CN112661988A - Preparation method of sodium alginate interpenetrating network hydrogel without ionic crosslinking - Google Patents
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Abstract
The invention discloses a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which comprises the following steps: mixing the biological macromolecule capable of being gelatinized or the biological macromolecule solution with sodium alginate to prepare a uniform solution, heating, standing, then soaking in an acid solution, and drying; then soaking the hydrogel in an acid solution, drying, and finally soaking the hydrogel in deionized water for swelling to obtain the sodium alginate interpenetrating network water without ionic crosslinkingAnd (4) gelling. The hydrogel prepared by the invention is crystalline cross-linked hydrogel, does not contain chemical cross-linking agents, can be dissolved and self-repaired, has certain salt solution stability and thermal stability, and has higher strength and toughness, the fracture stress and modulus of the hydrogel can reach more than 0.4MPa, and the damage energy can reach 300J/m2Therefore, the defect that the traditional ionic crosslinking hydrogel has larger dependence on the ionic environment is overcome.
Description
Technical Field
The invention belongs to the technical field of hydrogel material preparation, and particularly relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking.
Background
The hydrogel is a soft wet material consisting of cross-linked macromolecules and water, but is insoluble in water and has a three-dimensional network structure; has wide application prospect in the biomedical field, the food field, the engineering field and the like, so that the preparation of the high-strength and high-toughness pure biomass hydrogel material becomes a research hotspot in recent years. The alginate is a water-soluble natural polymer material, is nontoxic, has good biocompatibility and biodegradability, is environment-friendly and has low cost. Alginate-based hydrogels have wide applications in various fields. However, alginates are currently essentially cross-linked to form hydrogels by utilizing divalent and multivalent ion coordination. For example, Liu et al prepared a sodium alginate-based hydrogel with high mechanical strength using a trivalent ion coordination method (Liu, Shunli, Polymer Degradation & Stability,2016,133); zheng et al uses sodium alginate to compound with synthetic macromolecule, such as poly (acrylamide-co-acrylic acid), polyacrylamide, etc., and then cross-links by ion cross-linking or chemical bond to obtain hydrogel material with certain strength. However, alginate gel adopting ion crosslinking has strong ion concentration dependence, changes the ion environment, and obviously reduces the mechanical property and even converts into sol. This greatly limits the practical application of sodium alginate hydrogels in biomedical materials and food fields.
Disclosure of Invention
The invention aims to provide a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, wherein the sodium alginate network of the hydrogel takes an alginic acid crystalline region as a crosslinking point and does not contain a chemical crosslinking agent, and the hydrogel has higher strength and toughness.
The invention adopts the technical scheme that a preparation method of the sodium alginate interpenetrating network hydrogel without ion crosslinking is implemented according to the following steps:
step 1, mixing a biological macromolecule capable of being gelatinized or a biological macromolecule solution with sodium alginate to prepare a uniform solution, heating, cooling, and standing to crosslink the biological macromolecule capable of being gelatinized so as to obtain a biological macromolecule/sodium alginate semi-interpenetrating network hydrogel with weaker strength;
step 2, soaking the biomacromolecule/sodium alginate semi-interpenetrating network hydrogel obtained in the step 1 in an acid solution to enable part of sodium alginate to form alginic acid crystals, and crosslinking the sodium alginate to form a crystallized cross-linked sodium alginate biomacromolecule/sodium alginate interpenetrating network hydrogel;
step 3, drying the biological macromolecule/sodium alginate interpenetrating network hydrogel obtained in the step 2;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, and drying to obtain the sodium alginate mutual transmission network hydrogel with enhanced strength; and finally, soaking the hydrogel into deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking.
The present invention is also characterized in that,
in the step 1, the heating temperature is 40-100 ℃, the heating time is 10min-5h, the temperature is reduced to 1-30 ℃, and the standing time is 0.5-16 h.
In the step 1, the mass concentration of the biomacromolecule/sodium alginate solution is 5-25 wt%; the mass ratio of the biological macromolecules to the sodium alginate is 1: 0.1-1.5.
The biological macromolecule is any one of gelatin, agar, konjac polysaccharide, starch, soy protein, whey protein, beta-lac protein and serum protein.
In the step 2, the soaking time is 5-25 min; in step 4, the soaking time is 20-60 min.
In the step 2 and the step 4, the acid solution is any one of hydrochloric acid, acetic acid, citric acid, sorbic acid, fumaric acid, malic acid, gluconic acid and phosphoric acid; the volume concentration of the acid solution is 1-15%.
In the step 3, the drying time is 8-48 h.
In the step 4, the drying time is 10-36 h; the swelling temperature is 1-27 ℃, and the swelling time is 1-200 h.
The invention has the beneficial effects that:
the hydrogel prepared by the invention is crystalline cross-linked hydrogel, does not contain chemical cross-linking agent, has good biodegradability, self-repairing property, certain saline solution stability and thermal stability, higher strength and toughness, breaking stress and modulus of the hydrogel can reach more than 0.4MPa, and the breaking energy can reach 300J/m2Therefore, the defect that the traditional ionic crosslinking hydrogel has larger dependence on the ionic environment is overcome. In addition, the hydrogel is prepared by adopting the full-biomass polymer, has the advantages of environmental friendliness, biocompatibility, edibility and the like, is simple and feasible in steps and low in cost, and is suitable for large-scale popularization.
Drawings
FIG. 1 is a stress-strain test chart of sodium alginate interpenetrating network hydrogel prepared by the method of the present invention;
FIG. 2 is a stress-strain curve diagram of sodium alginate interpenetrating network hydrogel crosslinked by calcium ions and sodium alginate interpenetrating network hydrogel after swelling equilibrium in water environment and sodium alginate interpenetrating network hydrogel prepared by the method;
FIG. 3 is a schematic structural diagram of the sodium alginate interpenetrating network hydrogel prepared by the method of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which is implemented according to the following steps:
step 1, mixing a biological macromolecule capable of being gelatinized or a biological macromolecule solution with sodium alginate to prepare a uniform solution, heating, cooling to 1-30 ℃, standing, and crosslinking the biological macromolecule capable of being gelatinized to obtain a biological macromolecule/sodium alginate semi-interpenetrating network hydrogel with weaker strength;
heating at 40-100 deg.C for 10min-5h, and standing for 0.5-16 h;
the biomacromolecule/sodium alginate solution is formed by mixing biomacromolecules, sodium alginate and water; the mass concentration of the biomacromolecule/sodium alginate solution is 5-25 wt%; the biological macromolecule is any one of gelatin, agar, konjac polysaccharide, starch, soy protein, whey protein, beta-lac protein and serum protein;
the mass ratio of the biological macromolecules to the sodium alginate is 1: 0.1-1.5;
step 2, soaking the sodium alginate semi-interpenetrating network hydrogel obtained in the step 1 in an acid solution to enable part of the sodium alginate to form alginic acid crystals, and crosslinking the sodium alginate to form a crystal crosslinked sodium alginate biomacromolecule/sodium alginate interpenetrating network hydrogel;
soaking for 5-25 min; the acid solution is any one of hydrochloric acid, acetic acid, citric acid, sorbic acid, fumaric acid, malic acid, gluconic acid and phosphoric acid; the volume concentration of the acid solution is 1-15%;
step 3, drying the biological macromolecule/sodium alginate interpenetrating network hydrogel obtained in the step 2;
the drying time is 8-48 h; the drying mode is room temperature drying or freeze drying;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, and drying to obtain the sodium alginate mutual transmission network hydrogel with enhanced strength; and finally, soaking the hydrogel into deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking.
Soaking for 20-60 min; the acid solution is any one of hydrochloric acid, acetic acid, citric acid, sorbic acid, fumaric acid, malic acid, gluconic acid and phosphoric acid; the volume concentration of the acid solution is 1-15%;
drying for 10-36 h; the swelling temperature is 1-27 ℃, and the swelling time is 1-200 h;
the drying method is room temperature drying or freeze drying.
The invention relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which adopts a one-pot method to prepare a sodium alginate/self-crosslinkable biological macromolecule solution, firstly, the self-crosslinkable biological macromolecule is crosslinked to form weak gel which is used as a bracket of a sodium alginate molecular chain, the pH value is adjusted by adding acid to partially acidify the sodium alginate, an insoluble alginic acid micro-region is formed to realize the crosslinking of the sodium alginate, and the insoluble alginic acid region is enlarged by a drying-repeated acid treatment-drying-swelling method to further improve the mechanical strength. The bracket method can effectively inhibit the movement of the molecular chain of the sodium alginate and avoid the formation of dispersed alginic acid precipitates. The sodium alginate interpenetrating network hydrogel prepared by the invention is a pure biomass sodium alginate interpenetrating network hydrogel without ionic crosslinking; as shown in FIG. 3, the hydrogel prepared by the invention has an interpenetrating network structure, the self-crosslinkable biomacromolecule gel is a first-layer network, and the second-layer network is a crystallized and crosslinked sodium alginate network structure.
Example 1
The invention relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which is implemented according to the following steps:
step 1, mixing 1g of gelatin and 0.6g of sodium alginate with deionized water, heating to 40 ℃ to prepare a gelatin/sodium alginate uniform solution with the mass concentration of 5 wt%, cooling to room temperature, and standing for 8 hours to obtain the sodium alginate semi-interpenetrating network hydrogel with weak strength;
step 2, soaking the sodium alginate interpenetrating network hydrogel obtained in the step 1 in an acid solution to form an alginic acid crystal cross-linked network;
soaking for 5 min; the acid solution is hydrochloric acid; the volume concentration of the acid solution is 1 percent;
step 3, drying the sodium alginate interpenetrating network hydrogel obtained in the step 2;
the drying time is 10 h; the drying mode is room temperature drying;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, drying, and finally soaking the hydrogel in deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking; soaking for 20 min; the acid solution is hydrochloric acid; the volume concentration of the acid solution is 5 percent;the drying time is 12 h; the swelling temperature is 1 ℃, and the swelling time is 1 h; the drying mode is room temperature drying; the sodium alginate interpenetrating network hydrogel has a modulus of 0.6MPa and a destruction energy of 279J/m2。
Example 2
The invention relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which is implemented according to the following steps:
step 1, mixing 1g of agar and 0.4g of sodium alginate with deionized water, heating to 80 ℃ to prepare a uniform agar/sodium alginate solution with the mass concentration of 10 wt%, cooling to room temperature, and standing for 10 hours to obtain a weaker sodium alginate semi-interpenetrating network hydrogel;
step 2, soaking the sodium alginate interpenetrating network hydrogel obtained in the step 1 in an acid solution to form an alginic acid crystal cross-linked network;
soaking for 7 min; the acid solution is citric acid; the volume concentration of the acid solution is 4 percent;
step 3, drying the sodium alginate interpenetrating network hydrogel obtained in the step 2;
the drying time is 16 h; the drying mode is room temperature drying;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, drying, and finally soaking the hydrogel in deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking; soaking for 20 min; the acid solution is citric acid; the volume concentration of the acid solution is 4 percent; the drying time is 12 h; the swelling temperature is 10 ℃, and the swelling time is 20 h; the drying mode is room temperature drying; the modulus of the sodium alginate interpenetrating network hydrogel is 0.5MPa, and the tensile breaking stress is 1.2 MPa.
Example 3
The invention relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which is implemented according to the following steps:
step 1, mixing 1g of starch, 0.9g of sodium alginate and deionized water, and heating to boil to gelatinize the starch; preparing a starch/sodium alginate uniform solution with the mass concentration of 15 wt%. Cooling to 4 ℃, standing for 12h to obtain the sodium alginate semi-interpenetrating network hydrogel with weaker strength;
step 2, soaking the sodium alginate interpenetrating network hydrogel obtained in the step 1 in an acid solution to form an alginic acid crystal cross-linked network;
soaking for 15 min; the acid solution is sorbic acid; the volume concentration of the acid solution is 4.7%;
step 3, drying the sodium alginate interpenetrating network hydrogel obtained in the step 2;
the drying time is 20 h; the drying mode is room temperature drying;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, drying, and finally soaking the hydrogel in deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking; soaking for 40 min; the acid solution is sorbic acid; the volume concentration of the acid solution is 5 percent; the drying time is 18 h; the swelling temperature is 12 ℃, and the swelling time is 25 h; the drying mode is room temperature drying. The sodium alginate interpenetrating network hydrogel has modulus of 1.1MPa, tensile breaking stress of 0.8MPa and breaking energy of 117J/m2。
Example 4
The invention relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which is implemented according to the following steps:
step 1, mixing 1g of gelatin and 1.2g of sodium alginate with deionized water, heating to 40 ℃ to prepare a gelatin/sodium alginate uniform solution with the mass concentration of 15 wt%, cooling to room temperature, and standing for 12 hours to obtain the sodium alginate interpenetrating network hydrogel with weak strength;
step 2, soaking the sodium alginate interpenetrating network hydrogel obtained in the step 1 in an acid solution to form an alginic acid crystal cross-linked network;
soaking for 8 min; the acid solution is acetic acid; the volume concentration of the acid solution is 15 percent;
step 3, drying the sodium alginate interpenetrating network hydrogel obtained in the step 2;
the drying time is 16 h; the drying mode is room temperature drying;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, drying, and finally soaking the hydrogel in deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking; the modulus of the sodium alginate interpenetrating network hydrogel is 0.4MPa, and the tensile breaking stress is 1.4 MPa;
soaking for 20 min; the acid solution is acetic acid; the volume concentration of the acid solution is 5 percent;
drying for 20 h; the swelling temperature is 20 ℃, and the swelling time is 100 h; the drying mode is room temperature drying.
Example 5
The invention relates to a preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking, which is implemented according to the following steps:
step 1, mixing 1g of serum protein and 1.5g of sodium alginate with deionized water to prepare a serum protein/sodium alginate uniform solution with the mass concentration of 10 wt%, heating to above 90 ℃, and continuously heating for 0.5h to obtain the sodium alginate interpenetrating network hydrogel with weaker strength;
step 2, soaking the sodium alginate interpenetrating network hydrogel obtained in the step 1 in an acid solution to form an alginic acid crystal cross-linked network;
soaking for 15 min; the acid solution is hydrochloric acid; the volume concentration of the acid solution is 15 percent;
step 3, drying the sodium alginate interpenetrating network hydrogel obtained in the step 2;
the drying time is 10 h; the drying mode is freeze drying;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, drying, and finally soaking the hydrogel in deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking; the modulus of the sodium alginate interpenetrating network hydrogel is 0.3MPa, the tensile breaking stress is 0.2MPa, and the breaking strain is 120 percent;
soaking for 45 min; the acid solution is hydrochloric acid; the volume concentration of the acid solution is 10 percent;
the drying time is 12 h; the swelling temperature is 27 ℃, and the swelling time is 1 h; the drying method is freeze drying.
The stress-strain test is carried out on the sodium alginate interpenetrating network hydrogel prepared by the method and the sodium alginate interpenetrating network hydrogel prepared by the one-step method after mixing, as shown in figure 1, it can be known that the stress and the strain of the sodium alginate interpenetrating network hydrogel prepared by the method are larger than those of the sodium alginate interpenetrating network hydrogel prepared by the one-step method, which shows that the mechanical property of the sodium alginate hydrogel is obviously improved by the acid treatment and the drying treatment of the method.
The sodium alginate hydrogel crosslinked by calcium ions, the sodium alginate hydrogel swollen in a water environment and the sodium alginate interpenetrating network hydrogel prepared by the method are subjected to stress-strain test, as shown in figure 2, it can be seen from the figure that the sodium alginate interpenetrating network hydrogel subjected to acid treatment and drying treatment in the method has low environmental dependence, and the defect of high environmental dependence of the traditional ionic crosslinking is overcome.
Claims (8)
1. A preparation method of a sodium alginate interpenetrating network hydrogel without ionic crosslinking is characterized by comprising the following steps:
step 1, mixing a biological macromolecule capable of being gelatinized or a biological macromolecule solution with sodium alginate to prepare a uniform solution, heating, cooling, and standing to crosslink the biological macromolecule capable of being gelatinized so as to obtain a biological macromolecule/sodium alginate semi-interpenetrating network hydrogel with weaker strength;
step 2, soaking the biomacromolecule/sodium alginate semi-interpenetrating network hydrogel obtained in the step 1 in an acid solution to enable part of sodium alginate to form alginic acid crystals, and crosslinking the sodium alginate to form a crystallized cross-linked sodium alginate biomacromolecule/sodium alginate interpenetrating network hydrogel;
step 3, drying the biological macromolecule/sodium alginate interpenetrating network hydrogel obtained in the step 2;
step 4, soaking the hydrogel obtained in the step 3 in an acid solution, and drying to obtain the sodium alginate mutual transmission network hydrogel with enhanced strength; and finally, soaking the hydrogel into deionized water for swelling to obtain the sodium alginate interpenetrating network hydrogel without ionic crosslinking.
2. The preparation method of the ion-free crosslinked sodium alginate interpenetrating network hydrogel as claimed in claim 1, wherein in the step 1, the heating temperature is 40-100 ℃, the heating time is 10min-5h, and the standing time is 0.5-16 h.
3. The preparation method of the ion-free crosslinked sodium alginate interpenetrating network hydrogel as claimed in claim 1, wherein in the step 1, the mass ratio of the biological macromolecule to the sodium alginate is 1: 0.1-1.5.
4. The method for preparing the non-ionic crosslinked sodium alginate interpenetrating network hydrogel as claimed in claim 3, wherein the biomacromolecule is any one of gelatin, agar, konjac polysaccharide, starch, soy protein, whey protein, beta-lac protein and serum protein.
5. The preparation method of the ion-free crosslinked sodium alginate interpenetrating network hydrogel according to claim 1, wherein in the step 2, the soaking time is 5-25 min; in the step 4, the soaking time is 20-60 min.
6. The method for preparing the ion-free crosslinked sodium alginate interpenetrating network hydrogel as claimed in claim 1, wherein in the step 2 and the step 4, the acid solution is any one of hydrochloric acid, acetic acid, citric acid, sorbic acid, fumaric acid, malic acid, gluconic acid and phosphoric acid; the volume concentration of the acid solution is 1-15%.
7. The preparation method of the ion-free crosslinked sodium alginate hydrogel with interpenetrating network as claimed in claim 1, wherein in the step 3, the drying time is 8-48 h.
8. The preparation method of the sodium alginate interpenetrating network hydrogel without ionic crosslinking according to claim 1, wherein in the step 4, the drying time is 10-36 h; the swelling temperature is 1-27 ℃, and the swelling time is 1-200 h.
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