CN105758551A - Time-temperature indicating device - Google Patents
Time-temperature indicating device Download PDFInfo
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- CN105758551A CN105758551A CN201610104207.2A CN201610104207A CN105758551A CN 105758551 A CN105758551 A CN 105758551A CN 201610104207 A CN201610104207 A CN 201610104207A CN 105758551 A CN105758551 A CN 105758551A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
- G01K11/12—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance
- G01K11/16—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance of organic materials
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Abstract
The invention relates to a time-temperature indicating device comprising a base layer, an indicating layer and a sealing switch layer which are sequentially laminated. The indicating layer comprises discoloring region. The sealing switch layer comprises a phase change material and a carrier layer carrying the phase-change material. By using the phase-change material and the microporous carrier layer cooperatively as the sealing switch layer of the time-temperature indicating device, the device is simple in structure and can quite conveniently detect whether the temperature of a product is below the critical temperature. According to the color change of the discoloring region of the indicating layer, the time-temperature indicating device can predict the cumulative time during which the temperature of the product is lower than a certain temperature value, easily achieves monitoring of lower critical temperature, and thus determines whether the supercooling of the product fails.
Description
Technical field
The present invention relates to instruction equipment technical field, particularly relate to a kind of time-temperature instruction device.
Background technology
The perishable product needed such as food, beverage, blood, vaccine, meat food preserve under specified temp environment.Such as, vaccine product need to keep (such as 2 DEG C～8 DEG C) under cold chain specified temp environment.When vaccine storage temperature is higher than upper critical temperature (such as 8 DEG C) or during lower than lower critical temperature (such as 2 DEG C), vaccine activity, by rapid decrease, exceedes certain period of time even complete failure.After using rotten article, bringing infringement to human body, severe patient even results in death.Therefore, it is necessary to the upper critical of cold chain and lower critical temperature are monitored, it is determined that product is in the time of abnormal temperature, thus judging whether product lost efficacy.
But, traditional time-temperature instruction device is generally used for instruction product and exceedes the cumulative time of certain particular temperature value, but cannot indicate the product cumulative time lower than certain temperature value, namely cannot lower critical temperature be monitored.
Summary of the invention
Based on this, it is necessary to provide a kind of and may indicate that product indicates device lower than the time-temperature of the cumulative time of certain temperature value.
A kind of time-temperature instruction device, including the basal layer stacked gradually, marker and enclosed switch layer；
Described marker includes color change interval, and the material of described color change interval is color shifting ink；
Described enclosed switch layer includes phase-change material and carries the carrier layer of described phase-change material, and described carrier layer is provided with multiple micropore, and described micropore is through hole, and described phase-change material is arranged in described micropore.
In one embodiment, described phase-change material is at least one in fatty acid and fatty acid ester.
In one embodiment, the thickness of described carrier layer is 50 μm～2000 μm.
In one embodiment, the aperture of described micropore is 10nm～5000nm.
In one embodiment, described carrier layer is provided with multiple uniformly coherent micropore.
In one embodiment, described marker also includes reference zone, and the color of color change interval is thus judging the response time of described color change interval described in comparison for described reference zone, and described reference zone has at least one fixing color.
In one embodiment, described color shifting ink is volatile acid sensitive color change ink, volatile base sensitive color change ink, carbon dioxide sensitive color change ink or oxygen sensitive color shifting ink.
In one embodiment, described time-temperature instruction device also includes protective layer, and described protective layer is layered on the described color change interval of the described marker surface away from described basal layer.
In one embodiment, described time-temperature instruction device also includes the first adhesive-layer, described first adhesive-layer is layered in described enclosed switch layer on the surface of described marker, and described first adhesive-layer is in region place hollow out corresponding to the described color change interval of described marker.
In one embodiment, described time-temperature instruction device also includes the second adhesive-layer and the peel ply that stack gradually, described second adhesive-layer is layered on the described enclosed switch layer surface away from described marker, and described peel ply is layered on described second adhesive-layer surface away from described enclosed switch layer.
Above-mentioned time-temperature instruction device, including the basal layer stacked gradually, marker and enclosed switch layer.Marker includes color change interval, and the material of color change interval is color shifting ink.Enclosed switch layer includes phase-change material and the carrier layer of carrying phase-change material.Phase-change material has certain freezing point, and when temperature is higher than this freezing point, phase-change material is in a liquid state, and when temperature is lower than this freezing point, phase-change material is solid-state.Phase-change material is arranged in the carrier layer with micropore, when ambient temperature is higher than the freezing point of phase-change material, the phase-change material of liquid state is filled in the micropore of carrier layer, and now enclosed switch layer is closed, gas cannot pass through enclosed switch layer, and instruction device is in unactivated state.When ambient temperature is lower than phase-change material freezing point, phase-change material is become solid-state from liquid, in the process of solidification, adsorption because of hole wall, it is close on micro-pore wall, and phase-change material molecule is from ordered arrangement to lack of alignment, intermolecular gap diminishes, volume-diminished, there is mesopore in inside, the gas that escaping gas can be overflowed in color shifting ink or environment by mesopore can enter color shifting ink by mesopore so that chromic ink colors changes, and instruction device is active.Changed by the color of color change interval and can show that product is in the cumulative time lower than particular temperature value, it is achieved lower critical temperature is monitored, thus judging product whether supercooling failure.
Accompanying drawing explanation
Fig. 1 is the structural representation of the time-temperature instruction device of an embodiment；
Fig. 2 is the structural representation of ampoule bottle；
Fig. 3 is the structural representation being attached on ampoule bottle after peeling off by the peel ply of temperature indicating device between as shown in Figure 1；
Fig. 4 is the structural representation of the time-temperature instruction device of another embodiment；
Fig. 5 is the structural representation being attached on ampoule bottle after peeling off by the peel ply of temperature indicating device between as shown in Figure 4；
Fig. 6 is the structural representation of the time-temperature instruction device of a further embodiment；
Fig. 7 is the structural representation being attached on ampoule bottle after peeling off by the peel ply of temperature indicating device between as shown in Figure 6.
Detailed description of the invention
Understandable for enabling the above-mentioned purpose of the present invention, feature and advantage to become apparent from, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.Elaborate a lot of detail in the following description so that fully understanding the present invention.But the present invention can implement being much different from alternate manner described here, and those skilled in the art can do similar improvement when without prejudice to intension of the present invention, therefore the present invention is by the restriction of following public detailed description of the invention.
It should be noted that be referred to as " being fixed on " another element when element, it can directly on another element or can also there is element placed in the middle.When an element is considered as and another element " connection " or " connection " that it can be directly to another element or may be simultaneously present centering elements.Term as used herein " on ", D score, " vertical ", " level ", "left", "right" and similar statement for illustrative purposes only, being not offered as is unique embodiment.
Referring to Fig. 1, the time-temperature instruction device 10 of an embodiment, including the basal layer 100 stacked gradually, marker 200, protective layer the 300, first adhesive-layer 400, enclosed switch layer the 500, second adhesive-layer 600 and peel ply 700.
The material of basal layer 100 can be at least one in polyethylene terephthalate (PET), polrvinyl chloride (PVC), polyethylene (PE) and polypropylene (PP).Basal layer 100 is used for carrying and protect marker 200, has transparent and good bubble-tight feature, it will be appreciated that other has good transparency and bubble-tight material also can as the substrate layer of the present invention.
Marker 200 includes color change interval 201, and in active state, the material of color change interval 201 is increase the color shifting ink presenting different colours in time.Color intensity of variation according to color shifting ink, it is possible to whether instruction time-temperature instruction device 10 is activated, and the instruction device cumulative time under supercooling temperature.
In present embodiment, marker 200 also includes reference zone 202, and reference zone 202 is used for the color of comparison color change interval 201 thus judging the response time of color change interval 201.By arranging reference zone 202, convenient and observe timely color change interval 201 color change.Reference zone 202 has at least one fixing color.Reference zone 202 can be a kind of color, it is also possible to for multiple color.Can increase in time according to the color shifting ink that many experiments draws and present different colours and obtain the color of reference zone 202.It is appreciated that in other embodiments, it is also possible to do not indicate at time-temperature and device 10 arranges reference zone 202, now, by color change interval 201 and standard color comparison card comparison.
Concrete, color shifting ink can be volatile acid sensitive color change ink, volatile base sensitive color change ink, carbon dioxide sensitive color change ink or oxygen sensitive color shifting ink etc..Ink material can be printed on basal layer 100 easily.Should be appreciated that other can occur the ink of variable color all can as the color shifting ink of the present invention in non-hermetic environments.When the concentration of the volatile acid in ink, volatile base, carbon dioxide or oxygen changes, color shifting ink can occur color to change, and presents different colors.And the material of reference zone 202 can be common ink, color will be occurred to change along with the concentration change of volatile acid, volatile base, carbon dioxide or oxygen.Whether consistent with the color of reference zone 202 by comparing color change interval 201, can determine whether whether time-temperature instruction device 10 activates.Further, the amplitude according to color change, show that time-temperature instruction device 10 is in the cumulative time lower than particular temperature value, thus judging whether product goes bad.
In present embodiment, color shifting ink is volatile acid sensitive color change ink.Volatile acid sensitive color change ink includes volatile acid, binding agent, plasticizer, solvent and pH sensitive dyestuff.Volatile acid can be the carboxylic acid of 2～12 for carbon number, specifically includes acetic acid, propanoic acid, butanoic acid etc..Binding agent can be at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.PH sensitive dyestuff is at least one in m-cresol purple, thymolphthalein, o-cresolphthalein, bromthymol blue, cresol red, cetyltrimethyl ammonium cation, dimethyl diaminophenazine chloride, phenol red unit, rhodamine, Sulforhodamine 101 and thymol blue.Reference zone 202 is formed by common ink printing, does not have colour change function.When ambient temperature is lower than the freezing point of phase-change material, enclosed switch layer 500 is opened, volatile acid in color change interval 201 is outwards volatilized by mesopore, pH value in color shifting ink raises, pH sensitive dye colour changes, color by comparison color change interval 201 and reference section 202, it is determined that whether enclosed switch layer 500 is opened, can speculate whether product is in the environment lower than specific temperature value.Amplitude according to color change, it was predicted that product is in the cumulative time lower than particular temperature value, thus judging product whether supercooling failure.
In another embodiment, color shifting ink is volatile base sensitive color change ink.Volatile base sensitive color change ink includes volatile base, plasticizer, binding agent, solvent and pH sensitive dyestuff.Volatile base is at least one in ammonium hydroxide, propylamine, n-butylamine, n-hexylamine and 1-Aminooctane.Binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.PH sensitive dyestuff is at least one in bromophenol blue, bromocresol green, bromocresol purple, bromthymol blue, bromothymol blue and m-cresol purple.Reference zone 202 is formed by common ink printing, does not have colour change function.When ambient temperature is lower than the freezing point of phase-change material, enclosed switch layer 500 is opened, volatile base in color change interval 201 can pass through mesopore and outwards volatilize, pH value in color shifting ink reduces, pH sensitive dye colour changes, color by comparison color change interval 201 and reference section 202, it is determined that whether enclosed switch layer 500 is opened, can speculate whether product is in the environment lower than specific temperature value.Amplitude according to color change, it was predicted that product is in the cumulative time lower than particular temperature value, thus judging product whether supercooling failure.
In another embodiment, the material of the color change interval 201 of marker 200 is carbon dioxide sensitive color change ink.Carbon dioxide sensitive color change ink includes phase transfer catalyst, binding agent, plasticizer, solvent and pH sensitive dyestuff.Phase transfer catalyst is at least one in quaternary ammonium salt, sodium hydroxide, Lithium hydrate, potassium hydroxide, barium hydroxide and sodium bicarbonate.Binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.PH sensitive dyestuff is at least one in m-cresol purple, thymolphthalein, o-cresolphthalein, bromthymol blue, cresol red, cetyltrimethyl ammonium cation, dimethyl diaminophenazine chloride, phenol red, rhodamine, Sulforhodamine 101 and thymol blue.Reference zone 202 is formed by common ink printing, does not have colour change function.When ambient temperature is lower than the freezing point of phase-change material, enclosed switch layer 500 is opened, carbon dioxide in environment enters the color change interval 201 of marker 200 by mesopore, and the phase transfer catalyst in color change interval 201 absorbs acid carbon dioxide, and the pH value in color shifting ink reduces.PH sensitive dye colour changes, and consumer can pass through the color of comparison color change interval 201 and reference section 202, it is determined that whether enclosed switch layer 500 is opened, can speculate whether product is in the environment lower than specific temperature value.Amplitude according to color change, it was predicted that product is in the cumulative time lower than particular temperature value, thus judging product whether supercooling failure.
In other embodiments, the material of the color change interval 201 of marker 200 can also be oxygen sensitive color shifting ink, and oxygen sensitive color shifting ink includes photocatalyst, electron donor, binding agent, plasticizer, water-repelling agent, solvent and oxygen sensitive dyestuff.Photocatalyst is at least one in nano titanium oxide, nano strontium titanate, nano tin dioxide, nanometer tungsten oxide and nano zine oxide.Electron donor is at least one in disodiumedetate, triethanolamine, glucose, fructose, polyvinyl alcohol, polyhydric alcohol, dihydroxyhexane and citric acid.Binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Water-repelling agent is sulfonated polystyrene.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.Oxygen sensitive dyestuff is at least one in thiazine, oxazines, azine and indophenols.After photocatalyst is irradiated by the UV light of suitable wavelength, its electronics being in valence band is stimulated and crosses forbidden band and enter conduction band and form free light induced electron, produces photohole in valence band simultaneously.On the one hand, free light induced electron has stronger reproducibility, the oxygen sensitive reactive dye of reducible oxidation state；On the other hand, photohole has stronger oxidisability, oxidable electron donor material.The oxygen sensitive reactive dye of oxidation state can be reduced by light induced electron, and photohole can be reduced by electron donor simultaneously.Oxygen sensitive reactive dye are in reduction-state after being reduced, and possess and the ability of oxygen generation redox reaction, and course of reaction generation color changes.
Oxygen sensitive color shifting ink may also comprise reducing agent, binding agent, plasticizer, water-repelling agent, solvent and oxygen sensitive dyestuff.At least one in reducing agent dithionite, thiosulfate, bisulfites, sulphite, borohydride salts and ascorbic acid.Further, dithionite are sodium dithionite, and thiosulfate is sodium thiosulfate, and borohydride salts is sodium borohydride.Binding agent is described binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Water-repelling agent is sulfonated polystyrene.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.Oxygen sensitive dyestuff is at least one in thiazine, oxazines, azine and indophenols.In ink formulation process, the oxygen sensitive reactive dye of oxidation state are reduced agent reduction.Oxygen sensitive reactive dye are in reduction-state after being reduced, and possess and the ability of oxygen generation redox reaction, and course of reaction generation color changes.
Reference zone 202 is formed by common ink printing, does not have colour change function.When ambient temperature is lower than the freezing point of phase-change material, enclosed switch layer 500 is opened, and the oxygen in environment enters the color change interval 201 of marker 200 by mesopore, in color change interval 201.It is in oxygen sensitive reactive dye and the oxygen generation oxidation reaction of reduction-state, in oxidizing process, oxygen sensitive reactive dye occur that color changes, consumer can pass through the color of comparison color change interval 201 and reference section 202, determine that whether enclosed switch layer 500 is opened, can speculate whether product is in the environment lower than specific temperature value.Amplitude according to color change, it was predicted that product is in the cumulative time lower than particular temperature value, thus judging product whether supercooling failure.
Concrete, protective layer 300 is for protecting the color change interval 201 of marker 200 so that it is from pH value in the first acid adhesive layer 400 or the negative effect of non-neutral phase-change material in enclosed switch layer 500.Linkage change can be there is with color change interval 201 in the pH value of protective layer 300 in neutral or its pH value.The material of protective layer 300 can be thin film or the coating with breathability, for instance polyethylene film, polypropylene film, mylar and transparent ink etc..
When the material of protective layer 300 is transparent ink; the color shifting ink difference of transparent ink and color change interval 201 is in that in the transparent ink of protective layer 300 do not comprise pH sensitive dyestuff; all the other compositions and ratio are identical; both have identical pH value; marker 200 is constituted protection; avoid the phase-change material in the first adhesive layer of pH value non-neutral and enclosed switch that marker is constituted negative effect, cause instruction failure of apparatus.
Concrete; protective layer 300 can be indicate the transparent ink of device, the transparent ink suitable in volatile base sensitivity complexion changed instruction device, the transparent ink suitable in carbon dioxide sensitivity complexion changed instruction device suitable in volatile acid sensitivity complexion changed, or is applicable to the transparent ink etc. of oxygen sensitive complexion changed instruction device.
In present embodiment, protective layer 300 is the transparent ink indicating device suitable in volatile acid sensitivity complexion changed complexion changed.The transparent ink indicating device suitable in volatile acid sensitivity complexion changed complexion changed includes volatile acid, binding agent, plasticizer and solvent.Volatile acid can be the carboxylic acid of 2～12 for carbon number, specifically includes acetic acid, propanoic acid, butanoic acid etc..Binding agent can be at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.
In another embodiment, protective layer 300 is the transparent ink indicating device suitable in volatile base sensitivity complexion changed.The transparent ink indicating device suitable in volatile base sensitivity complexion changed includes volatile base, plasticizer, binding agent and solvent.Volatile base is at least one in ammonium hydroxide, propylamine, n-butylamine, n-hexylamine and 1-Aminooctane.Binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.
In another embodiment, protective layer 300 is the transparent ink indicating device suitable in carbon dioxide sensitivity complexion changed.The transparent ink indicating device suitable in carbon dioxide sensitivity complexion changed includes phase transfer catalyst, binding agent, plasticizer and solvent.Phase transfer catalyst is at least one in quaternary ammonium salt, sodium hydroxide, Lithium hydrate, potassium hydroxide, barium hydroxide and sodium bicarbonate.Binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.
In other embodiments, protective layer 300 can also be the transparent ink indicating device suitable in oxygen sensitive complexion changed, it is adaptable to the transparent ink of oxygen sensitive complexion changed instruction device includes photocatalyst, electron donor, binding agent, plasticizer, water-repelling agent and solvent.Photocatalyst is at least one in nano titanium oxide, nano strontium titanate, nano tin dioxide, nanometer tungsten oxide and nano zine oxide.Electron donor is at least one in disodiumedetate, triethanolamine, glucose, fructose, polyvinyl alcohol, polyhydric alcohol, dihydroxyhexane and citric acid.Binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Water-repelling agent is sulfonated polystyrene.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.
The transparent ink indicating device suitable in oxygen sensitive complexion changed may also comprise reducing agent, binding agent, plasticizer, water-repelling agent and solvent.At least one in reducing agent dithionite, thiosulfate, bisulfites, sulphite, borohydride salts and ascorbic acid.Further, dithionite are sodium dithionite, and thiosulfate is sodium thiosulfate, and borohydride salts is sodium borohydride.Binding agent is described binding agent is at least one in polyvinyl butyral resin, nitrocotton, polyvinyl alcohol, hydroxyethyl cellulose or hydroxypropyl cellulose.Plasticizer is at least one in diisodecyl adipate (DIDA), tributyl phosphate, dimethyl phthalate or glycerol.Water-repelling agent is sulfonated polystyrene.Solvent is at least one in methanol, ethanol, acetoneand ethyl acetate.
Concrete, protective layer 300 is layered on the color change interval 201 of marker 200 surface away from basal layer 100.Protective layer 300 can also be layered on the reference zone 202 of marker 200 simultaneously, and namely protective layer 300 covers color change interval 201 and the reference zone 202 of marker 200, so to facilitate location, simple for production.
Concrete, the first adhesive-layer 400 is layered in enclosed switch layer 500 on the surface of marker 200.First adhesive-layer 400 is for being bonded together protective layer 300 and enclosed switch layer 500.The material of the first adhesive-layer 400 can be at least one in acrylic resin, polyurethane and epoxy resin.
In present embodiment, the first adhesive-layer 400 forms the first adhesive-layer hollow-out parts 401 in the region place hollow out of color change interval 201 correspondence of marker 200.First adhesive-layer hollow-out parts 401 can be located at the underface of color change interval 201, and the first adhesive-layer 400 can be avoided after hollow out to intercept gas, and after enclosed switch layer 500 is opened, what gas can be without hindrance enters people or effusion color change interval 201.
Being appreciated that and indicate in device 10 at time-temperature, protective layer 300 and the first adhesive-layer 400 all can save, and now, enclosed switch layer 500 is layered on marker 200, and both are connected by methods such as hot melt laminatings.
Enclosed switch layer 500 includes phase-change material and the carrier layer of carrying phase-change material, and carrier layer is provided with multiple micropore, and micropore is through hole, and phase-change material is arranged in micropore.
Concrete, the thickness of carrier layer can be 50 μm～2000 μm.The ability of the carrier layer carrying phase-change material of 50 μm～2000 μ m thick is strong, when phase-change material is aqueous, plays the effect sealing marker 200.
Further, the thickness of carrier layer is 100 μm～1000 μm.
Concrete, the aperture of micropore is 10nm～5000nm.Aqueous phase-change material can be adsorbed in micropore, plays the effect sealing marker 200.When temperature is lower than the freezing point of phase-change material, phase-change material solidify, be close on micro-pore wall, phase-change material because mesopore occurs inside volume contraction, activationary time temperature indicating device 10.
Further, the aperture of micropore is 100nm～500nm.
Concrete, carrier layer is provided with multiple uniformly coherent micropore.Phase-change material is had affinity by carrier layer, and the phase-change material of liquid can be filled in the micropore of carrier layer.
Phase-change material can vary with temperature and change state of matter, and when temperature is higher than predetermined temperature value, phase-change material shows as liquid.When temperature is lower than predetermined temperature value, phase-change material shows as solid.Concrete, phase-change material is at least one in fatty acid and fatty acid ester.Phase-change material can also be the mixture of several material, such as mixture that different fatty acids form etc..The material with suitable freezing point and difficult volatilization all can as the phase-change material of the present invention.
In present embodiment, phase-change material is freezing point is the fatty acid of 2 DEG C, and fatty acid has a safe and nontoxic feature, particularly suitable does phase-change material.In other embodiments, it would however also be possible to employ the material of different freezing pointes is as phase-change material.
Concrete, it is possible to by the carrier layer with micropore is immersed in liquid phase change material, thus obtaining the enclosed switch layer 500 of the saturated filling of phase-change material.When ambient temperature is higher than the freezing point of phase-change material, phase-change material is saturated in fluid form to be filled in the carrier layer with micropore, is closed by micropore, and now enclosed switch layer 500 is closed, time-temperature instruction device 10 un-activation.When ambient temperature is lower than the freezing point of phase-change material, phase-change material solidifies, and occurs mesopore inside phase-change material, and now enclosed switch layer 500 is in open mode, and time-temperature instruction device 10 is activated state.Gas can be entered by mesopore or overflow the color change interval 201 of marker 200, the color change interval 201 making marker 200 occurs color to change, the color of contrast color change interval 201 and the color of reference zone 202, can show that product is in the cumulative time lower than particular temperature value, realize lower critical temperature is monitored, thus judging product whether supercooling failure.The phase-change material that adopts of the invention coordinates with the carrier layer being provided with micropore, indicates the enclosed switch layer 500 of device 10 as time-temperature, and product structure is simple, and easy achieves lower critical temperature monitoring, thus judging product whether supercooling failure.
Concrete, the second adhesive-layer 600 is layered on the enclosed switch layer 500 surface away from marker 200, and peel ply 700 is layered on second adhesive-layer 600 surface away from enclosed switch layer 500.The material of the second adhesive-layer 600 can be at least one in acrylic resin, polyurethane and epoxy resin.
In present embodiment, the second adhesive-layer 600 forms the second adhesive-layer hollow-out parts 601 in the region place hollow out of color change interval 201 correspondence of marker 200.Second adhesive-layer hollow-out parts 601 can be located at the underface of color change interval 201, and the second adhesive-layer 600 can be avoided after hollow out to intercept gas, and after enclosed switch layer 500 is opened, what gas can be without hindrance enters people or effusion color change interval 201.
Peel ply 700 is used for protecting the second adhesive-layer 600; optional peel ply 700 can be the peeling paper of silicon-coating oil; after removing peel ply 700; second adhesive-layer 600 indicates the surface of device 10 at time-temperature, by the second adhesive-layer 600, time-temperature can indicate device 10 be attached to the surface of detection product.
Being appreciated that and indicate in device 10 at time-temperature, the second adhesive-layer 600 and peel ply 700 all can save, and now, time-temperature indicate the enclosed switch layer 500 of device 10 be directly placed on detection product.
Above-mentioned time-temperature instruction device 10, the enclosed switch layer 500 indicating device 10 as time-temperature by using phase-change material to coordinate with the carrier layer being provided with micropore, apparatus structure is simple, Miniaturizable, whether detection product is lower than lower critical temperature very easily, is particularly suited for the product (ampoule bottle as equipped with vaccine) of detection smaller size smaller.By the amplitude that the color of color change interval 201 changes, showing that product is in the cumulative time lower than particular temperature value, easy achieves the monitoring to lower critical temperature, thus judging product whether supercooling failure.
It it is below specific embodiment.
Embodiment 1
The structural representation of the time-temperature instruction device 10 of the present embodiment can referring to Fig. 1.Forming marker 200 on basal layer 100, marker 200 is divided into color change interval 201 and reference zone 202.The material of color change interval 201 is volatile acid sensitive color change ink, and this volatile acid sensitive color change ink includes volatile acid (anhydrous acetic acid), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol) and pH sensitive dyestuff (m-cresol purple).Reference zone 202 is formed by common ink printing, does not possess colour change function.Being arranged below one layer of pH value protective layer 300 at color change interval 201 and reference zone 202, protective layer 300 is the transparent ink indicating device suitable in volatile acid sensitivity complexion changed.This protective layer transparent ink includes volatile acid (anhydrous acetic acid), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate) and solvent (ethanol).Protective layer transparent ink and color shifting ink difference are in that transparent ink does not comprise pH sensitive dyestuff, and all the other compositions and ratio are identical, and both have identical pH value.First adhesive-layer 400 is set in local, the lower section of protective layer 300, does hollow out process at color change interval 201 corresponding part and form the first adhesive-layer hollow-out parts 401.Being arranged below enclosed switch layer 500 at the first adhesive layer 400, enclosed switch layer 500 is soaked, by the carrier layer with micropore, the phase-change material that freezing point is 2 DEG C and makes.Being arranged below the second adhesive layer 600 at enclosed switch layer 500, transformation region corresponding part does hollow out process and forms the second adhesive layer hollow-out parts 601.It is arranged below peel ply 700 at the second adhesive layer 600 and the second adhesive layer hollow-out parts 601, namely makes the lower critical time-temperature instruction device 10 that critical temperature is 2 DEG C.
The structure of ampoule bottle 20 is as in figure 2 it is shown, the top of ampoule bottle 20 is provided with air-vent 021.The structural representation that the peel ply 700 that time-temperature indicates device 10 is attached on ampoule bottle after peeling off is as shown in Figure 3.Ampoule bottle is built with vaccine, time-temperature instruction device 10 enters cold chain with vaccine product, when cold chain temperature is in normal interval (such as 2 DEG C～8 DEG C), the phase-change material of saturated filling liquid in the micropore of the carrier layer of enclosed switch layer 500, not there is breathability.In color change interval 201, volatile acid cannot outwardly discharge, and its pH value remains unchanged, and namely color change interval 201 color remains unchanged.When cold chain temperature is lower than lower critical temperature 2 DEG C, phase-change material in the micropore of carrier layer solidifies gradually, in process of setting, adsorption due to hole wall, phase-change material is close on micro-pore wall, and its molecules align is from order to unordered, and intermolecular distance reduces,, there is mesopore in volume contraction inside phase-change material.Now, color change interval 201 and in protective layer 300 escaping gas molecular acid can pass through the middle lyriform pore of enclosed switch layer 500 and synchronize outwards volatilization, and be diffused in environment by air-vent 021, cause that the pH value of color change interval 201 and protective layer 300 ink synchronizes to raise.And then cause pH sensitive dye colour in color change interval 201 to change.Because of in protective layer 300 ink without pH sensitive dyestuff, its color keep water white transparency, color change interval 201 will not be adversely affected.The time opened to enclosed switch layer 500 hole due to the shade of color change interval 201 is directly proportional, when the vaccine the longest holding time under supercooled state is consistent with the variable color duration of color change interval 201, color by comparison color change interval 201 and reference zone 202, it is judged that whether vaccine is because of supercooling failure.Namely, when the color of color change interval 201 and the solid colour of reference zone 202, vaccine is because of supercooling failure, and otherwise, vaccine still can use.
Embodiment 2
The structural representation of the time-temperature instruction device 10 of the present embodiment can referring to Fig. 4.Forming marker 200 on basal layer 100, marker 200 is divided into color change interval 201 and reference zone 202.Reference zone 202 is further divided into the first reference zone 2021 and the second reference zone 2022.The material of color change interval 201 is volatile base sensitive color change ink, and this volatile base sensitive color change ink includes volatile base (propylamine), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol) and pH sensitive dyestuff (phenol red).Reference zone 202 is formed by common ink printing, does not possess colour change function.Being arranged below one layer of pH value protective layer 300 at color change interval 201 and reference zone 202, protective layer 300 is the transparent ink indicating device suitable in volatile base sensitive color change.This protective layer transparent ink includes volatile base (propylamine), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate) and solvent (ethanol).Protective layer transparent ink and color shifting ink difference are in that transparent ink does not comprise pH sensitive dyestuff, and all the other compositions and ratio are identical, and both have identical pH value.First adhesive-layer 400 is set in local, the lower section of protective layer 300, does hollow out process at color change interval 201 corresponding part and form the first adhesive-layer hollow-out parts 401.Being arranged below enclosed switch layer 500 at the first adhesive layer 400, enclosed switch layer 500 is soaked, by the carrier layer with micropore, the phase-change material that freezing point is 6 DEG C and makes.Being arranged below the second adhesive layer 600 at enclosed switch layer 500, transformation region corresponding part does hollow out process and forms the second adhesive layer hollow-out parts 601.It is arranged below peel ply 700 at the second adhesive layer 600 and the second adhesive layer hollow-out parts 601, namely makes the lower critical time-temperature instruction device 10 that critical temperature is 6 DEG C.
The structural representation that the peel ply 700 that time-temperature indicates device 10 is attached on ampoule bottle after peeling off is as shown in Figure 5.Ampoule bottle is built with vaccine, and time-temperature instruction device 10 enters cold chain with vaccine product, when cold chain temperature is in normal interval, and the phase-change material of saturated filling liquid in the micropore of the carrier layer of enclosed switch layer 500, not there is breathability.In color change interval 201, volatile base cannot outwardly discharge, and its pH value remains unchanged, and namely color change interval 201 color remains unchanged.When cold chain temperature is lower than lower critical temperature 6 DEG C, phase-change material in the micropore of carrier layer solidifies gradually, in process of setting, adsorption due to hole wall, phase-change material is close on micro-pore wall, and its molecules align is from order to unordered, and intermolecular distance reduces,, there is mesopore in volume contraction inside phase-change material.Now, color change interval 201 and in protective layer 300 escaping gas propylamine can pass through enclosed switch layer 500 mesopore and synchronize outwards volatilization, and be diffused in environment by air-vent 021, cause that the pH value of the ink of color change interval 201 and protective layer 300 synchronizes to reduce.And then cause pH sensitive dye colour in color change interval 201 to change.Because of in protective layer 300 ink without pH sensitive dyestuff, its color keep water white transparency, color change interval 201 will not be adversely affected.The time opened to enclosed switch layer 500 hole due to the shade of color change interval 201 is directly proportional, when the vaccine the longest holding time under supercooled state is consistent with the variable color duration of color change interval 201, color by comparison color change interval 201 and reference zone 202, it is judged that whether vaccine is because of supercooling failure.When the color of color change interval 201 and the solid colour of the first reference zone 2021 or close to time represent that cold chain ambient temperature is not less than lower critical temperature, vaccine can relieved use.When the color of color change interval 201 and the solid colour of the second reference zone 2022 or close to time represent that cold chain ambient temperature exceedes lower critical temperature, vaccine is because of supercooling failure.
Embodiment 3
The structural representation of the time-temperature instruction device 10 of the present embodiment can referring to Fig. 6.Forming marker 200 on basal layer 100, marker 200 is divided into color change interval 201 and reference zone 202.Reference zone 202 is further divided into the first reference zone the 2021, second reference zone 2022 and the 3rd reference zone 2023.The material of color change interval 201 is volatile base sensitive color change ink, and volatile base sensitive color change ink includes volatile base (ammonium hydroxide), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol) and pH sensitive dyestuff (Bromothymol blue).Reference zone 202 has common ink printing to form, and does not have colour change function.Being arranged below one layer of pH value protective layer 300 at color change interval 201 and reference zone 202, protective layer 300 is the polyethylene film stretched.First adhesive-layer 400 is set in local, the lower section of protective layer 300, does hollow out process at color change interval 201 corresponding part and form the first adhesive-layer hollow-out parts 401.Being arranged below enclosed switch layer 500 at the first adhesive layer 400, enclosed switch layer 500 is soaked, by the carrier layer with micropore, the phase-change material that freezing point is 4 DEG C and makes.Being arranged below the second adhesive layer 600 at enclosed switch layer 500, transformation region corresponding part does hollow out process and forms the second adhesive layer hollow-out parts 601.It is arranged below peel ply 700 at the second adhesive layer 600 and the second adhesive layer hollow-out parts 601, namely makes the lower critical time-temperature instruction device 10 that critical temperature is 4 DEG C.
The structural representation that the peel ply 700 that time-temperature indicates device 10 is attached on ampoule bottle after peeling off is as shown in Figure 7.Ampoule bottle is built with vaccine, and time-temperature instruction device 10 enters cold chain with vaccine product, when cold chain temperature is in normal interval, and the phase-change material of saturated filling liquid in the micropore of the carrier layer of enclosed switch layer 500, not there is breathability.In color change interval 201, volatile base cannot outwardly discharge, and its pH value remains unchanged, and namely color change interval 201 color remains unchanged.When cold chain temperature is lower than lower critical temperature 4 DEG C, phase-change material in the micropore of carrier layer solidifies gradually, in process of setting, adsorption due to hole wall, phase-change material is close on micro-pore wall, and its molecules align is from order to unordered, and intermolecular distance reduces,, there is mesopore in volume contraction inside phase-change material.Now; in color change interval 201 and protective layer 300, escaping gas ammonium hydroxide molecule can pass through enclosed switch layer 500 mesopore synchronization outwards volatilization; and it is diffused in environment by air-vent 021, cause that the pH value of the ink of color change interval 201 and protective layer 300 synchronizes to reduce.And then cause pH sensitive dye colour in color change interval 201 to change.Because of in protective layer 300 ink without pH sensitive dyestuff, its color keep water white transparency, color change interval 201 will not be adversely affected.The time opened to enclosed switch layer 500 hole due to the shade of color change interval 201 is directly proportional, when the vaccine the longest holding time under supercooled state is consistent with the variable color duration of color change interval 201, color by comparison color change interval 201 and reference zone 202, it is judged that whether vaccine is because of supercooling failure.When the color of color change interval 201 and the solid colour of the first reference zone 2021 or close to time represent that cold chain ambient temperature is not less than lower critical temperature, vaccine can relieved use.When the color of color change interval 201 and the solid colour of the second reference zone 2022 or close to time represent that cold chain ambient temperature is once once supercool, but do not result in vaccine complete failure.When the color of color change interval 201 and the solid colour of the 3rd reference zone 2023 or close to time, represent that cold chain ambient temperature exceedes lower critical temperature, vaccine is because of supercooling failure.
Embodiment 4
The material of the color change interval 201 of time-temperature instruction device 10 is carbon dioxide sensitive color change ink, and this carbon dioxide sensitive color change ink includes phase transfer catalyst (sodium hydroxide), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol) and pH sensitive dyestuff (Bromothymol blue).Protective layer transparent ink 300 includes phase transfer catalyst (sodium hydroxide), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate) and solvent (ethanol).Protective layer transparent ink and color shifting ink difference are in that transparent ink does not comprise pH sensitive dyestuff, and all the other compositions and ratio are identical, and both have identical pH value.All the other are identical with embodiment 1.When ambient temperature is lower than the freezing point of phase-change material; enclosed switch layer 500 is opened; carbon dioxide in environment enters the color change interval 201 of marker 200 by mesopore; phase transfer catalyst in color change interval 201 and protective layer 300 absorbs sour gas carbon dioxide simultaneously, and the pH value of color shifting ink and protective layer 300 synchronizes to reduce.Because of in protective layer 300 ink without pH sensitive dyestuff, its color keep water white transparency, color change interval 201 will not be adversely affected.Color change is shown, by the color of comparison color change interval 201 and reference section 202, it is determined that whether enclosed switch layer 500 is opened, can speculate whether product is in the environment lower than specific temperature value by pH sensitive dyestuff.Amplitude according to color change, it was predicted that product is in the cumulative time lower than particular temperature value, thus judging product whether supercooling failure.
Embodiment 5
The material of the color change interval 201 of time-temperature instruction device 10 is oxygen sensitive color shifting ink, and this oxygen sensitive color shifting ink includes photocatalyst (nano titanium oxide), electron donor (disodiumedetate), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol) and oxygen sensitive dyestuff (methylene blue).Protective layer transparent ink 300 includes photocatalyst (nano titanium oxide), electron donor (disodiumedetate), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol).Protective layer transparent ink and color shifting ink difference are in that transparent ink does not comprise pH sensitive dyestuff, and all the other compositions and ratio are identical, and both have identical pH value.All the other are identical with embodiment 1.When ambient temperature is lower than the freezing point of phase-change material, enclosed switch layer 500 is opened, and the oxygen in environment is entered by mesopore in color change interval 201 and the protective layer 300 of marker 200.Early stage is under the effect of suitable wavelength UV light, oxygen sensitive reactive dye are in reduction-state, the oxygen sensitive reactive dye of reduction-state can with oxygen generation oxidation reaction, reflection process oxygen sensitive dyestuff shows color change, the color of comparison color change interval 201 and reference section 202, determine that whether enclosed switch layer 500 is opened, can speculate whether product is in the environment lower than specific temperature value.Amplitude according to color change, it was predicted that product is in the cumulative time lower than particular temperature value, thus judging product whether supercooling failure.
Embodiment 6
The material of the color change interval 201 of time-temperature instruction device 10 is oxygen sensitive color shifting ink, and this oxygen sensitive color shifting ink includes reducing agent (sodium dithionite), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol) and oxygen sensitive dyestuff (methylene blue).Protective layer transparent ink 300 includes reducing agent (sodium dithionite), binding agent (polyvinyl butyral resin), plasticizer (tributyl phosphate), solvent (ethanol).Protective layer transparent ink and color shifting ink difference are in that transparent ink does not comprise pH sensitive dyestuff, and all the other compositions and ratio are identical, and both have identical pH value.All the other are identical with embodiment 1.When ambient temperature is lower than the freezing point of phase-change material, enclosed switch layer 500 is opened, and the oxygen in environment is entered by mesopore in color change interval 201 and the protective layer 300 of marker 200.During ink formulation, under the effect of reducing agent, oxygen sensitive reactive dye are in reduction-state, the oxygen sensitive reactive dye of reduction-state can with oxygen generation oxidation reaction, reflection process oxygen sensitive dyestuff shows color change, the color of comparison color change interval 201 and reference section 202, it is determined that whether enclosed switch layer 500 is opened, can speculate whether product is in the environment lower than specific temperature value.Amplitude according to color change, it was predicted that product is in the cumulative time lower than particular temperature value, thus judging product whether supercooling failure.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, it is also possible to making some deformation and improvement, these broadly fall into protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a time-temperature instruction device, it is characterised in that include the basal layer, marker and the enclosed switch layer that stack gradually；
Described marker includes color change interval, and the material of described color change interval is color shifting ink；
Described enclosed switch layer includes phase-change material and carries the carrier layer of described phase-change material, and described carrier layer is provided with multiple micropore, and described micropore is through hole, and described phase-change material is arranged in described micropore.
2. time-temperature according to claim 1 instruction device, it is characterised in that described phase-change material is at least one in fatty acid and fatty acid ester.
3. time-temperature according to claim 1 instruction device, it is characterised in that the thickness of described carrier layer is 50 μm～2000 μm.
4. time-temperature according to claim 1 instruction device, it is characterised in that the aperture of described micropore is 10nm～5000nm.
5. time-temperature according to claim 1 instruction device, it is characterised in that described carrier layer is provided with multiple uniformly coherent micropore.
6. time-temperature according to claim 1 instruction device, it is characterized in that, described marker also includes reference zone, and the color of color change interval is thus judging the response time of described color change interval described in comparison for described reference zone, and described reference zone has at least one fixing color.
7. time-temperature according to claim 1 instruction device, it is characterised in that described color shifting ink is volatile acid sensitive color change ink, volatile base sensitive color change ink, carbon dioxide sensitive color change ink or oxygen sensitive color shifting ink.
8. time-temperature according to claim 1 instruction device, it is characterised in that described time-temperature instruction device also includes protective layer, and described protective layer is layered on the described color change interval of the described marker surface away from described basal layer.
9. time-temperature according to claim 1 instruction device, it is characterized in that, described time-temperature instruction device also includes the first adhesive-layer, described first adhesive-layer is layered in described enclosed switch layer on the surface of described marker, and described first adhesive-layer is in region place hollow out corresponding to the described color change interval of described marker.
10. time-temperature according to claim 1 instruction device, it is characterized in that, described time-temperature instruction device also includes the second adhesive-layer and the peel ply that stack gradually, described second adhesive-layer is layered on the described enclosed switch layer surface away from described marker, and described peel ply is layered on described second adhesive-layer surface away from described enclosed switch layer.
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| CN106768462A (en) * | 2016-11-21 | 2017-05-31 | 深圳九星印刷包装集团有限公司 | Temperature-sensitive time-indicating arrangement |
| CN108279076A (en) * | 2017-12-19 | 2018-07-13 | 江南大学 | A kind of critical temperature indicator based on Microencapsulated Slow effect |
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