CN111533928A - Preparation method of polyvinyl alcohol ionic conductive hydrogel with high strength and high sensitivity - Google Patents
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- 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
- A61B5/1116—Determining posture transitions
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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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
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
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- G01N2203/0017—Tensile
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N2203/0067—Fracture or rupture
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0069—Fatigue, creep, strain-stress relations or elastic constants
- G01N2203/0075—Strain-stress relations or elastic constants
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
Abstract
A process for preparing the high-strength and-sensitivity ionic-conducting polyvinyl alcohol hydrogel includes such steps as preparing polyvinyl alcohol and NaCl, and preparing the hydrogel. The preparation method comprises the following steps: 1) preparing PVA hydrogel with different crystallization times; 2) and (3) preparing PVA ionic conductive hydrogel. The invention has the advantages that: the polyvinyl alcohol ionic conductive hydrogel contains a large amount of high molecular chain entanglement caused by hydrogen bond interaction and salting-out effect, so that the polyvinyl alcohol ionic conductive hydrogel has controllable high mechanical strength. The water content in the system is high, and the directional movement of ions enables the system to have quick strain responsiveness and high sensitivity, and can realize applications such as motion monitoring and voice recognition. The gel is simple in preparation method and rich in raw materials, has adjustable and controllable performances such as high mechanical strength, high sensitivity and biodegradability compared with the traditional hydrogel, and has potential application values in the fields of tissue engineering, medical electrodes, flexible electronic skins, intelligent sensors and the like.
Description
Technical Field
The invention belongs to the field of functional polymers and tissue engineering materials, and particularly relates to a preparation method and application of polyvinyl alcohol ion conductive hydrogel with high strength and high sensitivity.
Background
The hydrogel is a flexible material with a three-dimensional network structure, has high water content and good biocompatibility, is similar to human tissues, and is widely applied to tissue engineering, medical electrodes, wound repair, flexible electronic skin, intelligent sensors and the like. However, the traditional gel material free radical polymerization preparation process is complex, the synthesis conditions are harsh, the problems of poor mechanical property, slow response speed, low sensitivity and the like exist, and the application in the field of novel wearable devices cannot be met. Polyvinyl alcohol (PVA) hydrogel is a high molecular material with good biocompatibility and biodegradability, and can be used as an artificial cornea or a human articular cartilage material and the like.
Biological bodies mainly transmit electric signals by using ions, and gel materials based on an ion conduction mechanism are widely applied to flexible electronic and sensor materials.
The development of the hydrogel material with rapid, controllable, high strength and high sensitivity has wide application prospects in the fields of flexible electronic skin, intelligent sensors, motion monitoring, voice recognition and the like.
Disclosure of Invention
The invention aims to solve the problems of complex preparation process, harsh synthesis conditions, low and uncontrollable mechanical strength of materials, slow response speed and low sensitivity of the existing hydrogel, and provides a preparation method and application of polyvinyl alcohol ion-conductive hydrogel with high strength and high sensitivity.
The technical scheme of the invention is as follows:
a preparation method of polyvinyl alcohol ion conductive hydrogel with high strength and high sensitivity comprises the following steps:
step 1) preparation of PVA hydrogels with different crystallization times
Step 1.1) placing 3-20% of polyvinyl alcohol (PVA) in mass fraction into a container, adding deionized water, heating to 90-100 ℃, and violently stirring for 2-6 hours to completely dissolve the PVA.
Step 1.2) standing the PVA solution for 5-20min, degassing by using a vacuum pump, removing bubbles in the solution, quickly transferring the solution into a mold, and standing until the solution is cooled to room temperature.
And step 1.3) putting the mould into a refrigerator with the temperature of-20 ℃ for freezing for 2-6h, then placing the mould at room temperature for unfreezing for 6-12h, and controlling the cycle times of freezing and unfreezing to be 1-3 times to obtain the PVA hydrogel with different crystallization times.
Step 2) preparation of PVA ionic conduction hydrogel
And 2.1) weighing excessive NaCl in a container, adding deionized water, and dissolving to obtain a saturated NaCl solution.
And 2.2) completely soaking the PVA hydrogel prepared in the step 1.3) in the NaCl solution obtained in the step 2.1), and controlling the soaking time to be 0.5-90min to obtain the PVA ionic conductive hydrogels with different strengths.
The performance detection method of the prepared PVA ionic conduction hydrogel comprises the following steps:
1) detection of mechanical properties of PVA ion conductive hydrogel
The PVA ionic conduction hydrogel prepared by the method is cut into a standard dumbbell-shaped sample strip with the length of 3cm and the width of 5mm, and is stretched at the speed of 50mm/min by using an universal tensile machine (Shenzhen Sansi longitudinal and transverse science and technology Co., Ltd.), and the maximum load and the elongation at break are recorded. According to the formulaThe tensile strength was calculated, among others. The maximum load before breaking in the tensile test (unit: N), and S is the cross-sectional area of the gel (unit: mm)2). The strain was controlled to 50%, 100%, 200%, 300%, 400%, 500%, and the tensile rate was 50mm/min, and a cyclic loading-unloading test was performed. To ensure data accuracy, each set of samples was tested at least 3 times and the results averaged.
2) Strain-responsiveness detection of PVA ionically conductive hydrogels
The method comprises the steps of soaking 10% of PVA hydrogel with the thickness of 1mm in a saturated sodium chloride aqueous solution, controlling the soaking time, quickly preparing a high-toughness hydrogel sensor, fixing the hydrogel on a high-precision stepping motor, respectively controlling the small strain to be 0.2%, 0.4%, 0.8% and 1%, controlling the stretching rate to be 50mm/min, controlling the large strain to be 25%, 50% and 100%, controlling the stretching rate to be 200mm/min, combining the PVA hydrogel with a digital source meter with the model of GiTIMELI 2400, and recording the change of resistance along with deformation in real time.
3) Detection of different body part movements of PVA ionically conductive hydrogels
The prepared PVA ionic conductive hydrogel is cut into different lengths and is respectively fixed on each part of a body, including the parts of fingers, wrists, elbow joints, knee joints and the like, two ends of the prepared PVA ionic conductive hydrogel are respectively connected to a digital source meter with the model of Jishili 2400 through leads and are connected with a computer, and the resistance change of the hydrogel is monitored in real time. Each action was repeated at least 5 times.
4) PVA ionic conduction hydrogel language identification detection
The prepared PVA ionic conductive hydrogel is cut into 3 multiplied by 0.8 multiplied by 0.5cm, is fixed at the position of vocal cord vibration, emits different sounds, records the resistance change caused by the vocal cord vibration in real time, records the sounds emitted by different testers, distinguishes the change of tone and the difference of different country voices, and repeats at least 5 times each action.
The invention has the advantages and beneficial effects that:
the method of the invention prepares polyvinyl alcohol hydrogel with different mass fractions and different crystallization times, and obtains PVA ionic conduction hydrogel with different strengths by changing the soaking time in NaCl saturated solution. A large amount of hydrogen bond interaction and salting-out effect in the PVA ionic conduction hydrogel cause tight chain entanglement of a high molecular chain, so that the hydrogel has good mechanical strength and excellent biocompatibility. The PVA ionic conduction hydrogel prepared by the method fully exerts the synergistic interaction of a PVA high molecular chain and NaCl, realizes the quick and effective control of the mechanical property of the hydrogel by controlling the circulating freeze-thaw times and the soaking time, has good ionic conductivity and strain responsiveness, and can realize quick response, high-sensitivity motion monitoring, voice recognition and the like.
The PVA ionic conductive hydrogel prepared by the method has high strength and high sensitivity, can play an important role in the fields of flexible electronic skin, language identification and wearable electronic equipment, and has wide application prospect.
Drawings
FIG. 1 is a diagram illustrating the mechanical property detection of PVA ionic conduction hydrogel. Wherein, a is the tensile stress-strain curve of the PVA gel in the embodiment 3 in different soaking times, and b is the cyclic tensile curve of the PVA ionic conduction hydrogel in the embodiment 3 in different strains.
FIG. 2 is a measurement of the strain responsiveness of the PVA ionically conductive hydrogel of example 3. Wherein a is a relative resistance change curve of the PVA ionic conduction hydrogel under small strain, and b is a relative resistance change curve of the PVA ionic conduction hydrogel under large strain.
FIG. 3 shows the detection of the movement of different body parts of the PVA ionically conductive hydrogel according to example 3. Wherein a is a relative resistance change curve of the PVA ionic conductive hydrogel when a finger is bent by 30 degrees, 60 degrees and 90 degrees, and b-d are relative change curves of real-time resistance when a wrist, an elbow and a knee are bent respectively.
FIG. 4 is a speech recognition test of the PVA ionically conductive hydrogel of example 3. Wherein, a and b are relative resistance change curves recorded by the PVA ionic conductive hydrogel in Chinese "Nihao" and English "Hello", respectively, and c and d are relative resistance change curves recorded by the PVA ionic conductive hydrogel in "Thankyou" of male and female testers.
Detailed Description
Example 1:
a preparation method of polyvinyl alcohol ion conductive hydrogel with high strength and high sensitivity comprises the following steps:
step 1) preparation of PVA hydrogels with different crystallization times
Step 1.1) 0.6g of polyvinyl alcohol (PVA) (3% by mass) is taken in a single-neck flask, 19.4ml of deionized water is added, the temperature is raised to 90 ℃, and the mixture is vigorously stirred for 2 hours to be completely dissolved.
Step 1.2) the PVA solution is kept still for 5min and is degassed by a vacuum pump to remove air bubbles in the solution. Quickly transferring to a mold, and standing for cooling to room temperature.
And step 1.3) putting the mold into a refrigerator with the temperature of-20 ℃ for freezing for 2h, then putting the mold under the condition of 25 ℃ for unfreezing for 6h, and controlling the times of freezing and unfreezing to be 3 times to obtain the PVA hydrogel.
Step 2) preparation of PVA ionic conduction hydrogel
Step 2.1) weighing excess NaCl in a 100ml beaker, and adding deionized water to obtain a saturated NaCl solution.
And 2.2) completely soaking the PVA hydrogel prepared in the step 1.3) in the NaCl solution obtained in the step 2.1), and controlling the soaking time to be 0.5min to obtain the PVA ionic conduction hydrogel.
Example 2:
a preparation method of polyvinyl alcohol ion conductive hydrogel with high strength and high sensitivity comprises the following steps:
step 1) preparation of PVA hydrogels with different crystallization times
Step 1.1) 1.4g of polyvinyl alcohol (PVA) (7% by mass) is taken in a single-neck flask, 18.6ml of deionized water is added, the temperature is raised to 92 ℃, and the mixture is stirred vigorously for 3 hours to be completely dissolved.
Step 1.2) the PVA solution is kept still for 8min and is degassed by a vacuum pump to remove air bubbles in the solution. Quickly transferring to a mold, and standing for cooling to room temperature.
And step 1.3) putting the mold into a refrigerator with the temperature of-20 ℃ for freezing for 4h, then putting the mold under the condition of 25 ℃ for unfreezing for 8h, and controlling the times of freezing and unfreezing to be 3 times to obtain the PVA hydrogel.
Step 2) preparation of PVA ionic conduction hydrogel
Step 2.1) weighing excess NaCl in a 200ml beaker, and adding deionized water to obtain a saturated NaCl solution.
And 2.2) completely soaking the PVA hydrogel prepared in the step 1.3) in the solution in the step 2.1), and controlling the soaking time to be 10min to obtain the PVA ionic conduction hydrogel.
Example 3:
a preparation method of polyvinyl alcohol ion conductive hydrogel with high strength and high sensitivity comprises the following steps:
step 1) preparation of PVA hydrogels with different crystallization times
Step 1.1) 2g of polyvinyl alcohol (PVA) (10% by mass) is taken in a single-neck flask, 18ml of deionized water is added, the temperature is raised to 95 ℃, and the mixture is vigorously stirred for 4 hours to be completely dissolved.
Step 1.2) the PVA solution is kept still for 10min and is degassed by a vacuum pump to remove air bubbles in the solution. Quickly transferring to a mold, and standing for cooling to room temperature.
And step 1.3) putting the mold into a refrigerator with the temperature of-20 ℃ for freezing for 6h, then putting the mold under the condition of 25 ℃ for unfreezing for 12h, and controlling the times of freezing and unfreezing to be 3 times to obtain the PVA hydrogel.
Step 2) preparation of PVA ionic conduction hydrogel
Step 2.1) weighing excess NaCl in a 500ml beaker, and adding deionized water to obtain a saturated NaCl solution.
And 2.2) completely soaking the PVA hydrogel prepared in the step 1.3) in the solution in the step 2.1), and controlling the soaking time to be 10min to obtain the PVA ionic conduction hydrogel.
Example 4:
a preparation method of polyvinyl alcohol ion conductive hydrogel with high strength and high sensitivity comprises the following steps:
step 1) preparation of PVA hydrogels with different crystallization times
Step 1.1) 2g of polyvinyl alcohol (PVA) (10% by mass) is taken in a single-neck flask, 18ml of deionized water is added, the temperature is raised to 95 ℃, and the mixture is vigorously stirred for 6 hours to be completely dissolved.
Step 1.2) the PVA solution is kept still for 15min and is degassed by a vacuum pump to remove air bubbles in the solution. Quickly transferring to a mold, and standing for cooling to room temperature.
And step 1.3) putting the mold into a refrigerator with the temperature of-20 ℃ for freezing for 6h, then putting the mold under the condition of 25 ℃ for unfreezing for 12h, and controlling the times of freezing and unfreezing to be 3 times to obtain the PVA hydrogel.
Step 2) preparation of PVA ionic conduction hydrogel
Step 2.1) weighing excess NaCl in a 500ml beaker, and adding deionized water to obtain a saturated NaCl solution.
And 2.2) completely soaking the PVA hydrogel prepared in the step 1.3) in the solution obtained in the step 2.1), and controlling the soaking time to be 90min to obtain the PVA ionic conduction hydrogel.
Detection of the PVA ionic-conductive hydrogel:
1) detection of mechanical properties of PVA ion conductive hydrogel
The PVA ionic conduction hydrogel prepared in the example 3 is cut into a standard dumbbell-shaped sample bar, stretched at a speed of 50mm/min by using an universal tensile machine (Shenzhen Sansi technologies, Inc.), the maximum load and the elongation at break are recorded, the mechanical properties are measured, the strains are controlled to be 50%, 100%, 200%, 300%, 400% and 500%, and the stretching rate is 50mm/min, and a cyclic unloading-loading test is carried out. The detection results are shown in FIG. 1, wherein: FIG. a is a tensile stress-strain curve of the PVA gel of example 3 soaked for various periods of time, and FIG. b is a cyclic tensile curve of the PVA ionically conductive hydrogel of example 3 under various strains. From the results, it can be seen that the mechanical properties of the hydrogel gradually increased with the change of the soaking time, the tensile strength was 0.583MPa and the elongation at break was 230% without soaking, and after soaking for 10min, the tensile strength was 8.03MPa, the elongation at break was 730%, the mechanical strength was increased by 13.77 times, and the elongation at break was increased by 3.17 times. FIG. b is a cyclic extension curve of the PVA ion-conducting hydrogel of example 3, showing that the hydrogel has excellent mechanical properties.
2) Strain-responsiveness detection of PVA ionically conductive hydrogels
The PVA hydrogel with the thickness of 1mm in the embodiment 3 is soaked in a saturated sodium chloride aqueous solution, the soaking time is controlled, a high-toughness hydrogel sensor can be quickly prepared, the hydrogel is fixed on a high-precision stepping motor, the small strain is respectively controlled to be 0.2%, 0.4%, 0.8% and 1%, the stretching speed is 50mm/min, the large strain is controlled to be 25%, 50% and 100%, the stretching speed is 200mm/min, the PVA hydrogel is used with a digital source meter with the model of GiTIMELI 2400, and the change of the resistance along with the deformation is recorded in real time. The detection results are shown in FIG. 2, in which: the graph a is a relative resistance change curve of the PVA ionic conduction hydrogel when the strain is 0.2%, 0.4%, 0.8% and 1%, and the graph b is a relative resistance change curve of the PVA ionic conduction hydrogel when the strain is 25%, 50% and 100%. As can be seen from the results, the graphs a and b show that the PVA ionic conduction hydrogel prepared in the example 3 has rapid strain response to different strains, and when the fixed strain is maintained, the relative resistance change of the hydrogel is basically kept unchanged, which shows that the PVA ionic conduction hydrogel has good strain response stability.
3) Detection of different body part movements of PVA ionically conductive hydrogels
The PVA ionic conduction hydrogel with different lengths in the embodiment 3 is respectively fixed on each part of a body, including the parts of fingers, wrists, elbow joints, knee joints and the like, and two ends of the PVA ionic conduction hydrogel are respectively connected to a digital source meter with the model of Jishili 2400 through leads and are connected with a computer, so that the resistance change of the hydrogel is monitored in real time. The results of the tests are shown in FIG. 3, in which: FIG. a shows the relative resistance change curves of the PVA ionic conductive hydrogel in the embodiment 3 when the finger is bent at 30 degrees, 60 degrees and 90 degrees, and b-d show the relative resistance change curves when the wrist, elbow and knee are bent. The result shows that the gel has rapid strain responsiveness, can monitor the motion change of each part of the body in real time, can distinguish the change behavior of different parts of the body, and can recover the relative resistance change when the deformation recovers, thereby having high sensitivity and strain responsiveness.
4) PVA ionic conduction hydrogel language identification detection
The hydrogel of 3 × 0.8 × 0.5cm in size in example 3 was fixed at the position where the vocal cords vibrate and different sounds were emitted, the resistance change caused by the vocal cords vibration was recorded in real time, and the sounds emitted by different testers were recorded, and the change in tone color and the difference in different national voices were distinguished. The results of the measurements are shown in FIG. 4, in which: FIGS. a and b are the relative resistance change curves of Chinese "Nihao" and English "Hello" recorded by the PVA ion-conductive hydrogel in example 3, respectively, and FIGS. c and d are the relative resistance change curves of "Thankyou" of male and female testers recorded by the PVA ion-conductive hydrogel, respectively. As can be seen from the results, the hydrogel not only can distinguish different languages of Chinese and English, but also can identify the tone color changes of different testers. Therefore, the method has potential application value in the fields of wearable electronic equipment and motion monitoring language identification.
Claims (2)
1. A preparation method of polyvinyl alcohol ion conductive hydrogel with high strength and high sensitivity comprises the following steps:
step 1) preparation of PVA hydrogels with different crystallization times
Step 1.1) placing 3-20% of polyvinyl alcohol (PVA) in mass fraction in a container, adding deionized water, heating to 90-100 ℃, and violently stirring for 2-6 hours to completely dissolve the PVA;
step 1.2) standing the PVA solution for 5-20min, degassing by using a vacuum pump, removing bubbles in the solution, quickly transferring the solution into a mold, and standing until the solution is cooled to room temperature;
step 1.3) putting the mould into a refrigerator with the temperature of-20 ℃ for freezing for 2-6h, then putting the mould under the condition of room temperature, unfreezing for 6-12h, wherein the cycle times of freezing and unfreezing are 1-3 times, and obtaining PVA hydrogel with different crystallization times;
step 2) preparation of PVA ionic conduction hydrogel
Step 2.1) weighing excessive NaCl in a container, adding deionized water, and dissolving to obtain a saturated NaCl solution;
and 2.2) completely soaking the PVA hydrogel prepared in the step 1.3) in the NaCl solution obtained in the step 2.1), and controlling the soaking time to be 0.5-90min to obtain the PVA ionic conductive hydrogels with different strengths.
2. The method for preparing a high-strength and high-sensitivity polyvinyl alcohol ion-conducting hydrogel according to claim 1, wherein the method comprises the following steps: the molecular weight of the polyvinyl alcohol (PVA) is 146000-186000.
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CN113980296A (en) * | 2021-11-17 | 2022-01-28 | 江南大学 | High-tensile photocuring ionic-conductive hydrogel and preparation method thereof |
CN113999418A (en) * | 2021-11-23 | 2022-02-01 | 南京财经大学 | Polyvinyl alcohol material with multistage anisotropy as well as preparation method and application thereof |
CN115262027A (en) * | 2022-07-18 | 2022-11-01 | 浙江理工大学 | Preparation method of high-strength conductive hydrogel fiber with skin-core structure |
CN116178865A (en) * | 2023-03-03 | 2023-05-30 | 大连理工大学 | Transparent conductive hydrogel with high compressive strength and low energy dissipation and preparation method thereof |
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