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 PDFInfo
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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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- sodium alginate
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 74
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002304 perfume Substances 0.000 title claims description 15
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 52
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 52
- 239000000661 sodium alginate Substances 0.000 claims abstract description 52
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 52
- 239000000126 substance Substances 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 32
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 27
- 239000011734 sodium Substances 0.000 claims abstract description 27
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 27
- 239000003999 initiator Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000004108 freeze drying Methods 0.000 claims abstract description 17
- 230000000977 initiatory effect Effects 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 238000007710 freezing Methods 0.000 claims abstract description 14
- 230000008014 freezing Effects 0.000 claims abstract description 14
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000002202 Polyethylene glycol Substances 0.000 claims description 19
- 229920001223 polyethylene glycol Polymers 0.000 claims description 19
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 15
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 15
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 15
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 11
- 239000003205 fragrance Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 238000013268 sustained release Methods 0.000 claims description 8
- 239000012730 sustained-release form Substances 0.000 claims description 8
- 239000000796 flavoring agent Substances 0.000 claims description 7
- 235000019634 flavors Nutrition 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 230000002000 scavenging effect Effects 0.000 claims description 2
- 230000008961 swelling Effects 0.000 abstract description 5
- 239000002775 capsule Substances 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 28
- 235000013599 spices Nutrition 0.000 description 24
- 239000004743 Polypropylene Substances 0.000 description 15
- -1 polypropylene Polymers 0.000 description 15
- 229920001155 polypropylene Polymers 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 239000002994 raw material Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 239000000499 gel Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 229910021642 ultra pure water Inorganic materials 0.000 description 6
- 239000012498 ultrapure water Substances 0.000 description 6
- 240000000851 Vaccinium corymbosum Species 0.000 description 5
- 235000003095 Vaccinium corymbosum Nutrition 0.000 description 5
- 235000017537 Vaccinium myrtillus Nutrition 0.000 description 5
- 235000021014 blueberries Nutrition 0.000 description 5
- 238000001746 injection moulding Methods 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 235000005976 Citrus sinensis Nutrition 0.000 description 4
- 240000002319 Citrus sinensis Species 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 238000010556 emulsion polymerization method Methods 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 235000007516 Chrysanthemum Nutrition 0.000 description 2
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 2
- 238000013270 controlled release Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 238000013267 controlled drug release Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000003361 porogen Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised 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
- C08J2351/02—Characterised 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Cosmetics (AREA)
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
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.
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