CN105111341A - Sticky high-mechanical-strength nano hybrid hydrogel and preparation method thereof - Google Patents
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Abstract
The invention discloses a sticky high-mechanical-strength nano hybrid hydrogel and a preparation method thereof. The sticky hydrogel is obtained by polymerizing an acrylamide or N-alkyl substituted acrylamide derivative in aqueous dispersion of an inorganic nano crosslinking agent namely of laponite, polyvinyl alcohol and cyclodextrin, has high mechanical strength and stickiness and can adhere to surfaces of skins, metals, glasses and ceramics. The preparation method of the sticky hydrogel comprises the following steps: dispersing the inorganic nano crosslinking agent namely laponite and a monomer into water, and stirring to obtain uniform and transparent dispersion; adding polyvinyl alcohol into a reaction mixed solution, and stirring uniformly; then adding the cyclodextrin into the reaction mixed solution, and stirring uniformly; adding an initiating agent at last; and filling a mold with the reaction solution, sealing the mold, and putting the mold into an environment of 20-25 DEG C for reaction for 12-48 hours to obtain the sticky high-mechanical-strength nano hybrid hydrogel, wherein the tensile strength of the hydrogel is more than or equal to 100kPa, and the adhesive strength is more than or equal to 10kPa.
Description
Technical field
The present invention relates to the polymeric material field of functional polymer-inorganic lithium algae soil nano-hybrid material, be specifically related to sticking high strength nano hybridized hydrogel of a kind of tool and preparation method thereof.
Background technology
Hydrogel due to containing a large amount of water, and has the characteristic that its soft material given by perfect three-dimensional net structure, and this structure is similar to bio-tissue, has important application prospect in biomedical materials field.Wherein the sticking hydrogel of tool has unique advantage in organizational project, medical dressing and drug controlled release etc.Cohesive hydrogel, compared with conventional adhesive, can provide the intensity matched with substrate modulus, and have can the function of transmitter substance; The coupling of modulus effectively can avoid cracking, adsorbable and the function discharging molecule makes viscous gel have unique advantage in fields such as sensor, medicine controlled releasing, sealings.On the one hand hydrogel can keep stable contact by viscosity with biological tissue or surface adhesion, and another aspect hydrogel can medicine carrying, controlled release, realizes the control transmission of medicine, therefore has significant application value in medicine controlled releasing field.But owing to containing large quantity of moisture in hydrogel, therefore the mechanical strength of conventional hydrogels is very low, cannot bear larger stretching, compression or repeated deformation etc., greatly constrain the application of hydrogel at biomedicine field.
In recent years, there is the report of several high strength hydrogel, as Nanometer composite hydrogel, double-network hydrogel, topological framework hydrogel, polyampholyte hydrogel etc., the mechanical strength of hydrogel has been promoted to the kPa order of magnitude, even can reaches MPa.The appearance of these high strength hydrogels overcomes the low defect of conventional hydrogels mechanical strength, has widened the Application Areas of hydrogel.Wherein, Nanometer composite hydrogel replaces traditional chemical linking agent, a kind of high intensity hydrogel obtained by radical polymerization with acrylamide monomers by inorganic nano-particle lithium algae soil.But the high strength hydrogel of report scarcely has viscosity at present, only have on a small quantity about the report of high strength cohesive hydrogel, as based on Dopamine HCL (AdvancedMaterials, 2013,25:653), polyacrylamide (TheJournalofPhysicalChemistryB, 2013,117:441), polyoxyethylene glycol (MacromolecularBioscience, 2013, high intensity hydrogel 13:59) etc. has certain viscosity, preparation technology is quite complicated, and the application of high strength cohesive hydrogel is restricted.
For exploitation has the novel high-strength cohesive hydrogel of practical significance, simplify preparation technology, the invention provides one " one kettle way " preparation and there is viscosity nano hybridized hydrogel possessing high strength and preparation method thereof simultaneously; Prepared hybridized hydrogel had both had excellent mechanical strength, there is again good viscosity, can adhere to the surfaces such as skin, metal, glass, pottery, hydrogel also possesses biocompatibility simultaneously, can be used for the field that wound sealing, wound auxiliary material and medicine controlled releasing etc. need cohesive hydrogel.
Summary of the invention
For the deficiencies in the prior art, the invention provides sticking high strength nano hybridized hydrogel of a kind of tool and preparation method thereof.
Object of the present invention is achieved through the following technical solutions:
The sticking high strength nano hybridized hydrogel of a kind of tool, this hydrogel by acrylamide or
n-alkyl-substituted acrylamide derivative is polymerized in the aqueous dispersions of inorganic nano-particle lithium algae soil, polyvinyl alcohol and cyclodextrin; Described
n-alkyl-substituted acrylamide derivative is
n,
n-DMAA or
n-N-isopropylacrylamide; Described hydrolyzed pva degree is 80% ~ 99%, and molecular weight is 10,000 ~ 100,000.
Further, described inorganic nano-particle lithium algae soil adopts LaponiteXLS colloidal sol type product, LaponiteRDS colloidal sol type product, LaponiteXLG gel type products or LaponiteRD gel type products.
Further, described cyclodextrin is
α-cyclodextrin,
β-cyclodextrin or
γ-cyclodextrin.
Further, described hydrogel has high strength and viscosity, and can adhere to the surfaces such as skin, metal, glass, pottery, tensile strength is at 100-2000kPa, and cohesive strength is at 10-200kPa.
Further, described hydrogel tensile strength is at 100-500kPa, and cohesive strength is at 10-40kPa.
A preparation method for the sticking high strength nano hybridized hydrogel of tool, comprises the steps:
(1) successively by inorganic nano-particle lithium algae soil and monomer dispersion in water, stirring obtains the dispersion liquid of homogeneous transparent;
(2) in above-mentioned dispersion liquid, add polyvinyl alcohol and stir, then adding cyclodextrin and stir, obtaining reaction solution;
(3) remove the oxygen in reaction solution, then add initiator, obtain reaction mixture, finally reaction mixture to be loaded in mould and to seal, being placed in 10 ~ 25
oreact 12-48 hour in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.
Further, step (1) described inorganic nano-particle lithium algae soil adopts LaponiteXLS colloidal sol type product, LaponiteRDS colloidal sol type product, LaponiteXLG gel type products or LaponiteRD gel type products; Described inorganic nano-particle lithium algae soil property amount is 1% ~ 10% of added quality in dispersion liquid.
Further, step (1) described monomer be acrylamide,
n,
n-DMAA or
n-N-isopropylacrylamide; Described monomer mass is 10% ~ 40% of added quality in dispersion liquid.
Further, the described hydrolyzed pva degree of step (2) is 80% ~ 99%, and molecular weight is 10,000 ~ 100,000; The quality of described polyvinyl alcohol for add water in dispersion liquid 1 ~ 8% of quality.
Further, step (2) described cyclodextrin is
α-cyclodextrin,
β-cyclodextrin or
γ-cyclodextrin; The quality of described cyclodextrin is 3% ~ 15% of added quality in dispersion liquid.
Further, step (3) described initiator is redox initiation system, and wherein oxygenant is Potassium Persulphate or ammonium persulphate, and reductive agent is Tetramethyl Ethylene Diamine or tetrahydroxyethyl-ethylene diamine; The consumption of described initiator is 0.1% ~ 4% of monomer mass.
The present invention adopts inorganic nano-particle lithium algae soil to replace traditional chemical linking agent, and the introducing of lithium algae soil drastically increases the mechanical strength of hydrogel.Adding polyvinyl alcohol and cyclodextrin makes hydrogel produce adhesivity, and can play the effect regulating nano hybridized hydrogel mechanical strength, can according to using the intensity that need to regulate hydrogel, to promote that hydrogel mates with the modulus adhered between object.On the other hand, polyvinyl alcohol and cyclodextrin possess good biocompatibility, can also provide basis for hydrogel in the adhesion application of bioelectric interface.Therefore, the hydrogel that the present invention obtains can have adjustable high strength and the feature of viscosity simultaneously.
Compared with prior art, tool of the present invention has the following advantages and technique effect:
1. the viscosity nano hybridized hydrogel that prepared by the present invention has excellent mechanical strength, tensile strength is at more than 100kPa, cohesive strength, at more than 10kPa, overcomes the shortcoming that conventional hydrogels mechanical strength is low, also achieves the sticking function of high strength hydrogel tool simultaneously.
2. the present invention adopts " one kettle way " original position radical polymerization synthesis, and preparation method is simple, and polymerizing condition is gentle, can realize industrial production.
3. the present invention regulates the mechanical strength of product by the content controlling the components such as monomer, nanoparticle, polyvinyl alcohol, cyclodextrin, can provide and the cohesive hydrogel using object intensity to match according to use object difference.
4. the ductility of nano hybridized hydrogel prepared of the present invention and viscosity regulate by the content of polyvinyl alcohol and cyclodextrin, can meet the demand of different Adhesion Interface.
5. the nano hybridized hydrogel that prepared by the present invention has good biocompatibility, may be used for medical wound dressing, medicine controlled releasing etc.
Embodiment
Do further detailed description below in conjunction with embodiment to the present invention, these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.
The hybridized hydrogel obtained in following examples, all adopt the Macromolecules such as Xiong, 2009, method disclosed in 42:3811-3817 document measures mechanical property, adopt the MacromolecularBioscience such as Schmidt, method disclosed in 2013,13:59-66 document measures the cohesive strength on the surface such as hydrogel and pigskin, stainless steel, glass, pottery.
Embodiment 1
At room temperature 0.1g lithium algae soil LaponiteXLG gel type products is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then 1g monomer is added
n,
n-DMAA, stirs the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.1g degree of hydrolysis is 80%, and molecular weight is the polyvinyl alcohol of 10,000 and stirs 2h, then adds 0.3g
α-cyclodextrin stirs 1h; Pass into argon gas 10min again and remove oxygen; Finally add initiator potassium persulfate 0.03g and Tetramethyl Ethylene Diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 20
oreact 12h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 100kPa, and elongation at break is 1600%, and the cohesive strength of hydrogel and pigskin is 10kPa.
Embodiment 2
At room temperature 0.2g lithium algae soil LaponiteRD gel type products is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then add 3g monomeric acrylamide, stir the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.5g degree of hydrolysis is 83%, and molecular weight is the polyvinyl alcohol of 30,000 and stirs 2h, then adds 1g
β-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator ammonium persulfate 0.1g and Tetramethyl Ethylene Diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 10
oreact 24h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 120kPa, and elongation at break is 2300%, and hydrogel and stainless cohesive strength are 18kPa.
Embodiment 3
At room temperature 0.6g lithium algae soil LaponiteXLS colloidal sol type product is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then 2g monomer is added
n-N-isopropylacrylamide, stirs the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.2g degree of hydrolysis is 86%, and molecular weight is the polyvinyl alcohol of 100,000 and stirs 2h, then adds 1.5g
γ-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator ammonium persulfate 0.06g and Tetramethyl Ethylene Diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 25
oreact 48h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 200kPa, and elongation at break is 1800%, and the cohesive strength of hydrogel and pigskin is 20kPa.
Embodiment 4
At room temperature 0.8g lithium algae soil LaponiteRDS colloidal sol type product is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then 3g monomer is added
n,
n-DMAA, stirs the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.8g degree of hydrolysis is 90%, and molecular weight is the polyvinyl alcohol of 20,000 and stirs 2h, then adds 0.8g
β-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator ammonium persulfate 0.1g and tetrahydroxyethyl-ethylene diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 25
oreact 48h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 250kPa, and elongation at break is 2100%, and the cohesive strength of hydrogel and glass is 15kPa.
Embodiment 5
At room temperature 0.3g lithium algae soil LaponiteXLG gel type products is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then add 2.5g monomeric acrylamide, stir the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.3g degree of hydrolysis is 93%, and molecular weight is the polyvinyl alcohol of 80,000 and stirs 2h, then adds 0.9g
α-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator potassium persulfate 0.08g and Tetramethyl Ethylene Diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 15
oreact 24h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 110kPa, and elongation at break is 3000%, and the cohesive strength of hydrogel and pigskin is 18kPa.
Embodiment 6
At room temperature 1.0g lithium algae soil LaponiteXLS colloidal sol type product is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then 4g monomer is added
n-N-isopropylacrylamide, stirs the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.4g degree of hydrolysis is 96%, and molecular weight is the polyvinyl alcohol of 50,000 and stirs 2h, then adds 1.2g
γ-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator ammonium persulfate 0.15g and Tetramethyl Ethylene Diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 25
oreact 24h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 490kPa, and elongation at break is 1900%, and hydrogel is 31kPa with the cohesive strength of pottery.
Embodiment 7
At room temperature 0.4g lithium algae soil LaponiteRDS colloidal sol type product is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then 3g monomer is added
n,
n-DMAA, stirs the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.6g degree of hydrolysis is 99%, and molecular weight is the polyvinyl alcohol of 40,000 and stirs 2h, then adds 0.6g
β-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator ammonium persulfate 0.1g and tetrahydroxyethyl-ethylene diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 25
oreact 36h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 170kPa, and elongation at break is 2100%, and hydrogel and stainless cohesive strength are 13kPa.
Embodiment 8
At room temperature 0.5g lithium algae soil LaponiteXLG gel type products is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then 1g monomer is added
n,
n-DMAA, stirs the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.3g degree of hydrolysis is 88%, and molecular weight is the polyvinyl alcohol of 60,000 and stirs 2h, then adds 1.0g
γ-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator ammonium persulfate 0.02g and tetrahydroxyethyl-ethylene diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 20
oreact 40h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 140kPa, and elongation at break is 1900%, and the cohesive strength of hydrogel and pigskin is 23kPa.
Embodiment 9
At room temperature 0.7g lithium algae soil LaponiteXLS colloidal sol type product is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then add 2g monomeric acrylamide, stir the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.7g degree of hydrolysis is 95%, and molecular weight is the polyvinyl alcohol of 40,000 and stirs 2h, then adds 1.3g
α-cyclodextrin stirs 1h; Pass into argon gas 10min removing oxygen wherein again; Finally add initiator ammonium persulfate 0.06g and tetrahydroxyethyl-ethylene diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 20
oreact 30h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 350kPa, and elongation at break is 2000%, and the cohesive strength of hydrogel and pigskin is 25kPa.
Embodiment 10
At room temperature 0.9g lithium algae soil LaponiteRDS colloidal sol type product is dispersed in 10mL deoxygenation deionized water, stirs 2h and obtain uniform dispersion liquid; Then 1g monomer is added
n-N-isopropylacrylamide, stirs the mixed solution that 2h obtains homogeneous transparent; In above-mentioned mixed solution, add 0.3g degree of hydrolysis is 97%, and molecular weight is the polyvinyl alcohol of 90,000 and stirs 2h, then adds 1.4g
α-cyclodextrin stirs 1h; Argon gas 10min removes oxygen wherein again; Finally add initiator ammonium persulfate 0.02g and tetrahydroxyethyl-ethylene diamine 0.01g, obtain reaction solution, reaction solution to be loaded in mould and to seal, being placed in 20
oreact 24h in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.The tensile break strength of this hydrogel is 160kPa, and elongation at break is 2600%, and the cohesive strength of hydrogel and pigskin is 40kPa.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; the change done under other any does not deviate from spirit of the present invention and principle, modification, substitute, combine; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the sticking high strength nano hybridized hydrogel of tool, is characterized in that, this hydrogel by acrylamide or
n-alkyl-substituted acrylamide derivative is polymerized in the aqueous dispersions of inorganic nano-particle lithium algae soil, polyvinyl alcohol and cyclodextrin; Described
n-alkyl-substituted acrylamide derivative is
n,
n-DMAA or
n-N-isopropylacrylamide; Described hydrolyzed pva degree is 80% ~ 99%, and molecular weight is 10,000 ~ 100,000.
2. the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 1, it is characterized in that, described inorganic nano-particle lithium algae soil adopts LaponiteXLS colloidal sol type product, LaponiteRDS colloidal sol type product, LaponiteXLG gel type products or LaponiteRD gel type products.
3. the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 1, it is characterized in that, described cyclodextrin is
α-cyclodextrin,
β-cyclodextrin or
γ-cyclodextrin.
4. the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 1, is characterized in that, described hydrogel tensile strength is at 100-500kPa, and cohesive strength is at 10-40kPa.
5. prepare the method for the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 1, it is characterized in that, comprise the steps:
(1) successively by inorganic nano-particle lithium algae soil and monomer dispersion in water, stirring obtains the dispersion liquid of homogeneous transparent;
(2) in above-mentioned dispersion liquid, add polyvinyl alcohol and stir, then adding cyclodextrin and stir, obtaining reaction solution;
(3) remove the oxygen in reaction solution, then add initiator, obtain reaction mixture, finally reaction mixture to be loaded in mould and to seal, being placed in 10 ~ 25
oreact 12-48 hour in C environment, obtain the sticking high strength nano hybridized hydrogel of tool.
6. the preparation method of the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 5, it is characterized in that, step (1) described inorganic nano-particle lithium algae soil adopts LaponiteXLS colloidal sol type product, LaponiteRDS colloidal sol type product, LaponiteXLG gel type products or LaponiteRD gel type products; Described inorganic nano-particle lithium algae soil property amount is 1% ~ 10% of added quality in dispersion liquid.
7. the preparation method of the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 5, is characterized in that, step (1) described monomer be acrylamide,
n,
n-DMAA or
n-N-isopropylacrylamide; Described monomer mass is 10% ~ 40% of added quality in dispersion liquid.
8. the preparation method of the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 5, is characterized in that, the described hydrolyzed pva degree of step (2) is 80% ~ 99%, and molecular weight is 10,000 ~ 100,000; Described polyvinyl alcohol quality is 1 ~ 8% of added quality in dispersion liquid.
9. the preparation method of the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 5, is characterized in that, step (2) described cyclodextrin is
α-cyclodextrin,
β-cyclodextrin or
γ-cyclodextrin; Described cyclodextrin quality is 3% ~ 15% of added quality in dispersion liquid.
10. the preparation method of the sticking high strength nano hybridized hydrogel of a kind of tool according to claim 5, it is characterized in that, step (3) described initiator is redox initiation system, wherein oxygenant is Potassium Persulphate or ammonium persulphate, and reductive agent is Tetramethyl Ethylene Diamine or tetrahydroxyethyl-ethylene diamine; The consumption of described initiator is 0.1% ~ 4% of monomer mass.
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| CN113527558B (en) * | 2020-04-13 | 2023-06-20 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Nanocomposite hydrogel and preparation method and application thereof |
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