CN111393563B - Preparation method and monitoring die of temperature-sensitive hydrogel - Google Patents
Preparation method and monitoring die of temperature-sensitive hydrogel Download PDFInfo
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- CN111393563B CN111393563B CN201910002080.7A CN201910002080A CN111393563B CN 111393563 B CN111393563 B CN 111393563B CN 201910002080 A CN201910002080 A CN 201910002080A CN 111393563 B CN111393563 B CN 111393563B
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- 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
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to a preparation method of a temperature-sensitive hydrogel with volume rapidly eliminating swelling at low temperature, which comprises the following steps: placing the hydrogel prepolymerization solution in a preparation mold for polymerization for 2-24 hours; the components of the hydrogel pre-polymerization liquid comprise: the catalyst comprises 8-14% of comonomer, 0.09-0.36% of cross-linking agent, 0.02-0.07% of initiator, 0.01% of catalyst and the balance of deionized water. The method is simple, the cost is low, the diameter of the prepared hydrogel is 2.1cm at the temperature of 2-4 ℃, when the temperature is increased from 8 ℃ to 10 ℃, the gel rapidly swells, the diameter is reduced, and the volume is obviously changed along with the temperature change. The invention also discloses a detection mould matched with the hydrogel, and the temperature-sensitive hydrogel is placed in a specific mould, so that the temperature-sensitive hydrogel can be used for visual monitoring of temperature change in the vaccine storage and refrigeration transportation processes, and the monitoring mode has irreversibility.
Description
Technical Field
The invention relates to the technical field of hydrogel, in particular to a preparation method and a monitoring die of temperature-sensitive hydrogel.
Background
The quality of the vaccine depends not only on the production process but also on the transportation condition and the storage condition, the transportation and the storage condition of common vaccines such as hepatitis B vaccine, anthrax vaccine, leprosy vaccine and the like are 2-8 ℃, and when the temperature exceeds the threshold value, the vaccine has the risk of losing efficacy. After the inactivated vaccine caused by temperature is injected, the vaccine cannot achieve the due effect on the prevention of diseases and even endangers the health of human bodies or animals, so the method has important significance on the temperature monitoring of the transportation or storage of the vaccine.
Temperature-sensitive hydrogels are a special class of intelligent hydrogels, which can be called Temperature-sensitive gels, and these gels undergo a volume phase transition at a specific Temperature, which is called the Lower Critical Solution Temperature (LCST). The gel monomer comprises a hydrophilic group and a hydrophobic group, when the environmental temperature is lower than LCST, the hydrophilic group and water molecules form a large number of hydrogen bonds, and the multi-component system absorbs water and expands; when the ambient temperature is higher than the LCST, the hydrophobic group now dominates, the system loses water and causes volume shrinkage.
Chinese patent CN103408693A discloses a preparation method of temperature-sensitive hydrogel with adjustable response temperature, and the temperature-sensitive gel prepared by the patent has obvious light transmittance change in a higher temperature range of 25-90 ℃, and can be used as temperature-sensitive gel with temperature response.
At present, the research on low-temperature response gel is less, so that the design of a gel with low-temperature response, which is simple and convenient to operate, is of great significance based on the requirement of monitoring the vaccine transportation or storage temperature.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of temperature-sensitive hydrogel for vaccine storage and refrigerated transport monitoring, which comprises the steps of placing hydrogel prepolymerization liquid in a spherical mold for polymerization for 2-24 hours; the components of the hydrogel pre-polymerization liquid comprise: the catalyst comprises a comonomer, a cross-linking agent, an initiator, a catalyst and deionized water, wherein the mass fraction of the comonomer is 8-14%, the mass fraction of the cross-linking agent is 0.09-0.36%, the mass fraction of the initiator is 0.02-0.07%, the mass fraction of the catalyst is 0.01%, and the balance is the deionized water;
further, the preparation method of the temperature-sensitive hydrogel also comprises the following steps: taking the prepared hydrogel out of the preparation mold, placing the hydrogel in a 50ml beaker to fully swell at the temperature of 2-4 ℃, and then transferring the hydrogel to a monitoring mold filled with deionized water;
further, the hydrogel pre-polymerization solution was placed in the preparation mold at 60 ℃ for polymerization.
Further, the comonomer is N-tert-butyl acrylamide, N-isopropyl acrylamide and acrylamide;
further, the cross-linking agent is N, N' -methylene bisacrylamide, and the initiator is ammonium persulfate;
further, the catalyst is N, N, N, N' -tetramethyl ethylenediamine;
furthermore, the preparation mould is made of latex, the interior of the preparation mould is hollow and spherical, and the diameter of the sphere is 1-1.4cm.
The utility model provides a monitoring mould, the monitoring mould is the shape of falling the calabash, the shape of falling the calabash includes upper bottleneck, upper cavity, lower floor's cavity, the window between upper cavity and the lower floor's cavity.
Furthermore, the diameter of the upper layer bottle mouth is 2.0-2.5cm, the diameter of the upper layer cavity is 2.1-2.8cm, the diameter range of the window is 1.4-1.8cm, and the diameter of the lower layer cavity 4 is 2.0-2.5cm.
Furthermore, when the monitoring mold is placed at the temperature of 2-8 ℃ to be monitored, the hydrogel is positioned in the upper cavity of the mold, and when the temperature is higher than 8 ℃, the hydrogel dissipates swelling and contracts and sinks to the lower cavity of the detection mold.
The preparation method of the temperature-sensitive hydrogel provided by the embodiment of the invention is simple, the raw material source is easy to obtain, the cost is low, the method is suitable for batch production, and meanwhile, the temperature-sensitive hydrogel obtained by the invention has quick response to a certain temperature. Meanwhile, the temperature-sensitive hydrogel can be used for temperature monitoring in vaccine storage and refrigeration transportation processes, has irreversibility and visualization, and has high application value.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a graph of the diameter versus temperature of hydrogels prepared in examples 1-3 of the present invention.
Fig. 2 is a schematic view of a monitoring die in an embodiment of the present invention.
FIG. 3 is a graph of hydrogel diameter versus temperature for the hydrogel prepared in example 1 of the present invention.
Fig. 4 is a schematic view of monitoring the dimensions of a mold in example 1 of the present invention.
FIG. 5 is an SEM photograph of a hydrogel prepared in example 1 of the present invention after it has been sufficiently swollen at 4 ℃ and then freeze-dried.
FIG. 6 is an SEM photograph of a hydrogel prepared in example 1 of the present invention after swelling at 4 ℃ and then swelling at 10 ℃ and freeze-drying.
FIG. 7 is an SEM image of a hydrogel prepared in example 1 of the present invention after swelling at 4 ℃ and then swelling at 20 ℃ and freeze-drying.
FIG. 8 is a graph of hydrogel diameter versus temperature for the hydrogel prepared in example 2 of the present invention.
Fig. 9 is a schematic view of monitoring the dimensions of a mold in example 2 of the present invention.
FIG. 10 is an SEM photograph of a freeze-dried hydrogel prepared in example 2 of the present invention after it has been sufficiently swelled at 4 ℃.
FIG. 11 is a graph of hydrogel diameter versus temperature for example 3 of the present invention.
FIG. 12 is a schematic view of monitoring the dimensions of a mold in example 3 of the present invention.
FIG. 13 is an SEM photograph of a freeze-dried hydrogel fully swollen at 4 ℃ prepared in example 3 of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
Example 1
Adding 0.667g of N-tert-butyl acrylamide, 0.204g of N-isopropyl acrylamide, 0.199g of acrylamide, 0.036g of N, N ' -methylene bisacrylamide, 0.01g of ammonium persulfate and 10 mu L of N, N, N ', N ' -tetramethyl ethylenediamine into 10ml of deionized water, and fully and uniformly stirring to obtain a transparent hydrogel pre-polymerization liquid; transferring the hydrogel prepolymerization solution to a spherical mold with the diameter of 1.3cm, and reacting at 60 ℃ for 12 hours to obtain spherical temperature-sensitive hydrogel with the diameter of 1.3 cm; taking out the hydrogel pellet, placing the hydrogel pellet in a beaker filled with deionized water, and fully swelling the hydrogel pellet in an environment of 4 ℃ to obtain swollen gel with the diameter of 2.1 cm; spherical gel with the diameter of 2.1cm is transferred into a monitoring mold (shown in figure 2) filled with deionized water, the hydrogel ball is positioned on the upper layer of the mold, when the temperature is increased from 8 ℃ to 10 ℃, the diameter of the hydrogel ball can change obviously and is reduced from 2.05cm to 1.7cm, at the moment, the reduced hydrogel drops from the upper layer of the container to the lower layer of the container, and the temperature change can be monitored by observing the position of the hydrogel ball in the container. It can be seen that the response temperature of the hydrogel in this example is 8.0 ℃. As the temperature continues to increase, the hydrogel diameter continues to decrease, and the change in diameter of the spherical hydrogel with temperature is shown in FIG. 3. The hydrogel swelled at 4 deg.C is freeze-dried to form a three-dimensional porous structure, the scanning electron microscope image of the microstructure is shown in FIG. 5, the aperture of the hydrogel after freeze-drying at 10 deg.C is smaller than that of the hydrogel at 4 deg.C, the scanning electron microscope image of the microstructure is shown in FIG. 6, the aperture of the hydrogel after freeze-drying at 20 deg.C is not observed at 2000 times of 10 deg.C, and the scanning electron microscope image of the microstructure of the hydrogel at 20 deg.C is shown in FIG. 7.
Example 2
Adding 0.635g of N-tert-butylacrylamide, 0.17g of N-isopropylacrylamide, 0.156g of acrylamide, 0.018g of N, N ' -methylenebisacrylamide, 0.005g of ammonium persulfate and 10 mu L of N, N, N ', N ' -tetramethylethylenediamine into 10ml of water to obtain a transparent hydrogel pre-polymerization liquid; transferring the hydrogel prepolymerization solution to a spherical mold with the diameter of 1.3cm, reacting at 60 ℃ for 24 hours to obtain spherical temperature-sensitive hydrogel with the diameter of 1.3cm, taking out hydrogel pellets, placing the hydrogel pellets in a beaker containing deionized water, and fully swelling in an environment of 4 ℃ to obtain swollen gel with the diameter of 2.1 cm; the hydrogel is transferred to a monitoring mold filled with deionized water, as shown in fig. 9, a hydrogel ball is positioned on the upper layer of the mold, when the temperature is increased from 8 ℃ to 10 ℃, the diameter of the hydrogel ball is obviously changed, and is reduced from 1.9cm to 1.5cm, at the moment, the reduced hydrogel drops from the upper layer of the container to the lower layer of the container, the temperature change can be monitored by observing the position of the hydrogel ball in the container, when the temperature is continuously increased, the diameter of the hydrogel can be continuously reduced, the diameter of the spherical hydrogel is changed along with the temperature as shown in fig. 8, the swollen hydrogel is in a three-dimensional porous structure after being freeze-dried, and a scanning electron microscope image of the microstructure of the swollen hydrogel is shown in fig. 10.
Example 3
To 10ml of water were added 0.669g of N-t-butylacrylamide, 0.237g of N-isopropylacrylamide, 0.241g of acrylamide, 0.024g of N, N ' -methylenebisacrylamide, 0.01g of ammonium persulfate, and 10. Mu.L of N, N, N ', N ' -tetramethylethylenediamine to obtain a transparent hydrogel prepolymerization solution; transferring the hydrogel prepolymerization solution to a spherical mold with the diameter of 1.3cm, reacting at 60 ℃ for 12 hours to obtain spherical temperature-sensitive hydrogel with the diameter of 1.3cm, taking out hydrogel pellets, placing the hydrogel pellets in a beaker containing deionized water, and fully swelling in an environment of 4 ℃ to obtain swollen gel with the diameter of 2.1 cm; the hydrogel is transferred to a monitoring mold filled with deionized water, as shown in fig. 12, a hydrogel ball is positioned on the upper layer of the mold, when the temperature is increased from 8 ℃ to 10 ℃, the diameter of the hydrogel ball is obviously changed, and is reduced from 1.55cm to 1.2cm, at the moment, the reduced hydrogel drops from the upper layer of the container to the lower layer of the container, the temperature change can be monitored by observing the position of the hydrogel ball in the container, when the temperature is continuously increased, the diameter of the hydrogel can be continuously reduced, the diameter of the spherical hydrogel is changed along with the temperature as shown in fig. 11, the swollen hydrogel is in a three-dimensional porous structure after being freeze-dried, and a scanning electron microscope image of the microstructure of the swollen hydrogel is shown in fig. 13.
In some embodiments of the present invention, the monitoring mold is shown in fig. 2, and has an inverted gourd-shaped structure, which includes an upper bottle opening 4, an upper cavity 5, a lower cavity 7, and a window 6 between the upper cavity and the lower cavity. In some preferred embodiments of the invention, the diameter of the upper layer bottle mouth 4 is preferably 2.0-2.5cm, the diameter of the upper layer cavity 5 is preferably 2.1-2.8cm, the diameter range of the window is preferably 1.4-1.8cm, and the diameter of the lower layer cavity 7 is preferably 2.0-2.5cm. Therefore, when the swollen hydrogel is transferred to a monitoring mold filled with deionized water, the hydrogel ball is positioned in the upper cavity 4 of the mold, when the temperature is increased from 8 ℃ to 10 ℃, the diameter of the hydrogel can be obviously changed and reduced from a larger size to a smaller size, at the moment, the reduced hydrogel drops from the upper cavity 4 of the container to the lower cavity 7 of the container, and the temperature change can be monitored by observing the position of the hydrogel ball in the container.
In the description of the present specification, reference to the description of the terms "one embodiment", "some embodiments", "an illustrative embodiment", "an example", "a specific example", or "some examples", etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (7)
1. A monitoring mold is matched with a preparation method of temperature-sensitive hydrogel for use, and is characterized in that:
the monitoring mould is in an inverted gourd shape, and the inverted gourd shape comprises an upper-layer bottle mouth, an upper-layer cavity, a lower-layer cavity and a window between the upper-layer cavity and the lower-layer cavity;
the diameter of the upper layer bottle mouth is 2.0-2.5cm, the diameter of the upper layer cavity is 2.1-2.8cm, the diameter range of the window is 1.4-1.8cm, and the diameter of the lower layer cavity 4 is 2.0-2.5cm;
when the monitoring mold is placed at the temperature to be monitored, which is 2-8 ℃, the hydrogel is positioned in the upper cavity of the detection mold; when the monitoring mold is placed at the temperature to be monitored higher than 8 ℃, the hydrogel dissipates swelling and shrinks and sinks to the lower cavity of the monitoring mold;
the preparation method of the temperature-sensitive hydrogel comprises the following steps: placing the hydrogel prepolymerization solution in a preparation mold for polymerization for 2-24 hours; the components of the hydrogel pre-polymerization liquid comprise: the temperature-sensitive hydrogel is matched with the monitoring mold to be used for monitoring vaccine storage and refrigerated transport.
2. The monitoring mold according to claim 1, wherein the method for preparing the temperature sensitive hydrogel further comprises the steps of: and taking the prepared hydrogel out of the preparation mold, placing the hydrogel in a 50ml beaker to fully swell at the temperature of 2-4 ℃, and then transferring the hydrogel to a monitoring mold filled with deionized water.
3. The monitoring mold according to claim 1, wherein the temperature-sensitive hydrogel is prepared by polymerizing the hydrogel pre-polymerization solution in the preparation mold at 60 ℃.
4. A monitoring die as claimed in claim 1 wherein the comonomers are N-t-butylacrylamide, N-isopropylacrylamide and acrylamide.
5. The monitoring die of claim 1, wherein the crosslinking agent is N, N' -methylenebisacrylamide and the initiator is persulfuric acid.
6. The monitoring die of claim 1, wherein the catalyst is N, N' -tetramethylethylenediamine.
7. A monitoring die according to claim 1, wherein the preparation die is made of latex and has a hollow spherical shape with a diameter of 1-1.4cm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2363104A1 (en) * | 2001-03-13 | 2011-09-07 | Microvention, Inc. | Hydrogels that undergo volumetric expansion in response to changes in their environment and their methods of manufacture and use |
| CN103137013A (en) * | 2013-02-05 | 2013-06-05 | 南京天朗制药有限公司 | Temperature indication or multi-layer anti-fake indication tag based on shape memory polymers and temperature indication or multi-layer anti-fake indication method |
| CN103408693A (en) * | 2013-07-15 | 2013-11-27 | 东华大学 | Preparation method of response-temperature-adjustable temperature sensitive hydrogel |
| CN104845006A (en) * | 2015-05-11 | 2015-08-19 | 东华大学 | Magnetic acrylamide hydrogel and preparation method thereof |
| CN107101736A (en) * | 2017-06-08 | 2017-08-29 | 南京航空航天大学 | Temperature-detecting device |
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2019
- 2019-01-02 CN CN201910002080.7A patent/CN111393563B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2363104A1 (en) * | 2001-03-13 | 2011-09-07 | Microvention, Inc. | Hydrogels that undergo volumetric expansion in response to changes in their environment and their methods of manufacture and use |
| CN103137013A (en) * | 2013-02-05 | 2013-06-05 | 南京天朗制药有限公司 | Temperature indication or multi-layer anti-fake indication tag based on shape memory polymers and temperature indication or multi-layer anti-fake indication method |
| CN103408693A (en) * | 2013-07-15 | 2013-11-27 | 东华大学 | Preparation method of response-temperature-adjustable temperature sensitive hydrogel |
| CN104845006A (en) * | 2015-05-11 | 2015-08-19 | 东华大学 | Magnetic acrylamide hydrogel and preparation method thereof |
| CN107101736A (en) * | 2017-06-08 | 2017-08-29 | 南京航空航天大学 | Temperature-detecting device |
Non-Patent Citations (1)
| Title |
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| Stimuli sensitive copolymer poly(N-tert-butylacrylamide-ran-acrylamide): Synthesis and characterization;Save NS et al;《JOURNAL OF APPLIED POLYMER SCIENCE》;20050205;第95卷(第3期);第672-680页 * |
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