CN109337014B - High-elongation high-strength double-network hydrogel and preparation method thereof - Google Patents
High-elongation high-strength double-network hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of hydrogel, in particular to a high-elongation high-strength double-network hydrogel which comprises the following raw materials in parts by weight: 20-45 parts of acrylamide, 1-4 parts of curdlan, 0.4227-3.2143 parts of octadecyl methacrylate, 0.448 part of initiator, 7.435-8.747 parts of cetyl trimethyl ammonium bromide, 0-1.038 parts of sodium dodecyl sulfate and 100 parts of high-purity water. The invention also discloses a preparation method of the high-elongation high-strength double-network hydrogel. The curdlan and the polyacrylamide are used as base materials, and the prepared hydrogel has high strength and good fracture toughness.
Description
Technical Field
The invention relates to the technical field of hydrogel, in particular to high-elongation high-strength double-network hydrogel and a preparation method thereof.
Background
The polymer hydrogel is a material capable of absorbing a large amount of water into an internal three-dimensional space network structure, and the hydrogel is soft and elastic after absorbing water, and the characteristic is similar to that of a plurality of biological soft tissues, so that the hydrogel has wide potential application in the field of tissue engineering.
At present, most of high polymer hydrogels have the defects of low mechanical strength, poor toughness, poor recoverability and fatigue resistance and the like due to non-uniform structures or lack of an effective energy dissipation mechanism, and the defects greatly limit the high polymer hydrogels from becoming biomaterials for soft tissue repair and even regeneration. Therefore, the improvement of the mechanical strength, toughness, self-repairing capability and fatigue resistance of the polymer hydrogel is a major problem to be solved urgently when the polymer hydrogel is applied to the field of tissue engineering.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides a high-elongation high-strength double-network hydrogel and a preparation method thereof, so as to make up for the defects of low mechanical strength, poor toughness, poor recoverability and poor fatigue resistance of the conventional hydrogel.
The invention provides a high-elongation high-strength double-network hydrogel which comprises the following raw materials in parts by weight: 20-45 parts of acrylamide, 1-4 parts of curdlan, 0.4227-3.2143 parts of octadecyl methacrylate, 0.448 part of initiator, 7.435-8.747 parts of cetyl trimethyl ammonium bromide, 0-1.038 parts of sodium dodecyl sulfate and 100 parts of high-purity water.
Preferably, the initiator is the photoinitiator Irgacure 2959.
The invention also provides a preparation method of the high-elongation high-strength double-network hydrogel, which comprises the following steps:
s1, sequentially dissolving sodium dodecyl sulfate, cetyl trimethyl ammonium bromide, stearyl methacrylate, an initiator and acrylamide in the high-purity water in a water bath according to the parts by weight to obtain a mixed solution; cooling the mixed solution to room temperature, adding curdlan, and uniformly mixing to obtain a suspension;
s2, introducing argon gas into the suspension for 10min for exhausting, stirring the suspension at room temperature in an inert gas atmosphere, then sequentially vacuumizing the suspension under the conditions of standing and magnetic stirring by using a vacuum pump, and removing bubbles in the suspension to obtain a mixed material;
s3, pouring the mixed material into an acrylic mold, covering a quartz cover glass and removing bubbles, sealing the material, heating the sealed material, cooling to room temperature, placing the sealed material under an ultraviolet lamp for irradiation, controlling the height of the ultraviolet lamp from the material to be 6.5cm, and carrying out cross-linking polymerization under the ultraviolet condition to obtain the high-elongation high-strength double-network hydrogel.
Preferably, in S1, the temperature of the water bath is 30-40 ℃.
Preferably, in S1, the cetyl trimethyl ammonium bromide is dissolved by stirring, and the stirring time is 20-30 min.
Preferably, in S1, the octadecyl methacrylate is dissolved by stirring, and the stirring time is 2-4 h.
Preferably, in S2, the suspension is stirred for 20-24 h.
Preferably, in S2, the vacuum-pumping time is 10-15 min.
Preferably, in S3, the heating temperature of the material is 90-120 deg.C, and the heating time is 5-15 min.
Preferably, in S3, the wavelength of the ultraviolet lamp is 300-400nm, the power is 20-40W, and the irradiation time is 0.5-1.5 h.
Preferably, the wavelength of the ultraviolet lamp is 365nm, the power is 30W, and the irradiation time is 1 h.
The high-purity water is high-purity water subjected to deoxidization treatment, and the deoxidization treatment specifically comprises the following operations: pumping high purity water for 20min by a vacuum pump, inserting the gas guide tube into the bottom of the high purity water, and introducing argon for 1 h.
Has the advantages that: the curdlan and the acrylamide are crosslinked through physical action, the micelles of the curdlan are crosslinked through hydrophobic action, and the acrylamide is crosslinked through hydrophobic action between copolymerized stearyl methacrylate and surfactant micelles; the double-network physical crosslinking mode improves the mechanical strength, toughness, self-repairing capability and fatigue resistance of the invention.
Drawings
Fig. 1 is a stress-strain curve comparison diagram of a high-elongation and high-strength double-network hydrogel prepared by cetyl trimethyl ammonium bromide (abbreviated as CTAB) and Sodium dodecyl sulfate (abbreviated as SDS) according to different mixture ratios of the present invention.
FIG. 2 is a graph showing the stress-strain curve of a high-elongation and high-strength double-network hydrogel prepared by mixing Stearyl Methacrylate (SMA) and Acrylamide (AAm) according to the present invention.
FIG. 3 is a graph comparing stress-strain curves of high-elongation, high-strength, two-network hydrogels made with different amounts of acrylamide and stearyl methacrylate.
FIG. 4 is a graph comparing stress-strain curves of high elongation, high strength, dual network hydrogels made with different amounts of Curdlan gum according to the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A high-elongation high-strength double-network hydrogel comprises the following raw materials in parts by weight: 28 parts of acrylamide, 3 parts of curdlan, 2 parts of octadecyl methacrylate, 0.448 part of initiator, 7.872 parts of hexadecyl trimethyl ammonium bromide, 0.692 part of sodium dodecyl sulfate and 100 parts of high-purity water;
wherein the initiator is a photoinitiator Irgacure 2959.
The preparation method of the high-elongation high-strength double-network hydrogel comprises the following steps:
s1, sequentially dissolving sodium dodecyl sulfate, cetyl trimethyl ammonium bromide, stearyl methacrylate, an initiator and acrylamide in the high-purity water in a water bath according to the parts by weight to obtain a mixed solution; cooling the mixed solution to room temperature, adding curdlan, and uniformly mixing to obtain a suspension;
s2, introducing argon gas into the suspension for 10min for exhausting, stirring the suspension at room temperature in an inert gas atmosphere, then sequentially vacuumizing the suspension under the conditions of standing and magnetic stirring by using a vacuum pump, and removing bubbles in the suspension to obtain a mixed material;
s3, pouring the mixed material into an acrylic mold, covering a quartz cover glass and removing bubbles, sealing the material, heating the sealed material, cooling to room temperature, placing the sealed material under an ultraviolet lamp for irradiation, controlling the height of the ultraviolet lamp from the material to be 6.5cm, and performing cross-linking polymerization under the ultraviolet condition to obtain the high-elongation high-strength double-network hydrogel;
wherein in S1, the temperature of the water bath is 35 ℃;
in S1, the hexadecyl trimethyl ammonium bromide is stirred and dissolved for 20 min;
in S1, stirring and dissolving the octadecyl methacrylate for 2 h;
in S2, stirring the suspension for 20 h;
in S2, vacuumizing for 10 min;
in S3, heating the material at 100 ℃ for 10 min;
in S3, the wavelength of the ultraviolet lamp is 365nm, the power is 30W, and the irradiation time is 1 h.
Comparative example 1
A high-elongation high-strength double-network hydrogel, which comprises 8.747 parts of hexadecyl trimethyl ammonium bromide and 0 part of lauryl sodium sulfate, and the rest of the components and the preparation method are the same as those in the example 1.
Comparative example 2
A high-elongation high-strength double-network hydrogel, which comprises 8.309 parts of cetyltrimethylammonium bromide and 0.346 part of sodium dodecyl sulfate and has the same components and preparation method as example 1.
Comparative example 3
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 7.872 parts of cetyltrimethylammonium bromide and 0.692 part of sodium lauryl sulfate were used.
Comparative example 4
A high-elongation high-strength double-network hydrogel, which comprises 7.435 parts of hexadecyl trimethyl ammonium bromide and 1.038 parts of sodium dodecyl sulfate, and the rest of the components and the preparation method are the same as those in the example 1.
Test example 1
The performance tests of the high-elongation high-strength double-network hydrogel obtained in comparative examples 1-4 are respectively carried out, and the obtained stress (S) -strain (lambda) curve contrast graph is shown in FIG. 1; as can be seen from FIG. 1, the Young's modulus of the high-elongation high-strength double-network hydrogel remained substantially unchanged while the fracture strain decreased gradually, that is, the mechanical strength of the hydrogel remained substantially unchanged and the fracture toughness decreased gradually, with the increase of the amount of cetyltrimethylammonium bromide and the decrease of the amount of sodium lauryl sulfate.
Comparative example 5
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 29.58 parts of acrylamide and 0.4227 parts of octadecyl methacrylate were used.
Comparative example 6
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 29.30 parts of acrylamide and 0.6973 parts of octadecyl methacrylate were used.
Comparative example 7
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 28.64 parts of acrylamide and 1.363 parts of octadecyl methacrylate were used.
Comparative example 8
A high-elongation high-strength double-network hydrogel is prepared by the same steps as example 1 except that 28 parts of acrylamide and 2 parts of octadecyl methacrylate are added.
Comparative example 9
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 27.39 parts of acrylamide and 2.609 parts of octadecyl methacrylate were used.
Comparative example 10
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 26.81 parts of acrylamide and 3.191 parts of octadecyl methacrylate were used.
Test example 2
Respectively carrying out performance tests on the high-elongation high-strength double-network hydrogel obtained in the comparative examples 5-10, and obtaining a stress-strain curve contrast diagram as shown in FIG. 2; as can be seen from FIG. 2, with the decrease of the amount of acrylamide and the increase of the amount of stearyl methacrylate, the Young's modulus of the high-elongation high-strength double-network hydrogel gradually increases, the breaking strain gradually increases and then gradually decreases, that is, the mechanical strength of the hydrogel gradually increases, and the fracture toughness gradually increases and then gradually decreases.
Comparative example 11
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 20 parts of acrylamide and 1.4286 parts of octadecyl methacrylate were used.
Comparative example 12
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 25 parts of acrylamide and 1.7857 parts of octadecyl methacrylate were used.
Comparative example 13
A high-elongation high-strength double-network hydrogel is prepared from the following components in parts by weight, except that 30 parts of acrylamide and 2.1429 parts of octadecyl methacrylate, and the preparation method is the same as that of example 1.
Comparative example 14
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 35 parts of acrylamide and 2.0588 parts of octadecyl methacrylate were used.
Comparative example 15
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that the amount of acrylamide was 40 parts and the amount of octadecyl methacrylate was 2.8571 parts.
Comparative example 16
A high-elongation high-strength double-network hydrogel was prepared by following the same procedures as in example 1, except that 45 parts of acrylamide and 3.2143 parts of octadecyl methacrylate were used.
Test example 3
Respectively carrying out performance tests on the high-elongation high-strength double-network hydrogel obtained in comparative examples 11-16, and obtaining a stress-strain curve contrast diagram as shown in FIG. 3; as can be seen from FIG. 3, the Young's modulus of the high-elongation high-strength double-network hydrogel gradually increases with the increase of the amount of acrylamide, the strain at break gradually increases and then gradually decreases, that is, the mechanical strength of the hydrogel gradually increases, and the fracture toughness gradually increases and then gradually decreases.
Comparative example 17
A high-elongation high-strength double-network hydrogel, the other components and the preparation method are the same as those in example 1 except that 1 part of curdlan is used.
Comparative example 18
The components and the preparation method of the double-network hydrogel with high elongation and high strength are the same as those in example 1 except that 2 parts of curdlan is used.
Comparative example 19
The components and preparation method of the double-network hydrogel with high elongation and high strength are the same as those in example 1 except that 3 parts of curdlan is adopted.
Comparative example 20
A high-elongation high-strength double-network hydrogel, the other components and the preparation method are the same as those of the example 1 except that 3.5 parts of curdlan is adopted.
Comparative example 21
The components and preparation method of the double-network hydrogel with high elongation and high strength are the same as those in example 1 except that the curdlan is 4 parts.
Test example 4
Respectively carrying out performance tests on the high-elongation high-strength double-network hydrogel obtained in the comparative examples 17-21, and obtaining a stress-strain curve comparison diagram as shown in FIG. 4; as can be seen from fig. 4, as the amount of the curdlan increases, the young's modulus of the high-elongation high-strength double-network hydrogel gradually increases, the breaking strain gradually increases and then gradually decreases, that is, the mechanical strength of the hydrogel gradually increases, and the fracture toughness gradually increases and then gradually decreases.
Example 2
A high-elongation high-strength double-network hydrogel comprises the following raw materials in parts by weight: 20 parts of acrylamide, 1 part of curdlan, 3.2143 parts of octadecyl methacrylate, 0.448 part of initiator, 7.435 parts of hexadecyl trimethyl ammonium bromide, 1.038 parts of sodium dodecyl sulfate and 100 parts of high-purity water;
the initiator is a photoinitiator Irgacure 2959.
The preparation method of the high-elongation high-strength double-network hydrogel comprises the following steps:
s1, sequentially dissolving sodium dodecyl sulfate, cetyl trimethyl ammonium bromide, stearyl methacrylate, an initiator and acrylamide in the high-purity water in a water bath according to the parts by weight to obtain a mixed solution; cooling the mixed solution to room temperature, adding curdlan, and uniformly mixing to obtain a suspension;
s2, introducing argon gas into the suspension for 10min for exhausting, stirring the suspension at room temperature in an inert gas atmosphere, then sequentially vacuumizing the suspension under the conditions of standing and magnetic stirring by using a vacuum pump, and removing bubbles in the suspension to obtain a mixed material;
s3, pouring the mixed material into an acrylic mold, covering a quartz cover glass and removing bubbles, sealing the material, heating the sealed material, cooling to room temperature, placing the sealed material under an ultraviolet lamp for irradiation, controlling the height of the ultraviolet lamp from the material to be 6.5cm, and performing cross-linking polymerization under the ultraviolet condition to obtain the high-elongation high-strength double-network hydrogel;
wherein in S1, the temperature of the water bath is 40 ℃;
in S1, the hexadecyl trimethyl ammonium bromide is stirred and dissolved for 20 min;
in S1, stirring and dissolving the octadecyl methacrylate for 4 h;
in S2, stirring the suspension for 20 h;
in S2, vacuumizing for 15 min;
in S3, heating the material at 90 ℃ for 15 min;
in S3, the wavelength of the ultraviolet lamp is 300nm, the power is 40W, and the irradiation time is 0.5 h.
Example 3
A high-elongation high-strength double-network hydrogel comprises the following raw materials in parts by weight: 45 parts of acrylamide, 4 parts of curdlan, 0.4227 parts of octadecyl methacrylate, 0.448 part of initiator, 8.747 parts of hexadecyl trimethyl ammonium bromide, 0 part of sodium dodecyl sulfate and 100 parts of high-purity water;
the initiator is a photoinitiator Irgacure 2959.
The preparation method of the high-elongation high-strength double-network hydrogel comprises the following steps:
s1, sequentially dissolving sodium dodecyl sulfate, cetyl trimethyl ammonium bromide, stearyl methacrylate, an initiator and acrylamide in the high-purity water in a water bath according to the parts by weight to obtain a mixed solution; cooling the mixed solution to room temperature, adding curdlan, and uniformly mixing to obtain a suspension;
s2, introducing argon gas into the suspension for 10min for exhausting, stirring the suspension at room temperature in an inert gas atmosphere, then sequentially vacuumizing the suspension under the conditions of standing and magnetic stirring by using a vacuum pump, and removing bubbles in the suspension to obtain a mixed material;
s3, pouring the mixed material into an acrylic mold, covering a quartz cover glass and removing bubbles, sealing the material, heating the sealed material, cooling to room temperature, placing the sealed material under an ultraviolet lamp for irradiation, controlling the height of the ultraviolet lamp from the material to be 6.5cm, and performing cross-linking polymerization under the ultraviolet condition to obtain the high-elongation high-strength double-network hydrogel;
wherein in S1, the temperature of the water bath is 30 ℃;
in S1, the hexadecyl trimethyl ammonium bromide is stirred and dissolved for 30 min;
in S1, stirring and dissolving the octadecyl methacrylate for 2 h;
in S2, stirring the suspension for 24 h;
in S2, vacuumizing for 10 min;
in S3, heating the material at 120 ℃ for 5 min;
in S3, the wavelength of the ultraviolet lamp is 400nm, the power is 20W, and the irradiation time is 1.5 h.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The high-elongation high-strength double-network hydrogel is characterized by comprising the following raw materials in parts by weight: 20-45 parts of acrylamide, 1-4 parts of curdlan, 0.4227-3.2143 parts of octadecyl methacrylate, 0.448 part of initiator, 7.435-8.747 parts of cetyl trimethyl ammonium bromide, 0-1.038 parts of sodium dodecyl sulfate and 100 parts of high-purity water;
the preparation method of the high-elongation high-strength double-network hydrogel comprises the following steps:
s1, sequentially dissolving sodium dodecyl sulfate, cetyl trimethyl ammonium bromide, stearyl methacrylate, an initiator and acrylamide in the high-purity water in a water bath according to the parts by weight to obtain a mixed solution; cooling the mixed solution to room temperature, adding curdlan, and uniformly mixing to obtain a suspension;
s2, stirring the suspension at room temperature in an inert gas atmosphere, and then sequentially vacuumizing the suspension under the conditions of standing and magnetic stirring to obtain a mixed material;
and S3, pouring the mixed material into a mold, sealing the material after bubble removing treatment, heating the sealed material, cooling to room temperature, and then placing under an ultraviolet lamp for irradiation to obtain the high-elongation high-strength double-network hydrogel.
2. The high-elongation high-strength double-network hydrogel according to claim 1, wherein the initiator is a photoinitiator Irgacure 2959.
3. The method for preparing a high-elongation high-strength double-network hydrogel according to claim 1 or 2, wherein the temperature of the water bath in S1 is 30-40 ℃.
4. The method for preparing the double-network hydrogel with high elongation and high strength according to claim 1 or 2, wherein in S1, cetyl trimethyl ammonium bromide is dissolved by stirring, and the stirring time is 20-30 min.
5. The method for preparing the double-network hydrogel with high elongation and high strength according to claim 1 or 2, wherein in S1, the octadecyl methacrylate is dissolved by stirring, and the stirring time is 2-4 h.
6. The method for preparing a high-elongation high-strength double-network hydrogel according to claim 1 or 2, wherein the suspension is stirred for 20-24 hours in S2.
7. The method for preparing a high-elongation high-strength double-network hydrogel according to claim 1 or 2, wherein the evacuation time in S2 is 10-15 min.
8. The method for preparing the high-elongation high-strength double-network hydrogel according to claim 1 or 2, wherein in S3, the heating temperature of the material is 90-120 ℃, and the heating time is 5-15 min.
9. The method for preparing the double-network hydrogel with high elongation and high strength as claimed in claim 1 or 2, wherein in S3, the wavelength of the ultraviolet lamp is 300-400nm, the power is 20-40W, and the irradiation time is 0.5-1.5 h.
10. The method for preparing the high-elongation high-strength double-network hydrogel according to claim 1 or 2, wherein in S3, the wavelength of the ultraviolet lamp is 365nm, the power is 30W, and the irradiation time is 1 h.
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| CN103739861A (en) * | 2014-01-02 | 2014-04-23 | 河南理工大学 | Preparation method of high-strength hydrogel |
| CN107057087A (en) * | 2017-05-19 | 2017-08-18 | 安徽大学 | A kind of mask matrix adjustable hydrogel of high elongation rate intensity and preparation method thereof |
| CN108276590A (en) * | 2018-01-17 | 2018-07-13 | 湖北工业大学 | Can 3D printing agar/polyacrylamide dihydrogen bond collaboration crosslinking high tenacity hydrogel preparation method |
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| CN103739861A (en) * | 2014-01-02 | 2014-04-23 | 河南理工大学 | Preparation method of high-strength hydrogel |
| CN107057087A (en) * | 2017-05-19 | 2017-08-18 | 安徽大学 | A kind of mask matrix adjustable hydrogel of high elongation rate intensity and preparation method thereof |
| CN108276590A (en) * | 2018-01-17 | 2018-07-13 | 湖北工业大学 | Can 3D printing agar/polyacrylamide dihydrogen bond collaboration crosslinking high tenacity hydrogel preparation method |
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