CN108424532B - Preparation method of magnetic hydrogel with high strength and high fracture toughness - Google Patents
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- C08K3/346—Clay
Abstract
The invention provides a preparation method of magnetic hydrogel with high strength and high fracture toughness, wherein divalent and trivalent iron ions enter a three-dimensional polymer network of poly (N, N-dimethylacrylamide) nano composite hydrogel through the permeation diffusion effect, and then the divalent and trivalent iron ions are subjected to in-situ generation of ferroferric oxide magnetic particles through a sodium hydroxide coprecipitation method, and the magnetic particles are precipitated on the three-dimensional polymer network of the hydrogel in situ and are uniformly distributed; in a high-concentration sodium hydroxide solution, the poly N, N-dimethylacrylamide nano composite hydrogel can undergo volume phase change, so that the strength and fracture toughness of the magnetic hydrogel are greatly improved; the method can be popularized to different types of hydrogel, and is a universal preparation method of the magnetic hydrogel with high strength and high fracture toughness; the magnetic hydrogel prepared by the method can simultaneously solve two material problems: the mechanical property is poor, the magnetic particles are not uniformly distributed, and the fracture toughness of the magnetic hydrogel is as high as 11000Jm‑2Is one of the strongest magnetic hydrogels in the world at present.
Description
Technical Field
The invention belongs to the technical field of functional polymer material preparation, and particularly relates to a preparation method of a magnetic hydrogel with high strength and high fracture toughness.
Background
The magnetic hydrogel is formed by compounding magnetic particles and a hydrogel matrix, wherein the hydrogel matrix comprises polyacrylamide, poly-N-isopropylacrylamide, alginate, chitosan, hemicellulose and the like, and the magnetic particles comprise ferroferric oxide, gamma ferric oxide, cobalt ferrite and the like. The magnetic hydrogel is developed rapidly in recent years, and has good application prospects in the aspects of drug release, photonic crystals, drivers, artificial muscles and the like. The magnetic hydrogel with the porous structure can generate volume deformation of up to 70% under a magnetic field, so that the medicine is extruded out along with water, the medicine release amount under the magnetic field is 7 times that under the non-magnetic field, and the controllable release of stem cells in a mouse body can be realized. The magnetic particles with the core-shell structure move in the gel solvent under the excitation of a magnetic field to form periodic arrangement, present different colors and patterns, are response type photonic crystals, and can be used for manufacturing flexible display screens. The magnetic hydrogel cantilever beam bends under the action of a magnetic field and can be used for preparing a magnetic driver. The magnetic hydrogel can be stretched, contracted and curled under a magnetic field, and the artificial muscle can be prepared by utilizing the diversified deformation modes of the magnetic hydrogel.
At present, most of magnetic hydrogels have extremely poor mechanical properties, and practical application of the magnetic hydrogels is limited. There are two general international strategies for improving the mechanical properties of hydrogels. One is the addition of inorganic nanoparticles such as nanoclay, silica particles; the other is a dual network design, one layer of short network and one layer of long network. However, these toughening methods have not been expanded to the field of magnetic hydrogels.
The preparation method of the magnetic hydrogel mainly comprises a blending method and an in-situ precipitation method. In the blending method, magnetic particles are directly dispersed into a hydrogel monomer solution, and a macromolecule crosslinking reaction is excited to obtain the magnetic hydrogel. The drawback of the blending method is the non-uniform distribution of the magnetic particles. In the in-situ precipitation method, the hydrogel prepared in advance is soaked in a divalent and trivalent iron ion solution until the swelling balance is achieved, and then the swollen hydrogel is soaked in a reducing agent solution, so that the magnetic particles are precipitated on a polymer network of the hydrogel in situ to form uniform particle distribution. How to combine the hydrogel toughening method with the magnetic hydrogel preparation method to prepare the magnetic hydrogel with high strength and high fracture toughness is still an unbroken technical bottleneck.
Disclosure of Invention
Aiming at the defects of the mechanical property of the existing magnetic hydrogel, the invention provides a preparation method of the magnetic hydrogel with high strength and high fracture toughness. The fracture toughness of the magnetic hydrogel is as high as 11000Jm-2Is one of the strongest magnetic hydrogels in the world at present; the method provided by the invention is convenient to operate, can solve the problems of poor mechanical property and uneven distribution of magnetic particles in one step, can be popularized to different types of hydrogel, and is a universal preparation method of the magnetic hydrogel with high strength and high fracture toughness.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a magnetic hydrogel with high strength and high fracture toughness comprises the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with clay content of 3-5 mol% by taking N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through a thermally initiated free radical polymerization reaction;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
Compared with the prior art, the invention has the following advantages:
1. the method can prepare the high-strength and high-toughness magnetic hydrogel with uniformly distributed magnetic particles, and the fracture toughness is as high as 11000Jm-2Is one of the strongest magnetic hydrogels in the world at present. In the preparation method, divalent and trivalent iron ions enter a three-dimensional polymer network of the poly N, N-dimethylacrylamide nano composite hydrogel through the permeation diffusion effect, and then the divalent and trivalent iron ions are subjected to in-situ generation of ferroferric oxide magnetic particles through a simple and mild sodium hydroxide coprecipitation method, and the magnetic particles are precipitated on the three-dimensional polymer network of the hydrogel in situ and are uniformly distributed. In a high-concentration sodium hydroxide solution, the poly N, N-dimethylacrylamide nano composite hydrogel can undergo volume phase change, so that the strength and fracture toughness of the magnetic hydrogel are greatly improved.
2. The method can be popularized to different types of hydrogel, and is a universal preparation method of the magnetic hydrogel with high strength and high fracture toughness.
Drawings
FIG. 1 is a schematic diagram of a method for preparing a magnetic hydrogel used in the present invention.
FIG. 2 is a photograph of the magnetic hydrogel prepared in example 3 showing tensile strain at break.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific embodiments.
The preparation method comprises the following steps: as shown in fig. 1, firstly, preparing poly N, N-dimethylacrylamide nanocomposite hydrogel; secondly, placing the poly-N, N-dimethylacrylamide nano composite hydrogel in a solution of divalent and trivalent iron ions to swell to an equilibrium state; and finally, soaking the swelled hydrogel in NaOH solution to obtain the magnetic hydrogel with high strength and high fracture toughness.
Example 1
The preparation method of the high-strength high-toughness magnetic hydrogel comprises the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with clay content of 3 mol% by taking N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through thermally initiated free radical polymerization;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
The fracture toughness of the magnetic hydrogel prepared in the embodiment is 6929.71Jm through the characterization of mechanical experiments-2. The magnetic hydrogel prepared in the example was confirmed to have a saturation magnetization of 31.80emu/g at room temperature and to exhibit superparamagnetism by alternating gradient magnetometer characterization.
Example 2
The preparation method of the high-strength high-toughness magnetic hydrogel comprises the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with clay content of 4 mol% by using N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through a thermally initiated free radical polymerization reaction;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
The fracture toughness of the magnetic hydrogel prepared in the embodiment is 8100.61Jm through the characterization of mechanical experiments-2. The magnetic hydrogel prepared in the example was confirmed to have a saturation magnetization of 29.54emu/g at room temperature and to exhibit superparamagnetism by alternating gradient magnetometer characterization.
Example 3
The preparation method of the high-strength high-toughness magnetic hydrogel comprises the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with the clay content of 5 mol% by taking N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through a thermally initiated free radical polymerization reaction;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
The mechanical experiment characterization proves that the preparation method of the embodimentThe magnetic hydrogel prepared has a fracture toughness of 10984.57Jm-2. As shown in FIG. 2, the magnetic hydrogel prepared in this example can be stretched 13 times in the notched state. The magnetic hydrogel prepared in the example was confirmed to have a saturation magnetization of 23.68emu/g at room temperature and to exhibit superparamagnetism by alternating gradient magnetometer characterization.
Claims (4)
1. A preparation method of a magnetic hydrogel with high strength and high fracture toughness is characterized by comprising the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with clay content of 3-5 mol% by taking N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through a thermally initiated free radical polymerization reaction;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
2. The method for preparing the magnetic hydrogel with high strength and high fracture toughness according to claim 1, wherein the method comprises the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with clay content of 3 mol% by taking N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through thermally initiated free radical polymerization;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
3. The method for preparing the magnetic hydrogel with high strength and high fracture toughness according to claim 1, wherein the method comprises the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with clay content of 4 mol% by using N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through a thermally initiated free radical polymerization reaction;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
4. The method for preparing the magnetic hydrogel with high strength and high fracture toughness according to claim 1, wherein the method comprises the following steps:
step 1: forming poly N, N-dimethylacrylamide nano composite hydrogel with the clay content of 5 mol% by taking N, N-dimethylacrylamide as a monomer and hectorite nano clay particles as a physical cross-linking agent through a thermally initiated free radical polymerization reaction;
step 2: FeCl is added3·6H2O and FeCl2·4H2Mixing O according to the molar ratio of 2:1, and adding deionized water to prepare an iron ion solution;
and step 3: soaking the poly N, N-dimethylacrylamide nano composite hydrogel obtained in the step 1 into the iron ion solution obtained in the step 2 at room temperature for 24 hours to ensure that the hydrogel is fully swelled in the iron ion solution to an equilibrium state;
and 4, step 4: preparing NaOH solution with the concentration of 5 mol/L;
and 5: and (4) washing the hydrogel adsorbed with the divalent and trivalent iron ions in the step (3) by using deionized water, immersing the hydrogel into the NaOH solution in the step (4), and immersing the hydrogel for 24 hours at room temperature to obtain the high-strength and high-toughness magnetic hydrogel.
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