CN103435951B - A kind of Nanometer composite high-molecular dual-network hydrogel and preparation method thereof - Google Patents
A kind of Nanometer composite high-molecular dual-network hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of high-strength nano composite high-molecular double-network hydrogel and preparation method thereof, belong to the technical field composite modified to hydrogel.The preparation process of this Nanometer composite high-molecular dual-network hydrogel is as follows: be first dissolved in first network monomer, linking agent and initiator containing in nanoparticle aqueous dispersions, pour the mixing solutions obtained in mould heated polymerizable, obtain first network hydrogel.Second network monomer, linking agent and initiator are dissolved in the water, then first network hydrogel is put into this solution, swelling 24 hours, then heated polymerizable, obtain high-strength nano composite high-molecular double-network hydrogel.Hydrogel preparation process of the present invention is simple, and gained hydrogel superior performance, is strengthened by nanometer, not only can improve the compressive strength of double-network hydrogel, and can also keep its comparatively high tensile.Be widely used in fields such as biological medicine, agricultural, construction industry, chemical industry, mining industry.
Description
Technical field
The present invention relates to a kind of high-strength Nanometer composite high-molecular dual-network hydrogel and preparation method thereof, belong to technical field of polymer materials.
Background technology
Macromolecule hydrogel is a class take water as dispersion medium, the macromolecular material body with space three-dimensional network structure formed by chemistry or physical crosslinking effect.It can absorb rapidly large water gaging, but is not dissolved in water, and water retention capacity is strong, can maintain definite shape in water, even if after applying certain force, also can restore to the original state.As a kind of special " water material ", itself and bio-tissue structure are very similar, take a broad view organic sphere, hydrogel structure can be found in nearly all bio-tissue, therefore, hydrogel is that the first develops the biomaterial for tissue, has great application prospect in organizational project and regenerative medicine field.In addition, hydrogel also has a wide range of applications potentiality in agricultural, building, petrochemical complex, mining industry, food, makeup, agricultural gardening.
The research of hydrogel has driven related discipline as the development of medical science, physiotechnology, water and soil, Materials science etc.But when hydrogel is used for these fields, usually all require that it has certain intensity, to meet as load or to keep its functional requirement.And traditional synthesizing high-hydroscopicity gel mainly with vinylformic acid, acrylamide for raw material, the hydrogel of single-material is because crosslink density is low and crosslinking structure is uneven, and after water suction, gel Tension and Compression intensity is low waits not enough, seriously limits its development.Relative to conventional synthesis hydrogel, organism hydrogel then has superior mechanical strength, prepares the hydrogel that similar organism hydrogel is such, then can solve the barrier of hydrogel application, give full play to its function.
Since entering 21st century, high strength macromolecule hydrogel achieves very large development, and wherein, the preparation process of double-network hydrogel is simple, and be easy to industrialization, its large-scale application has a extensive future and receives much concern.Double-network hydrogel is first proposed by scholars such as Gong Jianping, (J.P.Gong, Y.Katsuyama, T.Kurokawa, Y.Osada.AdvanceMaterials, 2003,15 (14): 1155-1158).Why double-network hydrogel has excellent properties so, structure owing to itself and biological articular cartilage tissue is closely similar, and cartilaginous tissue is by collegen filament skeleton and is attached at hyaluronic acid around collegen filament by covalency, non covalent bond effect and aggrecanase aggregate is formed.Double-network hydrogel similar to the netted structure function of collegen filament skeleton in articular cartilage tissue compared with the first network of high crosslink density, rigidity, is the principal element of opposing external force, and gives the shape certain with hydrogel; Its low cross-linking or crosslinked flexible second network and hyaluronic acid and aggrecanase aggregate functional similarity, make stress effectively be relaxed by the distortion of loose network configuration.The present invention is a kind of superhigh tenacity and intensity polymer double-network hydrogel that combining nano Material reinforcement effect and dual network structure strengthen prepared by principle, improves resistance to compression and the creep-resistant property of double-network hydrogel further.Number of patent application is that CN201110092271.0 discloses a kind of double network polymer hydrogel and preparation method thereof with pH, temperature, electric field-sensitive, and its component is the multipolymer that polyoxyethylene glycol toxilic acid joins two vinegar, NIPA or acrylamide.Number of patent application is the hydrogel that CN201110092271.0 discloses high strength, and this hydrogel is prepared by uv-radiation method.But the mechanical property that above method prepares double-network hydrogel also far can not meet service requirements.
Summary of the invention
The method that the object of the invention is to strengthen by introducing nanoparticle the rigidity of first network provides a kind of preparation method of high strength polymer double-network hydrogel.Particularly, by Nanocomposites in the first network of hydrogel, improved the mechanical property of double-network hydrogel by the intensity strengthening first network.
The object of this invention is to provide a kind of Nanometer composite high-molecular dual-network hydrogel, this hydrogel has the advantages such as high-strength, high-ductility.
Another object of the present invention is to provide a kind of preparation method of Nanometer composite high-molecular dual-network hydrogel.
Nanometer composite high-molecular dual-network hydrogel of the present invention, this hydrogel is made up of double-network hydrogel and inorganic nano-particle, and wherein, the weight ratio between double-network hydrogel and nanoparticle is: 100:1-50.
Prepare monomer needed for first network hydrogel in double-network hydrogel of the present invention, it is selected from following material one or a combination set of: 2-acrylamide-2-methyl propane sulfonic, methacrylic sulfonic acid, p styrene sulfonic acid, vinyl sulfonic acid, methacrylic sulfonic acid salt, p styrene sulfonic acid salt, vinylsulfonate.
Prepare the monomer needed for second network hydrogel in double-network hydrogel of the present invention, it is selected from following material one or a combination set of: vinylformic acid and derivative, methacrylic acid and derivative thereof, acrylamide and derivative, N-vinyl formamide, vinyl pyridine, NVP.
Linking agent required in double-network hydrogel preparation of the present invention, it is selected from following material one or a combination set of: ethylene glycol dimethacrylate, dimethacrylate, N, N '-methylene-bisacrylamide.
Initiator required in double-network hydrogel preparation of the present invention, it is selected from one of following material: ammonium persulphate, Potassium Persulphate, hydrogen peroxide.
Nanoparticle of the present invention: graphene oxide, halloysite, carbon nanotube, green stone, polynite, talcum powder, beidellite, hectorite, silica, halloysite, cage-type silsesquioxane, cellulose crystallite, Graphene, oxide/carbon nanometer tube, hydroxyapatite, metal and oxide compound, soccerballene.
Needed for first network of the present invention, the molar concentration rate of monomer and linking agent is 100:2 ~ 6, prepare monomer needed for first network hydrogel and initiator molar concentration rate is 100:0.1 ~ 0.6, the mass ratio preparing monomer and nanoparticle needed for first network hydrogel is 100:0.1 ~ 5.
Needed for second network of the present invention, the molar concentration rate of monomer and linking agent is 100:0.01 ~ 0.2, and the molar concentration rate preparing monomer and initiator needed for second network hydrogel is 100:0.01 ~ 0.1.
First network monomer of the present invention and second network monomer molar concentration ratio are 100:50 ~ 500.
The preparation method of Nanometer composite high-molecular dual-network hydrogel provided by the invention comprises the following steps:
(1) be dissolved in preparing monomer, linking agent and initiator needed for first network hydrogel containing in nanoparticle aqueous dispersions, the mixing solutions obtained pours silicon rubber mould into, reacts 6 ~ 20 hours, obtain hydrogel at 50 ~ 80 DEG C.
(2) be dissolved in the water preparing monomer, linking agent and initiator needed for second network hydrogel, the hydrogel that step (1) obtains is put into this solution, swelling 24 ~ 30 hours, then react 6 ~ 20 hours at 50 ~ 80 DEG C, obtain Nanometer composite high-molecular dual-network hydrogel.
Nanometer composite high-molecular dual-network hydrogel prepared by the present invention has higher compression intensity and tensile strength.
Embodiment
Further describe the present invention below in conjunction with embodiment, scope of the present invention is not by the restriction of these embodiments.Scope of the present invention proposes in detail in the claims.
Comparative example 1
Take 2-acrylamide-2-methyl propane sulfonic 1.243g, linking agent N, N '-methylene-bisacrylamide 0.037g, initiator potassium persulfate 0.006g, add 6ml deionized water, after being uniformly dissolved, this solution is poured in silicon rubber mould, react 10 hours at 60 DEG C, obtain first network hydrogel.Take acrylamide 14.216g again, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, adds 100ml deionized water, after being uniformly dissolved, first network hydrogel is put into this solution, swelling 24 hours, then react 10 hours at 60 DEG C, obtain polymer double-network hydrogel.Then with cut-off knife hydrogel is cut into long 35mm, wide 10mm, thick 2mm, the long 15mm of gauge length, wide 4mm dumbbell shape batten carry out Elongation test, draw speed: 40mm/min; Hydrogel is cut into diameter 8mm, the cylinder shape sample of high 8mm carries out compression verification, compression speed: 0.8mm/min, its result is as shown in table 1.
Embodiment 1
Take nano graphene oxide 0.012g, add 6ml deionized water, stir 0.5 hour, ultrasonic 0.5 ~ 1 hour, take 2-acrylamide-2-methyl propane sulfonic 1.243g again, linking agent N, N '-methylene-bisacrylamide 0.037g, initiator potassium persulfate 0.006g, uniform dissolution, this solution is poured in silicon rubber mould, reacts 10 hours at 60 DEG C, obtain first network hydrogel.Take acrylamide 14.216g, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, adds 100ml deionized water, uniform dissolution, first network hydrogel is put into this solution, swelling 24 hours, then react 10 hours at 60 DEG C, obtain Nanometer composite high-molecular dual-network hydrogel.Then with cut-off knife hydrogel is cut into long 35mm, wide 10mm, thick 2mm, the long 15mm of gauge length, wide 4mm dumbbell shape batten carry out Elongation test, draw speed: 40mm/min; Hydrogel is cut into diameter 8mm, the cylinder shape sample of high 8mm carries out compression verification, compression speed: 0.8mm/min, it the results are shown in table 1.
Embodiment 2
Except changing into except nano level sodium-based montmorillonite by nano graphene oxide described in embodiment 1, all the other conditions are identical with embodiment 1.The hydrogel of preparation carries out various Mechanics Performance Testing, the results are shown in table 1.
Embodiment 3
Except changing into except 0.062g by the consumption of nano level sodium-based montmorillonite described in embodiment 2, all the other conditions are identical with embodiment 2.The hydrogel of preparation carries out various Mechanics Performance Testing, the results are shown in table 1.
Embodiment 4
Except changing into except nanometer halloysite by nano graphene oxide described in embodiment 1, all the other conditions are identical with embodiment 1.The hydrogel of preparation carries out various Mechanics Performance Testing, the results are shown in table 1.
Embodiment 5
Take carbon nanotube 0.012g, add 6ml deionized water, the surfactant sodium dodecyl base benzene sulfonic acid sodium salt of weight such as to add simultaneously, stir 0.5 hour, ultrasonic 0.5 ~ 1 hour, then take 2-acrylamide-2-methyl propane sulfonic 1.243g, linking agent N, N '-methylene-bisacrylamide 0.037g, initiator potassium persulfate 0.006g, uniform dissolution, pours in silicon rubber mould by this solution, react 10 hours at 60 DEG C, obtain first network hydrogel.Take acrylamide 14.216g, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, adds 100ml deionized water, uniform dissolution, first network hydrogel is put into this solution, swelling 24 hours, then react 10 hours at 60 DEG C, obtain Nanometer composite high-molecular dual-network hydrogel.Then with cut-off knife hydrogel is cut into long 35mm, wide 10mm, thick 2mm, the long 15mm of gauge length, wide 4mm dumbbell shape batten carry out Elongation test, draw speed: 40mm/min; Hydrogel is cut into diameter 8mm, the cylinder shape sample of high 8mm carries out compression verification, compression speed: 0.8mm/min, it the results are shown in table 1.
Embodiment 6
Except changing into except 0.049g by the consumption of carbon nanotube described in embodiment 5, all the other conditions are identical with embodiment 5.The hydrogel of preparation carries out various Mechanics Performance Testing, the results are shown in table 1.
Table 1
Claims (2)
1. the preparation method of a Nanometer composite high-molecular dual-network hydrogel, it is characterized in that, comprise the steps: to take carbon nanotube 0.012g, add 6ml deionized water, the surfactant sodium dodecyl base benzene sulfonic acid sodium salt of weight such as to add simultaneously, stir 0.5 hour, ultrasonic 0.5 ~ 1 hour, then take 2-acrylamide-2-methyl propane sulfonic 1.243g, linking agent N, N '-methylene-bisacrylamide 0.037g, initiator potassium persulfate 0.006g, uniform dissolution, pours in silicon rubber mould by this solution, react 10 hours at 60 DEG C, obtain first network hydrogel; Take acrylamide 14.216g, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, adds 100ml deionized water, uniform dissolution, first network hydrogel is put into this solution, swelling 24 hours, then react 10 hours at 60 DEG C, obtain Nanometer composite high-molecular dual-network hydrogel.
2. the preparation method of a Nanometer composite high-molecular dual-network hydrogel, it is characterized in that, comprise the steps: to take carbon nanotube 0.049g, add 6ml deionized water, the surfactant sodium dodecyl base benzene sulfonic acid sodium salt of weight such as to add simultaneously, stir 0.5 hour, ultrasonic 0.5 ~ 1 hour, then take 2-acrylamide-2-methyl propane sulfonic 1.243g, linking agent N, N '-methylene-bisacrylamide 0.037g, initiator potassium persulfate 0.006g, uniform dissolution, pours in silicon rubber mould by this solution, react 10 hours at 60 DEG C, obtain first network hydrogel; Take acrylamide 14.216g, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, adds 100ml deionized water, uniform dissolution, first network hydrogel is put into this solution, swelling 24 hours, then react 10 hours at 60 DEG C, obtain Nanometer composite high-molecular dual-network hydrogel.
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Application publication date: 20131211 Assignee: ANQING JIAXIN MEDICAL PRODUCTS Co.,Ltd. Assignor: Jiangnan University Contract record no.: X2021980003791 Denomination of invention: Nano composite polymer double network hydrogel and preparation method thereof Granted publication date: 20160427 License type: Common License Record date: 20210520 |