CN117467079A - Temperature-sensitive NIPAM/SA hydrogel, preparation method thereof and essence and perfume slow-release system - Google Patents

Temperature-sensitive NIPAM/SA hydrogel, preparation method thereof and essence and perfume slow-release system Download PDF

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CN117467079A
CN117467079A CN202311440713.5A CN202311440713A CN117467079A CN 117467079 A CN117467079 A CN 117467079A CN 202311440713 A CN202311440713 A CN 202311440713A CN 117467079 A CN117467079 A CN 117467079A
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hydrogel
sodium alginate
temperature
isopropyl acrylamide
substance
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苗丽坤
程书锋
张雨迎
陈�胜
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WUHAN YELLOW CRANE TOWER NEW MATERIAL TECHNOLOGY DEVELOPMENT CO LTD
China Tobacco Hubei Industrial LLC
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WUHAN YELLOW CRANE TOWER NEW MATERIAL TECHNOLOGY DEVELOPMENT CO LTD
China Tobacco Hubei Industrial LLC
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Priority to CN202311440713.5A priority Critical patent/CN117467079A/en
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2351/00Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/02Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides

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Abstract

The invention provides a preparation method of temperature-sensitive NIPAM/SA hydrogel, which comprises the following steps: a) Adding water into sodium alginate and N-isopropyl acrylamide to dissolve to obtain sodium alginate-N-isopropyl acrylamide solution; b) Adding a cross-linking agent into a sodium alginate-N-isopropyl acrylamide solution, stirring and mixing the mixture with a pore-forming agent, and heating the mixture for reaction to obtain a reaction solution; c) Freezing the reaction liquid, adding an initiating auxiliary agent, stirring, deoxidizing, adding an initiator, and reacting to obtain a gel-like substance; d) Freeze-drying the gel-like substance to obtain an aerogel-like substance; e) And mixing the aerogel-like substance with water for re-swelling to obtain the temperature-sensitive NIPAM/SA hydrogel. Experimental results show that the deswelling rate prepared by the invention can reach (93.76+/-0.22)%. The prepared fragrance-carrying capsules have the same swelling eliminating rate, the release rate of the essence is more than 90% when heated at 60 ℃ for 10min, and the temperature control release of the water-based essence is realized.

Description

Temperature-sensitive NIPAM/SA hydrogel, preparation method thereof and essence and perfume slow-release system
Technical Field
The invention relates to the technical field of essence and spice slow release, in particular to a temperature-sensitive NIPAM/SA hydrogel, a preparation method thereof and an essence and spice slow release system.
Background
Poly-N-isopropyl acrylamide (PNIAPM) hydrogel is a typical heat-shrinkable temperature-sensitive intelligent hydrogel, contains hydrophilic amide groups and hydrophobic isopropyl groups, and changes the interaction of the groups and water molecules when stimulated by external temperature, so that the hydrogel changes phase, and has special swelling and imbibition properties. Is widely applied to the fields of controlled drug release, biochemical system separation, medical materials, foods and the like.
It would therefore be highly desirable to provide a temperature sensitive NIPAM/SA hydrogel capable of adsorbing water soluble fragrance and flavor to form a fragrance and flavor hydrogel sustained release system.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a temperature-sensitive NIPAM/SA hydrogel, which can realize the temperature-controlled release of essence (applied to cigarettes, can realize the temperature-controlled release of the cigarette essence and achieve the effect of improving the taste of the cigarettes).
The invention provides a preparation method of temperature-sensitive NIPAM/SA hydrogel, which comprises the following steps:
a) Adding water into sodium alginate and N-isopropyl acrylamide to dissolve to obtain sodium alginate-N-isopropyl acrylamide solution;
b) Adding a cross-linking agent into a sodium alginate-N-isopropyl acrylamide solution, stirring and mixing the mixture with a pore-forming agent, and heating the mixture for reaction to obtain a reaction solution;
c) Freezing the reaction liquid, adding an initiating auxiliary agent, stirring, deoxidizing, adding an initiator, and reacting to obtain a gel-like substance;
d) Freeze-drying the gel-like substance to obtain an aerogel-like substance;
e) And mixing the aerogel-like substance with water for re-swelling to obtain the temperature-sensitive NIPAM/SA hydrogel.
Preferably, the mass ratio of the sodium alginate to the N-isopropyl acrylamide in the step A) is 1:1; the mass fraction of the solute in the sodium alginate-N-isopropyl acrylamide solution is 15-20wt%. (preferably, step B) the cross-linking agent is (calcium chloride) calcium chloride and N, N' -methylenebisacrylamide; the added mass of the calcium chloride is 0.08-0.12 wt% of sodium alginate-N-isopropyl acrylamide solution; the adding mass of the N, N' -methylene bisacrylamide is 0.08-0.15 wt% of the sodium alginate-N-isopropyl acrylamide solution;
the pore-forming agent is polyethylene glycol;
the addition amount of the pore-forming agent is 1.2-1.8wt% of the sodium alginate-N-isopropyl acrylamide solution.
Preferably, the heating temperature in the step B) is 50-70 ℃; the heating time is 50-70 min.
Preferably, the freezing in step C) is freezing to room temperature; the initiation auxiliary agent is N, N, N' -tetramethyl ethylenediamine; the addition amount of the initiation auxiliary agent is 0.02-0.05 wt% of the reaction solution;
the oxygen scavenging is specifically N 2 Deoxidizing for 30-60 min;
the initiator is ammonium persulfate; the concentration of the ammonium persulfate is 10%; the addition amount of the initiator is 0.15-0.3wt% of the reaction solution;
the reaction specifically comprises the following steps: reacting at room temperature for 4-6 h.
Preferably, the freeze-drying in step D) is specifically: freeze drying at-50 to-80 ℃;
the temperature of the water in the step E) is 20-30 ℃.
The invention provides a temperature-sensitive NIPAM/SA hydrogel, which is prepared by the preparation method according to any one of the technical schemes.
The invention provides a essence and spice slow-release system which comprises hydrogel and essence and spice.
The invention provides a preparation method of an essence and spice slow-release system, which comprises the following steps:
the aerogel-like substance prepared by the preparation method according to any one of the technical schemes is re-swelled in water added with essence and spice, and the aerogel-like substance is obtained.
The invention provides a perfume sustained-release device, which comprises a device for bearing the perfume sustained-release system and a perfume sustained-release system arranged in the device.
Compared with the prior art, the invention provides a preparation method of temperature-sensitive NIPAM/SA hydrogel, which comprises the following steps: a) Adding water into sodium alginate and N-isopropyl acrylamide to dissolve to obtain sodium alginate-N-isopropyl acrylamide solution; b) Adding a cross-linking agent into a sodium alginate-N-isopropyl acrylamide solution, stirring and mixing the mixture with a pore-forming agent, and heating the mixture for reaction to obtain a reaction solution; c) Freezing the reaction liquid, adding an initiating auxiliary agent, stirring, deoxidizing, adding an initiator, and reacting to obtain a gel-like substance; d) Freeze-drying the gel-like substance to obtain an aerogel-like substance; e) And mixing the aerogel-like substance with water for re-swelling to obtain the temperature-sensitive NIPAM/SA hydrogel. Experimental results show that the deswelling rate prepared by the invention can reach (93.76+/-0.22)%. The prepared fragrance-carrying capsules have the same swelling eliminating rate, the release rate of the essence is more than 90% when heated at 60 ℃ for 10min, and the temperature control release of the water-based essence is realized.
Drawings
Fig. 1 is a schematic view of a cup-shaped container.
Detailed Description
The invention provides a temperature-sensitive NIPAM/SA hydrogel, a preparation method thereof and an essence and perfume slow-release system, and the technical parameters can be properly improved by the technicians in the field with reference to the content of the composition. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and they are intended to be within the scope of the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that the invention can be practiced and practiced with modification and alteration and combination of the methods and applications herein without departing from the spirit and scope of the invention.
In the present application, the term "and/or" describes an association relationship of an association object, which means that three relationships may exist, for example, a and/or B may mean that a exists alone, a and B exist together, and B exists alone. Wherein A, B may be singular or plural.
In the present application, "at least one" means one or more, and "a plurality" means two or more. "at least one of" or the like means any combination of these items, including any combination of single item(s) or plural items(s).
It should be understood that, in various embodiments of the present application, the sequence number of each process does not mean that the sequence of execution is sequential, and some or all of the steps may be executed in parallel or sequentially, where the execution sequence of each process should be determined by its functions and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
The invention provides a preparation method of temperature-sensitive NIPAM/SA hydrogel, which comprises the following steps:
a) Adding water into sodium alginate and N-isopropyl acrylamide to dissolve to obtain sodium alginate-N-isopropyl acrylamide solution;
b) Adding a cross-linking agent into a sodium alginate-N-isopropyl acrylamide solution, stirring and mixing the mixture with a pore-forming agent, and heating the mixture for reaction to obtain a reaction solution;
c) Freezing the reaction liquid, adding an initiating auxiliary agent, stirring, deoxidizing, adding an initiator, and reacting to obtain a gel-like substance;
d) Freeze-drying the gel-like substance to obtain an aerogel-like substance;
e) And mixing the aerogel-like substance with water for re-swelling to obtain the temperature-sensitive NIPAM/SA hydrogel.
The preparation method of the temperature-sensitive NIPAM/SA hydrogel comprises the steps of firstly adding water into sodium alginate and N-isopropyl acrylamide to dissolve the sodium alginate and the N-isopropyl acrylamide to obtain sodium alginate-N-isopropyl acrylamide solution.
Wherein the water is preferably ultrapure water, and the water is commercially available.
The invention takes ultrapure water as a solvent, and adds the reaction raw materials Sodium Alginate (SA) and N-isopropyl acrylamide (NIPAM), and the materials are stirred and mixed.
In some embodiments, the mass ratio of sodium alginate to N-isopropylacrylamide is 1:1;
in some embodiments, the total mass fraction of solute in the sodium alginate-N-isopropylacrylamide solution is 15-20 wt%.
Adding a cross-linking agent into the sodium alginate-N-isopropyl acrylamide solution, stirring and mixing the mixture with a pore-forming agent, and heating the mixture for reaction to obtain a reaction solution.
The cross-linking agent is calcium chloride and N, N' -methylene bisacrylamide;
wherein the addition mass of the calcium chloride is 0.08-0.12 wt% of sodium alginate-N-isopropyl acrylamide solution; preferably 0.7 to 0.2wt%.
In some embodiments, the added mass of the N, N' -methylene bisacrylamide is 0.08-0.15 wt% of the sodium alginate-N-isopropyl acrylamide solution.
Preferably, the addition mass of the N, N' -methylene bisacrylamide is 0.09-0.14 wt% of the sodium alginate-N-isopropyl acrylamide solution.
The reaction liquid is heated by a magnetic stirring water bath kettle. Wherein the heating temperature is 50-70 ℃; the heating time is 50-70 min.
The pore-forming agent is polyethylene glycol;
in some embodiments, the porogen is added in an amount of 1.2 to 1.8 weight percent of the sodium alginate-N-isopropylacrylamide solution.
The reaction solution was frozen and an initiator aid was added.
After the reaction is finished, freezing to room temperature, adding an initiating auxiliary agent N, N, N 'N' -tetramethyl ethylenediamine (TEMED), controlling the mass fraction to be 0.02-0.05 wt%,
the room temperature of the invention can be 20-35 ℃.
And adding an initiating aid, stirring, deoxidizing, adding an initiator, and reacting to obtain a gel substance.
The deoxidization of the invention is specifically N 2 Deoxidizing for 30-60 min.
The initiator is ammonium persulfate; the mass concentration of the ammonium persulfate is 10%; the addition amount of the initiator is 0.15-0.3 wt% of the reaction solution.
According to the invention, the reaction is specifically: reacting at room temperature for 4-6 h.
Freeze-drying the gel-like substance to obtain aerogel-like substance.
In some embodiments, the freeze-drying is specifically: freeze drying at-50 to-80 deg.c for 1-2 hr;
and mixing the aerogel-like substance with water for re-swelling to obtain the temperature-sensitive NIPAM/SA hydrogel.
Adding aerogel-like substances into deionized water at 20-30 ℃ for re-swelling to obtain hydrogel, taking out the hydrogel at certain intervals to dry the water, and thus forming a hydrogel slow-release system.
The invention provides a temperature-sensitive NIPAM/SA hydrogel, which is prepared by the preparation method according to any one of the technical schemes.
The preparation method of the temperature-sensitive NIPAM/SA hydrogel has been clearly described, and is not repeated here.
The invention provides a essence and spice slow-release system which comprises hydrogel and essence and spice.
The essence perfume of the present invention is a perfume known to those skilled in the art, and is not limited herein, and includes, but is not limited to, blueberry, orange, red date or Shennong essence.
The invention provides a preparation method of an essence and spice slow-release system, which comprises the following steps:
the aerogel-like substance prepared by the preparation method according to any one of the technical schemes is re-swelled in water added with essence and spice, and the aerogel-like substance is obtained.
The prepared aerogel-like substance is added into deionized water with the temperature of 20-30 ℃ to be re-swelled into hydrogel, and the hydrogel is taken out to be wiped with water at certain intervals, so that a hydrogel slow-release system can be formed. In the process, water-soluble essence and spice can be added into deionized water to form an essence and spice hydrogel slow-release system.
The invention provides a perfume sustained-release device, which comprises a device for bearing the perfume sustained-release system and a perfume sustained-release system arranged in the device.
In one embodiment, it may be added to the apparatus of FIG. 1. Fig. 1 is a schematic view of a cup-shaped container. For patent publication (grant) No.: CN 217593423U.
The hydrogel slow-release system formed by the invention can be put into containers with various shapes which are made of polypropylene materials by injection molding, and can play a role in slow-release of essence and perfume. The hydrogel and polypropylene containers are used in a variety of situations by adjusting the dimensions of the hydrogel and polypropylene containers.
The invention provides a preparation method of temperature-sensitive NIPAM/SA hydrogel, which comprises the following steps: a) Adding water into sodium alginate and N-isopropyl acrylamide to dissolve to obtain sodium alginate-N-isopropyl acrylamide solution; b) Adding a cross-linking agent into a sodium alginate-N-isopropyl acrylamide solution, stirring and mixing the mixture with a pore-forming agent, and heating the mixture for reaction to obtain a reaction solution; c) Freezing the reaction liquid, adding an initiating auxiliary agent, stirring, deoxidizing, adding an initiator, and reacting to obtain a gel-like substance; d) Freeze-drying the gel-like substance to obtain an aerogel-like substance; e) And mixing the aerogel-like substance with water for re-swelling to obtain the temperature-sensitive NIPAM/SA hydrogel. Experimental results show that the deswelling rate prepared by the invention can reach (93.76+/-0.22)%. The prepared fragrance-carrying capsules have the same swelling eliminating rate, the release rate of the essence is more than 90% when heated at 60 ℃ for 10min, and the temperature control release of the water-based essence is realized.
In order to further illustrate the invention, the following is a detailed description of the temperature-sensitive NIPAM/SA hydrogel, the preparation method thereof and the essence and perfume slow release system provided by the invention by combining the examples.
Example 1
1. Sodium Alginate (SA) and N-isopropyl acrylamide (NIPAM) are used as reaction raw materials, calcium chloride N, N '-Methylene Bisacrylamide (MBA) is used as a cross-linking agent, ammonium Persulfate (APS) is used as an initiator, N, N, N' -tetramethyl ethylenediamine (TEMED) is used as an initiator auxiliary agent, polyethylene glycol (PEG) is used as a pore-forming agent, and a freeze-drying-re-swelling auxiliary soap-free emulsion polymerization method is used for preparing the temperature-sensitive NIPAM/SA hydrogel.
2. 1000ml of ultrapure water is taken, 120g of Sodium Alginate (SA) and 120g of N-isopropyl acrylamide (NIPAM) serving as reaction raw materials are added in equal proportion, and the mixture is stirred and mixed for 20min by magnetic force until the mixture is uniform.
3. And then adding 1.3g of cross-linking agent calcium chloride (CaCL 2) and 1.3g of N, N' -Methylene Bisacrylamide (MBA) into the step 2, and magnetically stirring and mixing 17g of pore-forming agent polyethylene glycol (PEG) until the mixture is uniform.
4. And (3) heating the mixture obtained in the step (3) by using a magnetic stirring water bath kettle. Wherein the heating temperature is controlled at 50deg.C, and the heating time is controlled at 50min.
5. After the reaction in the step 4 is completed, freezing to room temperature, adding 0.5ml of initiating additive N, N, N 'N' -tetramethyl ethylenediamine (TEMED), stirring uniformly, and deoxidizing by N2 for 30min.
6. Then, 20ml of 10% APS of an initiator is added into the step 5 to react at room temperature, and after 4 hours, the generated gel substance is cleaned for standby.
7. And (3) freeze-drying the gel-like substance generated in the step (6), controlling the temperature at-50 ℃ and the time at 1h to form an aerogel-like substance.
8. And (3) adding the aerogel-like substance formed in the step (7) into deionized water at 20 ℃ for re-swelling to obtain hydrogel, taking out the hydrogel at certain intervals, and wiping off the water to obtain the hydrogel slow-release system. In the process, water-soluble essence and spice such as blueberry, sweet orange, red date essence and Shennong essence can be added into deionized water with the addition amount of 0.5%, so that the essence and spice hydrogel slow-release system can be formed.
9. The hydrogel slow-release system formed in the step 8 is put into containers with various shapes which are made of polypropylene materials through injection molding, so that the essence and spice slow-release effect can be achieved. The hydrogel and polypropylene containers are used in a variety of situations by adjusting the dimensions of the hydrogel and polypropylene containers.
Example 2
1. Sodium Alginate (SA) and N-isopropyl acrylamide (NIPAM) are used as reaction raw materials, calcium chloride N, N '-Methylene Bisacrylamide (MBA) is used as a cross-linking agent, ammonium Persulfate (APS) is used as an initiator, N, N, N' -tetramethyl ethylenediamine (TEMED) is used as an initiator auxiliary agent, polyethylene glycol (PEG) is used as a pore-forming agent, and a freeze-drying-re-swelling auxiliary soap-free emulsion polymerization method is used for preparing the temperature-sensitive NIPAM/SA hydrogel.
2. 1000ml of ultrapure water is taken, 90g of Sodium Alginate (SA) and 90g of N-isopropyl acrylamide (NIPAM) serving as reaction raw materials are added in equal proportion, and the mixture is stirred and mixed for 40min by magnetic force until the mixture is uniform.
3. And then adding 1.0g of cross-linking agent calcium chloride (CaCL 2) and 1.0g of N, N' -Methylene Bisacrylamide (MBA) into the step 2, and magnetically stirring and mixing 15g of pore-forming agent polyethylene glycol (PEG) until the mixture is uniform.
4. And (3) heating the mixture obtained in the step (3) by using a magnetic stirring water bath kettle. Wherein the heating temperature is controlled at 70 ℃, and the heating time is controlled at 70min.
5. After the reaction in the step 4 is completed, freezing to room temperature, adding 0.7ml of initiating additive N, N, N 'N' -tetramethyl ethylenediamine (TEMED), stirring uniformly, and deoxidizing for 60min by N2.
6. Then, 23ml of 10% APS of an initiator is added into the step 5 to react at room temperature, and after 6 hours, the generated gel substance is cleaned for standby.
7. And (3) freeze-drying the gel-like substance generated in the step (6), controlling the temperature to minus 80 ℃ and the time to 2 hours, so as to form aerogel-like substance.
8. And (3) adding the aerogel-like substance formed in the step (7) into deionized water at 25 ℃ for re-swelling to obtain hydrogel, taking out the hydrogel at certain intervals, and wiping off the water to obtain the hydrogel slow-release system. In the process, water-soluble essence and spice (blueberry, sweet orange, red date essence and Shennong essence) can be added into deionized water with the addition amount of 0.5 percent, so that the essence and spice hydrogel slow-release system can be formed.
9. The hydrogel slow-release system formed in the step 8 is put into containers with various shapes which are made of polypropylene materials through injection molding, so that the essence and spice slow-release effect can be achieved. The hydrogel and polypropylene containers are used in a variety of situations by adjusting the dimensions of the hydrogel and polypropylene containers.
Example 3
1. Sodium Alginate (SA) and N-isopropyl acrylamide (NIPAM) are used as reaction raw materials, calcium chloride N, N '-Methylene Bisacrylamide (MBA) is used as a cross-linking agent, ammonium Persulfate (APS) is used as an initiator, N, N, N' -tetramethyl ethylenediamine (TEMED) is used as an initiator auxiliary agent, polyethylene glycol (PEG) is used as a pore-forming agent, and a freeze-drying-re-swelling auxiliary soap-free emulsion polymerization method is used for preparing the temperature-sensitive NIPAM/SA hydrogel.
2. 1000ml of ultrapure water is taken, 100g of Sodium Alginate (SA) and 100g of N-isopropyl acrylamide (NIPAM) serving as reaction raw materials are added in equal proportion, and the mixture is stirred and mixed for 30min by magnetic force until the mixture is uniform.
3. And then adding 1.3g of cross-linking agent calcium chloride (CaCL 2) and 1.3g of N, N' -Methylene Bisacrylamide (MBA) into the step 2, and magnetically stirring and mixing 16g of pore-forming agent polyethylene glycol (PEG) for 30min until the mixture is uniform.
4. And (3) heating the mixture obtained in the step (3) by using a magnetic stirring water bath kettle. Wherein the heating temperature is controlled at 60 ℃, and the heating time is controlled at 60min.
5. After the reaction in the step 4 is completed, freezing to room temperature, adding 0.7ml of initiating additive N, N, N 'N' -tetramethyl ethylenediamine (TEMED), stirring uniformly, and deoxidizing by N2 for 40min.
6. Then 30ml of 10% APS of initiator is added into the step 5, the mixture is reacted at room temperature for 4.5 hours, and the formed gel substance is cleaned for standby.
7. And (3) freeze-drying the gel substance generated in the step (6), controlling the temperature at-60 ℃ and the time at 1.5h to form aerogel-like substances.
8. And (3) adding the aerogel-like substance formed in the step (7) into deionized water at 30 ℃ for re-swelling to obtain hydrogel, taking out the hydrogel at certain intervals, and wiping off the water to obtain the hydrogel slow-release system. In the process, water-soluble essence and spice (blueberry, sweet orange, red date essence and Shennong chrysanthemum essence with the addition amount of 0.5%) can be added into deionized water to form an essence and spice hydrogel slow-release system.
9. The hydrogel slow-release system formed in the step 8 is put into containers with various shapes which are made of polypropylene materials through injection molding, so that the essence and spice slow-release effect can be achieved. The hydrogel and polypropylene containers are used in a variety of situations by adjusting the dimensions of the hydrogel and polypropylene containers.
Example 4
1. Sodium Alginate (SA) and N-isopropyl acrylamide (NIPAM) are used as reaction raw materials, calcium chloride N, N '-Methylene Bisacrylamide (MBA) is used as a cross-linking agent, ammonium Persulfate (APS) is used as an initiator, N, N, N' -tetramethyl ethylenediamine (TEMED) is used as an initiator auxiliary agent, polyethylene glycol (PEG) is used as a pore-forming agent, and a freeze-drying-re-swelling auxiliary soap-free emulsion polymerization method is used for preparing the temperature-sensitive NIPAM/SA hydrogel.
2. 1000ml of ultrapure water is taken, 105g of Sodium Alginate (SA) and N-isopropyl acrylamide (NIPAM) serving as reaction raw materials are added in equal proportion, and the mixture is stirred and mixed for 35min by magnetic force until uniform.
3. And then adding 1.2g of cross-linking agent calcium chloride (CaCL 2) and 1.2g of N, N' -Methylene Bisacrylamide (MBA) into the step 2, and magnetically stirring and mixing 14g of pore-forming agent polyethylene glycol (PEG) for 30min until the mixture is uniform.
4. And (3) heating the mixture obtained in the step (3) by using a magnetic stirring water bath kettle. Wherein the heating temperature is controlled at 65 ℃ and the heating time is controlled at 60min.
5. After the reaction in the step 4 is completed, freezing to room temperature, adding 0.65ml of initiating additive N, N, N 'N' -tetramethyl ethylenediamine (TEMED), stirring uniformly, and deoxidizing by N2 for 50min.
6. Then, 28ml of 10% APS of an initiator is added into the step 5, the mixture is reacted at room temperature for 5.5 hours, and the formed gel substance is cleaned for later use.
7. And (3) freeze-drying the gel-like substance generated in the step (6), controlling the temperature at-70 ℃ and the time at 1h to form an aerogel-like substance.
8. And (3) adding the aerogel-like substance formed in the step (7) into deionized water at 25 ℃ for re-swelling to obtain hydrogel, taking out the hydrogel at certain intervals, and wiping off the water to obtain the hydrogel slow-release system. In the process, water-soluble essence and spice (blueberry, sweet orange, red date essence and Shennong chrysanthemum essence with the addition amount of 0.5%) can be added into deionized water to form an essence and spice hydrogel slow-release system.
9. The hydrogel slow-release system formed in the step 8 is put into containers with various shapes which are made of polypropylene materials through injection molding, so that the essence and spice slow-release effect can be achieved. The hydrogel and polypropylene containers are used in a variety of situations by adjusting the dimensions of the hydrogel and polypropylene containers.
The implementation effect is as follows:
the results of the examples under four different conditions show that the deswelling rate of the example 1 can reach 81.43%, the deswelling rate of the example 2 can reach 90.82%, the deswelling rate of the example 3 can reach 91.71% and the deswelling rate of the gel material obtained in the example 4 can reach 93.76%. The 4 kinds of fragrance-carrying capsules prepared by the invention have the same swelling eliminating rate, the release rate of the fragrance is more than 90% when heated for 10min at 60 ℃, and the temperature control release of the water-based fragrance is realized.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (10)

1. The preparation method of the temperature-sensitive NIPAM/SA hydrogel is characterized by comprising the following steps of:
a) Adding water into sodium alginate and N-isopropyl acrylamide to dissolve to obtain sodium alginate-N-isopropyl acrylamide solution;
b) Adding a cross-linking agent into a sodium alginate-N-isopropyl acrylamide solution, stirring and mixing the mixture with a pore-forming agent, and heating the mixture for reaction to obtain a reaction solution;
c) Freezing the reaction liquid, adding an initiating auxiliary agent, stirring, deoxidizing, adding an initiator, and reacting to obtain a gel-like substance;
d) Freeze-drying the gel-like substance to obtain an aerogel-like substance;
e) And mixing the aerogel-like substance with water for re-swelling to obtain the temperature-sensitive NIPAM/SA hydrogel.
2. The preparation method according to claim 1, wherein the mass ratio of sodium alginate to N-isopropyl acrylamide in the step A) is 1:1; the total mass fraction of the solute in the sodium alginate-N-isopropyl acrylamide solution is 15-20wt%.
3. The method of claim 1, wherein the cross-linking agent of step B) is calcium chloride and N, N' -methylenebisacrylamide; the added mass of the calcium chloride is 0.08-0.12 wt% of sodium alginate-N-isopropyl acrylamide solution; the adding mass of the N, N' -methylene bisacrylamide is 0.08-0.15 wt% of the sodium alginate-N-isopropyl acrylamide solution;
the pore-forming agent is polyethylene glycol;
the addition amount of the pore-forming agent is 1.2-1.8wt% of the sodium alginate-N-isopropyl acrylamide solution.
4. The method of claim 1, wherein the heating temperature in step B) is 50-70 ℃; the heating time is 50-70 min.
5. The method of claim 1, wherein the freezing in step C) is to room temperature; the initiation auxiliary agent is N, N, N' -tetramethyl ethylenediamine; the addition amount of the initiation auxiliary agent is 0.02-0.05 wt% of the reaction solution;
the oxygen scavenging is specifically N 2 Deoxidizing for 30-60 min;
the initiator is ammonium persulfate; the concentration of the ammonium persulfate is 10%; the addition amount of the initiator is 0.15-0.3wt% of the reaction solution;
the reaction specifically comprises the following steps: reacting at room temperature for 4-6 h.
6. The method according to claim 1, wherein the freeze-drying of step D) is specifically: freeze drying at-50 to-80 ℃;
the temperature of the water in the step E) is 20-30 ℃.
7. A temperature-sensitive NIPAM/SA hydrogel prepared by the method of any one of claims 1-6.
8. A fragrance and flavor slow release system comprising the hydrogel of claim 7 and a fragrance and flavor.
9. A method for preparing a perfume sustained-release system, which is characterized by comprising the following steps:
the aerogel-like material prepared by the method according to any one of claims 1 to 6 is obtained by re-swelling in water added with essence and perfume.
10. A fragrance and flavor slow release device, which is characterized by comprising a device for bearing the fragrance and flavor slow release system as claimed in claim 8 and a fragrance and flavor slow release system arranged in the device.
CN202311440713.5A 2023-10-31 2023-10-31 Temperature-sensitive NIPAM/SA hydrogel, preparation method thereof and essence and perfume slow-release system Pending CN117467079A (en)

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