CN110690062B - Preparation method of polyacrylic acid flexible composite hydrogel electrolyte - Google Patents
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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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
- C08J3/075—Macromolecular gels
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- 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
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of a polyacrylic acid flexible composite hydrogel electrolyte, which comprises the following steps: (1) dissolving sodium alginate in distilled water, stirring, and dispersing with ultrasonic wave to obtain solution; (2) adding acrylic acid, N-N' methylene bisacrylamide, octavinyl polyhedral oligomeric silsesquioxane and an emulsifier into the solution obtained in the step (1), stirring and dispersing by utilizing ultrasonic waves to form a reaction system; (3) adding an initiator into the reaction system obtained in the step (2), and stirring for dissolving; (4) placing the product obtained in the step (3) in an oven at 60 ℃ for standing reaction for 5 hours to obtain hydrogel; (5) naturally airing the hydrogel obtained in the step (4) for 36-54 h; (6) and (4) soaking the hydrogel obtained in the step (5) in a redox active substance solution for 18-48h to obtain the polyacrylic acid flexible composite hydrogel electrolyte.
Description
Technical Field
The invention belongs to the technical field of materials for super capacitor electrolytes, and particularly relates to a preparation method of a polyacrylic acid flexible composite hydrogel electrolyte.
Background
With the rapid development of flexible electronic science and electronic product miniaturization technology, flexible, wearable, foldable and portable electronic devices are coming out in succession. As one kind of flexible power supply, the flexible super capacitor meets the energy requirements of wearable and portable electronic devices due to the excellent electrochemical properties such as high charging and discharging speed, high power density, long cycle life and the like and the mechanical deformation properties such as stretching, bending and folding. The electrolyte as a main component of the super capacitor directly influences the use performance of the super capacitor. Common electrolytes for supercapacitors include liquid-based electrolytes, organic electrolytes, ionic liquid electrolytes, and solid electrolytes. Wherein, the liquid electrolyte is easy to leak and has low energy density; the flexibility of the solid electrolyte is limited, the stretching and bending limits are very small, and the requirements of the flexible supercapacitor are difficult to meet.
Hydrogels are a particular class of wet, soft materials. The polymer is a three-dimensional network polymer which contains a large amount of hydroxyl, amino and carboxyl and is moderately crosslinked, can generate swelling behavior in water, can keep a certain shape before and after water absorption, has excellent elasticity and tensile property, and has attractive application prospects in the fields of drug release, chemical sensors, artificial muscles and the like. In recent years, polymer hydrogels have been used in supercapacitors, which are polymer-based hydrogels having flexibility and stretchability, such as oxidized polyethylene-based hydrogels, polyacrylic-based hydrogels, and polyvinyl alcohol hydrogels, mainly used as supercapacitor electrolytes. Tang et al immerse the crosslinked polyacrylic acid hydrogel in an aniline monomer to allow aniline to penetrate the polyacrylic acid before initiating polymerization. The obtained polyaniline/polyacrylic acid 3D interpenetrating network polymer has good ionic conductivity and can be used as an electrolyte of a super capacitor (Tang ZY, Wu J H, Liu Q, Zheng M, Tang QW, Lan Z, Lin JM. Preparation of poly (acrylic acid)/gelatin/polyannine gel-electrolyte and its application in quadrature-solid-state-sensed magnetic cells, J. Power Source, 2012, 203: 282-287.). Li et al reinforced polyacrylic acid hydrogel with cellulose nanofibrils to obtain electrolyte with high mechanical strength and high ionic conductivity which can be used as super capacitor (Li L, Liu L, Qing Y, Zhang Z, Yan N, Wu YQ, Tian CH. Stretchable alkali poly (acrylic acid) electrolyte with high ionic conductivity enhanced by cellulose nanofibers. electrochemical Acta, 2018, 270: 302-. Poosaptati et al, which uses polyacrylic acid and potassium hydroxide to prepare polymer gel electrolyte, have the properties of flexibility, stability and high ionic conductivity, and can be used as the electrolyte of super capacitors (Poosaptati A, Jang E, Madan D, Jang N, Hu LB, Lan YC. cell hydrogel as a flexible gel electrolyte layer, MRS Communications, 2019, 9(1): 122-. In summary, the flexible stretchable composite hydrogel electrolyte has a certain application foundation, but the ionic conductivity and mechanical properties (stretching and flexible bending properties) of the current flexible electrolyte material cannot meet the requirements of future portable electronic products.
Disclosure of Invention
In order to solve the above problems, the present invention aims to introduce sodium alginate having multiple crosslinking sites, octavinyl cage silsesquioxane (POSS), and redox active materials having electrochemical activity such as phosphomolybdic acid, copper chloride, etc. into the three-dimensional network structure of a polyacrylic acid hydrogel. The method has not been reported at home and abroad.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of a polyacrylic acid flexible composite hydrogel electrolyte comprises the following steps:
(1) dissolving sodium alginate in distilled water, stirring, and dispersing with ultrasonic wave to obtain solution;
(2) adding acrylic acid, N-N '-methylene bisacrylamide, octavinyl POSS and OP-10 into the solution obtained in the step (1), stirring and dispersing by using ultrasonic waves to form a reaction system, wherein the concentration of the acrylic acid is 150-250mg/mL, the mass ratio of the acrylic acid to sodium alginate is 20:1-5:1, the mass ratio of the acrylic acid to the N, N' -methylene bisacrylamide is 200:1-50:1, the mass ratio of the acrylic acid to the octavinyl POSS is 50:1-10:1, and the mass ratio of the acrylic acid to an emulsifier is 20:1-10: 1;
(3) adding an initiator into the reaction system obtained in the step (2), stirring and dissolving, wherein the mass ratio of the acrylic acid to the initiator is 200:1-50:1, and the initiator is ammonium persulfate or azodiisobutyl amidine hydrochloride;
(4) standing the reaction system obtained in the step (3) in an oven at 60 ℃ for 5 hours;
(5) naturally airing the hydrogel obtained in the step (4) for 36-54 h;
(6) and (5) soaking the hydrogel obtained in the step (5) in a redox active substance solution for 18-48h to obtain the polyacrylic acid flexible composite hydrogel electrolyte. The active substance is a solution of phosphomolybdic acid, phosphotungstic acid, p-benzoquinone, copper chloride or anthraquinone-2, 6-disulfonic acid sodium, and the concentration of the solution is 0.1-0.5 mmol/L.
The invention adopts alginate and hydrophilic acrylic acid as raw materials, the acrylic acid forms a three-dimensional network structure through polymerization, and octavinyl POSS is introduced to increase chemical crosslinking points. At the moment, the molecular chain of the sodium alginate is inserted in the network, and the molecular motion of the sodium alginate is limited by the formed polyacrylic acid network to a certain extent; and forming a sodium alginate network by the G segment in the sodium alginate molecular chain and the adjacent G segment to obtain the polyacrylic acid/sodium alginate interpenetrating network gel. Then introducing a redox active substance into the polyacrylic acid/sodium alginate gel interpenetrating network to improve the ionic conductivity of the gel electrolyte; in the charge and discharge process of the super capacitor, the redox active substances provide additional pseudo capacitance through redox reaction, so that the specific total capacitance of the super capacitor is improved, and the energy density of the super capacitor is further improved.
The invention has the following beneficial effects:
1. according to the invention, natural high-molecular sodium alginate is used as a reinforcing material, and the flexibility, the uniformity and the active functional groups of the natural high-molecular sodium alginate are utilized to increase the physical crosslinking points of the gel to form an interpenetrating network, so that the composite hydrogel has good mechanical properties.
2. According to the invention, the octavinyl POSS is used as a reinforcing material, and the active functional groups of the octavinyl POSS are used for increasing chemical crosslinking points of the gel to form a more compact network structure, so that the composite hydrogel has good mechanical properties.
3. The invention adopts a soaking mode to disperse the redox active substance into the interpenetrating network structure of the composite hydrogel, thereby improving the conductivity of the gel and the electrochemical performance of the gel.
4. The composite hydrogel prepared by the method has good flexibility, bending property and tensile property, the volume of the hydrogel is reduced and hardened after the hydrogel is dried, the volume is increased and the flexibility is recovered after the hydrogel absorbs moisture again, and the 3D network structure of the hydrogel has good memory effect.
5. The method of the invention carries out polymerization reaction at low temperature and under static state, has simple equipment and easy operation, and is easy to enlarge large-scale production.
Drawings
FIG. 1 is a schematic view of the shape recovery of the composite hydrogel prepared by the present invention.
FIG. 2 is an SEM photograph of a composite hydrogel of the present invention.
FIG. 3 is a structural diagram of a crosslinked network of a composite hydrogel prepared by the method of the present invention.
Detailed Description
The invention is explained in more detail below with reference to the figures and the specific embodiments.
Fig. 1 is a schematic diagram of shape recovery of the composite hydrogel prepared in example 1 of the present invention, and as shown in the figure, the prepared composite hydrogel shrinks and hardens after being dried in the air, and then recovers flexibility after absorbing water again, and a 3D network structure thereof has a good memory effect.
FIG. 2 is an SEM photograph of a composite hydrogel electrolyte prepared in example 1 of the present invention. As shown in the figure, the composite hydrogel forms a network structure with regular pore size, which is beneficial to the immersion of redox active substances, is convenient for the transmission of ions, increases the conductivity of the composite hydrogel and improves the electrochemical performance of the composite hydrogel.
FIG. 3 is a structural diagram of a crosslinked network of a composite hydrogel prepared by the method of the present invention. On one hand, the introduction of sodium alginate and octavinyl POSS can form a proper amount of physical/chemical crosslinking points, so that the mechanical property of the composite hydrogel is further regulated and controlled; on the other hand, the pseudocapacitance provided by the redox active material may increase the total specific capacitance of the supercapacitor, thereby further increasing its energy density.
Example 1
A preparation method of a polyacrylic acid flexible composite hydrogel electrolyte comprises the following steps:
(1) dissolving 0.075g of sodium alginate in 10ml of distilled water, stirring and dispersing by utilizing ultrasonic waves to form a solution for later use;
(2) adding 1.5g of acrylic acid, 0.0075g of N-N' methylene bisacrylamide, 0.03g of octavinyl POSS and 0.075gOP-10 into the solution obtained in the step (1), stirring and dispersing for 10min by using ultrasonic waves;
(3) adding 0.0075g of ammonium persulfate into the solution obtained in the step (2), stirring and dispersing for 10min by using ultrasonic waves;
(4) standing the reaction system obtained in the step (3) in an oven at 60 ℃ for 5 hours;
(5) naturally airing the hydrogel obtained in the step (4) for 36 hours;
(6) and (4) soaking the hydrogel obtained in the step (5) in a phosphomolybdic acid solution of 0.1mmol/L for 18h to obtain the polyacrylic acid flexible composite hydrogel electrolyte.
Example 2
A preparation method of a polyacrylic acid flexible composite hydrogel electrolyte is different from example 1 in that 0.075g of sodium alginate in step (1) is changed to 0.100g, 1.5g of acrylic acid in step (2) is changed to 2.0g, 0.0075g of N-N' methylene bisacrylamide is changed to 0.0250g, 0.03g of octavinyl POSS is changed to 0.04g, 0.075gOP-10 is changed to 0.100g, 0.0075g of ammonium persulfate in step (3) is changed to 0.0200g of azodiisobutyl hydrochloride, 36h in step (5) is naturally aired to 42h, 0.1mmol/L of phosphomolybdic acid in step (6) is changed to 0.2mmol/L of phosphotungstic acid, and 18h in step (6) is soaked for 24 h.
Example 3
A preparation method of a polyacrylic acid flexible composite hydrogel electrolyte is different from that of example 1 in that 0.075g of sodium alginate in step (1) is changed to 0.200g, 1.5g of acrylic acid in step (2) is changed to 2.0g, 0.0075g of N-N' methylene bisacrylamide is changed to 0.0250g, 0.03g of octavinyl POSS is changed to 0.10g, 0.075gOP-10 is changed to 0.125g, 0.0075g of ammonium persulfate in step (3) is changed to 0.0250g, natural airing in step (5) is changed to 48h, 0.1mmol/L of phosphomolybdic acid in step (6) is changed to 0.3mmol/L of p-benzoquinone, and soaking in step (6) is changed to 30 h.
Example 4
A preparation method of a polyacrylic acid flexible composite hydrogel electrolyte is different from example 1 in that 0.075g of sodium alginate in step (1) is changed to 0.300g, 1.5g of acrylic acid in step (2) is changed to 2.0g, 0.0075g of N-N' methylene bisacrylamide is changed to 0.0300g, 0.03g of octavinyl POSS is changed to 0.10g, 0.075gOP-10 is changed to 0.150g, 0.0075g of ammonium persulfate in step (3) is changed to 0.0300g, natural airing in step (5) is changed to 48h, 0.1mmol/L of phosphomolybdic acid in step (6) is changed to 0.1mmol/L of copper chloride, and soaking in step (6) is changed to 18h to 42 h.
Example 5
A preparation method of a polyacrylic acid flexible composite hydrogel electrolyte is different from example 1 in that 0.075g of sodium alginate in step (1) is changed into 0.400g, 1.5g of acrylic acid in step (2) is changed into 2.5g, 0.0075g of N-N' methylene bisacrylamide is changed into 0.0400g, 0.03g of octavinyl POSS is changed into 0.20g, 0.075gOP-10 is changed into 0.200g, 0.0075g of ammonium persulfate in step (3) is changed into 0.0400g, natural airing in step (5) is changed into 50h, 0.1mmol/L of phosphomolybdic acid in step (6) is changed into 0.4mmol/L of anthraquinone-2, 6-disulfonic acid, and soaking in step (6) is changed into 44 h.
Example 6
A preparation method of a polyacrylic acid flexible composite hydrogel electrolyte is different from example 1 in that 0.075g of sodium alginate in step (1) is changed to 0.500g, 1.5g of acrylic acid in step (2) is changed to 2.5g, 0.0075g of N-N' methylene bisacrylamide is changed to 0.0500g, 0.03g of octavinyl POSS is changed to 0.25g, 0.075gOP-10 is changed to 0.25g, 0.0075g of ammonium persulfate in step (3) is changed to 0.0500g, natural airing in step (5) is changed to 54h, phosphomolybdic acid concentration of 0.1mmol/L in step (6) is changed to 0.5mmol/L, and soaking in step (6) is changed to 48 h.
The performance parameters of the polyacrylic acid flexible composite hydrogel electrolytes prepared in examples 1 to 6 are shown in table 1.
TABLE 1
| Examples | 1 | 2 | 3 | 4 | 5 | 6 |
| Ion conductivity (mS/cm) | 125 | 65 | 80 | 110 | 90 | 185 |
| Elongation delta (%) | 100 | 110 | 150 | 200 | 140 | 130 |
The elongation shown in table 1 was calculated according to the following formula:
wherein, delta is elongation, L is maximum elongation length, and s is original length
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.
Claims (10)
1. The preparation method of the polyacrylic acid flexible composite hydrogel electrolyte is characterized by comprising the following steps:
(1) dissolving sodium alginate in water to form a solution for later use;
(2) adding acrylic acid, N-N' methylene bisacrylamide, octavinyl polyhedral oligomeric silsesquioxane and an emulsifier into the solution obtained in the step (1) to form a reaction system;
(3) adding an initiator into the reaction system obtained in the step (2), and stirring for dissolving;
(4) placing the product obtained in the step (3) in an oven at 60 ℃ for standing reaction for 5 hours to obtain hydrogel;
(5) naturally airing the hydrogel obtained in the step (4) for 36-54 h;
(6) and (3) soaking the hydrogel obtained in the step (5) in a redox active substance solution for 18-48h to obtain the polyacrylic acid flexible composite hydrogel electrolyte, wherein the redox active substance is a solution of phosphomolybdic acid, phosphotungstic acid, p-benzoquinone, copper chloride or anthraquinone-2, 6-disulfonic acid sodium.
2. The method as claimed in claim 1, wherein the concentration of acrylic acid in the step (2) is 150 mg/mL-250 mg/mL.
3. The preparation method according to claim 1, wherein the mass ratio of acrylic acid to sodium alginate in the step (2) is 20:1 to 5: 1.
4. The preparation method according to claim 1, wherein the mass ratio of the acrylic acid to the N, N' -methylenebisacrylamide in the step (2) is 200:1 to 50: 1.
5. The production method according to claim 1, wherein the mass ratio of the acrylic acid to the octavinyl cage-type silsesquioxane in the step (2) is 50:1 to 10: 1.
6. The production method according to claim 1, wherein the mass ratio of the acrylic acid to the emulsifier in the step (2) is 20:1 to 10: 1.
7. The method according to claim 1, wherein the emulsifier in step (2) is OP-10.
8. The method according to claim 1, wherein the initiator in the step (3) is ammonium persulfate or azobisisobutylamidine hydrochloride.
9. The production method according to claim 1, wherein the mass ratio of the acrylic acid to the initiator in the step (3) is 200:1 to 50: 1.
10. The method according to claim 1, wherein the concentration of the solution in the step (6) is 0.1 to 0.5 mmol/L.
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