CN111192515B - Preparation and application methods of temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material - Google Patents
Preparation and application methods of temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material Download PDFInfo
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- CN111192515B CN111192515B CN201911317700.2A CN201911317700A CN111192515B CN 111192515 B CN111192515 B CN 111192515B CN 201911317700 A CN201911317700 A CN 201911317700A CN 111192515 B CN111192515 B CN 111192515B
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F3/00—Labels, tag tickets, or similar identification or indication means; Seals; Postage or like stamps
- G09F3/02—Forms or constructions
- G09F3/0291—Labels or tickets undergoing a change under particular conditions, e.g. heat, radiation, passage of time
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Abstract
The invention discloses a preparation and application method of a temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material, which is used for determining a target temperature to be indicated; dissolving or dispersing 0.2-10 per mill w/w of fluorescent material in the basic ink to prepare the intelligent fluorescent composite coating material; after brushing a PVAL glue layer on the back of substrate paper, soaking basic ink, placing the basic ink in a low-temperature environment to solidify the basic ink, spraying a specified mark layer with the thickness of more than 1 mu m on the surface of the treated substrate paper by using an intelligent fluorescent composite coating material, placing the substrate paper sprayed with the fluorescent mark in the low-temperature environment, and observing a specific fluorescent mark after the intelligent fluorescent composite coating material is solidified; the composite coating material and the fluorescent anti-counterfeiting label product have obvious fluorescent effect in a low-temperature state, the structure of the composite coating changes after a high-temperature process, so that the fluorescent effect is weakened, and the temperature-sensitive fluorescence change process is irreversible, so that the composite coating material and the fluorescent anti-counterfeiting label product are ideal intelligent composite materials for monitoring the whole process of cold-chain transportation products.
Description
Technical Field
The invention relates to a preparation method and an application method of a temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material, which are oriented to the requirements of monitoring and managing the whole process of cold-chain storage and transportation of foods and medicines.
Background
In the increasingly developed logistics industry, cold chain storage and transportation have become an extremely important component. Based on the particularity of cold chain transportation, the fact that the transported goods are kept in a low-temperature environment all the time in the transportation process is an important factor for guaranteeing the quality of the transported goods. The traditional cold chain uses an electronic temperature sensor as a temperature label of a containerized cargo, but has the problems of high use cost, difficulty in carrying out whole-course continuous temperature detection on a single commodity from a factory to a shelf process and the like. The conventional temperature indicating label is easy to obtain and replace or change the label display. If local goods are heated in the transportation link to cause product failure, the body health is influenced, and great risks exist for special goods such as medical vaccines.
Disclosure of Invention
The invention provides an efficiency indicating material and an anti-counterfeiting label application method which are low in cost and can record whether a single product is exposed in a high-temperature environment, aiming at the problem that the whole process monitoring of the cold chain storage and transportation process is difficult to carry out on the single product, so that the whole process monitoring and management of the single product from delivery to a goods shelf to consumer application are realized.
The invention adopts the technical scheme of preparation and application of a temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material.
The specific implementation of the process of preparing the "temperature efficacy indication label" can be performed in steps, and the preparation process of the result is mainly described with respect to fig. 1. The temperature efficiency indicating label comprises a PVAL adhesive layer 1, substrate paper 2, a bottom base ink layer 3 and an intelligent fluorescent anti-counterfeiting composite coating 4;
the preparation process comprises the following steps:
a. determining a target temperature to be indicated, and adopting solvents such as higher alkane (C8-18), higher alcohol and the like as base ink, wherein the target temperature is not lower than the freezing point of the adopted base ink; (the mixing ratio is adjusted according to the specific temperature)
b. Dissolving or dispersing 0.2-10 per mill w/w of fluorescent material in the basic ink to prepare the intelligent fluorescent composite coating material;
c. after brushing a PVAL glue layer on the back of substrate paper, soaking basic ink, placing the basic ink in a low-temperature environment to solidify the basic ink, spraying a specified mark layer with the thickness of more than 1 mu m on the surface of the treated substrate paper by using the intelligent fluorescent composite coating material, placing the substrate paper sprayed with the fluorescent mark in the low-temperature environment, and observing a specific fluorescent mark after the intelligent fluorescent composite coating material is solidified; (the size of the tag is sprayed on as needed).
The application process comprises the following steps:
and placing the label in an environment needing temperature indication for 2-5 minutes, observing whether the fluorescent mark changes, and judging whether the environment temperature reaches or exceeds the target temperature if the fluorescent mark changes or disappears.
The ink is not limited to alkanes and alcohols and other chemicals can be widely used.
The fluorescent material refers to organic molecules or inorganic nanoparticles with fluorescent characteristics.
The substrate paper refers to non-fluorescent paper or fabric with good stability and can not react with ink or fluorescent dye.
The temperature effect indicating label is square, round, triangular and the like.
The designated mark is a character, a figure or a special pattern.
The low-temperature environment is a low-temperature environment which is not less than 2 ℃ lower than the target temperature.
When the ambient temperature rises to the melting point of the basic ink, the basic ink on the bottom layer and the intelligent fluorescent composite coating material are mixed and diffused, so that the fluorescent material in the intelligent fluorescent composite coating material is subjected to irreversible changes such as diffusion and mixing. When the label is placed in a low-temperature environment again, the mixed basic ink cannot be separated from the fluorescence, and damaged fluorescent marks and the like cannot be recovered. Irreversible changes in the sensitivity to high temperatures can be achieved by this technique. In addition, the requirements of different corresponding temperatures are realized by adjusting the selection of the base ink; the requirement of different fluorescent colors is achieved by selecting different fluorescent dyes or multiple fluorescent dyes.
The temperature sensitive efficiency indicating label provided by the invention has the advantages of simple structure, low cost, high sensitivity and strong anti-counterfeiting property. The efficiency and the reliability of transportation goods temperature supervision are stored to the cold chain are improved.
The term "intelligent" as used herein means that the "tag" can autonomously record whether it has been exposed to high temperature and can easily read the result directly.
Drawings
Fig. 1 is a schematic cross-sectional view of a temperature performance indicator according to a first embodiment of the present invention.
In the figure: 1 is PVAL glue film, 2 is substrate paper, 3 is bottom basic printing ink layer, 4 is intelligent fluorescence anti-fake composite coating.
Fig. 2 is a photo of a temperature performance indicator label according to a first embodiment of the present invention and a change of fluorescent label during a temperature increase process.
Fig. 3 is a photo of a temperature performance indicator label according to a second embodiment of the present invention.
Detailed Description
In order to make the technical spirit and advantages of the present invention more clearly understandable to those skilled in the art and particularly to the public, the applicant shall describe in detail the following embodiments, but the description of the embodiments is not a limitation to the technical solution of the present invention, and any equivalent changes made according to the inventive concept, which are only in form and not substantial, shall be considered as the technical solution of the present invention.
The first embodiment is as follows: an elongated temperature performance indicating label with a size of 30mm gamma and 20mm is manufactured, and non-fluorescent paper, PVAL glue, tetradecane and hexaphenylsilole are selected as materials. As shown in fig. 2
And (3) label making:
1. 2-100mg of hexaphenylsilole and 10g of n-tetradecane are subjected to ultrasonic treatment at 30 ℃ for 10min to prepare the fluorescent material dispersion liquid.
2. And (4) brushing PVAL glue on one side of the non-fluorescent paper and drying. The non-fluorescent paper after being painted is cut into strips with the x of 30mm and the x of 20mm, and the non-painted surface is coated with tetradecane. After absorbing the excessive n-tetradecane by using filter paper, the treated fluorescence-free paper is frozen at the temperature of minus 20 ℃ for 10 min.
3. And taking out the fluorescent-free paper. Dipping the fluorescent material dispersion liquid by a cotton swab, drawing lines on the non-fluorescent paper at equal intervals, and immediately freezing the non-fluorescent paper at-20 ℃ for 10min after drawing. The temperature performance indication label can be obtained.
The label is used: when in use, the temperature efficiency indicating label is attached to a product package stored in a cold chain, and is placed in an environment of 2 ℃ for refrigeration, and fluorescent marks with equal intervals can be observed by using an ultraviolet lamp for irradiation. If the product is taken out from the refrigerated environment and placed in a room temperature environment (20 ℃), the tetradecane on the label is dissolved and mixed with the fluorescent material, so that the fluorescent material is fully diffused, and the fluorescent label cannot be shown by the irradiation of an ultraviolet lamp at the moment, thereby indicating that the product is exposed in an environment higher than the specified storage temperature, the product efficiency cannot be ensured and the product cannot be used. When the label which loses the fluorescent mark is frozen again, the fluorescent mark can not be recovered because the diffused fluorescent material can not be gathered again, namely, the process of disappearance of the fluorescent mark is irreversible, so that whether the product is invalid or not can be effectively indicated.
Example two: a round temperature efficiency indicating label with the size of phi 15mm is manufactured, and the material selected is non-fluorescent paper, PVAL glue, n-tetradecane and hexaphenylsilole. As shown in fig. 3
And (3) label making:
1. 2-100mg of hexaphenylsilole and 10g of n-tetradecane are subjected to ultrasonic treatment at 30 ℃ for 10min to prepare the fluorescent material dispersion liquid.
2. And (4) brushing PVAL glue on one side of the non-fluorescent paper and drying. Cutting the non-fluorescent paper after being brushed with the glue into a round label with the size of phi 15mm, and coating tetradecane on the surface without being brushed with the glue. After absorbing the excessive n-tetradecane by using filter paper, the treated fluorescence-free paper is frozen at the temperature of minus 20 ℃ for 10 min.
3. And taking out the fluorescent-free paper. Dipping a cotton swab into the fluorescent material dispersion liquid, drawing a 'number matching' mark on the non-fluorescent paper, and immediately freezing the non-fluorescent paper at-20 ℃ for 10min after drawing. The temperature performance indication label can be obtained.
The label is used: when in use, the temperature efficiency indicating label is attached to a product package stored in a cold chain, and is placed in a 2 ℃ environment for refrigeration, and the 'number matching' fluorescent label can be observed by irradiating with an ultraviolet lamp. If the product is removed from the refrigerated environment and placed in a room temperature environment (20℃), the tetradecane on the label dissolves and mixes with the fluorescent material, causing the AIEgens to diffuse, at which time the fluorescent label cannot be revealed by irradiation with an ultraviolet lamp, thereby indicating that the product has been exposed to temperatures above the specified storage temperature, and that the product is unusable because of its effectiveness. When the label which loses the fluorescent mark is frozen again, the fluorescent mark can not be recovered because the diffused fluorescent material can not be gathered again, namely, the process of disappearance of the fluorescent mark is irreversible, so that whether the product is invalid or not can be effectively indicated.
Example three: an elongated temperature efficiency indicating label with the size of 30mm gamma and 20mm is manufactured, and non-fluorescent paper, PVAL glue, tetradecane and tetraphenyl ethylene are selected as materials.
And (3) label making:
1. 2-100mg of tetraphenylethylene and 10g of n-tetradecane are subjected to ultrasonic treatment at 30 ℃ for 10min to prepare a fluorescent material dispersion liquid.
2. And (4) brushing PVAL glue on one side of the non-fluorescent paper and drying. The non-fluorescent paper after being painted is cut into strips with the x of 30mm and the x of 20mm, and the non-painted surface is coated with tetradecane. After absorbing the excessive n-tetradecane by using filter paper, the treated fluorescence-free paper is frozen at the temperature of minus 20 ℃ for 10 min.
3. And taking out the fluorescent-free paper. Dipping the fluorescent material dispersion liquid by a cotton swab, drawing lines on the non-fluorescent paper at equal intervals, and immediately freezing the non-fluorescent paper at-20 ℃ for 10min after drawing. The temperature performance indication label can be obtained.
The label is used: when in use, the temperature efficiency indicating label is attached to a product package stored in a cold chain, and is placed in an environment of 2 ℃ for refrigeration, and fluorescent marks with equal intervals can be observed by using an ultraviolet lamp for irradiation. If the product is taken out from the refrigerated environment and placed in a room temperature environment (20 ℃), the tetradecane on the label is dissolved and mixed with the fluorescent material, so that the fluorescent material is fully diffused, and the fluorescent label cannot be shown by the irradiation of an ultraviolet lamp at the moment, thereby indicating that the product is exposed in an environment higher than the specified storage temperature, the product efficiency cannot be ensured and the product cannot be used. When the label which loses the fluorescent mark is frozen again, the fluorescent mark can not be recovered because the diffused fluorescent material can not be gathered again, namely, the process of disappearance of the fluorescent mark is irreversible, so that whether the product is invalid or not can be effectively indicated.
Example four: an elongated temperature efficiency indicating label with a size of 30mm gamma and 20mm is manufactured, and non-fluorescent paper, PVAL glue, 1, 5-pentanediol and hexa-phenyl silole are selected as materials.
And (3) label making:
1. 2-100mg of hexaphenyl silole and 10g of 1, 5-pentanediol were subjected to ultrasonic treatment at 30 ℃ for 10min to prepare a fluorescent material dispersion.
2. And (4) brushing PVAL glue on one side of the non-fluorescent paper and drying. The non-fluorescent paper after being painted is cut into strips with the x of 30mm and the x of 20mm, and the non-painted surface is coated with tetradecane. After absorbing the excessive n-tetradecane by using filter paper, the treated fluorescence-free paper is frozen at the temperature of minus 40 ℃ for 10 min.
3. And taking out the fluorescent-free paper. Dipping the fluorescent material dispersion liquid by a cotton swab, drawing lines on the non-fluorescent paper at equal intervals, and immediately freezing the non-fluorescent paper at-40 ℃ for 10min after drawing. The temperature performance indication label can be obtained.
The label is used: when in use, the temperature efficiency indicating label is attached to a product package stored in a cold chain, and is frozen at the temperature of minus 20 ℃, and fluorescent marks with equal distance can be observed by using an ultraviolet lamp for irradiation. If the product is taken out from the freezing environment and placed in the cold storage environment (2 ℃), the 1, 5-pentanediol on the label is dissolved and mixed with the fluorescent material, so that the fluorescent material is fully diffused, and the fluorescent label cannot be shown by the irradiation of an ultraviolet lamp at the moment, so that the condition that the product is exposed in the environment higher than the specified storage temperature is indicated, the product efficiency cannot be ensured, and the product cannot be used. When the label which loses the fluorescent mark is frozen again, the fluorescent mark can not be recovered because the diffused fluorescent material can not be gathered again, namely, the process of disappearance of the fluorescent mark is irreversible, so that whether the product is invalid or not can be effectively indicated.
Claims (4)
1. A preparation method of a temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material is characterized by comprising the following steps: the preparation process of the method comprises the following steps:
a. determining a target temperature required to be indicated by the temperature effect indicating label, and adopting higher alkane C8-18 and higher alcohol solvent as base ink, wherein the target temperature is not lower than the freezing point of the adopted base ink;
b. dissolving or dispersing 0.2-10 per mill w/w of fluorescent material in the basic ink to prepare the intelligent fluorescent composite coating material;
c. brushing a PVAL glue layer on the back of substrate paper, soaking basic ink, placing the basic ink in a low-temperature environment to solidify the basic ink, spraying a specified mark layer with the thickness of more than 1 mu m on the surface of the treated substrate paper by using an intelligent fluorescent composite coating material, placing the substrate paper sprayed with the fluorescent mark in the low-temperature environment, and observing a specific fluorescent mark after the intelligent fluorescent composite coating material is solidified;
placing the temperature effect indicating label in an environment needing temperature indication for 2-5 minutes, observing whether the fluorescent mark changes, and judging whether the environment temperature reaches or exceeds the target temperature if the fluorescent mark changes or disappears;
the fluorescent composite coating material is organic molecules or inorganic nanoparticles with fluorescent characteristics; the low-temperature environment is a low-temperature environment which is not less than 2 ℃ lower than the target temperature;
when the environmental temperature rises to the melting point of the basic ink, the basic ink on the bottom layer and the intelligent fluorescent composite coating material are mixed and diffused, so that the fluorescent material in the intelligent fluorescent composite coating material is subjected to diffusion mixing irreversible change; the label is placed in a low-temperature environment again, the mixed basic ink cannot be separated from the fluorescence, the damaged fluorescence label cannot be recovered, and irreversible change of high-temperature sensitivity is realized; in addition, the requirements of different corresponding temperatures are realized by adjusting the selection of the base ink; different fluorescent dyes or multiple fluorescent dyes are selected to achieve the different fluorescent color requirements.
2. The preparation method of the temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material according to claim 1, which is characterized by comprising the following steps of: the substrate paper is non-fluorescent paper or fabric and does not react with ink or fluorescent dye.
3. The preparation method of the temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material according to claim 1, which is characterized by comprising the following steps of: the shape of temperature effect indicating label is square, circular or triangle-shaped.
4. The preparation method of the temperature-sensitive irreversible intelligent fluorescent anti-counterfeiting composite coating material according to claim 1, which is characterized by comprising the following steps of: the appointed mark layer is characters, figures or special patterns.
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