-18 | 2020-11-18 | High-strength graphene-polyacrylic acid composite conductive hydrogel and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112321852A true CN112321852A (en) | 2021-02-05 |
Family
ID=74322658
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011291876.8A Withdrawn CN112321852A (en) | 2020-11-18 | 2020-11-18 | High-strength graphene-polyacrylic acid composite conductive hydrogel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112321852A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457737A (en) * | 2021-06-30 | 2021-10-01 | 深圳齐锂纳米科技有限公司 | Preparation method of catalytic hydrogenation catalyst for double-network graphene hydrogel |
| CN113930055A (en) * | 2021-11-04 | 2022-01-14 | 合肥晋怡科技有限公司 | Preparation method of anti-lightning antistatic epoxy resin |
| CN114409950A (en) * | 2021-12-14 | 2022-04-29 | 徐州飞云泡沫制品有限责任公司 | High-conductivity graphene modified polystyrene foam board and preparation method thereof |
| CN114437369A (en) * | 2021-12-17 | 2022-05-06 | 晋江瑞碧科技有限公司 | Polyacrylic acid/graphene grafted polyaniline interpenetrating network hydrogel and preparation method of electrode thereof |
| CN114685817A (en) * | 2022-05-11 | 2022-07-01 | 武夷学院 | Preparation method and application of polyacrylic acid/nitrogen and sulfur co-doped graphene interpenetrating network polymer hydrogel |
-
2020
- 2020-11-18 CN CN202011291876.8A patent/CN112321852A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457737A (en) * | 2021-06-30 | 2021-10-01 | 深圳齐锂纳米科技有限公司 | Preparation method of catalytic hydrogenation catalyst for double-network graphene hydrogel |
| CN113930055A (en) * | 2021-11-04 | 2022-01-14 | 合肥晋怡科技有限公司 | Preparation method of anti-lightning antistatic epoxy resin |
| CN114409950A (en) * | 2021-12-14 | 2022-04-29 | 徐州飞云泡沫制品有限责任公司 | High-conductivity graphene modified polystyrene foam board and preparation method thereof |
| CN114437369A (en) * | 2021-12-17 | 2022-05-06 | 晋江瑞碧科技有限公司 | Polyacrylic acid/graphene grafted polyaniline interpenetrating network hydrogel and preparation method of electrode thereof |
| CN114437369B (en) * | 2021-12-17 | 2023-08-22 | 武夷学院 | Preparation method of polyacrylic acid/graphene grafted polyaniline interpenetrating network hydrogel and electrode thereof |
| CN114685817A (en) * | 2022-05-11 | 2022-07-01 | 武夷学院 | Preparation method and application of polyacrylic acid/nitrogen and sulfur co-doped graphene interpenetrating network polymer hydrogel |
| CN114685817B (en) * | 2022-05-11 | 2023-07-28 | 武夷学院 | Preparation method and application of polyacrylic acid/nitrogen-sulfur co-doped graphene interpenetrating network polymer hydrogel |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112321852A (en) | High-strength graphene-polyacrylic acid composite conductive hydrogel and preparation method thereof | |
| CN108516538B (en) | Preparation method of pi-bond and covalent-bond orderly-crosslinked superstrong high-conductivity graphene composite film | |
| CN110256694A (en) | A kind of stretchable electrically conducting transparent hydrogel and preparation method thereof | |
| CN109847602B (en) | Method for in-situ preparation of metal organic framework hybrid membrane and application of metal organic framework hybrid membrane | |
| CN112403282A (en) | Amphiphilic polypropylene porous membrane and preparation method and application thereof | |
| CN111592050A (en) | Biomass-based porous carbon in-situ growth nano Fe3O4Wave-absorbing material and preparation method thereof | |
| CN109233527B (en) | Preparation method of modified graphene/acrylate composite water-based paint | |
| Ding et al. | Properties of polyacrylamide hydrogel enhanced by kaolinite with expanded layer structure | |
| CN112863893B (en) | Composite biochar-based material, and preparation method and application thereof | |
| CN111584243B (en) | Mn (manganese)3O4-carbon nano tube-polyaniline super capacitor material and preparation method thereof | |
| CN113346097B (en) | Preparation method of graphite-based composite material bipolar plate for proton exchange membrane fuel cell | |
| CN115347203A (en) | Method for enhancing conductive carbon black conductive capacity and application of method in ORR catalyst | |
| CN1673272A (en) | Hydrophilic porous PTFE film and its production process | |
| CN114373935B (en) | Negative electrode binder for lithium battery, negative electrode, and lithium battery | |
| CN113843271B (en) | Main-auxiliary multi-electrode Cr (VI) contaminated soil remediation method based on ternary auxiliary electrode | |
| CN112607733A (en) | Preparation method and application of polymer-based nitrogen and phosphorus doped graphitized porous carbon | |
| CN114068893A (en) | Composite material and preparation method and application thereof | |
| CN111268673A (en) | Preparation method of supercapacitor electrode material taking foamed nickel as template | |
| CN112430338A (en) | High-strength graphene chemically-crosslinked polyacrylamide hydrogel and preparation method thereof | |
| CN113782751B (en) | Preparation method of high-flexibility carbon/resin composite material | |
| CN107799785B (en) | Bacterial cellulose membrane-based bipolar plate and preparation method thereof | |
| CN115999520B (en) | Method for preparing pH response lignin-based adsorbent | |
| CN116454307B (en) | Manufacturing method of composite graphite bipolar plate for fuel cell | |
| CN117410513B (en) | Flexible composite graphite bipolar plate and preparation method thereof | |
| CN108914556A (en) | A kind of antistatic finish technique of plasma modification sofa fabric |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20210205 |
|
| WW01 | Invention patent application withdrawn after publication |