CN112080020A - Preparation method and application of self-damage-identification type optical detection self-healing hydrogel - Google Patents
Preparation method and application of self-damage-identification type optical detection self-healing hydrogel Download PDFInfo
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Abstract
The invention discloses a preparation method and application of self-identifiable damage type photo-detection self-healing hydrogel, and belongs to the technical field of polymer hydrogel. The method comprises the following steps: soaking the self-healing hydrogel in a solution of water-soluble fluorescent quantum dots to obtain the light detection self-healing hydrogel; the self-healing hydrogel is prepared by dissolving acrylic acid, ferric trichloride hexahydrate, acrylamide and potassium persulfate in a glycerol aqueous solution and reacting; the water-soluble fluorescent quantum dots are luminescent materials combined with the self-healing hydrogel through hydrogen bonds. The light detection self-healing hydrogel not only has high mechanical strength and excellent self-healing performance, but also has adjustable and concealed fluorescence characteristics, and has great potential in the fields of tissue engineering coating, sensing, self-recognition damage and the like.
Description
Technical Field
The invention belongs to the technical field of polymer hydrogel, and particularly relates to a preparation method and application of self-identifiable damage type photo-detection self-healing hydrogel.
Background
Self-healing hydrogels have some self-healing capabilities, however, rapid self-healing at room temperature without external stimuli using existing methods remains challenging. Particularly, the compound self-healing material with optical response characteristic has extremely high application potential in more fields. However, when optical characteristics are generated in a matrix, luminescent molecular groups need to be introduced, but large-scale synthesis of the introduced chromogenic groups has great difficulty, so that development of the conveniently synthesized luminous hydrogel has great significance in optical damage measurement, biological materials, tissue engineering and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of self-identifiable damage type light detection self-healing hydrogel, which comprises the following steps: soaking the self-healing hydrogel in a solution of water-soluble fluorescent quantum dots to obtain the light detection self-healing hydrogel;
the self-healing hydrogel is prepared by dissolving acrylic acid, ferric trichloride hexahydrate, acrylamide and potassium persulfate in a glycerol aqueous solution and reacting;
the water-soluble fluorescent quantum dots are luminescent materials combined with the self-healing hydrogel through hydrogen bonds.
The water-soluble fluorescent quantum dots comprise carbon quantum dots, graphene quantum dots and silicon quantum dots.
The self-healing hydrogel is obtained by heat preservation reaction for 4 hours at the stirring speed of 600r/min and the temperature of 25 ℃.
The concentration of the solution of the water-soluble fluorescent carbon quantum dots is 1-10 wt%, the soaking time is 1-10h, and preferably, the concentration of the solution of the water-soluble fluorescent carbon quantum dots is 3 wt%, and the soaking time is 6 h.
The volume ratio of water to glycerol in the glycerol aqueous solution is 5:1-1: 1.
The adding mass ratio of the potassium persulfate to the acrylic acid is 1:100-20: 100; the adding mass ratio of the acrylic acid to the ferric trichloride hexahydrate is 1:100-5: 100; the adding mass ratio of the acrylamide to the acrylic acid is 1:100-5: 100.
The water-soluble fluorescent carbon quantum dots are synthesized by adopting a high-temperature kettle thermal method.
The self-identifiable damage type light detection self-healing hydrogel prepared by the preparation method.
The light detection self-healing hydrogel can be used for detecting the damaged part under ultraviolet light, and the reason is that the hydrogel is brought into the water-soluble fluorescent quantum dots and uniformly dispersed in the network structure on the surface of the hydrogel, and the self structure of the water-soluble fluorescent quantum dots is not damaged, so that the water-soluble fluorescent quantum dots can generate fluorescence under the excitation of the ultraviolet light, and the water-soluble fluorescent quantum dots are lost due to the damage of the network structure at the damaged part, and the damaged area is easily detected due to the fact that no fluorescence or weak fluorescence brightness exists in the ultraviolet light and is compared with the undamaged part.
The light detection self-healing hydrogel can perform self-healing action, and the main cross-linked network of the network consists of carboxylate radical and Fe3+Forming ion coordination bonds, and strengthening the secondary crosslinking network by weak hydrogen bonds N-H.H between amino bonds and hydrogen bonds between quantum dots and a network structure. When the network structure is damaged, the reversible ionic bond and weak hydrogen bond double network are utilized to repair.
The self-discriminable damage type light detection self-healing hydrogel is applied to medical materials, stretchable bioelectronic devices and soft robot materials.
The self-identifiable damage type optical detection self-healing hydrogel is soaked in a solution of water-soluble fluorescent quantum dots to obtain adjustable and covert fluorescence properties.
The self-identifiable damage type light detection self-healing hydrogel has the application of enhancing the fluorescence identification damage characteristic, the fluorescence adjustable concealment characteristic, the electrical conductivity, the stretchability, the plasticity, the self-healing property and the light transmittance of materials.
The invention has the beneficial effects that:
1. the self-healing hydrogel is endowed with adjustable and hidden fluorescence performance by introducing the water-soluble fluorescent quantum dots, the preparation method is simple and convenient, the fluorescence effect is good, the water-soluble fluorescent quantum dots in the light detection self-healing hydrogel are uniformly distributed, a specific color is displayed after the light detection self-healing hydrogel is excited by ultraviolet light, and the damaged part can be observed by utilizing the self-fluorescence characteristic so as to give early warning on material breakage.
2. The photo-detection self-healing hydrogel can be used for manufacturing stretchable electronic devices, soft robots or sensors (such as strain sensors), medical monitoring equipment and the like by utilizing the conductivity and the performance that the current changes when the hydrogel is stretched and bent.
3. The light detection self-healing hydrogel prepared by combining the water-soluble fluorescent quantum dots and the self-healing hydrogel matrix is a novel composite hydrogel material. Overcomes the balance limit between the mechanical property and the repair time of the prior hydrogel and the application range. The reversible action of the ion coordination bond is utilized to improve the self-healing performance of the hydrogel.
4. The light detection self-healing hydrogel can self-identify a damaged area under the condition that the fluorescence wavelength is 365nm, and meanwhile, the hydrogel self-heals within 15min at room temperature, so that the hydrogel has extremely high tensile strength (the tensile strength can reach 1.19 MPa); excellent tensile properties (elongation up to 1650%); plasticity, adhesion, conductivity, etc.
5. According to the preparation method of the light detection self-healing hydrogel, the light detection self-healing hydrogel can be prepared by a simple mixing method, and then the light detection self-healing hydrogel can be obtained by simple soaking, so that the preparation method is simple and convenient, and is convenient for large-scale production; the adopted raw materials exist in large quantity, are convenient and easy to obtain, and are green and environment-friendly.
6. The light detection self-healing hydrogel is applied as a self-healing material, and the cross-linking mode in the self-healing hydrogel is reversible ion coordination and weak hydrogen bond action between amino groups, so that the structure of the light detection self-healing hydrogel is damaged when the shear stress is 1-1000Pa, and the original mechanical property of the light detection self-healing hydrogel can be recovered within 15 min.
Drawings
Fig. 1 is a graph showing the stress-strain test results of the self-healing hydrogel of the present invention.
FIGS. 2 a-2 e are photographs showing the luminescence of the hydrogels prepared in examples 1-5 under UV light, respectively.
Fig. 3 a-3 f are top-down photographs of hydrogels loaded with different masses of fluorescent carbon quantum dot particles under an ultraviolet lamp.
FIG. 4 is a photograph of a cross section of a carbon quantum dot-loaded hydrogel under an ultraviolet lamp.
FIGS. 5a and 5b are photographs of the light emission of the carbon quantum dot loaded hydrogel under an ultraviolet lamp before and after breakage.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
citric acid, formamide, Acrylic Acid (AA), AR > 99%, manufacturer all mireline,
ferric chloride hexahydrate (FeCl)3·6H2O), analytically pure AR, chemical reagents of traditional chinese medicine stock control limited,
potassium persulfate, AR, national drug-controlled chemical reagents GmbH,
acrylamide AAm, AR > 99.0%, Ron reagent.
The above reagents were used as received without further purification.
Example 1
Preparation of self-healing hydrogel capable of self-identifying damage based on light detection
S1: at room temperature, 25mL of acrylic acid was weighed into a three-necked flask, and 1.5g of FeCl was respectively weighed3·6H2O, 0.45g of ammonium persulfate and 1.5g of acrylamide were dissolved in 50mL10% glycerol in water. And after complete dissolution, adding the mixture into a three-neck flask, uniformly stirring, mechanically stirring for 4 hours (stirring speed is 600r/min) at room temperature in a nitrogen atmosphere to obtain a solution, placing the solution into a mold to form 2 hours, and preparing to obtain the formed self-healing hydrogel.
S2: weighing 1.50g of citric acid, and dissolving the citric acid in 30mL of formamide and 20mL of deionized water to obtain a colorless transparent solution; then transferring the colorless and transparent uniform solution to a 100mL polytetrafluoroethylene reaction kettle to react for 5h at 180 ℃; and after the reaction kettle is naturally cooled to room temperature, carrying out centrifugal separation on the dark red solution, filtering the solution obtained by centrifugal separation by using a filter membrane of 0.22 mu m, and finally freeze-drying the solution in a freeze dryer to prepare the water-soluble fluorescent carbon quantum dot particles.
S3, dissolving 1g of water-soluble fluorescent carbon quantum dot particles prepared in the step S2 in 100mL of deionized water, and soaking the formed self-healing hydrogel prepared in the step S1 in a water-soluble fluorescent carbon quantum dot solution for 4 hours to obtain the light detection self-healing hydrogel.
Examples 2 to 9
The steps S1-S2 are the same as in example 1, and the mass of the fluorescent carbon quantum dot particles, the volume of deionized water, and the soaking time in the S3 process are shown in table 1, and the others are the same as in example 1.
Table 1S 3 Process parameters from examples 1-9
| Examples | Fluorescent carbon quantum dot particle mass/g | Deionized Water/mL | Soaking time/ |
| 1 | 1 | 100 | 4 |
| 2 | 2 | 100 | 4 |
| 3 | 3 | 100 | 4 |
| 4 | 4 | 100 | 4 |
| 5 | 5 | 100 | 4 |
| 6 | 3 | 100 | 2 |
| 7 | 3 | 100 | 6 |
| 8 | 3 | 100 | 8 |
| 9 | 3 | 100 | 10 |
Comparative example 1
25mL of acrylic acid was weighed into a three-necked flask, and 1.5g of FeCl was respectively weighed30.45g of ammonium persulfate and 1.5g of acrylamide were dissolved in 50mL of 10% aqueous glycerol solution. And after complete dissolution, adding the mixture into a three-neck flask, uniformly stirring, mechanically stirring for 4 hours (stirring speed is 600r/min) at room temperature in a nitrogen atmosphere to obtain a solution, placing the solution into a mold to form 2 hours, and preparing to obtain the formed self-healing hydrogel.
Example 10
Mechanical tests were performed on the photo-detection self-healing hydrogel obtained in example 1 and the photo-detection self-healing hydrogel after self-healing after external force failure in example 1, and it can be seen from fig. 1 that the photo-detection self-healing hydrogel had an original tensile stress of 1.19MPa and a tensile strain of 1650%. The initial self-healing hydrogel tensile stress is 0.85MPa, and the tensile strain is 1450%. The original mechanical properties are recovered within 15 min.
Example 11
The solutions of the water-soluble fluorescent quantum dot particles prepared in examples 1 to 5 were observed under an ultraviolet lamp.
The experimental results are shown in the attached figures 2 a-2 e: the solution concentrations of the water-soluble fluorescent quantum dots are respectively 1 wt%, 2 wt%, 3 wt%, 4 wt% and 5 wt%; as is apparent from the figure, in example 3, the solution of 3 wt% water-soluble fluorescent quantum dots has good fluorescence characteristics.
Meanwhile, the self-healing hydrogel prepared in comparative example 1 and the light detection self-healing hydrogel prepared in examples 1 to 5 were observed under an ultraviolet lamp. The experimental results are shown in the attached figures 3 a-3 f, and the concentrations of the water-soluble fluorescent quantum dots are respectively 0, 1 wt%, 2 wt%, 3 wt%, 4 wt% and 5 wt%; further proves that the solution of the 3 wt% water-soluble fluorescent quantum dots has good fluorescence characteristics.
Example 12
The photodetecting self-healing hydrogel prepared in example 3 and examples 6 to 9 was soaked for 2 hours, 4 hours, 6 hours, 8 hours, and 10 hours, respectively, and fluorescence detection was performed, and it was found from experimental results that the photodetecting self-healing hydrogel obtained in example 7 with the soaking time of 6 hours had excellent fluorescence characteristics.
Example 13
The light-detecting self-healing hydrogels prepared in examples 1 to 9 were observed in cross section.
The test method comprises the following steps: the prepared photo-detection self-healing hydrogel is used for incision and observation under ultraviolet rays and the like. Fig. 4 shows a cross-sectional photograph of a photo-detecting self-healing hydrogel: the fluorescence effect is only shown to exist on the surface layer of the hydrogel, and the internal hydrogel has no fluorescence.
Example 14
The photo-detecting self-healing hydrogels prepared in examples 1-9 were subjected to abrasion fluorescence testing.
The test method comprises the following steps: the photo-detection self-healing hydrogels prepared in examples 1 to 9 were subjected to surface partial abrasion, and after abrasion, they were observed under an ultraviolet lamp having a wavelength of 365 nm. FIGS. 5a and 5b show photographs of photo-detectable self-healing hydrogels before and after abrasion. The light detection self-healing hydrogel has a fluorescent characteristic on the surface before abrasion, and after abrasion, the fluorescent characteristic of an abraded part disappears, so that the defect part can be better confirmed.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention (for example, the quantum dot solution infiltration method is not limited to carbon quantum dots, but also graphene quantum dots, silicon quantum dots, and other luminescent materials capable of hydrogen bonding with hydrogel).
Claims (9)
1. A preparation method of self-damage-identification type optical detection self-healing hydrogel is characterized by comprising the following steps: soaking the self-healing hydrogel in a solution of water-soluble fluorescent quantum dots to obtain the light detection self-healing hydrogel;
the self-healing hydrogel is prepared by dissolving acrylic acid, ferric trichloride hexahydrate, acrylamide and potassium persulfate in a glycerol aqueous solution and reacting;
the water-soluble fluorescent quantum dots are luminescent materials combined with the self-healing hydrogel through hydrogen bonds.
2. The preparation method of claim 1, wherein the water-soluble fluorescent quantum dots comprise carbon quantum dots, graphene quantum dots and silicon quantum dots.
3. The method according to claim 1, wherein the self-healing hydrogel is prepared by stirring at 600r/min and maintaining at 25 ℃ for 4 hours.
4. The preparation method of claim 1, wherein the concentration of the solution of the water-soluble fluorescent carbon quantum dots is 1-10 wt%, and the soaking time is 1-10 h.
5. The method according to claim 1, wherein the ratio of water to glycerol in the aqueous glycerol solution is 5:1 to 1:1 by volume.
6. The production method according to claim 1, wherein the addition mass ratio of the potassium persulfate to the acrylic acid is from 1:100 to 20: 100; the adding mass ratio of the acrylic acid to the ferric trichloride hexahydrate is 1:100-5: 100; the adding mass ratio of the acrylamide to the acrylic acid is 1:100-5: 100.
7. The preparation method of claim 2, wherein the water-soluble fluorescent carbon quantum dots are synthesized by a high-temperature kettle thermal method.
8. The self-identifiable damage-type photodetecting self-healing hydrogel prepared by the preparation method according to any one of claims 1 to 7.
9. The use of the self-identifiable damage-type light-detecting self-healing hydrogel according to claim 8 in medical materials, stretchable bioelectronic devices, and soft robotic materials.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113603993A (en) * | 2021-07-13 | 2021-11-05 | 南京工业大学 | Preparation method of self-healing polymer-nano composite material |
| CN115575341A (en) * | 2022-12-07 | 2023-01-06 | 之江实验室 | Self-healing material characterization method based on transmission spectrum change |
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