CN102580633B - Preparation method of graphene oxide/poly(N-isopropylacrylamide) composite hydrogel - Google Patents
Preparation method of graphene oxide/poly(N-isopropylacrylamide) composite hydrogel Download PDFInfo
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- CN102580633B CN102580633B CN201110458092.4A CN201110458092A CN102580633B CN 102580633 B CN102580633 B CN 102580633B CN 201110458092 A CN201110458092 A CN 201110458092A CN 102580633 B CN102580633 B CN 102580633B
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Abstract
The invention discloses a preparation method of graphene oxide/poly(N-isopropylacrylamide) composite hydrogel. The preparation method comprises the steps of: firstly, placing the graphene oxide in water and ultrasonically dispersing the graphene oxide for 30-60 min to obtain a graphene oxide colloidal solution; then adding N-isopropylacrylamide, a cross-linking agent and an initiator 1 in the graphene oxide colloidal solution; stirring for dissolving so as to obtain a mixed solution; then inflating nitrogen in the mixed solution to deoxidize fully, then adding an initiator 2 in the deoxidized mixed solution, mixing uniformly and placing the mixture in a thermostatic water bath at 25+/-1 DEG C so as to obtain the graphene oxide/poly(N-isopropylacrylamide) composite hydrogel. The graphene oxide/poly(N-isopropylacrylamide) composite hydrogel prepared by the method disclosed by the invention has the advantages of good temperature responsiveness and mechanical property and wide application prospect in the biomedical field (such as tissue engineering and drug controlled release).
Description
Technical field
The preparation method who the present invention relates to a kind of graphene oxide/NIPA composite aquogel, belongs to material technology field.
Background technology
Intelligent aqueous gel capable is that a class stimulates (as temperature, pH value, solvent, salinity, optical, electrical etc.) can produce the hydrogel of responsive response to external world.Due to its unique stimulating responsive, especially bio-medical field (as aspects such as fixing, the organizational project of bio-sensing, molecular separation, organized enzyme, artificial muscle, pharmaceutical carriers) has critical role and unique applications in a lot of fields, paid close attention to widely.Wherein Thermo-sensitive NIPA (PNIPAM) hydrogel is because its volume phase transition temperature is of greatest concern near human normal physiological temp.But the poor mechanical property of traditional large scale PNIPAM hydrogel (macroscopic hydroge1s) when solvent swelling state, matter is crisp frangible, thereby has greatly limited its application.In order to improve the mechanical strength of hydrogel, researcher has done some research work, as strengthened the intensity of gel network by introduce the inorganic matters such as clay in polymer network; Structure has the hydrogel of rule structure; Form complete inierpeneirating network structure (full-IPN) or half interpenetrating network structure (Semi-IPN) hydrogel.But the research about graphene oxide (GO) enhancing PNIPAM hydrogel rarely has report so far.
Graphene is the carbon nanocapsule thin film material of two-dimensional structure, it is several microns that its thickness only has 0.34nm left and right, lamella width, almost completely transparent, there is the specific area of good electric conductivity, heat conductivility and super large, be the known the highest material of intensity at present.Since the employing micromechanics stripping methods such as British scientist Andre Geim in 2004 obtain Graphene first, because its performance with many uniquenesses becomes the focus that many field scientists pay close attention to very soon.Graphene oxide (GO) is part sp
2the networks of carbon atoms of hydridization is destroyed, in structure with the Graphene of hydroxyl, epoxy radicals and carboxyl isoreactivity group.With Graphene ratio, although the electrical properties of graphene oxide, mechanical property and thermal property decrease, but oxygen-content active group wherein makes it have better modifiability, in water and many organic solvents, can form stable dispersion liquid, and graphene oxide is that chemical stripping legal system is for the intermediate material of Graphene, easily obtain, therefore as macromolecular material nanometer reinforced modifier, graphene oxide has vast potential for future development.
Summary of the invention
Based on above-mentioned research background, the invention provides a kind of preparation method of graphene oxide/NIPA composite aquogel.
Its technical solution is:
A preparation method for graphene oxide/NIPA composite aquogel, it comprises the following steps:
(1) graphite oxide is placed in to water, ultrasonic dispersion 30～60min, obtains graphene oxide colloidal solution;
(2) in the graphene oxide colloidal solution obtaining in step (1), add NIPA, crosslinking agent, initator 1, stirring and dissolving, obtains mixed solution;
(3) in the mixed solution obtaining in step (2), be filled with nitrogen with abundant deoxygenation, in the mixed solution of removing after oxygen, add initator 2 again, fully mix, be placed in 25 ± 1 ℃ of constant temperature water baths, isothermal reaction 12 hours, obtains graphene oxide/NIPA composite aquogel.
In step (1), the mass concentration of graphene oxide colloidal solution is 0.003～0.03mg/L, is preferably 0.003～0.017mg/L.
In above-mentioned steps, the mass ratio of graphene oxide and NIPA is 1%～50%, is preferably 1%～30%.
In step (2), crosslinking agent is N, N '-methylene-bisacrylamide or multicondensed ethylene glycol diacrylate or Polyethylene glycol dimethacrylate, and the consumption of crosslinking agent is 2～5% of NIPA quality, is preferably 3～4%.
In step (2), initator 1 is sodium sulfite or sodium hydrogensulfite, and the consumption of initator 1 is 0.5～2% of NIPA quality, is preferably 1%.
In step (3), initator 2 is potassium peroxydisulfate or ammonium persulfate aqueous solution, and the consumption of potassium peroxydisulfate or ammonium persulfate is 0.5～2% of NIPA quality, is preferably 1%.
In step (1), selected graphite oxide makes according to the following steps: the mixture of 360mL sulfuric acid and 40mL phosphoric acid is added in 3.0g crystalline flake graphite and 18.0g potassium permanganate mixture, be warming up to 50 ℃, stir 12h, then reactant is cooled to room temperature, pours into and contain 3mL30%H
2o
2400mL frozen water in, centrifugation, centrifugal speed 4000rpm, remove supernatant, solids is used respectively 200mL water washing, centrifugation, 200mL 30%NCl washing, centrifugation, the washing of 200mL ethanol, centrifugation, finally obtain graphite oxide by the solid matter freeze drying obtaining.
Useful technique effect of the present invention is:
Graphene oxide/NIPA composite aquogel that the present invention makes has good temperature-responsive and mechanical property, and in bio-medical field, (as the aspects such as controlled release of organizational project, medicine) has wide practical use.
The specific embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, below the preferred embodiments of the present invention are described in detail.
Embodiment 1
The mixture of 360mL sulfuric acid and 40mL phosphoric acid is added in 3.0g crystalline flake graphite and 18.0g potassium permanganate mixture, be warming up to 50 ℃, stir 12h, then reactant is cooled to room temperature, pour into and contain 3mL30%H
2o
2400mL frozen water in, centrifugation, centrifugal speed 4000rpm, remove supernatant, solids is used respectively 200mL water washing, centrifugation, 200mL 30%NCl washing, centrifugation, the washing of 200mL ethanol, centrifugation, finally obtain graphite oxide by the solid matter freeze drying obtaining.
Get 0.0067g graphite oxide, 12mL water adds respectively in 15mL reaction tube, puts into the ultrasonic dispersion of ultrasonator 30 minutes; Then in reaction tube, add respectively 0.6750gN-N-isopropylacrylamide, 0.0270gN, N '-methylene-bisacrylamide, 0.0067g sodium sulfite, stirring and dissolving; Toward inflated with nitrogen in reaction tube, to remove oxygen, after abundant deoxygenation, with rubber stopper, reaction tube is sealed; In reaction tube, add persulfate aqueous solution again, persulfate aqueous solution is that 0.0067g potassium peroxydisulfate is dissolved in 2mL water and makes, then reaction tube is put into 25 ± 1 ℃ of constant temperature water baths and reacted 12 hours, obtain graphene oxide/NIPA composite aquogel.
Embodiment 2
Repeat embodiment 1, difference is: the addition of graphite oxide is 0.0335g.
Embodiment 3
Repeat embodiment 1, difference is: the addition of graphite oxide is 0.0670g, ultrasonic dispersion 45min.
Embodiment 4
Repeat embodiment 1, difference is: the addition of graphite oxide is 0.0945g, ultrasonic dispersion 45min.
Embodiment 5
Repeat embodiment 1, difference is: the addition of graphite oxide is 0.1350g, ultrasonic dispersion 45min.
Embodiment 6
Repeat embodiment 1, difference is: the addition of graphite oxide is 0.2025g, ultrasonic dispersion 60min.
Embodiment 7
Repeat embodiment 1, difference is: the addition of graphite oxide is 0.2700g, ultrasonic dispersion 60min.
Embodiment 8
Repeat embodiment 1, difference is: the addition of graphite oxide is 0.3375g, ultrasonic dispersion 60min.
Comparative example 1
By 0.6750gN-N-isopropylacrylamide, 0.0270gN, N '-methylene-bisacrylamide, 0.0067g sodium sulfite and 12mL water add in 15mL reaction tube, stirring and dissolving; Toward inflated with nitrogen in reaction tube, to remove oxygen, after abundant deoxygenation, with rubber stopper, reaction tube is sealed; In reaction tube, add persulfate aqueous solution again, persulfate aqueous solution is that 0.0067g potassium peroxydisulfate is dissolved in 2mL water and makes, then reaction tube is put into 25 ± 1 ℃ of constant temperature water baths and reacted 12 hours, obtain NIPA hydrogel.
In above embodiment and comparative example, volume phase transition temperature, equilibrium swelling ratio and the compressive strength of gained hydrogel listed in respectively table 1.
Table 1
Comparative example 1, for not adding the situation of graphite oxide, in embodiment 1～8, all adds graphite oxide.As can be seen from the table when the mass ratio of graphene oxide and NIPAM is less than 30: 100, the compressive strength of gained graphene oxide/NIPA hydrogel is all higher than the compressive strength of NIPA hydrogel, anti-compression properties is better, especially embodiment 1～5, and anti-compression properties is obviously better than comparative example 1.In addition, embodiment compares with the obtained hydrogel of comparative example, and volume phase transition temperature improves, and more approaches human normal physiological temp, is conducive to the application of biomedical aspect.
In order to make experimental result there is contrast, thereby further illustrate the present invention, the uniformity of the conservation condition of trying one's best in above embodiment.Certainly in the specific embodiment of the invention, also comprise following embodiment.
Embodiment 9
The preparation method of graphite oxide is with embodiment 1.Get 0.0067g graphite oxide, 12mL water adds respectively in 15mL reaction tube, puts into the ultrasonic dispersion of ultrasonator 30 minutes; Then in reaction tube, add respectively 0.6750gN-N-isopropylacrylamide, 0.0135g multicondensed ethylene glycol diacrylate, 0.0067g sodium sulfite, stirring and dissolving; Toward inflated with nitrogen in reaction tube, to remove oxygen, after abundant deoxygenation, with rubber stopper, reaction tube is sealed; In reaction tube, add persulfate aqueous solution again, persulfate aqueous solution is that 0.0067g potassium peroxydisulfate is dissolved in 2mL water and makes, then reaction tube is put into 25 ± 1 ℃ of constant temperature water baths and reacted 12 hours, obtain graphene oxide/NIPA composite aquogel.
Embodiment 10
The preparation method of graphite oxide is with embodiment 1.Get 0.0067g graphite oxide, 12mL water adds respectively in 15mL reaction tube, puts into the ultrasonic dispersion of ultrasonator 45 minutes; Then in reaction tube, add respectively 0.6750gN-N-isopropylacrylamide, 0.0337g Polyethylene glycol dimethacrylate, 0.0034g sodium hydrogensulfite, stirring and dissolving; Toward inflated with nitrogen in reaction tube, to remove oxygen, after abundant deoxygenation, with rubber stopper, reaction tube is sealed; In reaction tube, add persulfate aqueous solution again, persulfate aqueous solution is that 0.0067g potassium peroxydisulfate is dissolved in 2mL water and makes, then reaction tube is put into 25 ± 1 ℃ of constant temperature water baths and reacted 12 hours, obtain graphene oxide/NIPA composite aquogel.
Embodiment 11
The preparation method of graphite oxide is with embodiment 1.Get 0.0670g graphite oxide, 12mL water adds respectively in 15mL reaction tube, puts into the ultrasonic dispersion of ultrasonator 60 minutes; Then in reaction tube, add respectively 0.6750gN-N-isopropylacrylamide, 0.0337g Polyethylene glycol dimethacrylate, 0.0034g sodium hydrogensulfite, stirring and dissolving; Toward inflated with nitrogen in reaction tube, to remove oxygen, after abundant deoxygenation, with rubber stopper, reaction tube is sealed; In reaction tube, add persulfate aqueous solution again, persulfate aqueous solution is that 0.0337g ammonium persulfate is dissolved in 2mL water and makes, then reaction tube is put into 25 ± 1 ℃ of constant temperature water baths and reacted 12 hours, obtain graphene oxide/NIPA composite aquogel.
Embodiment 12
The preparation method of graphite oxide is with embodiment 1.Get 0.135g graphite oxide, 12mL water adds respectively in 15mL reaction tube, puts into the ultrasonic dispersion of ultrasonator 30 minutes; Then in reaction tube, add respectively 0.6750gN-N-isopropylacrylamide, 0.0135g multicondensed ethylene glycol diacrylate, 0.0067g sodium hydrogensulfite, stirring and dissolving; Toward inflated with nitrogen in reaction tube, to remove oxygen, after abundant deoxygenation, with rubber stopper, reaction tube is sealed; In reaction tube, add persulfate aqueous solution again, persulfate aqueous solution is that 0.0034g ammonium persulfate is dissolved in 2mL water and makes, then reaction tube is put into 25 ± 1 ℃ of constant temperature water baths and reacted 12 hours, obtain graphene oxide/NIPA composite aquogel.
Claims (4)
1. a preparation method for graphene oxide/NIPA composite aquogel, is characterized in that comprising the following steps:
(1) graphite oxide is placed in to water, ultrasonic dispersion 30～60min, obtains graphene oxide colloidal solution;
(2) in the graphene oxide colloidal solution obtaining in step (1), add NIPA, crosslinking agent, initator 1, stirring and dissolving, obtains mixed solution;
(3) in the mixed solution obtaining in step (2), be filled with nitrogen with abundant deoxygenation, in the mixed solution of removing after oxygen, add initator 2 again, fully mix, be placed in 25 ± 1 ℃ of constant temperature water baths, isothermal reaction 12 hours, obtains graphene oxide/NIPA composite aquogel;
Crosslinking agent is N, N '-methylene-bisacrylamide or multicondensed ethylene glycol diacrylate or Polyethylene glycol dimethacrylate, and the consumption of crosslinking agent is 2～5% of NIPA quality;
Initator 1 is sodium sulfite or sodium hydrogensulfite, and the consumption of initator 1 is 0.5～2% of NIPA quality;
Initator 2 is potassium peroxydisulfate or ammonium persulfate aqueous solution, and the consumption of potassium peroxydisulfate or ammonium persulfate is 0.5～2% of NIPA quality.
2. the preparation method of a kind of graphene oxide/NIPA composite aquogel according to claim 1, is characterized in that: the mass concentration of graphene oxide colloidal solution is 0.003～0.03mg/L.
3. the preparation method of a kind of graphene oxide/NIPA composite aquogel according to claim 1, is characterized in that: the mass ratio of graphene oxide and NIPA is 1%～50%.
4. the preparation method of a kind of graphene oxide/NIPA composite aquogel according to claim 1, it is characterized in that described graphite oxide makes according to the following steps: the mixture of 360mL sulfuric acid and 40mL phosphoric acid is added in 3.0g crystalline flake graphite and 18.0g potassium permanganate mixture, be warming up to 50 ℃, stir 12h, then reactant is cooled to room temperature, pours into and contain 3mL30%H
2o
2400mL frozen water in, centrifugation, centrifugal speed 4000rpm, remove supernatant, solids is used respectively 200mL water washing, centrifugation, 200mL30%HCl washing, centrifugation, the washing of 200mL ethanol, centrifugation, finally obtain graphite oxide by the solid matter freeze drying obtaining.
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