CN113603906A - Temperature-sensitive hydrogel and preparation method and application thereof - Google Patents
Temperature-sensitive hydrogel and preparation method and application thereof Download PDFInfo
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- CN113603906A CN113603906A CN202111003299.2A CN202111003299A CN113603906A CN 113603906 A CN113603906 A CN 113603906A CN 202111003299 A CN202111003299 A CN 202111003299A CN 113603906 A CN113603906 A CN 113603906A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/12—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance
- G01K11/16—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance of organic materials
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- C08J2305/04—Alginic acid; Derivatives thereof
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/325—Calcium, strontium or barium phosphate
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- C08K5/00—Use of organic ingredients
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- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
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Abstract
A temperature-sensitive hydrogel is prepared by the following steps: 1) dissolving sodium alginate in water, and stirring to obtain sodium alginate solution; 2) adding an ether ester copolymer into a sodium alginate solution, and uniformly stirring to obtain a sample solution; 3) adding insoluble calcium salt into the sample solution, and uniformly stirring; 4) adding an acidic compound, reacting with insoluble calcium salt, stirring uniformly, and standing to obtain the temperature-sensitive hydrogel. The temperature-sensitive polyether ester copolymer and the natural polymer sodium alginate with no toxicity and no stimulation are synthesized under mild conditions, so that the temperature-sensitive polyether ester copolymer has temperature-sensitive response performance, has thermal irreversible performance, and has the advantages of no toxicity, good biocompatibility and degradability.
Description
Technical Field
The invention relates to the field of functional materials, in particular to a temperature-sensitive hydrogel and a preparation method and application thereof.
Background
While the polymer material continues to attach importance to the development of high performance, the polymer material is also developed in the direction of integration, functionalization and intellectualization.
At present, temperature-sensitive hydrogel researched in the fields of intelligent windows, thermochromic sensor materials and the like mainly takes N-isopropylacrylamide as a main monomer to synthesize poly-N-isopropylacrylamide temperature-sensitive hydrogel through a polymerization reaction. The temperature-sensitive hydrogel or the monomers used by the temperature-sensitive hydrogel have certain toxicity, and the volume shrinkage phenomenon of the temperature-sensitive hydrogel can occur in the actual use process.
Therefore, it is of great significance to develop a thermally irreversible hydrogel with temperature sensitive function, which is used in the fields of intelligent windows, thermochromic sensor materials and the like, is environment-friendly, thermally irreversible, and low in cost.
Disclosure of Invention
The invention aims to provide a temperature-sensitive hydrogel aiming at the defects of the prior art, which is synthesized by an ether ester copolymer with a temperature-sensitive function and natural polymer sodium alginate with no toxicity and no stimulation under mild conditions, has temperature-sensitive response performance, has thermal irreversible performance, and also has the advantages of no toxicity, good biocompatibility and degradability.
The technical scheme for realizing the purpose of the invention is as follows: a temperature-sensitive hydrogel is prepared by the following steps:
1) dissolving sodium alginate in water, and stirring to obtain sodium alginate solution;
2) adding an ether ester copolymer into a sodium alginate solution, and uniformly stirring to obtain a sample solution;
3) adding insoluble calcium salt into the sample solution, and uniformly stirring;
4) adding an acidic compound, reacting with insoluble calcium salt, stirring uniformly, and standing to obtain the temperature-sensitive hydrogel.
Step 1), the water is deionized water, and the mass ratio of sodium alginate to deionized water is 1-2: 40-120 ℃, the stirring and dissolving temperature is 70-90 ℃, and the stirring and dissolving time is 3-5 h.
The ether ester copolymer in the step 2) is a copolymer of hydroxyethyl vinyl ether and vinyl acetate, and the mass ratio of the ether ester is 1.05-1.45: 1, the concentration of the ether ester copolymer in the sodium alginate solution is 0.5-2 wt%.
The copolymer is prepared by the following steps:
1) under the environment of protective atmosphere, adding hydroxyethyl vinyl ether and vinyl acetate as polymerization monomers, wherein the mass ratio of the hydroxyethyl vinyl ether to the vinyl acetate is 1.05-1.45: 1;
2) adding an initiator, wherein the mass ratio of the addition amount of the initiator to the polymerized monomer is 1: 200, the initiator is dimethyl azodiisobutyrate and/or azodiisobutyronitrile;
2) and raising the temperature from room temperature to 65 ℃ every 5min, reacting for 6-8h, and cooling overnight to obtain the ether ester copolymer.
The insoluble calcium salt in the step 3) is one or a mixture of more of calcium carbonate, calcium sulfate, calcium sulfite, calcium silicate and calcium phosphate, and the mass ratio of the addition amount of the insoluble calcium salt to the sodium alginate solution is 0.5-1: 10-30.
Preferably, the insoluble calcium salt in step 3) is calcium sulfite.
The acidic compound in the step 4) is any one or a mixture of more of succinic anhydride, acetic acid and gluconolactone, and the mass ratio of the addition amount of the acidic compound to the sodium alginate solution is 0.5-2: 10-30.
Preferably, the acidic compound in step 4) is gluconolactone.
And 4) standing for 3-5h at normal temperature or low temperature.
The invention also requests to protect the application of any temperature-sensitive hydrogel in intelligent windows, thermochromic sensors, environment detection and temperature control detection in medical treatment.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the sodium alginate temperature-sensitive hydrogel provided by the invention is prepared by blending the ether ester copolymer and sodium alginate, so that the temperature-sensitive response performance of the temperature-sensitive hydrogel is ensured, and the temperature-sensitive hydrogel has the characteristics of no toxicity, good biocompatibility, degradability and the like. The temperature-sensitive hydrogel can reduce heat conduction by changing the solar light transmittance according to temperature change; and temperature-sensitive gold compound hydrogel can be obtained by grafting gold nanoparticles according to temperature change and used as a thermochromic sensor material to monitor the temperature of a system and the like.
2. The temperature-sensitive hydrogel provided by the invention can be blended with different substances, grafted and the like according to different requirements, so that the possibility of modification of hydrogels with different properties is provided, and the development and application of the products in the fields of intelligent windows, thermochromic sensors, environmental monitoring, medical temperature control detection and the like are expanded.
3. The temperature-sensitive hydrogel provided by the invention is an interpenetrating network structure hydrogel formed by an ether ester copolymer and sodium alginate. The temperature-sensitive response temperature of the temperature-sensitive hydrogel is realized by mainly adjusting the proportion of hydrophilic groups and hydrophobic groups of the ether ester copolymer, namely, the higher the proportion of hydroxyethyl vinyl ether containing hydrophilic groups is, the higher the density of hydrogen bonds formed by the ether ester copolymer and water molecules in the hydrogel is, the higher the energy required for breaking the hydrogen bonds is, the higher the temperature-sensitive response temperature is, and on the contrary, the higher the proportion of vinyl acetate containing hydrophobic groups is, the lower the temperature-sensitive response temperature is.
4. The preparation method of the temperature-sensitive hydrogel comprises the following steps of firstly preparing a sodium alginate hydrogel from a precursor of a self-synthesized hydroxyethyl vinyl ether-vinyl acetate copolymer by adopting an in-situ release method with a good effect: 1) fully dissolving sodium alginate in hot water, cooling until the solution is free of bubbles at room temperature, 2) adding an ether ester copolymer into the sodium alginate solution, fully swelling and mixing, and standing until the mixed solution is free of bubbles, 3) adding an insoluble calcium salt into the mixed solution, fully mixing, and standing until the mixed solution is free of bubbles, and 4) adding gluconolactone into the mixed solution, fully mixing, and standing to obtain the temperature-sensitive hydrogel. The temperature-sensitive hydrogel prepared by the method has the advantages of simple preparation method, thermal irreversible property, environmental protection and the like.
The following is a further description with reference to specific examples.
Detailed Description
In the invention, the ether ester copolymer is self-synthesized, and the rest is a commercial reagent grade product. The synthesis method of the ether ester copolymer comprises the following steps: 1) self-assembling a deoxidation closed system, fixing a balloon filled with nitrogen on a switchable tee joint, and then installing the balloon and other common components in a three-neck flask; 2) hydroxyethyl vinyl ether: 1g of vinyl acetate which is 1.05-1.45g, serving as a polymerization monomer, is added into a three-neck flask; 3) adding an initiator, wherein the mass ratio of the initiator to the polymerization monomer is 1: 200, selecting dimethyl azodiisobutyrate and/or azodiisobutyronitrile as an initiator; 4) closing the three-neck flask after releasing the nitrogen; 4) and raising the temperature from room temperature to 65 ℃ every 5min, reacting for 6-8h, and cooling overnight to obtain the ether ester copolymer.
EXAMPLE 1 preparation of temperature-sensitive hydrogel
Sodium alginate: 50g of deionized water is fed into a 250ml beaker, and the sodium alginate is heated and stirred to dissolve for 3-5h at the temperature of 70-90 ℃ to obtain a sodium alginate solution. 20g of Sodium Alginate (SA) solution was taken out into a beaker, and 0.1g of ether ester copolymer was added to the beaker, followed by thorough mixing with stirring. To the mixed sample solution, 0.5g of calcium sulfite was added, followed by thorough mixing with stirring. And adding 1g of glucolactone into the mixed sample solution, fully stirring and mixing, and standing to obtain the uniform temperature-sensitive hydrogel.
The prepared temperature-sensitive hydrogel is detected at the temperature of 35-60 ℃ and then is found to have the temperature-sensitive function and the thermal irreversible performance.
EXAMPLE 2 preparation of temperature-sensitive hydrogel
Sodium alginate: feeding 400g of deionized water into a 250ml beaker, and heating and stirring to dissolve sodium alginate at the temperature of 70-90 ℃ for 3-5h to obtain a sodium alginate solution. 20g of Sodium Alginate (SA) solution was taken out into a beaker, and 0.1g of ether ester copolymer was added to the beaker, followed by thorough mixing with stirring. To the mixed sample solution, 0.5g of calcium silicate was added, followed by thorough mixing with stirring. And adding 1g of glucolactone into the mixed sample solution, fully stirring and mixing, and standing to obtain the uniform temperature-sensitive hydrogel.
The prepared temperature-sensitive hydrogel is detected at the temperature of 35-60 ℃ and then is found to have the temperature-sensitive function and the thermal irreversible performance.
EXAMPLE 3 preparation of temperature-sensitive hydrogel
Sodium alginate: feeding 400g of deionized water into a 250ml beaker, and heating and stirring to dissolve sodium alginate at the temperature of 70-90 ℃ for 3-5h to obtain a sodium alginate solution. 20g of Sodium Alginate (SA) solution was taken out into a beaker, and 0.1g of ether ester copolymer was added to the beaker, followed by thorough mixing with stirring. To the mixed sample solution was added 0.5g of calcium phosphate swollen with 5g of deionized water, followed by thorough mixing with stirring. And adding 1g of gluconolactone swelled by 5g of deionized water into the mixed sample solution, fully stirring and mixing, and standing to obtain the uniform temperature-sensitive hydrogel.
The prepared temperature-sensitive hydrogel is detected at the temperature of 35-60 ℃ and then is found to have the temperature-sensitive function and the thermal irreversible performance.
Example 4 preparation of Ether ester copolymer temperature sensitive hydrogels with different ratios
Sodium alginate: 50g of deionized water is fed into a 250ml beaker, and the sodium alginate is heated and stirred to dissolve for 3-5h at the temperature of 70-90 ℃ to obtain a sodium alginate solution. 20g of Sodium Alginate (SA) solution is taken out of different beakers, 0.1g of ether ester copolymer with the mass ratio of 1.05:1-1.45:1 is added into each beaker, and then the mixture is fully stirred and mixed. To the mixed sample solution, 0.5g of calcium sulfite was added, followed by thorough mixing with stirring. And adding 1g of glucolactone into the mixed sample solution, fully stirring and mixing, and standing to obtain the uniform temperature-sensitive hydrogel.
The mass ratio of the prepared ether ester is 1.05:1-1.25:1, and the temperature-sensitive hydrogel is detected at the temperature of 35-45 ℃ and then has the temperature-sensitive function and the thermal irreversible performance. The temperature-sensitive hydrogel with the mass ratio of ether ester being 1.25:1-1.45:1 is detected at the temperature of 45-60 ℃ and then is found to have the temperature-sensitive function and the thermal irreversible performance.
Claims (10)
1. The temperature-sensitive hydrogel is characterized by being prepared by the following steps:
1) dissolving sodium alginate in water, and stirring to obtain sodium alginate solution;
2) adding an ether ester copolymer into a sodium alginate solution, and uniformly stirring to obtain a sample solution;
3) adding insoluble calcium salt into the sample solution, and uniformly stirring;
4) adding an acidic compound, reacting with insoluble calcium salt, stirring uniformly, and standing to obtain the temperature-sensitive hydrogel.
2. The temperature-sensitive hydrogel according to claim 1, wherein the water in step 1) is deionized water, and the mass ratio of sodium alginate to deionized water is 1-2: 40-120 ℃, the stirring and dissolving temperature is 70-90 ℃, and the stirring and dissolving time is 3-5 h.
3. The temperature-sensitive hydrogel according to claim 1, wherein the ether ester copolymer in step 2) is a copolymer of hydroxyethyl vinyl ether and vinyl acetate, and the mass ratio of the ether ester is 1.05-1.45: 1, the concentration of the ether ester copolymer in the sodium alginate solution is 0.5-2 wt%.
4. The temperature-sensitive hydrogel according to claim 3, wherein the copolymer is prepared by the following steps:
1) under the environment of protective atmosphere, adding hydroxyethyl vinyl ether and vinyl acetate, wherein the mass ratio of the hydroxyethyl vinyl ether to the vinyl acetate is 1.05-1.45: 1;
2) adding an initiator, wherein the mass ratio of the addition amount of the initiator to the polymerized monomer is 1: 200, the initiator is dimethyl azodiisobutyrate and/or azodiisobutyronitrile;
3) and raising the temperature from room temperature to 65 ℃ every 5min, reacting for 6-8h, and cooling overnight to obtain the ether ester copolymer.
5. The temperature-sensitive hydrogel according to claim 1, wherein the insoluble calcium salt in step 3) is one or a mixture of calcium carbonate, calcium sulfate, calcium sulfite, calcium silicate and calcium phosphate, and the mass ratio of the addition amount of the insoluble calcium salt to the sodium alginate solution is 0.5-1: 10-30.
6. The temperature-sensitive hydrogel according to claim 5, wherein the insoluble calcium salt of step 3) is calcium sulfite.
7. The temperature-sensitive hydrogel according to claim 1, wherein the acidic compound in step 4) is any one or a mixture of succinic anhydride, acetic acid and gluconolactone, and the mass ratio of the added amount of the acidic compound to the sodium alginate solution is 0.5-2: 10-30.
8. The temperature-sensitive hydrogel according to claim 7, wherein the acidic compound of step 4) is gluconolactone.
9. The temperature-sensitive hydrogel according to claim 1, wherein the step 4) is allowed to stand at normal or low temperature for 3-5 hours.
10. Use of the temperature-sensitive hydrogel according to any one of claims 1 to 9 in smart windows, thermochromic sensors, environmental testing, temperature-controlled testing in medical treatment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114853931A (en) * | 2022-04-13 | 2022-08-05 | 四川大学 | Preparation method of temperature-sensitive intelligent window with response temperature adjusted through Hofmeis special effect |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796267A (en) * | 2012-09-06 | 2012-11-28 | 北京理工大学 | Sodium-alginate-based temperature-sensitive polymer aquagel smart dimming film and preparation method thereof |
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- 2021-08-30 CN CN202111003299.2A patent/CN113603906A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102796267A (en) * | 2012-09-06 | 2012-11-28 | 北京理工大学 | Sodium-alginate-based temperature-sensitive polymer aquagel smart dimming film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| SUGIHARA, S; YOSHIDA, A; MAEDA, Y: "《MACROMOLECULES》", 《DESIGN OF HYDROXY-FUNCTIONALIZED THERMORESPONSIVE COPOLYMERS: IMPROVED DIRECT RADICAL POLYMERIZATION OF HYDROXY-FUNCTIONAL VINYL ETHERS.SUGIHARA》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114853931A (en) * | 2022-04-13 | 2022-08-05 | 四川大学 | Preparation method of temperature-sensitive intelligent window with response temperature adjusted through Hofmeis special effect |
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Application publication date: 20211105 |