CN104311859A - Preparation method of high-strength dual-mesh nano-meter aluminum oxide composite hydrogel - Google Patents
Preparation method of high-strength dual-mesh nano-meter aluminum oxide composite hydrogel Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-strength dual-mesh nano-meter aluminum oxide composite hydrogel. The preparation method comprises the following steps: preparing a nanometer Al2O3 water solution by using cooled boiling distilled water, dissolving sodium alginate, acrylamide, a crosslinking agent, an initiator and a catalyst in the Al2O3 water solution, rapidly transferring the prepared solution into a glass mould, placing the sealed mould in an environment of a temperature of 45-55 DEG C for performing an insulation reactor for 2-6h; and taking hydrogel formed in the mould out and then dissolving the hydrogel in a CaCl2 water solution with a concentration of 0.1-1M for 2-6h, and taking out to obtain the high-strength dual-mesh nano-meter aluminum oxide composite hydrogel. Compared with a conventional hydrogel, the high-strength dual-mesh nano-meter aluminum oxide composite hydrogel disclosed by the invention is relatively high in strength and elongation so as to meet application demands of the high-strength dual-mesh nano-meter aluminum oxide composite hydrogel on aspects of human body cartilage repair, tissue engineering and the like.
Description
Technical field
The present invention relates to a kind of preparation field of high intensity hydrogel, especially the preparation of high strength dual network Nanometer composite hydrogel.
Technical background
Hydrogel is that a class has chemistry or physical crosslinking structure, Absorbable rod large quantity of moisture but water-fast polymer or macromolecular, and they can keep definite shape and three-dimensional space network structure in water.As a kind of water content up to 90%, and the soft material very similar with biologic soft tissue, hydrogel is widely used in biology, medical field, such as: organizational project, repair of cartilage etc.But conventional hydrogels is far below the mechanical strength of natural biological tissue, this severely limits the clinical application of hydrogel.So, reduce the performance gap between macromolecule hydrogel and biologic soft tissue, seeking the macromolecule hydrogel material with biologic soft tissue Performance Match, finally reach the object substituting impaired organism soft tissue with hydrogel material, is one of major issue of current macromolecule hydrogel research.In recent years, the mentality of designing of double-network hydrogel was significant to increasing substantially hydrogel mechanical property and promoting its applied research in biomaterial, and the research of high strength double-network hydrogel constantly obtains outstanding progress.Wherein, lock will has just waited people to adopt one-step synthesis method to have the hydrogel of high tensile property, this hydrogel with acrylamide and natural macromolecular sodium alginate for monomer, calcium sulfate is as the ion crosslinking agent of sodium alginate, N, N '-methylene-bisacrylamide, ammonium persulphate and Tetramethyl Ethylene Diamine are respectively the linking agent of acrylamide, thermal initiator and catalyzer, and a step prepares sodium alginate/polyacrylamide hydrophilic gel.This hydrogel is stretchable to about 20 times, but corresponding tensile strength is only about 156kPa.Tensile strength is improved and compressive strength prepares the needs of high intensity hydrogel further in the basis maintaining sodium alginate/polyacrylamide hydrophilic gel high tensile property.
High, the fabulous dispersion of nano aluminium oxide even particle size distribution, purity, its specific surface is high, has resistant to elevated temperatures inertia, high reactivity, belongs to activated alumina; Porousness; Hardness is high, good stability of the dimension, can be widely used in the strengthening and toughening of the products such as various plastics, rubber, pottery, refractory materials, the wear resisting property particularly improving the compactness of pottery, smooth finish, cool-hot fatigue, fracture toughness property, creep-resistant property and macromolecular material product is particularly remarkable.
The polymeric system of nano aluminium oxide with sodium alginate/polyacrylamide combines by the present invention, utilizes the performance of the nano-meter characteristic of nano aluminium oxide and its adsorpting polymerization thing long-chain to go to strengthen the Tension and Compression intensity of hydrogel.Thus prepare the Nanometer composite hydrogel of high strength.
Summary of the invention
For overcoming the defect that existing traditional sodium alginate/polyacrylamide double-network hydrogel stretches and compressive strength is little, the present invention utilizes the interaction between nano aluminium oxide and polymkeric substance to improve the mechanical stability of sodium alginate/polyacrylamide dual network, realizes the preparation of above-mentioned high strength dual network nano aluminium oxide composite aquogel.Prepared high intensity hydrogel tension strain can reach 2076%, and tensile strength can reach 0.329MPa, and compressive strength when shape becomes 0.9 can reach 3.38MPa.Have a distinct increment compared to tradition traditional sodium alginate/polyacrylamide double-network hydrogel.
In order to achieve the above object, the technical solution used in the present invention is as follows:
A kind of high strength dual network nano aluminium oxide composite aquogel, comprises natural polysaccharide, polymer monomer, linking agent, initiator, catalyzer, Nano filling;
Described natural polysaccharide is sodium alginate;
Described polymer monomer is acrylamide;
Described linking agent is selected from N, N '-methylene-bisacrylamide, Ethylene glycol dimethacrylate, Vinylstyrene;
Described initiator is selected from ammonium persulphate, Potassium Persulphate, Sodium Persulfate;
Described catalyzer is selected from Tetramethyl Ethylene Diamine, five methyl diethylentriamine;
Described Nano filling is nanometer Al
2o
3, and nanometer Al
2o
3particle diameter be 20 ~ 100nm.
A kind of concrete preparation process of high strength dual network nano aluminium oxide composite aquogel is as follows: wherein step 2 ~ 3 are carried out under vacuum, Keep agitation condition;
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 1 ~ 10% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 10 ~ 20%;
3) linking agent, initiator, catalyzer being added step 2) in the solution of gained, described linking agent, initiator, catalyzer account for 0.03 ~ 0.09%, 0.1 ~ 0.2%, 0.2 ~ 0.3% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 45 ~ 55 DEG C, insulation reaction 2 ~ 6h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.1 ~ 1M
22 ~ 6h in the aqueous solution, takes out and is finished product.
Sodium alginate and Ca in the present invention
2+carry out the first network that ionomer forms hydrogel, acrylamide and N, N '-methylene-bisacrylamide polymerization crosslinking forms the second network of hydrogel, and the amide group that the first network of sodium alginate and the second network of acrylamide are directly formed by the carboxyl on sodium alginate long-chain and the amino on polyacrylamide is cross-linked.First network provides main stress under less deformation, and provides main stress by second network under comparatively large deformation, and now first network is as " the sacrifice key " of dissipation energy.
Inorganic nano material, as a kind of material that is emerging, that possess a lot of good characteristic, is often applied to organic polymer polymerization product to play the advantage of inorganic-organic composite material, the overall performance of strongthener.The present invention is the intensity strengthening sodium alginate/polyacrylamide dual network further, and the present invention introduces the nanometer Al possessing good distribution performance, high-specific surface area
2o
3, utilize the physisorption between nano particle and polymer chain to provide more waste of energy when hydrogel generation deformation.
Beneficial effect of the present invention:
1, present invention utilizes nanometer Al
2o
3particle is to the enhancement of polymer network, and polymer chain is adsorbed on its surface by aluminum oxide, and when making hydrogel be subject to external compression or stretching, inorganic nanoparticles can also play the effect supporting and disperse external force, thus improves the mechanical strength of hydrogel.
2, in preparation method of the present invention, the whole process of the first step is carried out in the Erlenmeyer flask vacuumized; relative to traditional nitrogen protection, the carrying out that this mode vacuumized can not only prevent oxygen from entering solution obstruction polyreaction air can also be discharged reactor thus the solution inside making viscosity higher is not easy to produce bubble.There is birth defect and easily produce stress concentration in the hydrogel after the existence of bubble can make gel solidification, is namely destroyed under less external force.Therefore, method of the present invention can not only ensure the carrying out of reaction and avoid the generation of hydrogel defect.
In sum, the high strength dual network nano aluminium oxide composite aquogel that prepared by the present invention has the advantages such as stretching, compressive strength is large, preparation method is more simply effective.
Accompanying drawing explanation
Fig. 1 is product structure schematic diagram of the present invention.
Fig. 2 is the stress-strain curve that the hydrogel of the embodiment of the present invention 1 ~ 3 gained and conventional hydrogels sample extension are tested.
Fig. 3 is the stress-strain curve that the hydrogel of the embodiment of the present invention 1 ~ 3 gained and conventional hydrogels sample compression are tested.
Caption: 1-polyacrylamide, 2-Ca
2+, 3-sodium alginate, 4-nanometer Al
2o
3particle, 5-embodiment 1 gained sample test curve, 6-embodiment 2 gained sample test curve, 7-embodiment 3 gained sample test curve, 8-conventional hydrogels sample test curve.
Embodiment
For making those skilled in the art understand the present invention better, the preparation method of high strength dual network nano aluminium oxide composite aquogel in the application is described below by way of specific embodiment.
Embodiment 1
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 1% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 20 ~ 30nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 10%;
3) by N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine add step 2) in the solution of gained, described N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine account for 0.03%, 0.1%, 0.2% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 45 DEG C, insulation reaction 2h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.1M
22h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 2076%, and tensile strength can reach 0.3MPa, and compressive strength when shape becomes 0.9 can reach 2.97MPa.
Embodiment 2
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 10% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 90 ~ 100nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 20%;
3) by N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine add step 2) in the solution of gained, described N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine account for 0.09%, 0.2%, 0.3% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 55 DEG C, insulation reaction 6h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 1.0M
26h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 2042%, and tensile strength can reach 0.251MPa, and compressive strength when shape becomes 0.9 can reach 2.26MPa.
Embodiment 3
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 6% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 40 ~ 50nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 14%;
3) by N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine add step 2) in the solution of gained, described N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine account for 0.06%, 0.17%, 0.25% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 50 DEG C, insulation reaction 3h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.5M
23h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 2010%, and tensile strength can reach 0.329MPa, and compressive strength when shape becomes 0.9 can reach 3.38MPa.
Embodiment 4
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 8% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 50 ~ 60nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 12%;
3) Vinylstyrene, Potassium Persulphate, Tetramethyl Ethylene Diamine being added step 2) in the solution of gained, described Vinylstyrene, Potassium Persulphate, Tetramethyl Ethylene Diamine account for 0.08%, 0.13%, 0.22% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 52 DEG C, insulation reaction 4h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.2M
25h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 2010%, and tensile strength can reach 0.290MPa, and compressive strength when shape becomes 0.9 can reach 2.78MPa.
Embodiment 5
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 4% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 30 ~ 40nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 16%;
3) Ethylene glycol dimethacrylate, Sodium Persulfate, five methyl diethylentriamine being added step 2) in the solution of gained, described Ethylene glycol dimethacrylate, Sodium Persulfate, five methyl diethylentriamine account for 0.07%, 0.18%, 0.26% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 48 DEG C, insulation reaction 2h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.6M
24h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 2030%, and tensile strength can reach 0.295MPa, and compressive strength when shape becomes 0.9 can reach 2.86MPa.
Embodiment 6
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 9% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 60 ~ 70nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 11%;
3) by N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine add step 2) in the solution of gained, described N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine account for 0.04%, 0.12%, 0.22% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 49 DEG C, insulation reaction 6h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.8M
22h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 1950%, and tensile strength can reach 0.289MPa, and compressive strength when shape becomes 0.9 can reach 2.75MPa.
Embodiment 7
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 2% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 50 ~ 60nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 17%;
3) by N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine add step 2) in the solution of gained, described N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine account for 0.06%, 0.17%, 0.25% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 50 DEG C, insulation reaction 3h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.5M
23h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 1930%, and tensile strength can reach 0.291MPa, and compressive strength when shape becomes 0.9 can reach 2.71MPa.
Embodiment 8
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 8% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, nanometer Al used
2o
3particle diameter is 60 ~ 70nm, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 19%;
3) by N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine add step 2) in the solution of gained, described N, N '-methylene-bisacrylamide, ammonium persulphate, Tetramethyl Ethylene Diamine account for 0.08%, 0.18%, 0.27% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 50 DEG C, insulation reaction 3h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.5M
23h in the aqueous solution, takes out and is finished product.
The high intensity hydrogel tension strain that the present embodiment obtains can reach 1970%, and tensile strength can reach 0.279MPa, and compressive strength when shape becomes 0.9 can reach 2.70MPa.
Experimental example
Elongation test: adopt universal testing machine (LR10K Plus) to carry out Elongation test to the sheet-like hydrous gel sample that length, width, thickness are respectively 50mm, 10mm, 3mm, gauge length is 10mm, and rate of extension is 20mm/min.Same sample test three times, test result is averaged.In embodiment 1,2,3, gained sample and conventional hydrogels sample extension test result are as shown in Figure 2.
Compression verification: adopt universal testing machine (LR10K Plus) to carry out compression verification to diameter, the columnar water gel sample that is highly 15mm, compressive set is 90%, and compression speed is 3mm/min.Same sample test three times, test result.
Claims (2)
1. a preparation method for high strength dual network nano aluminium oxide composite aquogel, is characterized in that: comprise natural polysaccharide, polymer monomer, linking agent, initiator, catalyzer, Nano filling;
Described natural polysaccharide is sodium alginate;
Described polymer monomer is acrylamide;
Described linking agent is selected from N, N '-methylene-bisacrylamide, Ethylene glycol dimethacrylate, Vinylstyrene;
Described initiator is selected from ammonium persulphate, Potassium Persulphate, Sodium Persulfate;
Described catalyzer is selected from Tetramethyl Ethylene Diamine, five methyl diethylentriamine;
Described Nano filling is nanometer Al
2o
3, and nanometer Al
2o
3particle diameter be 20 ~ 100nm.
2. the preparation method of a kind of high strength dual network nano aluminium oxide composite aquogel according to claim 1, is characterized in that: concrete steps are as follows: wherein step 2) ~ 3) carry out under vacuum, Keep agitation condition;
1) distilled water being boiled sealing and be cooled to room temperature with except the oxygen in anhydrating, is 1 ~ 10% nanometer Al with cooled distilled water preparation massfraction
2o
3the aqueous solution, is uniformly dispersed through ultrasonic oscillation 10min, for subsequent use;
2) sodium alginate is got and acrylamide is dissolved in step 1) the nanometer Al for preparing
2o
3in the aqueous solution, described sodium alginate and the mass ratio of acrylamide are 1:6, and the massfraction of the total content of sodium alginate and acrylamide is 10 ~ 20%;
3) linking agent, initiator, catalyzer being added step 2) in the solution of gained, described linking agent, initiator, catalyzer account for 0.03 ~ 0.09%, 0.1 ~ 0.2%, 0.2 ~ 0.3% of acrylamide quality respectively;
4) by step 3) solution for preparing is transferred in glass mold, and after sealing, at being placed in 45 ~ 55 DEG C, insulation reaction 2 ~ 6h, namely obtains shaping hydrogel;
5) take out shaping hydrogel in glass mold and be immersed in the CaCl that concentration is 0.1 ~ 1M
22 ~ 6h in the aqueous solution, takes out and is finished product.
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