CN112521630A - Preparation method and application of green flexible conductive anti-freezing hydrogel - Google Patents
Preparation method and application of green flexible conductive anti-freezing hydrogel Download PDFInfo
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Abstract
The invention provides a preparation method and application of a green flexible conductive antifreeze hydrogel, which can monitor human motion at normal temperature and low temperature; the invention uses polyvinyl alcohol (PVA), Phytic Acid (PA) and woodSodium Lignosulfonate (LS), Polyacrylamide (PANI), FeCl3And glycerol are used as materials, PA, LS and PANI are added into PVA hydrogel, the defects of poor mechanical property and non-conductivity of pure PVA hydrogel can be greatly improved, PANI can also endow hydrogel with thermosensitive property, and FeCl3And the introduction of glycerin can improve the electric conduction, water retention and frost resistance of the composite hydrogel. Meanwhile, hydrogen bonds formed by interaction of the PA and the LS with the PVA and the glycerol also enable the composite hydrogel to have self-healing performance; the preparation method of the green flexible conductive antifreeze hydrogel is simple, the operation is convenient, the material source is green, and the prepared composite hydrogel can be reused.
Description
Technical Field
The invention belongs to the technical field of high polymer materials and flexible electronics, and particularly relates to a preparation method and application of a green flexible conductive anti-freezing hydrogel.
Background
The hydrogel is a material with high water content, can form a 3D network structure through physical or chemical crosslinking, has good biocompatibility, and is widely applied to the aspects of biomedicine, tissue engineering, wearable electronic equipment, flexible sensors and the like. However, the traditional hydrogel has poor mechanical properties and is not conductive, and some inorganic materials are required to be added to enhance the mechanical properties and conductivity of the traditional hydrogel, and the composite hydrogel is not degradable, so that the advantage of green color of the hydrogel is weakened, and the environment is adversely affected.
Disclosure of Invention
Aiming at the defects in the prior art, the primary object of the invention is to provide a preparation method of a green flexible conductive antifreeze hydrogel, in the preparation process, green materials with good biodegradability, namely sodium lignosulfonate and Phytic Acid (PA), are introduced into the conductive hydrogel, and polyaniline fiber with heat-sensitive property and glycerol, FeCl and FeCl with water retention and antifreeze properties are added simultaneously3The ionic conductivity in the hydrogel can be increased, and the addition of the materials also greatly improves the mechanical properties of the hydrogel, so that the composite hydrogel has greatly enriched properties.
It is a second object of the present invention to provide the above green flexible electrically conductive antifreeze hydrogel.
The third purpose of the invention is to provide the application of the green flexible conductive antifreeze hydrogel.
In order to achieve the above purpose, the solution of the invention is as follows:
a preparation method of a green flexible conductive antifreeze hydrogel comprises the following steps:
(1) stirring the mixture of PVA and LS in thionyl chloride (DMSO)/water cosolvent at the rotation speed of 200-350rpm at the temperature of 100-135 ℃ for 2.5-5h to obtain a solution A;
(2) mixing PVA and FeCl3Dissolving in PA water solution, and stirring the mixture at 75-90 deg.C for 2.5-5h to obtain solution B;
(3) uniformly mixing the solution A and the solution B, cooling to 40-60 ℃, pouring into a mold, and standing at low temperature for 10-20h to form hydrogel; then placing the obtained hydrogel into water for 2-5 days to displace DMSO from the hydrogel;
(4) adding aniline into ethanol/water solution, and uniformly dispersing into nano aniline suspension under the action of ultrasound. Dissolving Ammonium Persulfate (APS) in deionized water, adding the solution into aniline solution, uniformly mixing, and polymerizing to form polyaniline nano-fibers;
(5) transferring the hydrogel obtained in the step (3) into the mixed solution obtained in the step (4), and soaking for a period of time;
(6) and (4) transferring the hydrogel obtained in the step (5) into glycerol and placing for several days to obtain the green flexible conductive anti-freezing hydrogel.
Preferably, in step (1), the LS mass fraction of the LS/PVA mixture is 5.1-9.9 wt%, DMSO/H2The volume ratio of O is 5/5-7/3.
Preferably, in step (2), FeCl3The concentration of (A) is 0.002-0.03mol/L, and the mass fraction of PVA is 10% -30%.
Preferably, in step (3), the low temperature is-10-10 ℃.
Preferably, in the step (4), the volume ratio of ethanol to water is 1: 4-1: 1; the molar ratio of ammonium persulfate to aniline is 1.1: 1-1.8: 1.
preferably, in the step (5), the soaking time is 1.5-3 h.
Preferably, in step (6), the standing time is 2 to 3 days.
Polyvinyl alcohol (PVA) is used as a material and is widely applied in the process of preparing hydrogel, because the PVA is low in price and easy to obtain, and hydroxyl groups on a molecular chain are easy to form hydrogen bonds to form the hydrogel. Lignin (LS) is a second largest biomass resource cellulose, is low in cost, non-toxic and biodegradable, is rich in functional groups such as hydroxyl and carboxyl, can form hydrogen bond interaction with PVA chains, and can be chelated with metal ions. Phytic Acid (PA) is also a natural product in plants, has a large number of hydroxyl groups, can form hydrogen bonds with PVA chains, weakens PVA crystallization, and is ionized by PA+Excellent ionic conductivity can be imparted to the PVA-PA gel by migration. Polyaniline nanofibers (PANI NFs) can produce a transient response to transient temperature changes, and the transition speed of carriers between fibers is increased along with the increase of temperature. The introduction of the glycerin can form hydrogen bonds with water, so that the formation of ice crystals is prevented, the freezing point of the water is lowered, and the glycerin plays an important role in the aspects of epidermis water retention, skin elasticity maintenance, dermis restoration and the like, so that the glycerin can improve the water retention property of the hydrogel, and the hydrogel can be stored for a long time.
A green flexible conductive antifreeze hydrogel is prepared by the preparation method.
The green flexible conductive antifreeze hydrogel is applied to artificial intelligence and flexible electronic technology.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the material of the green flexible conductive antifreeze hydrogel disclosed by the invention is natural material, such as sodium lignosulfonate and phytic acid, which have good biodegradability, and when the material is introduced into the hydrogel, the transparency, the mechanical property, the conductivity, the sensitivity and the like of the hydrogel can be greatly improved, so that the material has wide application prospects in the aspects of flexible wearable equipment, intelligent artificial skin and the like.
Secondly, the green flexible conductive antifreeze hydrogel has abundant performance, besides the performance of the common flexible conductive hydrogel, the introduction of polyaniline fiber is that the hydrogel has heat sensitivity, and the addition of glycerol can greatly improve the antifreeze water retention effect of the hydrogel, so that the hydrogel can work at subzero temperature.
Thirdly, the preparation method of the green flexible conductive antifreeze hydrogel is simple and convenient to operate, and the prepared green flexible conductive antifreeze hydrogel has good self-healing performance and can be used repeatedly.
Drawings
FIG. 1 is a scanning electron micrograph of the green flexible electrically conductive antifreeze hydrogel of example 1.
FIG. 2 is a Differential Scanning Calorimetry (DSC) curve of the green flexible conductive antifreeze hydrogel of example 1.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1:
the preparation method of the green flexible conductive antifreeze hydrogel comprises the following steps:
(1) mixing 10g of PVA and 0.51g of LS in a DMSO/water cosolvent, wherein the DMSO and the water are both 50mL, and stirring at the rotating speed of 200-350rpm at the temperature of 100-135 ℃ for 2.5-5h to obtain a solution A;
(2) 10g of PVA and 0.032g of FeCl3Dissolving in 100ml of aqueous solution of LPA, and stirring the mixture at 75-90 ℃ for 2.5-5h to obtain solution B;
(3) uniformly mixing the solution A and the solution B, cooling to 40-60 ℃, pouring into a mould, and standing at-10 ℃ for 10-20h to form the hydrogel. Then placing the obtained hydrogel into water for 2-5 days to displace DMSO from the hydrogel;
(4) and 0.47g of aniline is added into an ethanol/water solution, wherein 20mL of ethanol and 80mL of water are uniformly dispersed under the action of ultrasound. Dissolving 1.25g of Ammonium Persulfate (APS) in deionized water, adding the solution into an aniline solution, and uniformly mixing;
(5) transferring the hydrogel obtained in the step (3) into the mixed solution obtained in the step (4), and soaking for 1.5 h;
(6) and (3) transferring the hydrogel obtained in the step (5) into glycerol and standing for 2 days to obtain the green flexible conductive anti-freezing hydrogel.
FIG. 1 is a scanning electron micrograph of the green flexible electrically conductive antifreeze hydrogel of example 1. The apparent porous structure can be seen from the figure, which illustrates the typical 3D interconnected network of hydrogels.
FIG. 2 is a Differential Scanning Calorimetry (DSC) curve of the green flexible conductive antifreeze hydrogel of example 1. As can be seen, the freezing point of the hydrogel was lowered to-28.5 deg.C, indicating that it has good freezing resistance and is stable even at temperatures greater than-20 deg.C.
Example 2:
the preparation method of the green flexible conductive antifreeze hydrogel comprises the following steps:
(1) mixing 10g of PVA and 0.99g of LS in a DMSO/water cosolvent, wherein the DMSO is 70mL, the water is 30mL, and stirring is carried out at the rotation speed of 200-350rpm at the temperature of 100-135 ℃ for 2.5-5h to obtain a solution A;
(2) 30g of PVA and 0.486g of FeCl3Dissolving in 100ml of aqueous solution of LPA, and stirring the mixture at 75-90 ℃ for 2.5-5h to obtain solution B;
(3) uniformly mixing the solution A and the solution B, cooling to 40-60 ℃, pouring into a mould, and standing at 10 ℃ for 10-20h to form the hydrogel. Then placing the obtained hydrogel into water for 2-5 days to displace DMSO from the hydrogel;
(4) and 0.47g of aniline is added into an ethanol/water solution, wherein 50mL of ethanol and 50mL of water are uniformly dispersed under the action of ultrasound. Dissolving 2.05g of Ammonium Persulfate (APS) in deionized water, adding the solution into an aniline solution, and uniformly mixing;
(5) transferring the hydrogel obtained in the step (3) into the mixed solution obtained in the step (4), and soaking for 3 hours;
(6) and (3) transferring the hydrogel obtained in the step (5) into glycerol and standing for 3 days to obtain the green flexible conductive anti-freezing hydrogel.
Example 3:
the preparation method of the green flexible conductive antifreeze hydrogel comprises the following steps:
(1) mixing 10g of PVA and 0.6g of LS in a DMSO/water cosolvent, wherein the DMSO and the water are both 50mL, and stirring at the rotating speed of 200-350rpm at the temperature of 100-135 ℃ for 2.5-5h to obtain a solution A;
(2) 10g of PVA and 0.1g of FeCl3Dissolving in 100ml of aqueous solution of LPA, and stirring the mixture at 75-90 ℃ for 2.5-5h to obtain solution B;
(3) uniformly mixing the solution A and the solution B, cooling to 40-60 ℃, pouring into a mold, and standing at 5 ℃ for 10-20h to form the hydrogel. Then placing the obtained hydrogel into water for 2-5 days to displace DMSO from the hydrogel;
(4) and 0.47g of aniline is added into an ethanol/water solution, wherein 35mL of ethanol and 65mL of water are uniformly dispersed under the action of ultrasound. Dissolving 2g of Ammonium Persulfate (APS) in deionized water, adding the solution into an aniline solution, and uniformly mixing;
(5) transferring the hydrogel obtained in the step (3) into the mixed solution obtained in the step (4), and soaking for 2 hours;
(6) and (3) transferring the hydrogel obtained in the step (5) into glycerol and standing for 2 days to obtain the green flexible conductive anti-freezing hydrogel.
Example 4:
the preparation method of the green flexible conductive antifreeze hydrogel comprises the following steps:
(1) mixing 10g of PVA and 0.75g of LS in a DMSO/water cosolvent, wherein the DMSO is 60mL, the water is 40mL, and stirring is carried out at the rotation speed of 200-350rpm at the temperature of 100-135 ℃ for 2.5-5h to obtain a solution A;
(2) 10g of PVA and 0.2g of FeCl3Dissolving in 100ml of aqueous solution of LPA, and stirring the mixture at 75-90 ℃ for 2.5-5h to obtain solution B;
(3) uniformly mixing the solution A and the solution B, cooling to 40-60 ℃, pouring into a mould, and standing at-5 ℃ for 10-20h to form the hydrogel. Then placing the obtained hydrogel into water for 2-5 days to displace DMSO from the hydrogel;
(4) and 0.47g of aniline is added into an ethanol/water solution, wherein 20mL of ethanol and 80mL of water are uniformly dispersed under the action of ultrasound. Dissolving 1.5g of Ammonium Persulfate (APS) in deionized water, adding the solution into an aniline solution, and uniformly mixing;
(5) transferring the hydrogel obtained in the step (3) into the mixed solution obtained in the step (4), and soaking for 1.5 h;
(6) and (3) transferring the hydrogel obtained in the step (5) into glycerol and standing for 3 days to obtain the green flexible conductive anti-freezing hydrogel.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (9)
1. A preparation method of a green flexible conductive antifreeze hydrogel is characterized by comprising the following steps: which comprises the following steps:
(1) stirring the mixture of PVA and LS in DMSO/water cosolvent at the rotation speed of 200-350rpm at the temperature of 100-135 ℃ for 2.5-5h to obtain a solution A;
(2) mixing PVA and FeCl3Dissolving in PA water solution, and stirring the mixture at 75-90 deg.C for 2.5-5h to obtain solution B;
(3) uniformly mixing the solution A and the solution B, cooling to 40-60 ℃, pouring into a mold, and standing at low temperature for 10-20h to form hydrogel; then placing the obtained hydrogel into water for 2-5 days to displace DMSO from the hydrogel;
(4) adding aniline into ethanol/water solution, and uniformly dispersing into nano aniline suspension under the action of ultrasound. Dissolving Ammonium Persulfate (APS) in deionized water, adding the solution into aniline solution, uniformly mixing, and polymerizing to form polyaniline nano-fibers;
(5) transferring the hydrogel obtained in the step (3) into the mixed solution obtained in the step (4), and soaking for a period of time;
(6) and (3) transferring the hydrogel obtained in the step (5) into glycerol and placing the glycerol for several days to obtain the green flexible conductive anti-freezing hydrogel.
2. The method of claim 1, wherein: in the step (1), the LS mass fraction in the LS/PVA mixture is 5.1-9.9 wt%, DMSO/H2The volume ratio of O is 5/5-7/3.
3. The method of claim 1, wherein: in the step (2), the FeCl3The concentration of (A) is 0.002-0.03mol/L, and the mass fraction of PVA is 10% -30%.
4. The method of claim 1, wherein: in the step (3), the low temperature is-10-10 ℃.
5. The method of claim 1, wherein: in the step (4), the volume ratio of the ethanol to the water is 1: 4-1: 1; and/or the presence of a gas in the gas,
in the step (4), the molar ratio of ammonium persulfate to aniline is 1.1: 1-1.8: 1.
6. the method of claim 1, wherein: in the step (5), the soaking time is 1.5-3 h.
7. The method of claim 1, wherein: in the step (6), the standing time is 2-3 days.
8. A green flexible conductive antifreeze hydrogel is characterized in that: which is obtained by the production method according to any one of claims 1 to 7.
9. Use of the green flexible electrically conductive antifreeze hydrogel of claim 8 in the manufacture of a medicament for treating a human or animal body.
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| CN112795029A (en) * | 2021-04-07 | 2021-05-14 | 同济大学 | Preparation method and application of double-network flexible conductive adhesive anti-freezing hydrogel |
| CN113248730A (en) * | 2021-04-22 | 2021-08-13 | 上海健康医学院 | Polyacrylamide-nanocellulose crystal-silver nanoparticle composite conductive anti-freezing organic hydrogel and preparation method and application thereof |
| CN113512209A (en) * | 2021-08-10 | 2021-10-19 | 吉林大学 | Preparation method of high-conductivity and high-sensitivity polyvinyl alcohol-based conductive hydrogel |
| CN114736477A (en) * | 2022-05-18 | 2022-07-12 | 浙江大学 | Anti-freezing hydrogel, preparation method thereof and flexible temperature sensor suitable for extremely low temperature response |
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| CN113248730A (en) * | 2021-04-22 | 2021-08-13 | 上海健康医学院 | Polyacrylamide-nanocellulose crystal-silver nanoparticle composite conductive anti-freezing organic hydrogel and preparation method and application thereof |
| CN113512209A (en) * | 2021-08-10 | 2021-10-19 | 吉林大学 | Preparation method of high-conductivity and high-sensitivity polyvinyl alcohol-based conductive hydrogel |
| CN113512209B (en) * | 2021-08-10 | 2022-04-15 | 吉林大学 | Preparation method of high-conductivity and high-sensitivity polyvinyl alcohol-based conductive hydrogel |
| CN114736477A (en) * | 2022-05-18 | 2022-07-12 | 浙江大学 | Anti-freezing hydrogel, preparation method thereof and flexible temperature sensor suitable for extremely low temperature response |
| JP2023171295A (en) * | 2022-05-18 | 2023-12-01 | 浙江大学 | Method for producing freeze-resistant hydrogel and method for producing flexible temperature sensor suitable for cryogenic response |
| JP7397542B2 (en) | 2022-05-18 | 2023-12-15 | 浙江大学 | Method for manufacturing freeze-resistant hydrogel and flexible temperature sensor suitable for cryogenic response |
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Application publication date: 20210319 |