CN114752257A - Carbon quantum dot fluorescent anti-counterfeiting ink and preparation method and application thereof - Google Patents
Carbon quantum dot fluorescent anti-counterfeiting ink and preparation method and application thereof Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
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Abstract
The invention belongs to the technical field of fluorescent ink, and particularly relates to carbon quantum dot fluorescent anti-counterfeiting ink as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) weighing anhydrous citric acid, diethylenetriamine and acrylamide, adding deionized water, and ultrasonically mixing. (2) Transferring the solution into a reaction kettle for hydrothermal reaction, and naturally cooling to room temperature; (3) and (3) centrifuging the product obtained in the step (2), taking supernatant, and dialyzing to obtain the fluorescent carbon quantum dot solution. Freeze drying to obtain solid powder, and dispersing in water solution to obtain the fluorescent ink. The raw material acrylamide can generate Polyacrylamide (PAM) with thickening property and surface activity, so that the surface tension of the liquid is reduced, the printability of the carbon quantum dot fluorescent ink on a fiber paper base is good, patterning is realized through an ink-jet printing technology, the prepared anti-counterfeiting pattern is good in stability, and the anti-counterfeiting ink can be well applied to the field of tobacco anti-counterfeiting packaging.
Description
Technical Field
The invention relates to the technical field of anti-counterfeiting materials, in particular to carbon quantum dot fluorescent anti-counterfeiting ink and a preparation method and application thereof.
Background
Counterfeiting is a widespread problem that poses a threat to individuals and society. It may have a significant negative impact on the public and even worsen economic growth through the distribution of illegal or counterfeit goods, documents and currency. Thus, counterfeiting can have serious environmental, health, economic and social impacts.
The fluorescent printing technology based on the anti-counterfeiting ink has wide application in the anti-counterfeiting aspect, and common fluorescent substances comprise organic luminescent dyes, semiconductor quantum dots, rare earth luminescent materials and the like. However, the preparation process of these materials is complex, the post-treatment is cumbersome, and the semiconductor quantum dots contain heavy metals such as lead and cadmium, which can affect the environment. The carbon quantum dots are novel environment-friendly carbon nano materials with unique optical properties discovered in recent years, can emit visible light under the irradiation of ultraviolet light, and have the advantages of environmental friendliness, low cost, excellent chemical stability and the like.
Most tobacco packing boxes are fiber paper-based materials and have a porous net structure, and carbon quantum dot ink can be relatively uniformly dispersed on fibers along with the penetration and spreading of liquid drops, so that a bright fluorescent effect is generated. However, the traditional carbon quantum dot solution has poor adhesion on the fiber paper base, and is easy to cause phase separation phenomenon, so that the anti-counterfeiting effect is lost. Patent publication No. CN 112391086A discloses a technical scheme of placing carbon quantum dot reaction suspension and cellulose paper into a reaction kettle together, using diethylenetriamine as a cellulose activator, and reacting to obtain fluorescent paper, but the technical scheme can only obtain paper with fluorescence, cannot form a specific fluorescent pattern on the paper, has poor anti-counterfeiting effect and is difficult to produce on a large scale.
Disclosure of Invention
In order to solve the problems that the traditional carbon quantum dot solution in the prior art has poor adhesion on a fiber paper base, is easy to generate phase separation phenomenon so as to lose anti-counterfeiting effect, and fluorescent patterns cannot be set at will, the invention aims to provide a preparation method of carbon quantum dot fluorescent anti-counterfeiting ink.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of carbon quantum dot fluorescent anti-counterfeiting ink comprises the following steps:
the preparation method of the fluorescent anti-counterfeiting ink as the carbon quantum dot is further improved:
(1) weighing anhydrous citric acid, diethylenetriamine and acrylamide, adding into water, and ultrasonically mixing uniformly;
(2) transferring the solution into a reaction kettle for hydrothermal reaction, and naturally cooling to room temperature;
(3) centrifuging the product obtained in the step (2), taking supernatant, and dialyzing to obtain a fluorescent carbon quantum dot solution;
(4) and (4) carrying out freeze drying treatment on the carbon quantum dot solution obtained in the step (3) to obtain solid powder, and dispersing the solid powder into water to obtain the carbon quantum dot fluorescent anti-counterfeiting ink.
Preferably, the mixing ratio of the anhydrous citric acid, the diethylenetriamine and the acrylamide in the step (1) to the water is 1g (1-5 ml) to 1-10 g (20-40 ml).
Preferably, the ultrasonic mixing conditions in step (1) are as follows: the power is 70-100W, and the time is 10-30 min.
Preferably, the temperature of the hydrothermal reaction in the step (2) is 100-200 ℃ and the time is 4-12 h.
Preferably, the reaction kettle in the step (2) is a polytetrafluoroethylene reaction kettle.
Preferably, the speed of the centrifugal treatment in the step (3) is 5000-10000 rpm, and the time is 5-15 min.
Preferably, a dialysis bag with the molecular weight cutoff of 500-3000 Da is adopted for dialysis in the step (3), and the dialysis time is 12-48 h.
Preferably, the temperature of the freeze-drying treatment in the step (4) is-35 to-45 ℃, and the time is 24 to 48 hours.
Preferably, the solid powder in step (4) is dispersed in water at a ratio of 1-10 mg/ml.
The invention also aims to provide the carbon quantum dot fluorescent anti-counterfeiting ink prepared by any one of the preparation methods.
The invention also aims to provide the application of the carbon quantum dot fluorescent anti-counterfeiting ink in printing of the tobacco anti-counterfeiting package.
Compared with the prior art, the invention has the beneficial effects that:
1) according to the invention, a water-soluble fluorescent product is obtained by a one-step hydrothermal method, the carbon quantum dot fluorescent ink is prepared firstly, and then the carbon quantum dot fluorescent ink is printed on the fiber paper base in an ink-jet printing mode, so that any desired fluorescent pattern can be printed, one paper and one code can be realized by a two-dimensional code technology, and the anti-counterfeiting effect is strong. The product can emit blue visible light under the excitation of ultraviolet light and has good stability. Diluted to a certain concentration and used as fluorescent ink.
In the scheme, diethylenetriamine is used as a nitrogen source to be doped into a system, -NH2Is beneficial to dehydration and carbonization among molecules and improves the fluorescence intensity. The pattern printed onto the fibrous paper base appeared bright blue fluorescence under uv light.
The added acrylamide generates Polyacrylamide (PAM) under the high temperature condition of 100-200 ℃, and the polyacrylamide plays a role in thickening the solution in the system on one hand, so that the carbon quantum dots are better attached to the fiber paper base; on the other hand, the surface activity of the carbon quantum dot solution is improved, the surface tension of the liquid is reduced, and the carbon quantum dot solution uniformly permeates into the cellulose-based paper, so that the phenomenon of phase separation after a period of time is avoided. The carbon quantum dot solution prepared by the raw materials without acrylamide is unstable and turns into green after being placed for 24-48 h. The carbon quantum dot fluorescent ink has good printability and good stability on the fiber paper base. The prepared fluorescent ink is printed on a tobacco packaging box, and printed characters or patterns can be clearly seen under sunlight after the tobacco packaging box is placed for 24-48 hours.
3) The raw materials of the fluorescent ink are low in cost and easy to obtain, and the prepared fluorescent ink has strong fluorescence and stability. The preparation process is simple, green and low in cost, and is suitable for large-scale production. The carbon quantum dot fluorescent ink prepared by the invention has good printability on a fiber paper base, and provides a new way for carrying out effective and safe anti-counterfeiting marking on packages such as tobacco and the like.
Drawings
FIG. 1 is a photograph of fluorescent ink prepared in example 1 of the present invention under sunlight (a) and ultraviolet light (b).
Fig. 2 is a fluorescence spectrum of the carbon quantum dot solution prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative effort based on the embodiments of the present invention belong to the protection scope of the present invention.
Comparative example 1
A preparation method of carbon quantum dot fluorescent anti-counterfeiting ink specifically comprises the following steps:
1) weighing 1g of anhydrous citric acid and 1ml of diethylenetriamine, dissolving the anhydrous citric acid and the 1ml of diethylenetriamine in 30ml of deionized water, performing ultrasonic dispersion for 20min under the power of 80W to obtain a mixed solution, then putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene inner container, placing the stainless steel reaction kettle in an oven at the temperature of 180 ℃ for hydrothermal reaction for 6h, and after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the reaction kettle to obtain the carbon quantum dot solution.
2) Transferring the carbon quantum dot solution in the reaction kettle into a centrifuge tube, centrifuging for 15min at the rotating speed of 8000r/min, and taking out the supernatant. Soaking a dialysis bag with molecular weight cutoff of 1000Da in deionized water for 10min, adding the supernatant obtained by centrifugation into the dialysis bag, dialyzing for 24h, and changing water every 4 h. And (4) freeze-drying the dialyzed solution at-35 ℃ for 24h to obtain the powdery carbon quantum dots.
3) And then adding the powdery carbon quantum dots into deionized water according to the proportion of 1g/1000ml to prepare the fluorescent anti-counterfeiting ink.
4) The anti-counterfeiting ink is added into a replaceable ink box of an ink-jet printer by a needle tube, the printer is connected with a computer, characters and patterns to be printed are designed, and the characters and the patterns are printed on the tobacco packaging box by the ink-jet printer.
In this comparative example a two-dimensional code is printed which can be linked to the corresponding content by a wechat scan. The printing content can not be seen under the sunlight, can be seen only by the ultraviolet irradiation, and can be observed on the packaging box under the sunlight after 24 hours, which indicates that the fluorescent anti-counterfeiting ink prepared by the comparative example has poor stability.
Example 1
A preparation method of carbon quantum dot fluorescent anti-counterfeiting ink specifically comprises the following steps:
1) weighing 1g of anhydrous citric acid, 1ml of diethylenetriamine and 2g of acrylamide, dissolving the anhydrous citric acid, the diethylenetriamine and the acrylamide in 30ml of deionized water, performing ultrasonic dispersion for 20min under the power of 80W to obtain a mixed solution, then putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene inner container, putting the stainless steel reaction kettle in an oven at the temperature of 180 ℃, performing hydrothermal reaction for 6h, naturally cooling to room temperature after the reaction is finished, and taking out the reaction kettle to obtain a carbon quantum dot solution.
2) Transferring the carbon quantum dot solution in the reaction kettle into a centrifuge tube, centrifuging for 15min at the rotating speed of 8000r/min, and taking out the supernatant. Soaking a dialysis bag with molecular weight cutoff of 1000Da in deionized water for 10min, adding the supernatant obtained by centrifugation into the dialysis bag, dialyzing for 24h, and changing water every 4 h. And (3) freeze-drying the dialyzed solution at-35 ℃ for 24 hours to obtain the powdery carbon quantum dots.
3) And then adding the powdery carbon quantum dots into deionized water according to the proportion of 1g/1000ml to prepare the fluorescent anti-counterfeiting ink.
4) The anti-counterfeiting ink is added into a replaceable ink box of an ink-jet printer by a needle tube, the printer is connected with a computer, characters and patterns to be printed are designed, and the characters and the patterns are printed on the tobacco packaging box by the ink-jet printer.
In this embodiment, a two-dimensional code is printed out, and the two-dimensional code can be linked to corresponding content by scanning the WeChat. The printed content is invisible under sunlight, can be seen only by ultraviolet irradiation, and has good stability and lasting fluorescence effect.
Example 2
A preparation method of carbon quantum dot fluorescent anti-counterfeiting ink specifically comprises the following steps:
1) weighing 1g of anhydrous citric acid, 1ml of diethylenetriamine and 2g of acrylamide, dissolving the citric acid, the diethylenetriamine and the acrylamide in 30ml of deionized water, performing ultrasonic dispersion for 20min under the power of 80W to obtain a mixed solution, then putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene inner container, placing the stainless steel reaction kettle in an oven at the temperature of 180 ℃ for hydrothermal reaction for 4h, and after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the reaction kettle to obtain the carbon quantum dot solution.
2) Transferring the carbon quantum dot solution in the reaction kettle into a centrifuge tube, centrifuging for 15min at the rotating speed of 8000r/min, and taking out the supernatant. Soaking a dialysis bag with molecular weight cutoff of 1000Da in deionized water for 10min, adding the supernatant obtained by centrifugation into the dialysis bag, dialyzing for 24h, and changing water every 4 h. And (4) freeze-drying the dialyzed solution at-35 ℃ for 24h to obtain the powdery carbon quantum dots.
3) And then adding the powdery carbon quantum dots into deionized water according to the proportion of 1g/1000ml to prepare the fluorescent anti-counterfeiting ink.
4) The anti-counterfeiting ink is added into a replaceable ink box of an ink-jet printer by a needle tube, the printer is connected with a computer, characters and patterns to be printed are designed, and the characters and the patterns are printed on the tobacco packaging box by the ink-jet printer.
In this embodiment, a two-dimensional code is printed out, and the two-dimensional code can be linked to corresponding content by scanning the WeChat. The printed content is invisible under sunlight, can be seen only by ultraviolet irradiation, and has good stability. Compared with example 1, the brightness of the pattern fluorescence under ultraviolet light is slightly reduced, mainly because the hydrothermal reaction time in step 1) is short and the carbonization of organic molecules in the solution is incomplete.
Example 3
In this embodiment, the carbon quantum dot fluorescent anti-counterfeiting ink is prepared by the following steps:
1) weighing 1g of anhydrous citric acid, 1ml of diethylenetriamine and 2g of acrylamide, dissolving the anhydrous citric acid, the diethylenetriamine and the acrylamide in 30ml of deionized water, performing ultrasonic dispersion for 20min under the power of 80W to obtain a mixed solution, then putting the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene inner container, putting the stainless steel reaction kettle in an oven at the temperature of 180 ℃, performing hydrothermal reaction for 8h, naturally cooling to room temperature after the reaction is finished, and taking out the reaction kettle to obtain a carbon quantum dot solution.
2) Transferring the carbon quantum dot solution in the reaction kettle into a centrifuge tube, centrifuging for 15min at the rotating speed of 8000r/min, and taking out the supernatant. Soaking a dialysis bag with molecular weight cutoff of 1000Da in deionized water for 10min, adding the supernatant obtained by centrifugation into the dialysis bag, dialyzing for 24h, and changing water every 4 h. And (4) freeze-drying the dialyzed solution at-35 ℃ for 24h to obtain the powdery carbon quantum dots.
3) And then adding the powdery carbon quantum dots into deionized water according to the proportion of 1g/1000ml to prepare the fluorescent anti-counterfeiting ink.
4) The anti-counterfeiting ink is added into a replaceable ink box of an ink-jet printer by a needle tube, the printer is connected with a computer, characters and patterns to be printed are designed, and the characters and the patterns are printed on the tobacco packaging box by the ink-jet printer.
In this embodiment, a two-dimensional code is printed and scanned by a wechat to link to the corresponding content. The printed content is invisible under sunlight, can be seen only by ultraviolet irradiation, and has good stability. The pattern fluorescence under uv light was slightly less bright than in example 1, mainly because the hydrothermal reaction time in step 1) was long and the solution had already started to form graphitized carbon nuclei.
It should be understood by those skilled in the art that the foregoing is only illustrative of several embodiments of the invention, and not of all embodiments. It should be noted that many variations and modifications are possible to those skilled in the art, and all variations and modifications that do not depart from the gist of the invention are intended to be within the scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of carbon quantum dot fluorescent anti-counterfeiting ink is characterized by comprising the following steps:
(1) weighing anhydrous citric acid, diethylenetriamine and acrylamide, adding into water, and ultrasonically mixing uniformly;
(2) transferring the solution into a reaction kettle for hydrothermal reaction, and naturally cooling to room temperature;
(3) centrifuging the product obtained in the step (2), taking supernatant, and dialyzing to obtain a fluorescent carbon quantum dot solution;
(4) and (4) carrying out freeze drying treatment on the carbon quantum dot solution obtained in the step (3) to obtain solid powder, and dispersing the solid powder into water to obtain the carbon quantum dot fluorescent anti-counterfeiting ink.
2. The method for preparing the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 1, wherein the mixing ratio of the anhydrous citric acid, the diethylenetriamine and the acrylamide to the water in the step (1) is 1g (1-5 ml) to 1-10 g (20-40 ml).
3. The preparation method of the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 1, wherein the ultrasonic mixing conditions in the step (1) are as follows: the power is 70-100W, and the time is 10-30 min.
4. The preparation method of the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 1, wherein the temperature of hydrothermal reaction in the step (2) is 100-200 ℃ and the time is 4-12 h.
5. The method for preparing the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 1, wherein the speed of the centrifugal treatment in the step (3) is 5000-10000 rpm, and the time is 5-15 min.
6. The preparation method of the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 1, wherein a dialysis bag with the molecular weight cutoff of 500-3000 Da is adopted in dialysis in the step (3), and the dialysis time is 12-48 h.
7. The preparation method of the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 1, wherein the temperature of the freeze-drying treatment in the step (4) is-35 to-45 ℃, and the time is 24 to 48 hours.
8. The method for preparing the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 1, wherein the solid powder in the step (4) is dispersed in water according to the proportion of 1-10 mg/ml.
9. A carbon quantum dot fluorescent anti-counterfeiting ink prepared by the preparation method of any one of claims 1 to 8.
10. Use of the carbon quantum dot fluorescent anti-counterfeiting ink according to claim 9 in printing of tobacco anti-counterfeiting packages.
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| CN115404074A (en) * | 2022-09-05 | 2022-11-29 | 南华大学 | Fluorescence detection nano probe, preparation method and application |
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