CN110183570B - Preparation method of temperature-sensitive gel - Google Patents
Preparation method of temperature-sensitive gel Download PDFInfo
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- CN110183570B CN110183570B CN201910416420.0A CN201910416420A CN110183570B CN 110183570 B CN110183570 B CN 110183570B CN 201910416420 A CN201910416420 A CN 201910416420A CN 110183570 B CN110183570 B CN 110183570B
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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Abstract
The invention relates to a preparation method of a temperature-sensitive gel, belonging to the technical field of materials. The invention takes cod skin and edible fly maggot as raw materials, grinding and crushing the raw materials, performing enzymolysis to obtain polypeptide and amino acid mixture, mixing the polypeptide and amino acid mixture with N-isopropylacrylamide, improving the sensitivity to poly (N-isopropylacrylamide) by modifying supernatant and additives in the polymerization process, crosslinking the supernatant by using a crosslinking agent, improving the swelling effect of temperature-sensitive gel, improving the biocompatibility of the temperature-sensitive gel, effectively increasing the antibacterial performance of the gel by using antibacterial polypeptide substances in the gel, mixing chlorophyll, hydroxyethyl methacrylate and N-vinyl pyrrolidone, performing magnesium removal treatment under an acidic condition, initiating polymerization graft polymer by using an initiator to form a crosslinked network structure, and increasing the temperature and the photosensitive performance, thereby improving the temperature sensitivity of the temperature sensitive gel.
Description
Technical Field
The invention relates to a preparation method of a temperature-sensitive gel, belonging to the technical field of materials.
Background
The hydrogel is a three-dimensional network structure formed by covalent bonds of macromolecules and is a common substance form commonly existing in nature. The intelligent hydrogel is a special hydrogel which can sense tiny chemical or physical stimuli in the surrounding environment, can respond quickly and can change a plurality of properties obviously. The hydrogel can swell and absorb a large amount of water in water, but is not dissolved in water, which has similarity with a plurality of structures of living organisms, in recent years, the hydrogel relates to the fields of biomedicine, material science, agriculture and the like, and a plurality of researchers carry out extensive research on the synthesis, properties and practical application of the hydrogel.
The temperature-sensitive hydrogel is a hydrogel with water (or solvent) absorption quantity having mutation at a certain temperature, and the temperature when the swelling ratio has mutation is the sensitive temperature. Because the temperature sensitivity is high, the swelling ratio is high, and the sensitive temperature is close to that of people, the method has wide application in the aspects of material separation, immobilized enzyme, immunoassay, drug release and the like. At present, although the temperature-sensitive gel is simple and convenient to operate and low in preparation cost, the temperature sensitivity and the swelling ratio of the temperature-sensitive gel are low, so that the application range of the temperature-sensitive gel is narrow.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the invention provides a preparation method of a temperature-sensitive gel, aiming at the problems of lower temperature sensitivity and lower swelling ratio of the existing temperature-sensitive gel.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of temperature-sensitive gel comprises the following steps:
(1) grinding the cod skin, the edible fly maggots and the mixed solvent according to the mass ratio of 3-6: 1-3: 10, collecting the ground materials, mixing the ground materials and the mixed enzyme according to the mass ratio of 14-16: 1-3, adjusting the pH value, standing and carrying out enzymolysis;
(2) centrifuging after enzymolysis is finished, collecting supernatant, and taking 120-130 parts of water, 30-40 parts of N-isopropylacrylamide, 12-15 parts of supernatant, 7-9 parts of additive, 1-3 parts of initiator and 1-2 parts of cross-linking agent according to parts by weight;
(3) putting water, N-isopropyl acrylamide and an additive into a reaction kettle, using nitrogen for protection, heating, adding an initiator, stirring, cooling, adding a supernatant and a crosslinking agent, stirring, standing, discharging, and collecting a discharged material;
(4) and uniformly mixing the discharged mixture and a surfactant according to the mass ratio of 17: 1-3, adjusting the pH, carrying out reduced pressure concentration, and sterilizing to obtain the temperature-sensitive gel.
The mixed solvent in the step (1) is formed by mixing water, sodium acetate, glycerol and citric acid according to a mass ratio of 9-11: 1-4: 6-8: 2.
The mixed enzyme in the step (1) is formed by mixing papain and serine protease according to the mass ratio of 3: 1-3.
The preparation method of the additive comprises the following steps:
A. putting the chlorophyll, the mixture and the diethyl ether into a reaction kettle according to the mass ratio of 3: 2-4: 17, preheating at 50-55 ℃, heating to 85-95 ℃, adjusting the pH to 3.0-3.5, and preserving heat;
B. and after the heat preservation is finished, adding a catalyst accounting for 1-1.5% of the mass of the mixture and an initiator A accounting for 2-4% of the mass of the hydroxyethyl methacrylate, heating for reaction, cooling, adjusting the pH value to be neutral, standing, filtering, washing and drying to obtain the additive.
The mixture in the step A is prepared by mixing hydroxyethyl methacrylate and N-vinyl pyrrolidone according to a mass ratio of 1: 1-3.
The catalyst in the B is dibutyltin dilaurate.
In the B, the initiator A is azodiisobutyronitrile.
The initiator is any one of potassium persulfate and ammonium persulfate.
The cross-linking agent is formed by mixing N, N-methylene acrylamide and genipin according to the mass ratio of 3: 1-4.
And (4) mixing the surfactant lecithin and the sorbitan fatty acid ester according to the mass ratio of 6: 1-5 to obtain the surfactant.
Compared with other methods, the method has the beneficial technical effects that:
the invention takes cod skin and edible fly maggot as raw materials, the mixture of polypeptide and amino acid is obtained by grinding, crushing and enzymolysis, then the mixture is mixed with N-isopropyl acrylamide, the poly (N-isopropyl acrylamide) is formed by mixing reaction with the N-isopropyl acrylamide, the sensitivity to the poly (N-isopropyl acrylamide) is improved by modification of supernatant and additive in the polymerization process, meanwhile, the cross-linking agent is utilized to be cross-linked with the supernatant, the swelling effect of temperature-sensitive gel is improved, the biocompatibility of the temperature-sensitive gel is improved, the antibacterial property of the gel can be effectively improved by the antibacterial polypeptide substance in the gel, meanwhile, the invention mixes chlorophyll with hydroxyethyl methacrylate and N-vinyl pyrrolidone, and the magnesium removal treatment is carried out under the acidic condition, and initiating polymerization of the graft polymer by using an initiator to form a cross-linked network structure, and further improving the temperature sensitivity of the temperature-sensitive gel by increasing the temperature and the photosensitive performance.
Detailed Description
The mixed solvent is formed by mixing water, sodium acetate, glycerol and citric acid according to the mass ratio of 9-11: 1-4: 6-8: 2.
The mixed enzyme is formed by mixing papain and serine protease according to the mass ratio of 3: 1-3.
The mixture is formed by mixing hydroxyethyl methacrylate and N-vinyl pyrrolidone according to the mass ratio of 1: 1-3.
The catalyst was dibutyltin dilaurate.
The initiator A is azodiisobutyronitrile.
The preparation method of the additive comprises the following steps:
A. putting the chlorophyll, the mixture and the diethyl ether into a reaction kettle according to the mass ratio of 3: 2-4: 17, preheating for 30min at 50-55 ℃, then heating to 85-95 ℃ for 2h, adjusting the pH value to 3.0-3.5, and preserving heat;
B. and after the heat preservation is finished, adding a catalyst accounting for 1-1.5% of the mass of the mixture and an initiator A accounting for 2-4% of the mass of the hydroxyethyl methacrylate, heating to 110-115 ℃ for reaction for 10 hours, cooling to room temperature, adjusting the pH value to be neutral, standing for 5 hours, filtering, washing filter residues, and drying to obtain the additive.
The initiator is any one of potassium persulfate and ammonium persulfate.
The cross-linking agent is formed by mixing N, N-methylene acrylamide and genipin according to the mass ratio of 3: 1-4.
The surfactant is prepared by mixing lecithin and sorbitan fatty acid ester according to the mass ratio of 6: 1-5.
A preparation method of temperature-sensitive gel comprises the following steps:
(1) grinding the cod skin, the edible fly maggots and the mixed solvent according to the mass ratio of 3-6: 1-3: 10, collecting the ground materials, mixing the ground materials and the mixed enzyme according to the mass ratio of 14-16: 1-3, adjusting the pH value to 8.0, standing, and performing enzymolysis for 5 hours;
(2) after enzymolysis is finished, centrifuging at 6000r/min for 10min, collecting supernatant, and taking 120-130 parts of water, 30-40 parts of N-isopropylacrylamide, 12-15 parts of supernatant, 7-9 parts of additive, 1-3 parts of initiator and 1-2 parts of cross-linking agent according to parts by weight;
(3) putting water, N-isopropyl acrylamide and an additive into a reaction kettle, heating to 70-80 ℃ under the protection of nitrogen, adding an initiator, stirring for 6 hours, cooling to 50-55 ℃, adding a supernatant and a crosslinking agent, stirring for 50 minutes, standing for 3 hours, discharging, and collecting a discharged material;
(4) uniformly mixing the discharged mixture and a surfactant according to a mass ratio of 17: 1-3 to obtain a mixture, adjusting the pH to be neutral, concentrating under reduced pressure to 60-70% of the volume of the mixture, and sterilizing to obtain the temperature-sensitive gel.
Example 1
The mixed solvent is prepared by mixing water, sodium acetate, glycerol and citric acid according to the mass ratio of 11:4:8: 2.
The mixed enzyme is formed by mixing papain and serine protease according to the mass ratio of 3: 3.
The mixture is prepared by mixing hydroxyethyl methacrylate and N-vinyl pyrrolidone according to the mass ratio of 1: 1.
The catalyst was dibutyltin dilaurate.
The initiator A is azodiisobutyronitrile.
The preparation method of the additive comprises the following steps:
A. putting the chlorophyll, the mixture and the diethyl ether into a reaction kettle according to the mass ratio of 3:2:17, preheating for 30min at 50 ℃, then heating to 85 ℃ for 2h, adjusting the pH value to 3.0, and preserving the heat for 3 h;
B. and after the heat preservation is finished, adding a catalyst accounting for 1% of the mass of the mixture and an initiator A accounting for 2% of the mass of the hydroxyethyl methacrylate, heating to 110 ℃ for reaction for 10 hours, cooling to room temperature, adjusting the pH value to be neutral, standing for 5 hours, filtering, washing filter residues, and drying to obtain the additive.
The initiator is potassium persulfate.
The cross-linking agent is prepared by mixing N, N-methylene acrylamide and genipin according to the mass ratio of 3: 4.
The surfactant is prepared by mixing lecithin and sorbitan fatty acid ester according to the mass ratio of 6: 5.
A preparation method of temperature-sensitive gel comprises the following steps:
(1) grinding the cod skin, the edible fly maggots and the mixed solvent according to the mass ratio of 6:3:10, collecting the ground material, mixing the ground material and the mixed enzyme according to the mass ratio of 16:3, adjusting the pH value to 8.0, standing, and performing enzymolysis for 5 hours;
(2) after enzymolysis is finished, centrifuging at 6000r/min for 10min, collecting supernatant, and taking 130 parts of water, 40 parts of N-isopropylacrylamide, 15 parts of supernatant, 9 parts of additive, 3 parts of initiator and 2 parts of cross-linking agent according to parts by weight;
(3) putting water, N-isopropyl acrylamide and an additive into a reaction kettle, heating to 80 ℃ under the protection of nitrogen, adding an initiator, stirring for 6 hours, cooling to 55 ℃, adding a supernatant and a cross-linking agent, stirring for 50 minutes, standing for 3 hours, discharging, and collecting a discharged material;
(4) and uniformly mixing the discharged mixture and a surfactant according to the mass ratio of 17:3 to obtain a mixture, adjusting the pH value to be neutral, concentrating under reduced pressure to 70% of the volume of the mixture, and sterilizing to obtain the temperature-sensitive gel.
Example 2
The mixed solvent is prepared by mixing water, sodium acetate, glycerol and citric acid according to the mass ratio of 10:3:7: 2.
The mixed enzyme is prepared by mixing papain and serine protease according to the mass ratio of 3: 2.
The mixture is prepared by mixing hydroxyethyl methacrylate and N-vinyl pyrrolidone according to the mass ratio of 1: 2.
The catalyst was dibutyltin dilaurate.
The initiator A is azodiisobutyronitrile.
The preparation method of the additive comprises the following steps:
A. putting the chlorophyll, the mixture and the diethyl ether into a reaction kettle according to the mass ratio of 3:3:17, preheating for 30min at 53 ℃, then heating to 90 ℃ for 2h, adjusting the pH value to 3.0, and preserving the heat for 3 h;
B. and after the heat preservation is finished, adding a catalyst accounting for 1.3% of the mass of the mixture and an initiator A accounting for 3% of the mass of the hydroxyethyl methacrylate, heating to 113 ℃ for reaction for 10 hours, cooling to room temperature, adjusting the pH value to be neutral, standing for 5 hours, filtering, washing filter residues, and drying to obtain the additive.
The initiator is ammonium persulfate.
The cross-linking agent is prepared by mixing N, N-methylene acrylamide and genipin according to the mass ratio of 3: 3.
The surfactant is prepared by mixing lecithin and sorbitan fatty acid ester according to the mass ratio of 6: 3.
A preparation method of temperature-sensitive gel comprises the following steps:
(1) grinding the cod skin, the edible fly maggots and the mixed solvent according to the mass ratio of 5:2:10, collecting the ground material, mixing the ground material and the mixed enzyme according to the mass ratio of 15:2, adjusting the pH value to 8.0, standing, and performing enzymolysis for 5 hours;
(2) after the enzymolysis is finished, centrifuging at 6000r/min for 10min, collecting supernatant, and taking 125 parts of water, 35 parts of N-isopropylacrylamide, 14 parts of supernatant, 8 parts of additive, 2 parts of initiator and 1.5 parts of cross-linking agent according to parts by weight;
(3) putting water, N-isopropyl acrylamide and an additive into a reaction kettle, heating to 75 ℃ under the protection of nitrogen, adding an initiator, stirring for 6 hours, cooling to 53 ℃, adding a supernatant and a cross-linking agent, stirring for 50 minutes, standing for 3 hours, discharging, and collecting a discharged material;
(4) and uniformly mixing the discharged mixture and a surfactant according to the mass ratio of 17:2 to obtain a mixture, adjusting the pH value to be neutral, concentrating under reduced pressure to 65% of the volume of the mixture, and sterilizing to obtain the temperature-sensitive gel.
Example 3
The mixed solvent is prepared by mixing water, sodium acetate, glycerol and citric acid according to the mass ratio of 9:1:6: 2.
The mixed enzyme is prepared by mixing papain and serine protease according to the mass ratio of 3: 1.
The mixture is prepared by mixing hydroxyethyl methacrylate and N-vinyl pyrrolidone according to the mass ratio of 1: 3.
The catalyst was dibutyltin dilaurate.
The initiator A is azodiisobutyronitrile.
The preparation method of the additive comprises the following steps:
A. putting the chlorophyll, the mixture and the diethyl ether into a reaction kettle according to the mass ratio of 3:4:17, preheating for 30min at 50-55 ℃, then heating to 95 ℃ for 2h, adjusting the pH value to 3.5, and keeping the temperature for 3 h;
B. and after the heat preservation is finished, adding a catalyst accounting for 1.5% of the mass of the mixture and an initiator A accounting for 4% of the mass of the hydroxyethyl methacrylate, heating to 115 ℃ for reaction for 10 hours, cooling to room temperature, adjusting the pH value to be neutral, standing for 5 hours, filtering, washing filter residues, and drying to obtain the additive.
The initiator is potassium persulfate.
The cross-linking agent is prepared by mixing N, N-methylene acrylamide and genipin according to the mass ratio of 3: 1.
The surfactant is prepared by mixing lecithin and sorbitan fatty acid ester according to the mass ratio of 6: 1.
A preparation method of temperature-sensitive gel comprises the following steps:
(1) grinding the cod skin, the edible fly maggots and the mixed solvent according to the mass ratio of 3:1:10, collecting the ground material, mixing the ground material and the mixed enzyme according to the mass ratio of 14:1, adjusting the pH value to 8.0, standing, and performing enzymolysis for 5 hours;
(2) after the enzymolysis is finished, centrifuging at 6000r/min for 10min, collecting supernatant, and taking 120 parts of water, 30 parts of N-isopropylacrylamide, 12 parts of supernatant, 7 parts of additive, 1 part of initiator and 1 part of cross-linking agent according to parts by weight;
(3) putting water, N-isopropyl acrylamide and an additive into a reaction kettle, heating to 70 ℃ under the protection of nitrogen, adding an initiator, stirring for 6 hours, cooling to 50 ℃, adding a supernatant and a cross-linking agent, stirring for 50 minutes, standing for 3 hours, discharging, and collecting a discharged material;
(4) uniformly mixing the discharged mixture and a surfactant according to the mass ratio of 17:1 to obtain a mixture, adjusting the pH to be neutral, concentrating under reduced pressure to 60% of the volume of the mixture, and sterilizing to obtain the temperature-sensitive gel.
Comparative example 1
The mixed solvent is prepared by mixing water, sodium acetate, glycerol and citric acid according to the mass ratio of 10:3:7: 2.
The mixed enzyme is prepared by mixing papain and serine protease according to the mass ratio of 3: 2.
The mixture is prepared by mixing hydroxyethyl methacrylate and N-vinyl pyrrolidone according to the mass ratio of 1: 2.
The catalyst was dibutyltin dilaurate.
The initiator A is azodiisobutyronitrile.
The preparation method of the additive comprises the following steps:
A. putting the chlorophyll, the mixture and the diethyl ether into a reaction kettle according to the mass ratio of 3:3:17, preheating for 30min at 53 ℃, then heating to 90 ℃ for 2h, adjusting the pH value to 3.0, and preserving the heat for 3 h;
B. and after the heat preservation is finished, adding a catalyst accounting for 1.3% of the mass of the mixture and an initiator A accounting for 3% of the mass of the hydroxyethyl methacrylate, heating to 113 ℃ for reaction for 10 hours, cooling to room temperature, adjusting the pH value to be neutral, standing for 5 hours, filtering, washing filter residues, and drying to obtain the additive.
The initiator is ammonium persulfate.
The cross-linking agent is prepared by mixing N, N-methylene acrylamide and genipin according to the mass ratio of 3: 3.
The surfactant is prepared by mixing lecithin and sorbitan fatty acid ester according to the mass ratio of 6: 3.
A preparation method of temperature-sensitive gel comprises the following steps:
(1) grinding the cod skin, the edible fly maggots and the mixed solvent according to the mass ratio of 5:2:10, collecting the ground material, mixing the ground material and the mixed enzyme according to the mass ratio of 15:2, adjusting the pH value to 8.0, standing, and performing enzymolysis for 5 hours;
(2) after the enzymolysis is finished, centrifuging at 6000r/min for 10min, collecting supernatant, and taking 125 parts of water, 35 parts of N-isopropylacrylamide, 8 parts of additive, 2 parts of initiator and 1.5 parts of cross-linking agent according to parts by weight;
(3) putting water, N-isopropyl acrylamide and an additive into a reaction kettle, heating to 75 ℃ under the protection of nitrogen, adding an initiator, stirring for 6 hours, cooling to 53 ℃, adding a cross-linking agent, stirring for 50min, standing for 3 hours, discharging, and collecting a discharged material;
(4) and uniformly mixing the discharged mixture and a surfactant according to the mass ratio of 17:2 to obtain a mixture, adjusting the pH value to be neutral, concentrating under reduced pressure to 65% of the volume of the mixture, and sterilizing to obtain the temperature-sensitive gel.
Comparative example 2
Essentially the same as example 2, except that the supernatant was absent.
Comparative example 3
A commercially available poly (N-isopropylacrylamide) temperature sensitive gel.
The temperature-sensitive gels in the examples and comparative examples were examined.
Placing the sol in a 1.5mL plastic centrifuge tube at room temperature, placing in a 37 ℃ water bath to gelatinize the sol, irradiating for a period of time at a certain power by using a physiotherapy probe of a microwave therapeutic apparatus, measuring the temperature by using an American import thermocouple wire, measuring the intermediate temperature of the gel, and detecting the conversion time of the sol to the gel;
characterization of Water absorption: taking a small block of freeze-dried gel (n = 5), weighing the mass as W1, soaking the gel in distilled water for 24h, taking out the gel, wiping off excessive surface water, weighing the mass as W2, and calculating the water absorption rate as follows: e = (W2-W1)/W1 × 100%, and the results are shown in the following table:
| transition time (min) | Water absorption (%) | |
| Example 1 | 2 | 568 |
| Example 2 | 1.2 | 593 |
| Example 3 | 1.8 | 572 |
| Comparative example 1 | 3.8 | 521 |
| Comparative example 2 | 3.2 | 558 |
| Comparative example 3 | 2.3 | 547 |
In conclusion, the temperature-sensitive gel prepared by the invention has better performance.
Claims (8)
1. The preparation method of the temperature-sensitive gel is characterized by comprising the following steps:
(1) grinding the cod skin, the edible fly maggots and the mixed solvent according to the mass ratio of 3-6: 1-3: 10, collecting the ground materials, mixing the ground materials and the mixed enzyme according to the mass ratio of 14-16: 1-3, adjusting the pH value, standing and carrying out enzymolysis;
(2) centrifuging after enzymolysis is finished, collecting supernatant, and taking 120-130 parts of water, 30-40 parts of N-isopropylacrylamide, 12-15 parts of supernatant, 7-9 parts of additive, 1-3 parts of initiator and 1-2 parts of cross-linking agent according to parts by weight;
the preparation method of the additive comprises the following steps:
A. putting the chlorophyll, the mixture and the diethyl ether into a reaction kettle according to the mass ratio of 3: 2-4: 17, preheating at 50-55 ℃, heating to 85-95 ℃, adjusting the pH to 3.0-3.5, and preserving heat; the mixture is formed by mixing hydroxyethyl methacrylate and N-vinyl pyrrolidone according to the mass ratio of 1: 1-3;
B. after the heat preservation is finished, adding a catalyst accounting for 1-1.5% of the mass of the mixture and an initiator A accounting for 2-4% of the mass of the hydroxyethyl methacrylate, heating for reaction, cooling, adjusting the pH value to be neutral, standing, filtering, washing and drying to obtain an additive;
(3) putting water, N-isopropyl acrylamide and an additive into a reaction kettle, using nitrogen for protection, heating, adding an initiator, stirring, cooling, adding a supernatant and a crosslinking agent, stirring, standing, discharging, and collecting a discharged material;
(4) and uniformly mixing the discharged mixture and a surfactant according to the mass ratio of 17: 1-3, adjusting the pH, carrying out reduced pressure concentration, and sterilizing to obtain the temperature-sensitive gel.
2. The preparation method of the temperature-sensitive gel according to claim 1, wherein the mixed solvent in the step (1) is prepared by mixing water, sodium acetate, glycerol and citric acid according to a mass ratio of 9-11: 1-4: 6-8: 2.
3. The preparation method of the temperature-sensitive gel according to claim 1, wherein the mixed enzyme in the step (1) is formed by mixing papain and serine protease in a mass ratio of 3: 1-3.
4. The method for preparing the temperature-sensitive gel according to claim 1, wherein the catalyst in the step B is dibutyltin dilaurate.
5. The method for preparing a temperature-sensitive gel according to claim 1, wherein the initiator A in the step B is azobisisobutyronitrile.
6. The preparation method of the temperature-sensitive gel according to claim 1, wherein the initiator is any one of potassium persulfate and ammonium persulfate.
7. The preparation method of the temperature-sensitive gel according to claim 1, wherein the cross-linking agent is prepared by mixing N, N-methylene acrylamide and genipin according to a mass ratio of 3: 1-4.
8. The preparation method of the temperature-sensitive gel according to claim 1, wherein in the step (4), the surfactant is prepared by mixing lecithin and sorbitan fatty acid ester according to a mass ratio of 6: 1-5.
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