CN107337927A - A kind of graphene oxide with self-repair function/polyamic acid hydrogel and preparation method thereof - Google Patents
A kind of graphene oxide with self-repair function/polyamic acid hydrogel and preparation method thereof Download PDFInfo
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- CN107337927A CN107337927A CN201710529430.6A CN201710529430A CN107337927A CN 107337927 A CN107337927 A CN 107337927A CN 201710529430 A CN201710529430 A CN 201710529430A CN 107337927 A CN107337927 A CN 107337927A
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- 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
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- 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
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- 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
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- 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
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
Abstract
The present invention relates to a kind of graphene oxide with self-repair function/polyamic acid hydrogel and preparation method thereof, composition includes：Graphene oxide, one or more water-soluble polyimide precursor polyamic acids.Preparation includes：Polycondensation prepares polyimides water-soluble precursor polyamic acid, then graphene oxide water solution is mixed with polyamic acid, and graphene oxide/polyamic acid hydrogel is obtained by way of vacuum drying, aging.After the graphene oxide of selfreparing prepared by the present invention/polyamic acid hydrogel damages, renovation agent is done by simple docking or several drip, can repairs breaking part again, remediation efficiency is high, cost is low, multiplicating repair function can be realized in same area, and material can carry out overlength stretching.Script pattern can be recovered by being mixed again with water after material dehydration, reused, be a kind of good self-repair material.
Description
Technical field
The invention belongs to self-repair material and its preparation field, more particularly to a kind of graphite oxide with self-repair function
Alkene/polyamic acid hydrogel and preparation method thereof.
Background technology
Hydrogel is the specific function material with spacial framework that WATER AS FLOW MEDIUM is filled with a kind of structural void.It
There are many similarities in structure and performance with organism soft tissue.It has very strong water holding capacity, even in compression
In the case of be not easy to dehydration, have extensively in fields such as garden craft, physiological hygiene, medicine, artificial organ, petrochemical industry, commodity
Wealthy prospect.
Self-repair material is mainly inspired and produced by the self-healing capability of organism, by introducing reversible hydrogen bond, hydrophobic
Interaction, host-guest interaction, pi-pi accumulation, the method for ionic bond or dynamic reversible chemical bond, assign hydrogel and review one's lessons by oneself
Multiple function, after material receives environmental damage, impaired place can be repaired again, so as to extend the service life of material and set
Standby security performance, widen the potential application foreground of hydrogel.
Polyimides (Polyimide) is that a kind of to have good moulding processability, high mechanical strength, heat endurance good etc. excellent
The special engineering plastics of point, it is widely used in the every field of national economy.Graphene oxide (Graphene Oxide) nanometer
Not only make oxidation containing abundant oxygen-containing functional group, such as carboxyl, hydroxyl, carbonyl and epoxy radicals, these oxygen-containing functional groups on piece
Graphene has good hydrophily, moreover it is possible to as physical crosslinking or the avtive spot of chemical reaction, participates in a variety of physics, chemistry
Reaction, form cross-linked network.Therefore graphene oxide is frequently used to as crosslinking agent and pore regulator.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of graphene oxide/polyamic acid with self-repair function
Hydrogel and preparation method thereof, the rubber pureed that preparation process of the present invention is simple, cost is cheap, to obtain self-healing properties excellent
Graphene oxide/polyamic acid hydrogel.
A kind of graphene oxide with self-repair function/polyamic acid hydrogel of the present invention, hydrogel raw material include
Graphene oxide and one or more water-soluble polyimide precursor-polyamic acids, pass through graphene oxide crosslinked polyamide
Acid obtains hydrogel.
A kind of preparation method of the graphene oxide with self-repair function/polyamic acid hydrogel of the present invention, including：
(1) graphite oxide is dispersed in water, ultrasound, obtains the graphene oxide dispersion of stable dispersion；
(2) water-soluble polyamic acid is dissolved in graphene oxide dispersion, stirs, obtain graphene oxide/polyamide
Acid solution；
(3) above-mentioned graphene oxide/polyamic acid solution is dried, stands, pass through sol-gel process, aging
Obtain graphene oxide/polyamic acid hydrogel.
Graphite oxide is prepared by Hummers methods in the step (1).
The concentration of graphene oxide dispersion is 2-10mg/mL in the step (1).
Contain triethylamine in graphene oxide dispersion in the step (1).
The mass ratio of graphene oxide and polyamic acid is in graphene oxide/polyamic acid solution in the step (2)
2:1~1:8.
Water-soluble polyamic acid is prepared as in the step (2)：First the diamine monomer of synthesis of polyimides is dissolved in
Polar solvent, binary anhydride monomer is added, reacted under ice-water bath, then add triethylamine, continued to react, obtain polyamide
Acid solution, then precipitating, freeze-drying, obtains water-soluble polyamic acid.
The diamine monomer is the one or more in phenylenediamine, 4,4 '-diaminodiphenyl ether；Binary anhydride monomer is equal
PMDA, biphenyl tetracarboxylic dianhydride or diphenyl ether tetracarboxylic dianhydride.
The polar solvent is dimethyl acetamide, 1-METHYLPYRROLIDONE or dimethylformamide.
The precipitating is poured slowly into precipitating in deionized water for polyamic acid solution and obtains polyamic acid fiber.
Drying is in the step (3)：Vacuum drying chamber is dried, and the time is 1~8h, and temperature is 30-80 DEG C.
Time of repose (the sol-gel process time is) is 12~48h in the step (3).
Polycondensation of the present invention prepares polyimides water-soluble precursor-polyamic acid, then by graphene oxide water solution with gathering
Imido water-soluble precursor polyamic acid mixing, graphene oxide/polyamide is obtained by way of vacuum drying, aging
Acid hydrogel.
After the graphene oxide of selfreparing prepared by the present invention/polyamic acid hydrogel damages, by simple
Docking or several drip do renovation agent, it is possible to repair breaking part again, remediation efficiency is high, and cost is low, can be realized in same area
Repair function is repeated several times, and material can carry out overlength stretching.Script shape can be recovered by being mixed again with water after material dehydration
Looks, reuse, be a kind of good self-repair material.
In order to carry out more comprehensively research and experiment to the composite, to the ratio of polyamic acid and graphene oxide
The regulation in respective range has been carried out, has as a result found that the preparation-obtained hydrogel of different embodiments (different proportion) is respectively provided with
Good self-healing properties, tensile property and bending fold performance, the performance no significant difference of gained sample between each embodiment,
Prove that the inspectable space of the method and material on self-healing properties is larger, and have wide range of applications.
Beneficial effect
(1) preparation process of the present invention is simple, environmental protection, easily operated, is a kind of green chemical preparation process；
(2) present invention is ingenious in design：Using friendship of the graphene oxide as polyamic acid for containing abundant oxygen-containing functional group
Join agent, graphene oxide is crosslinked reaction with polyamic acid, assign hydrogel with the function of selfreparing.
Brief description of the drawings
Fig. 1 is the synthesis schematic diagram of water-soluble polyamic acid in the present invention；
Fig. 2 is the selfreparing, stretching and bending photo of graphene oxide/polyamic acid hydrogel of embodiment 1.Wherein scheme
A is one piece of graphene oxide/polyamic acid hydrogel；Figure b is cut to two pieces；It is by the use of water as renovation agent to scheme c, makes two blocks of water
Gel is repaired as one piece again；It is graphene oxide/polyamic acid hydrogel after selfreparing to scheme d；It is the photograph curved it to scheme e
Piece；Figure f is the photo for being stretched to obtain.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
Using DMA as solvent, by equimolar than 4,4 '-diaminodiphenyl ether and terephthalic acid (TPA)
Acid anhydride carries out condensation polymerization reaction in ice-water bath and the polyamic acid that solid content is 15% is prepared.Detailed process is as follows：Will
4.31g4,4 '-diaminodiphenyl ether are dissolved in 51g DMAs, 4.69g terephthalic anhydrides are added, in ice-water bath
Middle reaction 5h.Then, 2.18g triethylamines are added, continue to react 5h, the water-soluble polyamic acid that solid content is 15% is prepared
Solution.By prepared water-soluble polyamic acid deionized water precipitating, then water solubility is obtained by washing and freeze-drying
Polyamic acid fiber is stand-by.
The graphene oxide water solution for the 5mg/mL that 10mL prepared is taken, adds 0.125g triethylamines, ultrasonic 0.5h.Will
0.25g water-soluble polyamic acid fibers are put into the graphene oxide water solution containing triethylamine, and stirring makes its dissolving.By its turn
Move on in a diameter of 3cm container, be put into vacuum drying chamber 60 DEG C, 5h.Then placed 24h and complete sol-gel mistake
Journey, it is 1 that aging, which obtains graphene oxide and polyamic acid mass ratio,:5 graphene oxide/polyamic acid hydrogel, is designated as GO-
PAA-1-5。
Embodiment 2
Graphene oxide in embodiment 1 and the mass ratio of polyamic acid are changed to 1:4, that is, the 5mg/ for taking 5mL to prepare
ML graphene oxide water solution, 0.05g triethylamines are added, ultrasonic 0.5h, 0.1g water-soluble polyamic acid fibers is put into and contained
Have in the graphene oxide water solution of triethylamine, stirring makes its dissolving, and remaining is the same as implementation 1.Final prepared graphene oxide/poly-
Acid amides acid hydrogel, is designated as GO-PAA-1-4.
Embodiment 3
Graphene oxide in embodiment 1 and the mass ratio of polyamic acid are changed to 1:3, that is, the 8mg/ for taking 10mL to prepare
ML graphene oxide water solution, 0.125g triethylamines are added, ultrasonic 0.5h, 0.25g water-soluble polyamic acid fibers are put into
In graphene oxide water solution containing triethylamine, stirring makes its dissolving, remaining same implementation 1, and final prepared graphene oxide/
Polyamic acid hydrogel, is designated as GO-PAA-1-3.
Embodiment 4
Graphene oxide in embodiment 1 and the mass ratio of polyamic acid are changed to 1:2, that is, the 5mg/ for taking 10mL to prepare
ML graphene oxide water solution, 0.05g triethylamines are added, ultrasonic 0.5h, 0.1g water-soluble polyamic acid fibers is put into and contained
Have in the graphene oxide water solution of triethylamine, stirring makes its dissolving, and remaining is the same as implementation 2, final prepared graphene oxide/poly-
Acid amides acid hydrogel, is designated as GO-PAA-1-2.
Embodiment 5
Graphene oxide in embodiment 1 and the mass ratio of polyamic acid are changed to 1:1, that is, the 5mg/ for taking 20mL to prepare
ML graphene oxide water solution, 0.05g triethylamines are added, ultrasonic 0.5h, 0.1g water-soluble polyamic acid fibers is put into and contained
Have in the graphene oxide water solution of triethylamine, stirring makes its dissolving, and remaining is the same as implementation 2, final prepared graphene oxide/poly-
Acid amides acid hydrogel, is designated as GO-PAA-1-1.
Embodiment 6
Graphene oxide in embodiment 1 and the mass ratio of polyamic acid are changed to 2:1, that is, take what 20mL was prepared
10mg/mL graphene oxide water solution, 0.05g triethylamines are added, ultrasonic 0.5h, 0.1g water-soluble polyamic acid fibers are put
Enter in the graphene oxide water solution containing triethylamine, stirring makes its dissolving, and remaining is the same as implementation 2, final prepared graphite oxide
Alkene/polyamic acid hydrogel, is designated as GO-PAA-2-1.
Embodiment 7
Control group.Synthesizing polyamides acid hydrogel, i.e., be not added with graphene oxide during preparation.Take 10mL deionizations
Water and 0.125g triethylamines, ultrasonic 0.5h, 0.25g water-soluble polyamic acid fibers are put into the aqueous solution containing triethylamine,
Stirring makes its dissolving, and remaining final prepared polyamic acid hydrogel, is designated as PAA with implementing 1.
The graphene oxide of gained rubber pureed/polyamic acid hydrogel has excellent self-healing properties, hydrogel hair
After raw damage, breaking part can be repaired again by simple docking or several lubrications dripped, remediation efficiency is high, and cost is low, in phase
Multiplicating repair function can be realized with position.It can still recover script pattern after contacting mixing with water again after material dehydration, can
Reuse, be a kind of good self-repair material on performance without influence.
Claims (10)
- A kind of 1. graphene oxide with self-repair function/polyamic acid hydrogel, it is characterised in that：Hydrogel raw material includes Graphene oxide and polyamic acid, hydrogel is obtained by graphene oxide crosslinked polyamide acid.
- A kind of 2. preparation side of graphene oxide/polyamic acid hydrogel as claimed in claim 1 with self-repair function Method, including：(1) graphite oxide is dispersed in water, ultrasound, obtains graphene oxide dispersion；(2) water-soluble polyamic acid is dissolved in graphene oxide dispersion, stirs, it is molten to obtain graphene oxide/polyamic acid Liquid；(3) above-mentioned graphene oxide/polyamic acid solution is dried, stands, obtain graphene oxide/polyamic acid water-setting Glue.
- A kind of 3. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 2 Method, it is characterised in that：The concentration of graphene oxide dispersion is 2-10mg/mL in the step (1).
- A kind of 4. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 2 Method, it is characterised in that：Contain triethylamine in graphene oxide dispersion in the step (1).
- A kind of 5. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 2 Method, it is characterised in that：Graphene oxide and polyamic acid in graphene oxide/polyamic acid solution in the step (2) Mass ratio is 2:1~1:8.
- A kind of 6. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 2 Method, it is characterised in that：Water-soluble polyamic acid is prepared as in the step (2)：Diamine monomer is dissolved in polar solvent, Binary anhydride monomer is added, is reacted under ice-water bath, then adds triethylamine, continues to react, obtains polyamic acid solution, so Precipitating afterwards, freeze-drying, obtains water-soluble polyamic acid.
- A kind of 7. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 6 Method, it is characterised in that：The diamine monomer is the one or more in phenylenediamine, 4,4 '-diaminodiphenyl ether；Binary acid anhydride Monomer is pyromellitic acid anhydride, biphenyl tetracarboxylic dianhydride or diphenyl ether tetracarboxylic dianhydride.
- A kind of 8. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 6 Method, it is characterised in that：The polar solvent is dimethyl acetamide, 1-METHYLPYRROLIDONE or dimethylformamide.
- A kind of 9. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 2 Method, it is characterised in that：Drying is in the step (3)：Vacuum drying chamber is dried, and the time is 1~8h, and temperature is 30-80 DEG C.
- A kind of 10. preparation of the graphene oxide with self-repair function/polyamic acid hydrogel according to claim 2 Method, it is characterised in that：Time of repose is 12~48h in the step (3).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108546334A (en) * | 2018-05-04 | 2018-09-18 | 东华大学 | A kind of preparation method of the graphene with self-repair function/polyamic acid conductive hydrogel |
| CN110511402A (en) * | 2019-09-12 | 2019-11-29 | 东华大学 | A kind of cobalt cross-linked hydrogel and preparation method thereof with high cross-link intensity |
| CN110620014A (en) * | 2019-09-12 | 2019-12-27 | 东华大学 | Graphene/polyamic acid all-solid-state supercapacitor and preparation method thereof |
| CN112280056A (en) * | 2020-11-06 | 2021-01-29 | 湖南科技大学 | Preparation method of repairable graphene oxide material based on hydrogen bond effect |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108546334A (en) * | 2018-05-04 | 2018-09-18 | 东华大学 | A kind of preparation method of the graphene with self-repair function/polyamic acid conductive hydrogel |
| CN110511402A (en) * | 2019-09-12 | 2019-11-29 | 东华大学 | A kind of cobalt cross-linked hydrogel and preparation method thereof with high cross-link intensity |
| CN110620014A (en) * | 2019-09-12 | 2019-12-27 | 东华大学 | Graphene/polyamic acid all-solid-state supercapacitor and preparation method thereof |
| CN112280056A (en) * | 2020-11-06 | 2021-01-29 | 湖南科技大学 | Preparation method of repairable graphene oxide material based on hydrogen bond effect |
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