CN116462860A - Conductive nanofiber double-network adhesive hydrogel and preparation method and sensing application thereof - Google Patents
Conductive nanofiber double-network adhesive hydrogel and preparation method and sensing application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 238000010257 thawing Methods 0.000 claims abstract description 32
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 23
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 238000003756 stirring Methods 0.000 claims description 35
- 239000000835 fiber Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 21
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 18
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- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
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- 238000003760 magnetic stirring Methods 0.000 claims description 2
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- WVAKRQOMAINQPU-UHFFFAOYSA-N 2-[4-[2-[5-(2,2-dimethylbutyl)-1h-imidazol-2-yl]ethyl]phenyl]pyridine Chemical compound N1C(CC(C)(C)CC)=CN=C1CCC1=CC=C(C=2N=CC=CC=2)C=C1 WVAKRQOMAINQPU-UHFFFAOYSA-N 0.000 description 2
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- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/103—Detecting, measuring or recording devices for testing the shape, pattern, colour, size or movement of the body or parts thereof, for diagnostic purposes
- A61B5/11—Measuring movement of the entire body or parts thereof, e.g. head or hand tremor, mobility of a limb
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
- C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
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- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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Abstract
The invention discloses a conductive nanofiber double-network adhesive hydrogel, a preparation method and sensing application thereof. According to the invention, polyvinyl alcohol composite BLG-Ag is subjected to freeze thawing cycle to form a first network, and acrylic acid is subjected to free radical polymerization to form a second network, so that the conductive nanofiber double-network adhesive hydrogel is prepared. By introducing a strategy of double-network crosslinking, conductive nanofiber compositing and interface non-covalent interaction, the formed hydrogel has excellent mechanical properties, adhesion properties, conductivity and biocompatibility, and the properties can be adjusted by controlling the addition amount of BLG-Ag. Due to its good adhesion properties and electrical conductivity to tissue, the material can be used for wearable sensors to monitor human tissue movement. The sensing experiment proves that the hydrogel can monitor large body actions, fine actions and physiological indexes in real time. The hydrogel is expected to be applied to health monitoring and disease treatment due to simple preparation, excellent performance and good biocompatibility.
Description
Technical Field
The invention belongs to the technical field of polymers, and particularly relates to a conductive nanofiber double-network adhesive hydrogel, a preparation method and sensing application thereof.
Background
Hydrogels are three-dimensional crosslinked networks with high water content formed from natural or synthetic polymeric materials through physical or chemical crosslinking, which, by virtue of their biomimetic mechanical properties and biocompatibility, can mimic the machinery of biological tissues to reduce micro-motions and minimize adverse biological reactions. The health monitoring device is used for replacing a traditional sensor in health monitoring, can be adhered to tissues, conforms to the surfaces of the tissues, realizes continuous real-time monitoring of the human health index throughout the day, and allows a user to perform self-monitoring in a normal environment.
Currently, various types of wearable sensors have been used to monitor human motion. However, the dispersion of the conductive filler in the hydrogel network is uneven, making it difficult for the dynamic mechanical properties to be compatible with conductivity, and at the same time, it is difficult to achieve strong adhesion and dynamic mechanical synergy in a humid and dynamic environment, which limit the application range of such sensors. To solve this problem, it is necessary to develop a hydrogel having both good dynamic mechanical properties and high conductivity as well as strong tissue adhesion to meet the application requirements.
Disclosure of Invention
In order to solve the related problems, the primary aim of the invention is to provide a preparation method of the conductive nanofiber double-network adhesive hydrogel.
The invention relates to a conductive hydrogel constructed based on conductive nano-silver modified beta-lactoglobulin fibers (BLG-Ag), polyvinyl alcohol (PVA) and Acrylic Acid (AA). The stability of BLG-Ag in the aqueous phase simultaneously endows the hydrogel with good dynamic mechanical properties and conductivity, PVA is subjected to freeze thawing cycle to form physical crosslinking to provide excellent dynamic mechanical properties, and carboxyl hydrophilic groups on a main chain after AA polymerization can be modified by EDC/NHS so as to form instant physical and covalent crosslinking with the tissue surface, so that tissue adhesiveness is improved. The nano silver modified beta-lactoglobulin fiber (BLG-Ag) is used as a conductive material, is compounded with polyvinyl alcohol (PVA) in a freeze thawing cycle to form a first network, and Acrylic Acid (AA) monomer is subjected to free radical polymerization and covalent crosslinking to form a second network, so that the conductive nano fiber double-network adhesive hydrogel is constructed, and the hydrogel is endowed with excellent mechanical property, strong tissue adhesion, excellent conductivity and excellent biocompatibility.
Another object of the present invention is to provide a conductive nanofiber double-network adhesive hydrogel obtained by the above preparation method.
The invention takes three polymers of BLG-Ag, PVA and AA as raw materials, and synthesizes the conductive nanofiber double-network adhesive hydrogel through hydrogen bond, electrostatic action and multiple physical/chemical crosslinking among the components, and the hydrogel adhesive has good dynamic mechanical property, high conductivity and strong tissue adhesion.
It is a further object of the present invention to provide the use of the conductive nanofiber dual network adhesive hydrogel described above.
In order to achieve the above object, the present invention adopts the following technical scheme:
a preparation method of a conductive nanofiber double-network adhesive hydrogel comprises the following steps:
s1, completely dissolving beta-lactoglobulin in water, regulating the pH value to 2+/-1, and reacting; dialyzing the obtained reaction liquid, and freeze-drying the dialyzed solution to obtain a light yellow flocculent product which is beta-lactoglobulin fiber;
s2, dissolving the beta-lactoglobulin fibers obtained in the step S1 in water, regulating the pH to 2+/-1, and adding a silver nitrate solution to dissolve the beta-lactoglobulin fibers completely; then adding sodium borohydride solution corresponding to the equivalent of silver nitrate for reaction; dialyzing the obtained reaction liquid, and freeze-drying the dialyzed solution to obtain a brownish black flocculent product which is the nano silver modified beta-lactoglobulin fiber;
s3, dissolving the nano-silver modified beta-lactoglobulin fibers obtained in the step S2 in water to prepare a nano-silver modified beta-lactoglobulin fiber solution; then adding polyvinyl alcohol (PVA), stirring uniformly, and preparing hydrogel precursor liquid;
s4, adding acrylic acid, a cross-linking agent, an initiator and an initiation accelerator into the hydrogel precursor liquid obtained in the step S3, uniformly stirring and deoxidizing; and (3) performing freeze thawing cycle on the obtained mixed solution to obtain the conductive nanofiber double-network adhesive hydrogel.
Further, the reaction in the step S1 is a magnetic stirring reaction at 90+ -5 ℃ for 12+ -2 h.
Further, in step S1, the reaction solution is cooled to room temperature (room temperature in the present invention means 20 to 30 ℃) before the dialysis is performed.
Further, the mass ratio of the beta-lactoglobulin fiber to the silver nitrate in the step S2 is 1.8-2.2:1; preferably 2:1.
Further, in the step S2, the silver nitrate solution is added and then stirred for reaction for 10+/-2 min, and the sodium borohydride solution is added and then stirred for reaction for 5+/-1 h.
Further, the reagent used for adjusting the pH in the step S1 and the step S2 is nitric acid, and the preferable pH is 2.
Further, dialysis bags used in the dialysis in the step S1 and the step S2 have a molecular weight cut-off of 8-14 kDa, a time of 7+ -2 d, water is changed 2+ -1 times a day, and dialysis is performed with a large amount of water to remove impurities and unreacted monomers.
Further, the freeze-drying temperature in the step S1 and the step S2 is-40 ℃ to-80 ℃.
Further, the molecular weight of the polyvinyl alcohol in the step S3 ranges from 50000 to 140000; preferably 80000 to 100000.
Further, the concentration of the nano-silver modified beta-lactoglobulin fiber solution in the step S3 is 2-5 wt%.
Further, after preparing the nano silver modified beta-lactoglobulin fiber solution in the step S3, regulating the pH of the system to 2-5, and stirring for 1-6 hours at the temperature of 30-60 ℃ and the speed of 100-300 rmp.
Further, the stirring conditions in step S3 are: the temperature is 90-100 ℃, the time is 20-60 min, and the speed is 100-300 rmp.
Further, the mass fraction of the nano silver modified beta-lactoglobulin fibers in the mixed solution in the step S4 is 0.25-2 wt%, and the mass fraction of the polyvinyl alcohol is 8-10 wt%.
Further, the initiator in the step S4 is Ammonium Persulfate (APS) or potassium persulfate (KPS).
Further, the mass fraction of the initiator in the mixed solution in the step S4 is 0.05 to 1wt%.
Further, the crosslinking agent in step S4 is N, N' -Methylenebisacrylamide (MBA) or polyethylene glycol and acrylate (PEGDA).
Further, the mass fraction of the cross-linking agent in the mixed solution in the step S4 is 0.01-0.5 wt%.
Further, the initiation accelerator in step S4 is tetramethyl ethylenediamine (TEMED) or sodium bisulphite.
Further, the mass fraction of the initiation accelerator in the mixed solution in the step S4 is 0.01-0.5 wt%.
Further, the stirring conditions described in step S4: the temperature is 0-10 ℃, the time is 5-20 min, and the speed is 100-300 rmp.
Further, the conditions of the freeze-thawing cycle described in step S4 are: freezing temperature is-10 to-20 ℃, freezing time is 10-15 h, thawing temperature is room temperature, and thawing time is 10-15 h; preferably, the freezing temperature is-20 ℃, the freezing time is 12 hours, the thawing temperature is room temperature, the thawing time is 12 hours, and the freezing and thawing cycle is three times.
The conductive nanofiber double-network adhesive hydrogel is obtained by the preparation method.
The application of the conductive nanofiber double-network adhesive hydrogel in preparing a sensor.
Further, the sensor is a flexible sensor.
Compared with the prior art, the invention has the following advantages and effects:
(1) The beta-lactoglobulin fibers used in the invention are derived from beta-lactoglobulin in animal bodies, and have good biocompatibility and stability;
(2) The conductive material nano silver modified beta-lactoglobulin fiber (BLG-Ag) used in the invention can be uniformly dispersed in a water phase, and can be compounded with PVA in a freeze thawing cycle, so that the conductive material nano silver modified beta-lactoglobulin fiber has excellent mechanical properties and high conductivity, and the problem that the conductive material is not uniform in hydrogel is solved;
(3) The conductive nanofiber double-network adhesive hydrogel prepared by the invention has good mechanical properties, high conductivity and excellent adhesive property;
(4) The structure, mechanical property, conductivity and adhesion property of the conductive nanofiber double-network adhesive hydrogel prepared by the invention can be regulated and controlled by changing the BLG-Ag content so as to meet the requirements of various applications;
(5) The conductive nanofiber double-network adhesive hydrogel prepared by the invention has higher sensitivity (1.8-3.69) in a strain range (0.5% -500%);
(6) The conductive nanofiber double-network adhesive hydrogel prepared by the invention can be assembled into a flexible self-adhesive electrode, so that the monitoring of the large-range motion (such as elbows) and tiny motion (such as vocal cord vibration) of a human body is realized, physiological signals are tracked and collected to a certain extent, no stimulation is caused to skin, the wound motion condition can be monitored in real time, and the wound healing condition can be indirectly known.
Drawings
FIG. 1 is a physical view of the conductive nanofiber dual network adhesive hydrogel prepared in examples 1-4;
FIG. 2 is a stress-strain curve of conductive nanofiber dual network adhesive hydrogels of different BLG-Ag content (BAg0.25wt% PP in the figure represents BLG-Ag0.25wt% and PVA/PAA, BAg0.5wt% PP in the figure represents BLG-Ag0.5wt% and PVA/PAA, and BAg1% PP in the figure represents BLG-Ag1% @ PVA/PAA);
FIG. 3 is a graphical representation of the adhesion of BLG-Ag1% @ PVA/PAA hydrogels prepared in example 4 to fresh porcine heart tissue;
FIG. 4 is an adhesion-displacement curve of a conductive nanofiber dual network tacky hydrogel lap shear test for different BLG-Ag contents (BAg0.25PP in the figure represents BLG-Ag0.25% @ PVA/PAA, BAg0.5PP in the figure represents BLG-Ag0.5% @ PVA/PAA, BAg1% PP in the figure represents BLG-Ag1% @ PVA/PAA);
FIG. 5 is a BLG-Ag1% @ PVA/PAA hydrogel prepared in example 4 for finger bending motion monitoring;
FIG. 6 is a BLG-Ag1% @ PVA/PAA hydrogel prepared in example 4 for electromyography;
FIG. 7 is a stress-strain curve of a hydrogel of BLG-Ag1% @ PVA/PAA without and with a freeze-thawing cycle (BAgPP in the figure represents BLG-Ag1% @ PVA/PAA with a freeze-thawing cycle and BAgPP without freeze-thaw in the figure represents BLG-Ag1% @ PVA/PAA without a freeze-thawing cycle).
FIG. 8 is the sensing application range and sensitivity of the BLG-Ag1% @ PVA/PAA hydrogel prepared in example 4.
Detailed Description
The advantages and features of the present invention will become more apparent from the following detailed description of the embodiments, which are given by way of example only and are not limiting in any way.
The following examples are illustrative of the sources of raw materials used:
polyvinyl alcohol (PVA) is purchased from Sigma-Aldrich, the molecular weight is 89000-98000, acrylic Acid (AA) is purchased from Alfa Aesar, cross-linking agent N, N' -Methylene Bisacrylamide (MBA) is purchased from MACHLIN biochemical technology company, initiator Ammonium Persulfate (APS) is purchased from Sigma-Aldrich, and initiator tetramethyl ethylenediamine (TEMED) is purchased from Aladin reagent company;
the nano-silver modified beta-lactoglobulin fiber is prepared by the following method:
synthesis of S1, beta-lactoglobulin fibers (BLG)
4.0g of beta-lactoglobulin is dissolved in 80mL of deionized water at room temperature and stirred magnetically for 30min to dissolve completely. After dissolution was completed, the pH was adjusted to 2 with nitric acid, and the reaction was magnetically stirred at 90℃for 12 hours. After cooling the reaction to room temperature, the resulting mixed solution was placed in a dialysis bag having a molecular weight cut-off of 8 to 14kDa, and dialyzed against a large amount of deionized water for one week (twice daily water change) to remove impurities and unreacted monomers. Freeze-drying the dialyzed solution at-50deg.C to obtain yellowish flocculent product, and storing in a drying cabinet.
S2, synthesis of nano silver modified beta-lactoglobulin fiber (BLG-Ag)
Beta-lactoglobulin fibers were dissolved in deionized water and the pH was adjusted to 2 with nitric acid. Adding silver nitrate solution according to the mass ratio of 2/1 of silver nitrate to beta-lactoglobulin fiber, mixing, magnetically stirring for 10min to dissolve completely, slowly adding sodium borohydride solution corresponding to the equivalent of silver nitrate, simultaneously accelerating the stirring speed, stirring and reacting for 5h at room temperature, putting the obtained mixed solution into a dialysis bag with the cut-off molecular weight of 8-14 kDa, and dialyzing with a large amount of deionized water for one week (changing water twice a day) to remove impurities and unreacted monomers. And freeze-drying the dialyzed solution at-50 ℃ by a freeze dryer to obtain a brownish black flocculent product, and storing the brownish black flocculent product in a drying cabinet.
Example 1
A preparation method of a conductive nanofiber double-network adhesive hydrogel comprises the following steps:
(1) Weighing 100mgPVA, dissolving in deionized water to prepare 0.7mL solution, stirring at 90 ℃ for 30min at a stirring speed of 200rmp;
(2) Adding 200 mu LAA,2mg initiator APS,0.2mg crosslinking agent MBA,1mg initiator accelerator TEMED into the mixed solution obtained in the step (1), stirring for 5min at 0 ℃ at a stirring speed of 200rmp, and deoxidizing for 5min;
(3) And (3) carrying out freeze thawing cycle on the mixed solution obtained in the step (2) for three times, wherein the freezing time is 12h at minus 20 ℃, the room temperature (25 ℃) and the thawing time is 12h, and obtaining the PVA/PAA hydrogel.
Example 2
A preparation method of a conductive nanofiber double-network adhesive hydrogel comprises the following steps:
(1) 200mgBLG-Ag is weighed and dissolved in deionized water to prepare 10mL of solution, the pH is adjusted to 2, the temperature is 60 ℃, and the solution is stirred for 30min at 200rpm to prepare 10mL of BLG-Ag solution with the concentration of 2%;
(2) Weighing 100mgPVA, dissolving 125 mu L of 2% BLG-Ag solution in the step (1) in deionized water to prepare 0.8mL solution, stirring at 90 ℃ for 30min, and stirring at 200rmp;
(3) Adding 200 mu LAA,2mg initiator APS,0.2mg crosslinking agent MBA,1mg initiator accelerator TEMED into the mixed solution obtained in the step (2), stirring for 5min at 0 ℃, wherein the stirring speed is 200rmp, and deoxidizing for 5min;
(4) And (3) carrying out freeze thawing cycle on the mixed solution obtained in the step (3) for three times, wherein the freezing time is 12h at minus 20 ℃, the room temperature (25 ℃) and the thawing time is 12h, and thus the BLG-Ag0.25% @ PVA/PAA hydrogel can be obtained.
Example 3
A preparation method of a conductive nanofiber double-network adhesive hydrogel comprises the following steps:
(1) 200mgBLG-Ag is weighed and dissolved in deionized water to prepare 10mL of solution, the pH is adjusted to 2, the temperature is 60 ℃, and the solution is stirred for 30min at 200rpm to prepare 10mL of BLG-Ag solution with the concentration of 2%;
(2) Weighing 100mgPVA, dissolving 250 mu L of 2% BLG-Ag solution in the step (1) in deionized water to prepare 0.8mL solution, stirring at 90 ℃ for 30min, and stirring at 200rmp;
(3) Adding 200 mu LAA,2mg initiator APS,0.2mg crosslinking agent MBA,1mg initiator accelerator TEMED into the mixed solution obtained in the step (2), stirring for 5min at 0 ℃, wherein the stirring speed is 200rmp, and deoxidizing for 5min;
(4) And (3) carrying out freeze thawing cycle on the mixed solution obtained in the step (3) for three times, wherein the freezing time is 12h at minus 20 ℃, the room temperature (25 ℃) and the thawing time is 12h, and thus the BLG-Ag0.5% @ PVA/PAA hydrogel can be obtained.
Example 4
A preparation method of a conductive nanofiber double-network adhesive hydrogel comprises the following steps:
(1) 200mgBLG-Ag is weighed and dissolved in deionized water to prepare 10mL of solution, the pH is adjusted to 2, the temperature is 60 ℃, and the solution is stirred for 30min at 200rpm to prepare 10mL of BLG-Ag solution with the concentration of 2%;
(2) Weighing 100mgPVA, dissolving 500 mu L of 2% BLG-Ag solution in the step (1) in deionized water to prepare 0.8mL solution, stirring at 90 ℃ for 30min at a stirring speed of 200rmp;
(3) Adding 200 mu L of AA,2mg of initiator APS,0.2mg of crosslinking agent MBA,1mg of initiation accelerator TEMED into the mixed solution obtained in the step (2), stirring for 5min at the temperature of 0 ℃ at the stirring speed of 200rmp, and deoxidizing for 5min;
(4) And (3) carrying out freeze thawing cycle on the mixed solution obtained in the step (3) for three times, wherein the freezing time is 12h at minus 20 ℃, the room temperature (25 ℃) and the thawing time is 12h, and thus the BLG-Ag1% @ PVA/PAA hydrogel can be obtained.
FIG. 1 is a physical view of the conductive nanofiber dual network adhesive hydrogel prepared in examples 1-4. It can be seen that the color of the hydrogel gradually deepens as the content of BLG-Ag increases.
The BLG-Ag1% @ PVA/PAA hydrogel prepared in example 4 was immersed in EDC/NHS solution (EDC 2mol/L, NHS:1 mol/L) for 24 hours, followed by immersing in PBS for 24 hours to allow the hydrogel to reach swelling equilibrium. The tissue fluid on the surface of the isolated heart was wiped dry, followed by rapid application of the hydrogel soaked in EDC/NHS solution, and pressing for 30s to form strong adhesion. FIG. 3 is a graphical representation of the adhesion of BLG-Ag1% @ PVA/PAA hydrogels to fresh porcine heart tissue. It can be seen that the hydrogel does not fall off even under the impact of water flow, indicating that the hydrogel of the invention can rapidly seal a wound of a heart.
The conductive nanofiber double-network adhesive hydrogels with different BLG-Ag contents prepared in examples 1-4 were subjected to tensile stress-strain test on long-strip hydrogel samples (20 mm long, 10mm wide and 2mm thick) at room temperature (25 ℃) by using a universal material tester (Instron 5967), the tensile rate was 100mm/min, and at least three samples were selected for each group to test, and the tensile properties of the BAgPP hydrogels were tested. FIG. 2 is a stress-strain curve of conductive nanofiber dual network adhesive hydrogels prepared in examples 1-4 with different BLG-Ag contents. As can be seen, as the BLG-Ag content increases, the Young's modulus increases from 20kPa to 102kPa, and the toughness increases from 200kJ/m 3 To 265kJ/m 3 While the maximum strain at break is reduced from 900% to 425%. This is due to the large number of hydrogen bonding interactions and physical crosslinks that can form between PVA crystallites and PVA chains and BLG-Ag.
Conducting nanofiber double-network adhesive hydrogels with different BLG-Ag contents prepared in examples 1-4 were subjected to lap shear testing at room temperature by using a universal material tester (Instron 5967), and the length, width and thickness of the hydrogels were controlled at 10mm, 5mm and 2mm. The hydrogel sample was sandwiched between two pigskin surfaces, and then the pigskin was pressed with a weight for 1 minute to ensure complete adhesion between the hydrogel and the pigskin surfaces. Fig. 4 is an adhesion-displacement curve of the conductive nanofiber dual network adhesive hydrogel lap shear test of different BLG-Ag contents prepared in examples 1-4. It can be seen that the adhesive strength of the pure PVA-PAA hydrogel to the pigskin is 12kPa, and the adhesive strength of the hydrogel to the pigskin is increased and then reduced along with the increase of the BLG-Ag content, but the adhesive strength is increased to 25-35kPa, which is higher than the adhesive strength of the pure PVA-PAA hydrogel to the pigskin. The self-adhesion of hydrogels is likely due to hydrogen bond interactions between hydroxyl groups on the substrate, carboxyl groups of the hydrogel, and different hydrogen bond donor/acceptor groups. With the introduction of BLG-Ag, the hydrogen bond interaction of amino, hydroxyl and carboxyl in the BLG-Ag and PVA-PAA improves the adhesion strength of the hydrogel to pigskin, but the content of the BLG-Ag is further improved, and the cohesive force and the adhesion force of the hydrogel are unbalanced due to the rapid increase of the mechanical strength and the increase of the crosslinking density of the hydrogel, so that the adhesion between the hydrogel and the pigskin is influenced, and the phenomenon of reduced adhesion strength is further presented.
The conductive nanofiber double-network adhesive hydrogels with different BLG-Ag contents prepared in example 4 were taken, the two ends of the hydrogel were assembled with a wire, the wire was connected to an electrochemical workstation (CHI 600E), and the length and width of the hydrogel were 15mm, 5mm and 2mm, respectively. The hydrogel is directly attached to the fingers of a human body, two ends of the hydrogel are connected to an electrochemical workstation through wires, and the change curve of the electric signal is recorded, so that the sensing characteristics of the hydrogel flexible sensor are analyzed. Fig. 5 is a conductive nanofiber dual network adhesive hydrogel for finger bending motion monitoring. The electromyographic signals of the hydrogel are recorded through a multichannel physiological signal acquisition system of the electromyography module, the hydrogel electrode is closely attached to the skin of a human body, the two detection electrodes are placed on the forearm muscle, and the reference electrode is placed on the bones of the arm. Fig. 6 is a conductive nanofiber dual network adhesive hydrogel for electromyography. It can be seen that the BAgPP hydrogel electrode can also detect myoelectric signals generated by different finger abductions, the forces generated by five fingers show distinct myoelectric signal amplitudes, and the movements of the finger abductions can be distinguished by recording the amplitudes, so that the BAgPP hydrogel electrode can be clinically used for physical therapists and biomedical engineers to evaluate muscle activation, and can be used for monitoring the rehabilitation process of a patient suffering from muscle weakness for a long time.
The conductive nanofiber double-network adhesive hydrogels with different BLG-Ag contents prepared in example 4 were taken, the two ends of the hydrogel were assembled with a wire, the wire was connected to an electrochemical workstation, the electrochemical workstation (CHI 600E) and a universal materials tester (Instron 5967) were used to record the resistance change during stretching of the hydrogel, and the sensitivity (GF) was calculated by fitting a curve, and the results are shown in FIG. 8. The length, width and thickness of the hydrogel are 15mm, 5mm and 2mm respectively.
The conductive nanofiber double-network adhesive hydrogel prepared by the invention is assembled into a flexible self-adhesive electrode which is attached to the elbow, vocal cords and other positions, so that the monitoring of the large-range motion of the elbow and the micro motion of the vocal cords vibration can be realized, and the physiological signals can be tracked and collected to a certain extent.
Comparative example 1
A preparation method of a conductive nanofiber double-network adhesive hydrogel comprises the following steps:
(1) 200mgBLG-Ag is weighed and dissolved in deionized water to prepare 10mL of solution, the pH is adjusted to 2, the temperature is 60 ℃, and the solution is stirred for 30min at 200rpm to prepare 10mL of BLG-Ag solution with the concentration of 2%;
(2) Weighing 100mgPVA, dissolving 500 mu L of 2% BLG-Ag solution in the step (1) in deionized water to prepare 0.8mL solution, stirring at 90 ℃ for 30min at a stirring speed of 200rmp;
(3) Adding 200 mu LAA,2mg initiator APS,0.2mg crosslinking agent MBA,1mg initiation accelerator TEMED into the mixed solution obtained in the step (2), stirring for 5min at 0 ℃, wherein the stirring speed is 200rmp, and deoxidizing for 5min, thus obtaining the BLG-Ag1% @ PVA/PAA hydrogel without freeze thawing cycle.
FIG. 7 is a stress-strain curve of a hydrogel of BLG-Ag1% @ PVA/PAA without and with freeze-thawing cycles. By comparing the mechanical properties of the hydrogel formed by the freeze-thawing cycle operation, the Young's modulus and toughness of the hydrogel can be obviously improved by the freeze-thawing cycle, and the fracture strain can be slightly improved.
The embodiments described above are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the embodiments described above, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the present invention should be made in the equivalent manner, and are included in the scope of the present invention.
Claims (10)
1. A preparation method of a conductive nanofiber double-network adhesive hydrogel is characterized by comprising the following steps of: the method comprises the following steps:
s1, completely dissolving beta-lactoglobulin in water, regulating the pH value to 2+/-1, and reacting; dialyzing the obtained reaction liquid, and freeze-drying the dialyzed solution to obtain a light yellow flocculent product which is beta-lactoglobulin fiber;
s2, dissolving the beta-lactoglobulin fibers obtained in the step S1 in water, regulating the pH to 2+/-1, and adding a silver nitrate solution to dissolve the beta-lactoglobulin fibers completely; then adding sodium borohydride solution corresponding to the equivalent of silver nitrate for reaction; dialyzing the obtained reaction liquid, and freeze-drying the dialyzed solution to obtain a brownish black flocculent product which is the nano silver modified beta-lactoglobulin fiber;
s3, dissolving the nano-silver modified beta-lactoglobulin fibers obtained in the step S2 in water to prepare a nano-silver modified beta-lactoglobulin fiber solution; then adding polyvinyl alcohol (PVA), stirring uniformly, and preparing hydrogel precursor liquid;
s4, adding acrylic acid, a cross-linking agent, an initiator and an initiation accelerator into the hydrogel precursor liquid obtained in the step S3, uniformly stirring and deoxidizing; and (3) performing freeze thawing cycle on the obtained mixed solution to obtain the conductive nanofiber double-network adhesive hydrogel.
2. The method for preparing the conductive nanofiber dual-network adhesive hydrogel according to claim 1, wherein:
the mass ratio of the beta-lactoglobulin fiber to the silver nitrate in the step S2 is 1.8-2.2:1.
3. The method for preparing the conductive nanofiber dual-network adhesive hydrogel according to claim 2, wherein:
the mass ratio of the beta-lactoglobulin fiber to the silver nitrate in the step S2 is 2:1;
the reaction in the step S1 is magnetic stirring reaction for 12+/-2 hours at the temperature of 90+/-5 ℃;
step S2, adding a silver nitrate solution, stirring and reacting for 10+/-2 min, adding a sodium borohydride solution, and stirring and reacting for 5+/-1 h;
the reagent used for regulating the pH in the step S1 and the step S2 is nitric acid;
the dialysis in the step S1 and the step S2 adopts a dialysis bag to obtain a molecular weight cutoff of 8-14 kDa, the time is 7+/-2 d, the water is changed for 2+/-1 times a day, and a large amount of water is used for dialysis to remove impurities and unreacted monomers;
the freeze-drying temperature in the step S1 and the step S2 is-40 ℃ to-80 ℃.
4. The method for preparing the conductive nanofiber dual-network adhesive hydrogel according to claim 1, wherein:
the molecular weight of the polyvinyl alcohol in the step S3 ranges from 50000 to 140000;
the concentration of the nano silver modified beta-lactoglobulin fiber solution in the step S3 is 2-5wt%.
5. The method for preparing the conductive nanofiber dual-network adhesive hydrogel according to claim 4, wherein:
the molecular weight range of the polyvinyl alcohol in the step S3 is 80000-100000;
step S3, preparing nano silver modified beta-lactoglobulin fiber solution, regulating the pH of the system to 2-5, and stirring at the temperature of 30-60 ℃ and the speed of 100-300 rmp for 1-6 h;
the stirring conditions in the step S3 are as follows: the temperature is 90-100 ℃, the time is 20-60 min, and the speed is 100-300 rmp.
6. The method for preparing the conductive nanofiber dual-network adhesive hydrogel according to claim 1, wherein:
the initiator in the step S4 is ammonium persulfate or potassium persulfate;
the cross-linking agent in the step S4 is N, N' -methylene bisacrylamide or polyethylene glycol and acrylic ester;
the initiation promoter in the step S4 is tetramethyl ethylenediamine or sodium bisulphite;
the conditions of the freeze-thaw cycle described in step S4 are: freezing temperature is-10 to-20 ℃, freezing time is 10-15 h, thawing temperature is room temperature, and thawing time is 10-15 h.
7. The method for preparing the conductive nanofiber dual-network adhesive hydrogel according to claim 6, wherein:
the mass fraction of the nano silver modified beta-lactoglobulin fibers in the mixed solution in the step S4 is 0.25-2 wt%, and the mass fraction of the polyvinyl alcohol is 8-10 wt%;
the mass fraction of the initiator in the mixed solution in the step S4 is 0.05-1 wt%;
the mass fraction of the cross-linking agent in the mixed solution in the step S4 is 0.01-0.5 wt%;
the mass fraction of the initiation accelerator in the mixed solution in the step S4 is 0.01-0.5 wt%;
the stirring conditions described in step S4: the temperature is 0-10 ℃, the time is 5-20 min, and the speed is 100-300 rmp;
the conditions of the freeze-thaw cycle described in step S4 are: freezing temperature is-20 ℃, freezing time is 12h, thawing temperature is room temperature, thawing time is 12h, and freezing and thawing cycle is three times.
8. A conductive nanofiber dual-network adhesive hydrogel, characterized in that: obtained by the production method as claimed in any one of claims 1 to 7.
9. Use of a conductive nanofiber dual network adhesive hydrogel as recited in claim 8 in the manufacture of a sensor.
10. The use according to claim 9, characterized in that: the sensor is a flexible sensor.
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