CN110105592A - A kind of preparation method of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel - Google Patents
A kind of preparation method of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
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- 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
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- C08J2329/00—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 at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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Abstract
The invention discloses a kind of preparation methods of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel.The specific steps of the preparation method are as follows: be first add to deionized water polyvinyl alcohol, 90-100 DEG C of heating and stirring and dissolving, obtain polyvinyl alcohol water solution, it is naturally cooling to room temperature, then it is kept stirring, in 0-5 DEG C of addition graphene oxide water solution, it is slow added into pyrrole monomer, ammonium persulfate solution then is added dropwise, continues to stir, mixture is cast in mold, after freezing, it takes out to place at room temperature and thaw, freeze-thaw circulation number is 4-7 times, finally obtains high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel.Polyvinyl alcohol-graphene oxide-polypyrrole composite hydrogel disclosed by the invention has excellent mechanical strength, and polyvinyl alcohol-graphene oxide-polypyrrole composite hydrogel preparation method is simple, without complex device, organic solvent, no pollution to the environment are not needed.
Description
Technical field
The present invention relates to a kind of preparation methods of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, belong to
In Functionally structure field.
Background technique
The polymer composites that conductive hydrogel is made of the conductive component containing high hydrated polymer network.It is conductive
Hydrogel is up-and-coming candidate material in biomedicine field.Because they show characteristic similar with soft tissue, such as
Flexibility, ductility and high-moisture.Conductive hydrogel has wide range of applications, such as artificial-muscle, cartilage, electronic skin and life
There is extensive application in object sensor.
Polyvinyl alcohol is the water-soluble polymer obtained after Polymerization of Vac through alkali catalyzed alcoholysis, very due to its toxicity
It is low and nonirritant, it has been applied to medicine and food industry in China.Contain great amount of hydroxy group on polyvinyl alcohol molecule chain, therefore poly-
Vinyl alcohol has good water-soluble, oil resistivity and solvent resistance.Polyvinyl alcohol can also pass through physical crosslinking other than easily forming a film
Method, chemical crosslink technique and radiation cross-linking process synthetic hydrogel, wherein physical crosslinking method is to study a kind of more mechanism at present, it can
The mechanical performance of hydrogel is improved using circulating frozen-defrosting method.Prepare the conduction with high-intensitive and chemical property
Hydrogel is one of the important topic in current conducting polymer field.She X report has directly synthesized polypyrrole-graphene oxide
Hydrogel [Journal of Inorganic and Organometallic Polymers and Materials, 2014,24
(5):884-889.].However, polypyrrole-graphene oxide hydrogel brittleness is big, poor mechanical property, therefore it is necessary to exploitation
A kind of simple and environmentally-friendly method prepares high-intensitive conductive composite hydrogel.
Summary of the invention
To overcome above-mentioned the shortcomings of the prior art, the purpose of the present invention is to provide a kind of poly- second of high intensity
Enol-graphene oxide-polypyrrole composite hydrogel preparation method.The high-strength polyethylene being prepared by the method
Alcohol-graphene oxide-polypyrrole composite hydrogel has excellent mechanical property, and preparation method is simple, sets without complexity
It is standby, do not need organic solvent, no pollution to the environment.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of preparation method of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, which is characterized in that
The following steps are included:
1) polyvinyl alcohol that alcoholysis degree is 85%-99% is add to deionized water, is heated to 90-100 DEG C and stirs
It makes it dissolve, cooled to room temperature obtains polyvinyl alcohol water solution, is kept stirring；
2) under the conditions of 0-5 DEG C of ice bath, first by polyvinyl alcohol water solution made from graphene oxide water solution and step 1)
Mixing, is slow added into pyrrole monomer, continues to stir, ammonium persulfate solution is then added dropwise, and continues to stir 0.5-2h, obtain poly-
Vinyl alcohol-graphene oxide-polypyrrole prepolymer；
3) polyvinyl alcohol-graphene oxide obtained by step 2)-polypyrrole prepolymer freezing is thawed again, recycles 4-7 times, obtains
Hydrogel；
4) the obtained hydrogel of step 3) was finally obtained into high-strength polyethylene with deionized water washing by soaking 2-6 days
Alcohol-graphene oxide-polypyrrole composite hydrogel.
According to the above scheme, it is preferable that the amount ratio of polyvinyl alcohol described in step 1) and the deionized water is 0.05~
0.2g:1mL.
According to the above scheme, it is preferable that the concentration of graphene oxide water solution described in step 2) is 2~4mg/mL；It is described
The concentration of ammonium persulfate solution is 0.01-0.1g/mL.
According to the above scheme, it is preferable that graphene oxide water solution described in polyvinyl alcohol described in step 1) and step 2),
Ammonium persulfate solution, pyrrole monomer amount ratio be (0.5g-1.5g): (2mL-20mL): (1mL-10mL): (60 μ L-180 μ
L)。
According to the above scheme, it is preferable that the temperature of freezing described in step 3) is -40 DEG C to -20 DEG C, and the time of freezing is 5-
15h。
According to the above scheme, it is preferable that the temperature of defrosting described in step 3) is room temperature (20-25 DEG C).
Compared with prior art, the present invention has following prominent effect:
1) interaction of hydrogen bond between polyvinyl alcohol, graphene oxide and polypyrrole, graphene oxide and polypyrrole it
Between conjugation so that composite hydrogel have good mechanical property and electric property；
2) content of graphene oxide is added by changing, the mechanical strength of composite hydrogel can be regulated and controled；
3) convenient experimental operation, process is environmentally protective, and experimental raw is safe and non-toxic and simple and easy to get.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
A kind of preparation of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, the specific steps are as follows:
1) polyvinyl alcohol that 1.5g alcoholysis degree is 99% is added in 20mL deionized water, 95 DEG C are heated and stirred molten
Solution, obtains polyvinyl alcohol water solution, is naturally cooling to room temperature, obtain the polyvinyl alcohol water solution of homogeneous transparent, be kept stirring；
2) under the conditions of 4 DEG C of ice bath, 20mL (concentration 2mg/mL) graphene oxide water solution is added obtained by step 1)
Polyvinyl alcohol water solution (being kept stirring) in, mixing, be slow added into 180 μ L pyrrole monomers, continue to stir, then dropwise plus
Enter 4mL (concentration 0.06g/mL) ammonium persulfate solution, stirs 1h, obtain polyvinyl alcohol-graphene oxide-polypyrrole pre-polymerization
Object；
3) polyvinyl alcohol-graphene oxide-polypyrrole prepolymer obtained by step 2) is cast in 25mL beaker, be placed in-
40 DEG C of freezing 14h take out to place at room temperature from beaker and thaw, freeze-thaw circulation 4 times, obtain primary polyvinyl alcohol-oxidation
Graphene-polypyrrole composite hydrogel；
4) finally by obtained primary polyvinyl alcohol-graphene oxide-polypyrrole composite hydrogel 500mL deionization
Water washing by soaking 3 days, finally obtain high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel.
High strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel made from the present embodiment is taken, diameter, which is made, is
3cm, it is highly the sample of 8cm, carries out compression with microcomputer controlled electronic universal tester and restore experiment, the results show that when compresses
When strain is 50%, corresponding stress is 16.6KPa.
High strength poly vinyl alcohol-graphene oxide made from the present embodiment-polypyrrole composite hydrogel is taken to carry out tabletting, system
Standby to go forward side by side the experiment of line cyclic voltammetry at working electrode, electrolyte is the sulfuric acid of 1mol/L, measurement voltage range is-
0.6V to 0.4V, sweep speed 5mVs-1.Measure polyvinyl alcohol-graphene oxide-polypyrrole Compound Water made from the present embodiment
The specific capacitance of gel is 151.2Fg-1。
Embodiment 2
A kind of preparation of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, the specific steps are as follows:
1) polyvinyl alcohol that 1.0g alcoholysis degree is 88% is added in 20mL deionized water, 95 DEG C are heated and stirred molten
Solution, obtains polyvinyl alcohol water solution, is naturally cooling to room temperature, obtain the polyvinyl alcohol water solution of homogeneous transparent, be kept stirring；
2) under the conditions of 5 DEG C of ice bath, it is resulting that step 1) is added in 5mL (concentration 4mg/mL) graphene oxide water solution
In polyvinyl alcohol water solution (being kept stirring), mixing is slow added into 120 μ L pyrrole monomers, continues to stir, then be added dropwise
7mL (concentration 0.05g/mL) ammonium persulfate solution stirs 0.5h, obtains polyvinyl alcohol-graphene oxide-polypyrrole pre-polymerization
Object；
3) polyvinyl alcohol-graphene oxide-polypyrrole prepolymer obtained by step 2) is cast in 25mL beaker, be placed in-
25 DEG C of freezing 5h take out to place at room temperature from beaker and thaw, and freeze-thaw follows 5 times, obtains primary polyvinyl alcohol-graphite oxide
Alkene-polypyrrole composite hydrogel；
4) finally by obtained primary polyvinyl alcohol-graphene oxide-polypyrrole composite hydrogel 500mL deionization
Water washing by soaking 2 days, finally obtain high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel.
High strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel made from the present embodiment is tested, is surveyed
When proper compression strain is 50%, corresponding stress is 7.1KPa；When Electrochemical Scanning rate is 5mVs-1When, specific capacitance is
109Fg-1。
Embodiment 3
A kind of preparation of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, the specific steps are as follows:
1) polyvinyl alcohol that 1.0g alcoholysis degree is 85% is added in 10mL ionized water, 95 DEG C are heated and stirred molten
Solution, obtains polyvinyl alcohol water solution, is naturally cooling to room temperature, obtain the polyvinyl alcohol water solution of homogeneous transparent, be kept stirring；
2) under the conditions of 3 DEG C of ice bath, it is resulting that step 1) is added in 9mL (concentration 3mg/mL) graphene oxide water solution
In polyvinyl alcohol water solution (being kept stirring), mixing is slow added into 120 μ L pyrrole monomers, continues to stir, then be added dropwise
10mL (concentration 0.03g/mL) ammonium persulfate solution stirs 1.5h, obtains polyvinyl alcohol-graphene oxide-polypyrrole prepolymer；
3) polyvinyl alcohol-graphene oxide-polypyrrole prepolymer obtained by step 2) is cast in 25mL beaker, be placed in-
30 DEG C of freezing 8h take out to place at room temperature from beaker and thaw, freeze-thaw circulation 6 times, obtain primary polyvinyl alcohol-oxidation stone
Black alkene-polypyrrole composite hydrogel；
4) finally by obtained primary polyvinyl alcohol-graphene oxide-polypyrrole composite hydrogel 500mL deionization
Water washing by soaking 4 days, finally obtain high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel.
High strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel made from the present embodiment is tested, is surveyed
When proper compression strain is 50%, corresponding stress is 8.2KPa；When Electrochemical Scanning rate is 5mVs-1When, specific capacitance is
63Fg-1。
Embodiment 4
A kind of preparation of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, the specific steps are as follows:
1) polyvinyl alcohol that 1.5g alcoholysis degree is 89% is added in 10mL ionized water, 95 DEG C are heated and stirred molten
Solution, obtains polyvinyl alcohol water solution, is naturally cooling to room temperature, obtain the polyvinyl alcohol water solution of homogeneous transparent, be kept stirring；
2) under the conditions of 2 DEG C of ice bath, 15mL (concentration 2mg/mL) graphene oxide water solution is added obtained by step 1)
Polyvinyl alcohol water solution (being kept stirring) in, be uniformly mixed, be slow added into 180 μ L pyrrole monomers, continue to stir, then by
It is added dropwise to 2mL (concentration 0.1g/mL) ammonium persulfate solution, 2h is stirred, obtains polyvinyl alcohol-graphene oxide-polypyrrole pre-polymerization
Object；
3) polyvinyl alcohol-graphene oxide-polypyrrole prepolymer obtained by step 2) is cast in 25mL beaker, be placed in-
35 DEG C of freezing 10h take out to place at room temperature from beaker and thaw, freeze-thaw circulation number 3 times, obtain primary polyvinyl alcohol-
Graphene oxide-polypyrrole composite hydrogel；
4) finally by obtained hydrogel with 500mL deionized water washing by soaking 5 days, high-strength polyethylene is finally obtained
Alcohol-graphene oxide-polypyrrole composite hydrogel.
High strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel made from the present embodiment is tested, is surveyed
When proper compression strain is 50%, corresponding stress is 15.7KPa；When Electrochemical Scanning rate is 5mVs-1When, specific capacitance is
50Fg-1。
Embodiment 5
A kind of preparation of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, the specific steps are as follows:
1) polyvinyl alcohol that 0.5g alcoholysis degree is 95% is added in 10mL deionized water, 95 DEG C are heated and stirred molten
Solution, obtains polyvinyl alcohol water solution, is naturally cooling to room temperature, obtain the polyvinyl alcohol water solution of homogeneous transparent, be kept stirring；
2) under the conditions of 2 DEG C of ice bath, 13mL (concentration 3mg/mL) graphene oxide water solution is added obtained by step 1)
Polyvinyl alcohol water solution (being kept stirring) in, be uniformly mixed, be slow added into 60 μ L pyrrole monomers, continue to stir, then by
It is added dropwise to 5mL (concentration 0.04g/mL) ammonium persulfate solution, 1.5h is stirred, it is pre- to obtain polyvinyl alcohol-graphene oxide-polypyrrole
Polymers；
3) polyvinyl alcohol-graphene oxide-polypyrrole prepolymer mixed solution obtained by step 2) is cast in 25mL beaker
In, -20 DEG C of freezings are placed in, time 12h takes out to place at room temperature from beaker and thaw, freeze-thaw circulation 4 times, obtains just
Grade polyvinyl alcohol-graphene oxide-polypyrrole composite hydrogel；
4) finally by obtained hydrogel with 500mL deionized water washing by soaking 6 days, high-strength polyethylene is finally obtained
Alcohol-graphene oxide-polypyrrole composite hydrogel.
High strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel made from the present embodiment is tested, is surveyed
When proper compression strain is 50%, corresponding stress is 6.4KPa；When Electrochemical Scanning rate is 5mVs-1When, specific capacitance is
93Fg-1。
Each raw material cited by the present invention can realize that the bound value of the present invention and each raw material, interval value can
Realize the present invention；Embodiment numerous to list herein.The bound value of technological parameter (such as temperature, time) of the invention,
Interval value can realize the present invention, embodiment numerous to list herein.
Claims (6)
1. a kind of preparation method of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel, which is characterized in that packet
Include following steps:
1) polyvinyl alcohol is add to deionized water, is heated to 90-100 DEG C and stirred to dissolve, be cooled to 20-25 DEG C,
Obtain polyvinyl alcohol water solution；
2) first that polyvinyl alcohol water solution obtained in graphene oxide water solution and step 1) is mixed under the conditions of 0-5 DEG C of ice bath
It closes, adds pyrrole monomer, stir, ammonium persulfate solution is then added, continue to stir 0.5-2h, obtain polyvinyl alcohol-oxidation stone
Black alkene-polypyrrole prepolymer；
3) polyvinyl alcohol-graphene oxide obtained by step 2)-polypyrrole prepolymer freezing is thawed again, recycles 4-7 times, obtains water-setting
Glue；
4) the obtained hydrogel of step 3) was obtained into high strength poly vinyl alcohol-graphite oxide with deionized water washing by soaking 2-6 days
Alkene-polypyrrole composite hydrogel.
2. the preparation side of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel according to claim 1
Method, which is characterized in that the amount ratio of polyvinyl alcohol described in step 1) and the deionized water is 0.05-0.2g:1mL.
3. the preparation side of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel according to claim 1
Method, which is characterized in that the concentration of graphene oxide water solution described in step 2) is 2-4mg/mL；The ammonium persulfate solution
Concentration is 0.01-0.1g/mL.
4. the preparation side of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel according to claim 3
Method, which is characterized in that graphene oxide water solution, the ammonium persulfate described in polyvinyl alcohol described in step 1) and step 2)
The amount ratio of solution and the pyrrole monomer is (0.5g-1.5g): (2mL-20mL): (1mL-10mL): (60 μ L-180 μ L).
5. the preparation side of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel according to claim 1
Method, which is characterized in that the temperature of freezing described in step 3) is -40 DEG C to -20 DEG C, and the time of freezing is 5-15h.
6. the preparation side of high strength poly vinyl alcohol-graphene oxide-polypyrrole composite hydrogel according to claim 1
Method, which is characterized in that the temperature of defrosting described in step 3) is 20-25 DEG C.
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| CN110698856A (en) * | 2019-09-23 | 2020-01-17 | 江苏理工学院 | Graphene/polypyrrole/water-soluble polymer ternary composite material and preparation method thereof |
| CN111729623A (en) * | 2020-05-24 | 2020-10-02 | 同济大学 | Preparation method and application of three-dimensional copper ferricyanide composite polypyrrole/polyvinyl alcohol conductive hydrogel material |
| CN111803466A (en) * | 2020-04-17 | 2020-10-23 | 中山大学 | Preparation method and application of polypyrrole nanoparticles with controllable particle size |
| CN112113498A (en) * | 2020-09-14 | 2020-12-22 | 山西大学 | Preparation method of high-sensitivity piezoresistive strain sensor |
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