CN103435951A - Nanometer composite high-molecular dual-network hydrogel and preparation method thereof - Google Patents
Nanometer composite high-molecular dual-network hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-strength nanometer composite high-molecular dual-network hydrogel and a preparation method thereof, and belongs to the technical field of composite modification of hydrogels. The preparation method of the high-strength nanometer composite high-molecular dual-network hydrogel comprises the following steps of: firstly dissolving a first network monomer, a cross-linking agent and an initiating agent into a water dispersion liquid which contains nanometer particles, and pouring an obtained mixed solution into a mould for heating polymerization to obtain a first network hydrogel; dissolving a second network monomer, the cross-linking agent and the initiating agent into water, placing the first network hydrogel into the solution, swelling for 24 hours, and then carrying out the heating polymerization to obtain the high-strength nanometer composite high-molecular dual-network hydrogel. The high-strength nanometer composite high-molecular dual-network hydrogel provided by the invention is simple in preparation process and superior in property, can be used for enhancing the compression strength of the dual-network hydrogel and keeping higher tensile strength through nanometer enhancement and is widely applied to the fields of biological medicine, agriculture, a building industry, a chemical industry, a mining industry, and the like.
Description
Technical field
The present invention relates to a kind of high-strength nano composite polymeric double-network hydrogel and preparation method thereof, belong to technical field of polymer materials.
Background technology
Macromolecule hydrogel is that a class be 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, in water, can maintain definite shape, even 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, can find hydrogel structure in nearly all bio-tissue, therefore, hydrogel is that the first is developed the biomaterial for tissue, in organizational project and regenerative medicine field, great application prospect is arranged.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 the development of related discipline as medical science, physiotechnology, water and soil, Materials science etc.Yet when hydrogel is used for these fields, usually all require it to there is certain intensity, using and meet as load or keep its functional requirement.And traditional synthesizing high-hydroscopicity gel mainly to take vinylformic acid, acrylamide be raw material, the hydrogel of single-material is low and crosslinking structure is inhomogeneous due to crosslink density, after water suction, gel stretches and the deficiency such as compressive strength is low, has seriously limited its development.With respect to traditional synthetic water gel, the organism hydrogel has superior mechanical strength, prepares the such hydrogel of similar organism hydrogel, can solve the barrier of hydrogel application, gives full play to its function.
Since entering 21st century, the high strength macromolecule hydrogel has been obtained very large development, and wherein, the preparation process of double-network hydrogel is simple, is easy to industrialization, and its large-scale application has a extensive future and receives much concern.Double-network hydrogel is at first to be proposed by scholars such as Gong Jianping, (J.P.Gong, Y.Katsuyama, T.Kurokawa, Y.Osada.Advance Materials, 2003,15 (14): 1155-1158).Why double-network hydrogel has so excellent properties, structure owing to itself and biological articular cartilage tissue is closely similar, and cartilaginous tissue is to consist of collegen filament skeleton and the hyaluronic acid and the aggrecanase aggregate that are attached at around collegen filament by covalency, non covalent bond effect.Double-network hydrogel similar to the netted structure function of collegen filament skeleton in articular cartilage tissue than the first network of high crosslink density, rigidity, be the principal element of opposing external force, and give the shape certain with hydrogel; Its low cross-linking or not crosslinked flexible second network and hyaluronic acid and aggrecanase aggregate functional similarity, the distortion by the loose network configuration is effectively relaxed stress.The present invention is a kind of superhigh tenacity and intensity polymer double-network hydrogel prepared by combining nano Material reinforcement effect and dual network structural reinforcing principle, further improves resistance to compression and the creep-resistant property of double-network hydrogel.Number of patent application is CN201110092271.0 double network polymer hydrogel of having announced a kind of pH of having, temperature, electric field-sensitive and preparation method thereof, and its component is the multipolymer that the polyoxyethylene glycol toxilic acid is joined two vinegar, NIPA or acrylamide.Number of patent application is that CN201110092271.0 has announced high-intensity hydrogel, by the uv-radiation method, prepared by this hydrogel.Yet 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 objective of the invention is the rigidity by introducing nanoparticle enhancing first network provides a kind of preparation method of high strength polymer double-network hydrogel.Particularly, Nanocomposites, in the first network of hydrogel, is improved to the mechanical property of double-network hydrogel by the intensity that strengthens first network.
The purpose of this invention is to provide a kind of nano composite polymeric double-network hydrogel, the advantage such as that this hydrogel has is high-strength, high-ductility.
Another object of the present invention is to provide a kind of preparation method of nano composite polymeric double-network hydrogel.
Nano composite polymeric double-network hydrogel of the present invention, this hydrogel is comprised of double-network hydrogel and inorganic nano-particle, and wherein, the weight ratio between double-network hydrogel and nanoparticle is: 100:1-50.
Prepare the required monomer of 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 sulfonate, p styrene sulfonic acid salt, vinylsulfonate.
Prepare the required monomer of 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 thereof, methacrylic acid and derivative thereof, acrylamide and derivative thereof, N-vinyl formamide, vinyl pyridine, NVP.
Required linking agent in double-network hydrogel preparation of the present invention, it is selected from following material one or a combination set of: ethylene glycol dimethacrylate, Diethylene Glycol dimethacrylate, N, N '-methylene-bisacrylamide.
Required initiator 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 thereof, soccerballene.
The molar concentration rate of the required monomer of first network of the present invention and linking agent is 100:2～6, preparing the required monomer of first network hydrogel and initiator molar concentration rate is 100:0.1～0.6, and the mass ratio for preparing the required monomer of first network hydrogel and nanoparticle is 100:0.1～5.
The molar concentration rate of the required monomer of second network of the present invention and linking agent is 100:0.01～0.2, and the molar concentration rate for preparing the required monomer of second network hydrogel and initiator 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 nano composite polymeric double-network hydrogel provided by the invention comprises the following steps:
(1) will prepare the required monomer of first network hydrogel, linking agent and initiator and be dissolved in containing in the nanoparticle aqueous dispersions, the mixing solutions obtained is poured silicon rubber mould into, reacts 6～20 hours under 50～80 ℃, obtains hydrogel.
(2) will prepare the required monomer of second network hydrogel, linking agent and initiator is dissolved in the water, the hydrogel that step (1) is obtained is put into this solution, swelling 24～30 hours is then reacted 6～20 hours under 50～80 ℃, obtains the nano composite polymeric double-network hydrogel.
Nano composite polymeric double-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 subject to the restriction of these embodiment.Scope of the present invention proposes in claims.
Comparative Examples 1
Take 2-acrylamide-2-methyl propane sulfonic 1.243g, linking agent N, N '-methylene-bisacrylamide 0.037g, initiator potassium persulfate 0.006g, add the 6ml deionized water, after being uniformly dissolved, this solution is poured in silicon rubber mould, under 60 ℃, reaction is 10 hours, obtains the first network hydrogel.Take again acrylamide 14.216g, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, add the 100ml deionized water, after being uniformly dissolved, the first network hydrogel is put into to this solution, swelling 24 hours is then reacted 10 hours under 60 ℃, obtains the polymer double-network hydrogel.Then the dumbbell shape batten that with cut-off knife, hydrogel is cut into to long 35mm, wide 10mm, thick 2mm, the long 15mm of gauge length, wide 4mm carries out Elongation test, draw speed: 40mm/min; The cylinder shape sample that hydrogel is cut into to diameter 8mm, 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 the 6ml deionized water, stir 0.5 hour, ultrasonic 0.5～1 hour, take again 2-acrylamide-2-methyl propane sulfonic 1.243g, linking agent N, N '-methylene-bisacrylamide 0.037g, initiator potassium persulfate 0.006g, uniform dissolution, this solution is poured in silicon rubber mould, and reaction is 10 hours under 60 ℃, obtains the first network hydrogel.Take acrylamide 14.216g, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, add the 100ml deionized water, uniform dissolution, the first network hydrogel is put into to this solution, swelling 24 hours is then reacted 10 hours under 60 ℃, obtains the nano composite polymeric double-network hydrogel.Then the dumbbell shape batten that with cut-off knife, hydrogel is cut into to long 35mm, wide 10mm, thick 2mm, the long 15mm of gauge length, wide 4mm carries out Elongation test, draw speed: 40mm/min; The cylinder shape sample that hydrogel is cut into to diameter 8mm, high 8mm carries out compression verification, compression speed: 0.8mm/min, it the results are shown in table 1.
Embodiment 2
Except nano graphene oxide described in embodiment 1 is changed into the nano level sodium-based montmorillonite, all the other conditions are identical with embodiment 1.The hydrogel of preparation carries out various Mechanics Performance Testings, the results are shown in table 1.
Embodiment 3
Except the consumption by nano level sodium-based montmorillonite described in embodiment 2 changes into 0.062g, all the other conditions are identical with embodiment 2.The hydrogel of preparation carries out various Mechanics Performance Testings, the results are shown in table 1.
Embodiment 4
Except nano graphene oxide described in embodiment 1 is changed into the nanometer halloysite, all the other conditions are identical with embodiment 1.The hydrogel of preparation carries out various Mechanics Performance Testings, the results are shown in table 1.
Embodiment 5
Take carbon nanotube 0.012g, add the 6ml deionized water, the tensio-active agent Sodium dodecylbenzene sulfonate of weight such as 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, pour this solution in silicon rubber mould into, under 60 ℃, reaction is 10 hours, obtains the first network hydrogel.Take acrylamide 14.216g, linking agent N, N '-methylene-bisacrylamide 0.015g, initiator potassium persulfate 0.054g, add the 100ml deionized water, uniform dissolution, the first network hydrogel is put into to this solution, swelling 24 hours is then reacted 10 hours under 60 ℃, obtains the nano composite polymeric double-network hydrogel.Then the dumbbell shape batten that with cut-off knife, hydrogel is cut into to long 35mm, wide 10mm, thick 2mm, the long 15mm of gauge length, wide 4mm carries out Elongation test, draw speed: 40mm/min; The cylinder shape sample that hydrogel is cut into to diameter 8mm, high 8mm carries out compression verification, compression speed: 0.8mm/min, it the results are shown in table 1.
Embodiment 6
Except the consumption by carbon nanotube described in embodiment 5 changes into 0.049g, all the other conditions are identical with embodiment 5.The hydrogel of preparation carries out various Mechanics Performance Testings, the results are shown in table 1.
Table 1
Claims (7)
1. a nano composite polymeric double-network hydrogel, is characterized in that, described nano composite polymeric double-network hydrogel comprises double-network hydrogel and nanoparticle, and wherein, the weight ratio between double-network hydrogel and nanoparticle is: 100:1-50; Double-network hydrogel comprises first network hydrogel and second network hydrogel; Wherein, preparing the required monomer of first network hydrogel is one or more in 2-acrylamide-2-methyl propane sulfonic, methacrylic sulfonic acid, p styrene sulfonic acid, vinyl sulfonic acid, methacrylic sulfonate, p styrene sulfonic acid salt, vinylsulfonate;
Wherein, preparing the required monomer of second network hydrogel is one or more in vinylformic acid and derivative, methacrylic acid and derivative thereof, acrylamide and derivative thereof, N-vinyl formamide, vinyl pyridine, NVP;
Wherein, inorganic nano-particle is one or more in 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 thereof, soccerballene.
2. nano composite polymeric double-network hydrogel according to claim 1, it is characterized in that, prepare the required linking agent of double-network hydrogel and be selected from ethylene glycol dimethacrylate, Diethylene Glycol dimethacrylate, N, one or more in N '-methylene-bisacrylamide.
3. nano composite polymeric double-network hydrogel according to claim 2, is characterized in that, prepares the required initiator of double-network hydrogel to be: ammonium persulphate, Potassium Persulphate or hydrogen peroxide.
4. nano composite polymeric double-network hydrogel according to claim 3, it is characterized in that, the described molar concentration rate for preparing the required monomer of first network hydrogel and linking agent is 100:2～6, preparing the required monomer of first network hydrogel and initiator molar concentration rate is 100:0.1～0.6, and the mass ratio for preparing the required monomer of first network hydrogel and inorganic nano-particle is 100:0.1～50.
5. nano composite polymeric double-network hydrogel according to claim 3, it is characterized in that, the described molar concentration rate for preparing the required monomer of second network hydrogel and linking agent is 100:0.01～0.2, and the molar concentration rate for preparing the required monomer of second network hydrogel and initiator is 100:0.01～0.1.
6. according to the described nano composite polymeric double-network hydrogel of claim 1-5 any one, it is characterized in that, the described volumetric molar concentration for preparing the required monomer of first network hydrogel is 100:50～500 with the molar concentration rate for preparing the required monomer of second network hydrogel.
7. according to the preparation method of the arbitrary described nano composite polymeric double-network hydrogel of claim 1-7, it is characterized in that, comprise the steps:
(1) by the first network hydrogel, required monomer, linking agent and initiator is dissolved in containing in the nanoparticle aqueous dispersions, and the mixing solutions obtained is poured silicon rubber mould into, reacts 6～20 hours under 50～80 ℃, obtains the first network hydrogel;
(2) by the second network hydrogel, required monomer, linking agent and initiator is dissolved in the water, the first network hydrogel that step (1) is obtained is put into this solution, swelling 24～30 hours is then reacted 6～20 hours under 50～80 ℃, obtains the nano composite polymeric double-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 |