CN114714792A - Fluorescent anti-counterfeiting film and preparation method and application thereof - Google Patents
Fluorescent anti-counterfeiting film and preparation method and application thereof Download PDFInfo
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- CN114714792A CN114714792A CN202210201937.XA CN202210201937A CN114714792A CN 114714792 A CN114714792 A CN 114714792A CN 202210201937 A CN202210201937 A CN 202210201937A CN 114714792 A CN114714792 A CN 114714792A
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- B42D25/00—Information-bearing cards or sheet-like structures characterised by identification or security features; Manufacture thereof
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses a fluorescent anti-counterfeiting film and a preparation method and application thereof. The fluorescent anti-counterfeiting film comprises nanofibers and nitrogen-doped carbon quantum dots, wherein the nanofibers are interwoven into a film, and the nitrogen-doped carbon quantum dots are attached to the surfaces of the nanofibers. The preparation method of the fluorescent anti-counterfeiting film comprises the following steps: dispersing the nano-fiber and the amino acid in a solvent, carrying out microwave reaction, dialyzing in water, and carrying out suction filtration to obtain the fluorescent anti-counterfeiting film. The fluorescent anti-counterfeiting film disclosed by the invention has the advantages of high luminous intensity, good stability, high mechanical strength and the like, is simple in preparation process, green and environment-friendly, and has wide application prospects in the technical field of fluorescent anti-counterfeiting.
Description
Technical Field
The invention relates to the technical field of anti-counterfeiting films, in particular to a fluorescent anti-counterfeiting film and a preparation method and application thereof.
Background
The anti-fake technology is a measure for the user to distinguish true from false for anti-fake purpose and has wide application. The traditional anti-counterfeiting technologies such as scratch-off, bar codes and watermarks generally have the problems of single mode, easiness in counterfeiting and the like, and are not high in safety, and the advanced anti-counterfeiting technologies such as radio frequency identification and laser holography have the problems of high cost and are greatly limited in application although the advanced anti-counterfeiting technologies are high in safety. In recent years, fluorescent anti-counterfeiting technology becomes the leading edge and hot spot of research, and fluorescent anti-counterfeiting films are important materials in the field of fluorescent anti-counterfeiting. At present, common fluorescent anti-counterfeiting films are mainly prepared by printing fluorescent ink on the surface of the existing film material, and the luminescence of the fluorescent ink is realized by toxic fluorescent pigments, so that the fluorescent anti-counterfeiting films are harmful to human bodies and pollute the environment.
Therefore, the development of the fluorescent anti-counterfeiting film with good fluorescent effect, no toxicity, no harm, green and environmental protection is of great significance.
Disclosure of Invention
The invention aims to provide a fluorescent anti-counterfeiting film and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
a fluorescent anti-counterfeiting film comprises nanofibers and nitrogen-doped carbon quantum dots; the nanofibers are interwoven into a film; the nitrogen-doped carbon quantum dots are attached to the surfaces of the nanofibers.
Preferably, the nanofiber is selected from at least one of cellulose nanofibrils, cellulose nanocrystals, bacterial cellulose.
Preferably, the length of the nanofiber is 100nm to 500 nm.
The preparation method of the fluorescent anti-counterfeiting film comprises the following steps: dispersing the nano-fiber and the amino acid in a solvent, carrying out microwave reaction, dialyzing in water, and carrying out suction filtration to obtain the fluorescent anti-counterfeiting film.
Preferably, the mass ratio of the nano fibers to the amino acid is 1: 0.25-4.00.
Preferably, the amino acid is at least one selected from histidine, leucine, alanine, lysine, glutamic acid and threonine. And the amino acid is used as a carbon-nitrogen source and is used for preparing the nitrogen-doped carbon quantum dot.
Preferably, the dispersion mode is ultrasonic dispersion, and the time of the ultrasonic dispersion is 15 min-30 min.
Preferably, the solvent is water.
Preferably, the microwave reaction is carried out under the conditions that the microwave power is 500W-800W and the temperature is 100 ℃ to 105 ℃, and the reaction time is 2min to 10 min.
Preferably, the molecular weight cut-off of the dialysis bag used for dialysis is 500D-1000D.
Preferably, the dialysis time is 24-72 h, and the water changing interval is 6-12 h.
The fluorescent anti-counterfeiting material comprises the fluorescent anti-counterfeiting film.
The action mechanism of the invention is as follows: the invention takes the nano fiber as a carrier, nitrogen-doped carbon quantum dots are attached to the nano fiber and then manufactured into a film, the film system has better stability, the coagulation and sedimentation of the nitrogen-doped carbon quantum dots are avoided, the nitrogen-doped carbon quantum dots in the manufactured fluorescent anti-counterfeiting film can absorb the energy of light to be excited after being irradiated by ultraviolet light, and when the lowest vibration energy level transition of a first electronic excitation state is reduced to different vibration energy levels of a ground state, the film is emitted in a light form to generate a fluorescence phenomenon.
The invention has the beneficial effects that: the fluorescent anti-counterfeiting film disclosed by the invention has the advantages of high luminous intensity, good stability, high mechanical strength and the like, is simple in preparation process, green and environment-friendly, and has wide application prospects in the technical field of fluorescent anti-counterfeiting.
Specifically, the method comprises the following steps:
1) the fluorescent anti-counterfeiting film has the advantages of uniformity, stability, high mechanical strength, strong fluorescent light-emitting effect and the like, and meets the performance standard of related industries;
2) the fluorescent anti-counterfeiting film has high fluorescence intensity and good color rendering property, has obvious fluorescent light-emitting effect when being used for detecting anti-counterfeiting, and is convenient for direct observation;
3) the preparation process of the fluorescent anti-counterfeiting film is convenient and rapid, no organic solvent is volatilized, and the prepared product does not contain radioactive elements, is nontoxic and harmless to the environment and human bodies, and is green and environment-friendly.
Drawings
FIG. 1 is an appearance picture of the fluorescent security film and the pure nanofiber film of example 1 under the irradiation of a fluorescent lamp.
FIG. 2 is a picture of the appearance of the fluorescent security film and the pure nanofiber film of example 1 under the irradiation of an ultraviolet lamp.
FIG. 3 is an SEM image of the fluorescent security film of example 1.
FIG. 4 is a graph showing the effect of the fluorescent anti-counterfeit film of example 1 covering the surface of the picture with patterns.
FIG. 5 is a UV-VIS spectrum of the fluorescent security film of example 1.
FIG. 6 is a fluorescence spectrum of the fluorescent security film of example 1.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a fluorescent anti-counterfeiting film is prepared by the following steps:
adding 1g of cellulose nanofibrils (the length is 100 nm-500 nm) and 4g of histidine into 10mL of deionized water, placing the mixture into a KH3200E ultrasonic cleaner (Kunshan standing grass ultrasonic instruments, Inc.) for ultrasonic treatment for 30min, transferring the obtained mixture into an XH100B microwave catalytic synthesis/extraction instrument (Beijing Xiangkun scientific and technological development, Inc.), setting the reaction power to be 800W and the reaction time to be 10min, automatically recording the heat preservation time when the temperature reaches 100 ℃, reacting for 4min, transferring the reaction product into a dialysis bag (the molecular weight is intercepted 500D), dialyzing the product with water for 36h, changing water once during the period of 12h, performing vacuum filtration by using an SHZ-D (III) circulating water type vacuum pump (Jianyi Cihua instruments, Inc.), placing the product into a 101 type electrothermal blowing drying box (Tongzhou Branch of Shanghai Jinyan instruments, Inc.), the fluorescent anti-counterfeiting film is obtained.
And (3) performance testing:
1) the appearance pictures of the fluorescent anti-counterfeiting film and the pure nanofiber film (obtained by adding water to cellulose nanofibrils, performing ultrasonic dispersion and then performing vacuum filtration) under the irradiation of the fluorescent lamp in the embodiment are as shown in fig. 1(a is the fluorescent anti-counterfeiting film, and b is the pure nanofiber film), and are shown in the ultraviolet lamp (shenzhen luvor electromechanical limited company, model number: RW-UVA type) as shown in fig. 2(a is a fluorescent security film and b is a pure nanofiber film).
As can be seen from fig. 1: the pure nanofiber film is colorless and transparent, while the fluorescent anti-counterfeiting film of the embodiment is yellow and transparent, which is related to the color of the nitrogen-doped carbon quantum dots.
As can be seen from fig. 2: the fluorescent anti-counterfeiting film of the embodiment shows bright blue fluorescence under ultraviolet light, and the pure nanofiber film has no fluorescence phenomenon.
2) The Scanning Electron Microscope (SEM) image of the fluorescent anti-counterfeiting film of the present example is shown in fig. 3 (tested by using an EVO 18 thermal field emission SEM).
As can be seen from fig. 3: the surface of the fluorescent anti-counterfeiting film of the embodiment is relatively flat, and only a few raised nano fibers can be observed.
3) The effect graph of the fluorescent anti-counterfeiting film covered on the surface of the picture with the pattern is shown in fig. 4.
As can be seen from fig. 4: the fluorescent anti-counterfeiting film has good transparency, and patterns in pictures below the film can be clearly seen.
4) The ultraviolet-visible spectrum of the fluorescent anti-counterfeiting film of the embodiment (the detection of the ultraviolet-visible spectrum adopts a carry 60 ultraviolet-visible spectrophotometer) is shown in fig. 5.
As can be seen from fig. 5: the peak at 230nm is assigned to the pi → pi transition absorption peak of C-C bond, the peak at 275nm is assigned to the n → pi transition absorption peak of C-O bond, and the chemical bonds corresponding to the two peaks are the main reasons that the carbon quantum dots can generate fluorescence after absorbing ultraviolet light.
5) The fluorescence spectrum of the fluorescent anti-counterfeiting film of the embodiment (fluorescence spectrum detection adopts a FluoroMax-4 fluorescence spectrometer) is shown in FIG. 6.
As can be seen from fig. 6: the maximum emission wavelength of the nitrogen-doped carbon quantum dots in the fluorescent anti-counterfeiting film of the embodiment is 430nm under the excitation wavelength of 365nm, and the emission peak is wide, which indicates that the fluorescent anti-counterfeiting film of the embodiment can exhibit a color development effect in a wide wavelength range.
6) The fluorescent anti-counterfeiting film of the embodiment is stored and kept stand for 10 days at room temperature, the state of the film is observed and detected, and the film is tested to find that the film has no abnormal conditions such as discoloration, curling and the like.
Example 2:
a fluorescent anti-counterfeiting film is prepared by the following steps:
adding 1g of cellulose nanofibrils (the length is 100 nm-500 nm) and 2.33g of leucine into 10mL of deionized water, placing the mixture into a KH3200E ultrasonic cleaner (Kunshan cereal ultrasonic apparatus Limited) for ultrasonic treatment for 25min, transferring the obtained mixture into an XH100B microwave catalytic synthesis/extraction apparatus (Beijing Xiangkun scientific and technological development Limited), setting the reaction power to be 800W and the reaction time to be 10min, automatically recording the heat preservation time when the temperature reaches 100 ℃, reacting for 4min, transferring the reaction product into a dialysis bag (the molecular weight cut-off is 500D), dialyzing the product with water for 24h, changing water once during the period of 8h, performing vacuum filtration by using an SHZ-D (III) circulating water type vacuum pump (Hiziwa apparatus Limited), placing the product into a 101 type electrothermal blowing drying box (Tongzhou division of Shanghai Jinyan apparatus Instrument Limited), thus obtaining the fluorescent anti-counterfeiting film.
Through tests (the test method is the same as that of the example 1), the appearance, the transparency, the color generation effect under an ultraviolet lamp, the ultraviolet-visible light spectrum, the fluorescence spectrum and the storage stability of the fluorescent anti-counterfeiting film of the example are similar to those of the fluorescent anti-counterfeiting film of the example 1.
Example 3:
a fluorescent anti-counterfeiting film is prepared by the following steps:
adding 1g of cellulose nanofibrils (the length is 100 nm-500 nm) and 4g of alanine into 10mL of deionized water, placing the mixture into a KH3200E ultrasonic cleaner (Kunshan standing grain ultrasonic apparatus Co., Ltd.) for ultrasonic treatment for 20min, transferring the obtained mixture into an XH100B microwave catalytic synthesis/extraction apparatus (Beijing Xiangkun scientific and technological development Co., Ltd.), setting the reaction power to be 800W and the reaction time to be 10min, automatically recording the heat preservation time when the temperature reaches 100 ℃, reacting for 4min, transferring the reaction product into a dialysis bag (the molecular weight is intercepted 1000D), dialyzing the product with water for 48h, changing water once during the period of 8h, performing vacuum filtration by using an SHZ-D (III) circulating water type vacuum pump (Jiancheng Hua apparatus Co., Ltd.), and placing the product into a 101 type electrothermal blowing drying box (Tongzhou Suo Branch of Shanghai Jinyan apparatus Co., Ltd.) for drying, the fluorescent anti-counterfeiting film is obtained.
Through tests (the test method is the same as that of the example 1), the appearance, the transparency, the color generation effect under an ultraviolet lamp, the ultraviolet-visible light spectrum, the fluorescence spectrum and the storage stability of the fluorescent anti-counterfeiting film of the example are similar to those of the fluorescent anti-counterfeiting film of the example 1.
Example 4:
a fluorescent anti-counterfeiting film is prepared by the following steps:
adding 10g of cellulose nanocrystals (with the length of 100 nm-500 nm) and 2.33g of lysine into 10mL of deionized water, placing the mixture in a KH3200E ultrasonic cleaner (Kunshan grass ultrasonic instruments, Inc.) for ultrasonic treatment for 20min, transferring the obtained mixture into an XH100B microwave catalytic synthesis/extraction apparatus (Beijing Xiangkun scientific and technological development, Inc.), setting the reaction power to be 800W and the reaction time to be 10min, automatically recording the heat preservation time when the temperature reaches 100 ℃, reacting for 5min, transferring the reaction product into a dialysis bag (with the molecular weight cutoff of 500D), dialyzing the product with water for 36h, changing water once during the period of 12h, performing vacuum filtration by using an SHZ-D (III) circulating water type vacuum pump (Hiziwa instruments, Inc.), placing the product into a 101 type electrothermal blowing drying box (Tongzhou Branch of Shanghai Jinyan instruments, Inc.), the fluorescent anti-counterfeiting film is obtained.
Through tests (the test method is the same as that of the example 1), the appearance, the transparency, the color generation effect under an ultraviolet lamp, the ultraviolet-visible light spectrum, the fluorescence spectrum and the storage stability of the fluorescent anti-counterfeiting film of the example are similar to those of the fluorescent anti-counterfeiting film of the example 1.
Example 5:
a fluorescent anti-counterfeiting film is prepared by the following steps:
adding 1g of cellulose nanocrystals (with the length of 100 nm-500 nm) and 1.5g of glutamic acid into 10mL of deionized water, placing the mixture in a KH3200E ultrasonic cleaner (Kunshan standing grass ultrasonic apparatus Co., Ltd.) for ultrasonic treatment for 30min, transferring the obtained mixture into an XH100B microwave catalytic synthesis/extraction apparatus (Beijing Xiangkun scientific and technological development Co., Ltd.), setting the reaction power to 800W and the reaction time to 10min, automatically recording the heat preservation time when the temperature reaches 100 ℃, reacting for 4min, transferring the reaction product into a dialysis bag (with the molecular weight cutoff of 1000D), dialyzing with water for 48h, changing water once during the period of 12h, performing vacuum filtration by using an SHZ-D (III) circulating water type vacuum pump (Otsuwa apparatus Co., Ltd.), and drying in a 101 type electrothermal blowing drying box (Tongzhou division, Shanghai Jinyan apparatus Co., Ltd.), the fluorescent anti-counterfeiting film is obtained.
Through tests (the test method is the same as that of the example 1), the appearance, the transparency, the color generation effect under an ultraviolet lamp, the ultraviolet-visible light spectrum, the fluorescence spectrum and the storage stability of the fluorescent anti-counterfeiting film of the example are similar to those of the fluorescent anti-counterfeiting film of the example 1.
Example 6:
a fluorescent anti-counterfeiting film is prepared by the following steps:
adding 1g of bacterial cellulose (the length is 200 nm-300 nm) and 1g of threonine into 10mL of deionized water, placing the mixture into a KH3200E ultrasonic cleaner (Kunshan grass ultrasonic instruments, Inc.) for ultrasonic treatment for 20min, transferring the obtained mixture into an XH100B microwave catalytic synthesis/extraction instrument (Beijing Xiangkun scientific and technological development, Inc.), setting the reaction power to 800W and the reaction time to 10min, automatically recording the heat preservation time when the temperature reaches 100 ℃, reacting for 6min, transferring the reaction product into a dialysis bag (the molecular weight cut-off is 500D), dialyzing the product with water for 36h, changing the water once during the period of 8h, performing vacuum filtration by using an SHZ-D (III) circulating water type vacuum pump (consolidation Yuanhua instruments, Inc.), placing the product into a 101 type electrothermal blowing drying box (Shanghai Jinyan instruments, Inc. Tongzhou Branch Co., Ltd.) and drying the product, thus obtaining the fluorescent anti-counterfeiting film.
Through tests (the test method is the same as that of the example 1), the appearance, the transparency, the color generation effect under an ultraviolet lamp, the ultraviolet-visible light spectrum, the fluorescence spectrum and the storage stability of the fluorescent anti-counterfeiting film of the example are similar to those of the fluorescent anti-counterfeiting film of the example 1.
Example 7:
a fluorescent anti-counterfeiting film is prepared by the following steps:
adding 1g of bacterial cellulose (the length is 200 nm-300 nm) and 4g of histidine into 10mL of deionized water, placing the mixture in a KH3200E ultrasonic cleaner (Kunshan grass ultrasonic instrument, Inc.) for ultrasonic treatment for 30min, transferring the obtained mixture into an XH100B microwave catalytic synthesis/extraction instrument (Beijing Xiangkun scientific and technological development, Inc.), setting the reaction power to 800W and the reaction time to 10min, automatically recording the heat preservation time when the temperature reaches 100 ℃, reacting for 6min, transferring the reaction product into a dialysis bag (the molecular weight cut-off is 1000D), dialyzing with water for 24h, changing water once during the period of 6h, performing vacuum filtration by using an SHZ-D (III) circulating water type vacuum pump (consolidation Yuanhua instruments, Inc.), placing the mixture into a 101 type electrothermal blowing drying box (Shanghai Jinyan instruments, Inc. Tongzhou Branch), thus obtaining the fluorescent anti-counterfeiting film.
Through tests (the test method is the same as that of the example 1), the appearance, the transparency, the color generation effect under an ultraviolet lamp, the ultraviolet-visible light spectrum, the fluorescence spectrum and the storage stability of the fluorescent anti-counterfeiting film of the example are similar to those of the fluorescent anti-counterfeiting film of the example 1. Test example:
the tensile strength of the fluorescent anti-counterfeiting films of examples 1 to 7 was tested by using an INSTRON 5565 tensile compression material testing machine, and the test results are shown in the following table:
TABLE 1 tensile Strength test results of fluorescent anti-counterfeiting films of examples 1 to 7
As can be seen from Table 1: the fluorescent anti-counterfeiting films of examples 1 to 7 all had tensile strength of more than 40MPa, high mechanical strength and excellent mechanical properties.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A fluorescent anti-counterfeiting film is characterized by comprising nanofibers and nitrogen-doped carbon quantum dots; the nano-fibers are interwoven into a film shape; the nitrogen-doped carbon quantum dots are attached to the surfaces of the nanofibers.
2. The fluorescent security film of claim 1, wherein: the nano-fiber is selected from at least one of cellulose nano-fibril, cellulose nano-crystal and bacterial cellulose.
3. The fluorescent security film according to claim 1 or 2, wherein: the length of the nano fiber is 100 nm-500 nm.
4. The preparation method of the fluorescent anti-counterfeiting film according to any one of claims 1 to 3, which is characterized by comprising the following steps: dispersing the nano-fiber and the amino acid in a solvent, carrying out microwave reaction, dialyzing in water, and carrying out suction filtration to obtain the fluorescent anti-counterfeiting film.
5. The method for preparing a fluorescent anti-counterfeiting film according to claim 4, characterized in that: the mass ratio of the nano fibers to the amino acid is 1: 0.25-4.00.
6. The method for preparing the fluorescent anti-counterfeiting film according to claim 4 or 5, characterized in that: the dispersion mode is ultrasonic dispersion, and the ultrasonic dispersion time is 15-30 min.
7. The method for preparing the fluorescent anti-counterfeiting film according to claim 4 or 5, characterized in that: the microwave reaction is carried out under the conditions that the microwave power is 500W-800W and the temperature is 100 ℃ to 105 ℃, and the reaction time is 2min to 10 min.
8. The method for preparing the fluorescent anti-counterfeiting film according to claim 4 or 5, characterized in that: the molecular weight cut-off of the dialysis bag adopted by dialysis is 500D-1000D.
9. The method for preparing the fluorescent anti-counterfeiting film according to claim 4 or 5, characterized in that: the dialysis time is 24-72 h, and the water changing interval is 6-12 h.
10. The use of the fluorescent anti-counterfeiting film according to any one of claims 1 to 3 in the preparation of fluorescent anti-counterfeiting materials.
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| CN112697757A (en) * | 2020-12-10 | 2021-04-23 | 浙江理工大学 | Preparation method of fluorescent sensor for Cr (VI) instant detection and product thereof |
| CN113338076A (en) * | 2021-06-03 | 2021-09-03 | 华南理工大学 | Detection paper containing nitrogen-doped carbon quantum dots and preparation method and application thereof |
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