CN114108374A - Preparation method of carbon quantum dot fluorescent paper - Google Patents
Preparation method of carbon quantum dot fluorescent paper Download PDFInfo
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- CN114108374A CN114108374A CN202111039326.1A CN202111039326A CN114108374A CN 114108374 A CN114108374 A CN 114108374A CN 202111039326 A CN202111039326 A CN 202111039326A CN 114108374 A CN114108374 A CN 114108374A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 116
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- 239000001913 cellulose Substances 0.000 claims abstract description 72
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
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- 239000007864 aqueous solution Substances 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
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- 229920002873 Polyethylenimine Polymers 0.000 claims description 6
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- MJYQFWSXKFLTAY-OVEQLNGDSA-N (2r,3r)-2,3-bis[(4-hydroxy-3-methoxyphenyl)methyl]butane-1,4-diol;(2r,3r,4s,5s,6r)-6-(hydroxymethyl)oxane-2,3,4,5-tetrol Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O.C1=C(O)C(OC)=CC(C[C@@H](CO)[C@H](CO)CC=2C=C(OC)C(O)=CC=2)=C1 MJYQFWSXKFLTAY-OVEQLNGDSA-N 0.000 claims description 4
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims 2
- 235000017060 Arachis glabrata Nutrition 0.000 claims 1
- 244000105624 Arachis hypogaea Species 0.000 claims 1
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
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- 150000002910 rare earth metals Chemical class 0.000 description 1
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- 230000005476 size effect Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
Images
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/02—Material of vegetable origin
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/07—Nitrogen-containing compounds
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/14—Carboxylic acids; Derivatives thereof
- D21H17/15—Polycarboxylic acids, e.g. maleic acid
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
- D21H17/56—Polyamines; Polyimines; Polyester-imides
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- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/40—Agents facilitating proof of genuineness or preventing fraudulent alteration, e.g. for security paper
- D21H21/44—Latent security elements, i.e. detectable or becoming apparent only by use of special verification or tampering devices or methods
- D21H21/48—Elements suited for physical verification, e.g. by irradiation
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Abstract
The invention provides a preparation method of carbon quantum dot fluorescent paper, which specifically comprises the following steps: s1, preparing a carbon quantum dot reaction solution; s2, inverting the prepared carbon quantum dot reaction suspension liquid into a tetrafluoroethylene tank of a high-temperature high-pressure reaction kettle, soaking a cellulose paper base into the carbon quantum dot reaction suspension liquid, and then putting the high-temperature high-pressure reaction kettle into an oil bath kettle at 180 ℃ for keeping for 10 hours; and S3, after the reaction is finished, naturally cooling the high-temperature high-pressure reaction kettle to room temperature to obtain an intermediate paper sample, washing the intermediate paper sample for 3-4 times by using deionized water and absolute ethyl alcohol respectively, and then placing the intermediate paper sample in a forced air drying oven at 40 ℃ for drying for 2-8 hours to obtain the carbon quantum dot fluorescent paper. The preparation method of the carbon quantum dot fluorescent paper is simple in process, the carbon quantum dot fluorescent paper which has excellent fluorescence performance of the carbon quantum dots and also has flexibility and excellent mechanical properties of the cellulose base material can be prepared, the fluorescence intensity is high, and the anti-counterfeiting performance is excellent.
Description
Technical Field
The invention relates to a preparation method of fluorescent paper, in particular to a preparation method of carbon quantum dot fluorescent paper.
Background
The quantum dot is a tiny crystal with the particle size of 1-10 nm, and electrons and holes in the crystal structure of the quantum dot are limited by the size of a quantum, so that a unique discrete energy level structure can be generated under the action of exciting light with a specific wavelength to be excited to generate a photoluminescence phenomenon. The quantum size effect and the edge effect of the quantum dots enable the quantum dots to generate photoelectric properties related to crystal size, namely, the particle size of the quantum dots is regulated and controlled, so that the wavelength range of emitted light generating photoluminescence effect can cover a visible light region, and fluorescence of different colors can be emitted under the action of excitation light of different wavelengths. Although quantum dots have excellent fluorescent performance, most of the raw materials for preparing quantum dots contain cadmium, selenium and other elements, so that the quantum dots are high in toxicity, have great harm to the environment and human health, and do not accord with the national development concept of green and environment protection.
As a novel zero-dimensional fluorescent carbon nano material, the carbon quantum dot is green and environment-friendly because the carbon quantum dot does not contain high-toxicity heavy metals, and is a novel quantum dot material harmless to the environment and human health. Due to size limitation, carbon quantum dots have strong quantum confinement effect and boundary effect, excite strong and stable fluorescence under the illumination of specific wavelength, and have excellent biocompatibility, water solubility, low cytotoxicity and chemical inertness, so that the carbon quantum dots gradually replace traditional quantum dot materials in various fields such as biomedical imaging, photon sensors, nano electronic devices, energy storage and luminescent devices, and become a hotspot of research. The carbon quantum dots have stable crystal structures, the surfaces of the carbon quantum dots are easy to functionalize, the structures of the carbon quantum dots can be changed by doping of the non-metal elements, so that the carbon quantum dots have fluorescence emission of different colors, and the application range of the quantum dots is widened.
With the rapid development of economy and the continuous upgrading of medium and high-grade products, such as tobacco, wine, cosmetics, medicines and other commodity fields, the products are extremely easy to counterfeit, harm the physical health of consumers and cause serious economic loss. In order to protect the property rights of products, counterfeit and counterfeit are attacked, the anti-counterfeiting technology is increasingly updated, and fluorescent anti-counterfeiting paper is an effective mode. At present, functional anti-counterfeiting materials commonly used in anti-counterfeiting paper are generally organic fluorescent materials or lanthanide complexes and other rare earth substances, are high in cost and have certain toxicity, and the addition amount of the functional anti-counterfeiting materials reaches a certain amount, so that a good fluorescent anti-counterfeiting effect can be achieved, the color of the fluorescent paper is influenced, and the subsequent packaging printing is not facilitated. The carbon quantum dots not only have higher fluorescence intensity than that of the traditional fluorescent material by dozens of times, but also can obtain excellent fluorescent effect by only needing little addition amount in the paper, and basically do not influence the color of the fluorescent paper. Compared with the traditional fluorescent material, the carbon quantum dots have higher light stability, can resist stronger exciting light, and can have a fluorescent emission effect lasting for several hours.
However, the preparation of the current carbon quantum dot fluorescent paper has 3 problems: firstly, the preparation process is complicated, the flow time is long, the solution of the carbon quantum dots needs to be prepared firstly, the powder of the carbon quantum dots is obtained by a method of dialysis for several days and rotary evaporation, then the powder is dispersed in a medium and coated on paper, or the paper is soaked in the dispersion liquid of the carbon quantum dots, so that the carbon quantum dots are attached to the paper, and the fluorescent paper is prepared; secondly, in the method, the preparation of the carbon quantum dots is easy to agglomerate to cause fluorescence quenching, and the carbon quantum dots are too small in size and are easy to agglomerate in the process of being dispersed in a medium, so that the fluorescence emission performance is weakened, the photoluminescence performance is unstable, and the effect of the prepared carbon quantum dot fluorescent paper is greatly influenced; thirdly, graphene oxide is prepared by adopting a hummer method as a raw material in the preparation of the carbon quantum dots at present, and dangerous chemicals such as concentrated sulfuric acid, potassium permanganate and the like are used in the hummer method, so that the process has certain danger, explosion is easy to occur in the actual production, and the method is not environment-friendly.
Therefore, the preparation of the green and environment-friendly carbon quantum dot anti-counterfeiting paper prepared from the raw materials is very important, and the application of the carbon quantum dots in the anti-counterfeiting paper can be widened.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of carbon quantum dot fluorescent paper, which is simple in process, can be used for preparing the carbon quantum dot fluorescent paper with excellent fluorescence performance of carbon quantum dots, flexibility of a cellulose base material and excellent mechanical property, and is high in fluorescence intensity and excellent in anti-counterfeiting performance.
In order to realize the technical scheme, the invention provides a preparation method of carbon quantum dot fluorescent paper, which specifically comprises the following steps:
s1, weighing 4-20g of carbon source substances of carbon quantum dots, dissolving the carbon source substances in 50-200mL of carbon source substance solvent, uniformly stirring to prepare a carbon source substance solution of the carbon quantum dots, weighing 10-50mL of cellulose activator by a dropper, adding 50-250mL of deionized water, magnetically stirring to prepare an aqueous solution, slowly dripping the aqueous solution of the cellulose activator into the carbon source substance solution of the carbon quantum dots, continuously stirring for 20-30min to form a uniform mixed solution, weighing 0.4-2g of cellulose modifier, adding 5-20mL of deionized water, magnetically stirring to prepare a cellulose modifier aqueous solution, dripping into the uniform mixed solution under the condition of magnetic stirring, continuously stirring for 20-30min, and preparing to obtain a carbon quantum dot reaction suspension;
s2, inverting the carbon quantum dot reaction suspension liquid prepared in the step S1 into a tetrafluoroethylene tank of a high-temperature high-pressure reaction kettle, soaking a cellulose paper base into the carbon quantum dot reaction suspension liquid, and then putting the high-temperature high-pressure reaction kettle into an oil bath kettle at the temperature of 180 ℃ for 10 hours;
and S3, after the reaction is finished, naturally cooling the high-temperature high-pressure reaction kettle to room temperature to obtain an intermediate paper sample, washing the intermediate paper sample for 3-4 times by using deionized water and absolute ethyl alcohol respectively, and then placing the intermediate paper sample in a forced air drying oven at 40 ℃ for drying for 2-8 hours to obtain the carbon quantum dot fluorescent paper.
Preferably, the carbon source material of the carbon quantum dots is one or more of sucrose, linseed and citric acid.
Preferably, the carbon source substance solvent is one of water or ethanol or a water/ethanol mixed solution.
Preferably, the cellulose activator is one of diethylenetriamine and urea.
Preferably, the cellulose modifier is one of polydiallyldimethylammonium chloride and polyethyleneimine.
Preferably, the cellulose paper base is one or more of filter paper, cellulose dissolving and regenerating paper base film and cellulose dissolving and regenerating composite paper.
The preparation method of the carbon quantum dot fluorescent paper provided by the invention has the beneficial effects that: the preparation method of the carbon quantum dot fluorescent paper is simple in process, after the cellulose activator is activated and the cellulose modifier is used for modifying fibers in a cellulose paper base, active functional groups are introduced, the grafting rate and the coating rate of the cellulose surface are greatly improved, the surface of the cellulose paper base which is originally chemically inert is activated, the carbon quantum dot fluorescent paper can be used as an excellent carrier loaded by carbon quantum dots, the carbon quantum dots can be prevented from being agglomerated, the carbon quantum dots can be uniformly distributed, optical annihilation is avoided, uniform and strong fluorescence is emitted, the carbon quantum dot fluorescent paper which has the excellent fluorescence performance of the carbon quantum dots and the flexibility and the excellent mechanical performance of a cellulose base material can be prepared, the fluorescence intensity is high, and the anti-counterfeiting performance is excellent.
Drawings
FIG. 1 is a comparison of carbon quantum dot fluorescent paper prepared by the present invention and blank filter paper under UV lamp irradiation.
FIG. 2 is an X-ray photoelectron spectrum of carbon quantum dot fluorescent paper.
Fig. 3 is a fluorescence emission spectrum of the carbon quantum dot fluorescent paper prepared in example 1.
FIG. 4 is a comparison of carbon quantum dot fluorescent paper and blank filter paper by fluorescent metallographic microscopy.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of the present invention.
Example 1
The preparation method of the carbon quantum dot fluorescent paper comprises the following specific steps:
s1, weighing 10g of sucrose and 100mL of deionized water, uniformly stirring to prepare a sucrose aqueous solution, measuring 20mL of diethylenetriamine (produced by Guangzhou Qing Biotech Co., Ltd.) as a cellulose activator by using a burette, adding 100mL of deionized water to prepare an aqueous solution, slowly dropping the diethylenetriamine aqueous solution into the sucrose aqueous solution under the condition of magnetic stirring to form a uniform mixed solution after continuously stirring for 30min, measuring 1g of polydiallyldimethylammonium chloride (produced by Wuxi blue wave chemical Co., Ltd.) by using the burette, adding 10mL of deionized water to prepare a cellulose modifier aqueous solution, dropping the cellulose modifier aqueous solution into the uniform mixed solution under the condition of magnetic stirring, and continuously stirring for 30min to prepare a carbon quantum dot reaction suspension;
s2, inverting the carbon quantum dot reaction suspension liquid prepared in the step S1 into a tetrafluoroethylene tank of a high-temperature high-pressure reaction kettle, dipping conventional quantitative filter paper in the carbon quantum dot reaction suspension liquid, and then putting the high-temperature high-pressure reaction kettle into an oil bath kettle at 180 ℃ for 10 hours;
and S3, after the reaction is finished, naturally cooling the high-temperature high-pressure reaction kettle to room temperature to obtain a slightly yellow paper sample, washing the slightly yellow paper sample with deionized water and absolute ethyl alcohol for 4 times respectively, and then placing the slightly yellow paper sample in a forced air drying oven at 40 ℃ for drying for 4 hours to obtain the carbon quantum dot fluorescent paper.
And S4, washing the yellow brown dispersion liquid in the high-pressure kettle, washing the yellow brown dispersion liquid for 4 times respectively by using deionized water and absolute ethyl alcohol, centrifuging the yellow brown dispersion liquid at 6000r/h, and drying the yellow brown dispersion liquid to obtain the carbon quantum dots which are not loaded on the filter paper and are used for detecting the performance of the quantum dots.
Wherein, the sucrose as a natural food additive is soluble in water, has no harm to the environment and human health, and is a green and environment-friendly carbon source; according to the preparation method, the carbon quantum dots are prepared by a one-step hydrothermal method, and water is selected as a solvent, so that the atmospheric pollution caused by solvent volatilization is avoided; the method is characterized in that diethylenetriamine is used as a cellulose activator to activate the surface of a filter paper fiber, so that more active position points are generated on the surface of the filter paper fiber, and the cellulose modifier polydiallyldimethylammonium chloride is matched to modify the fiber in the filter paper, and then active functional groups are introduced, so that the grafting rate and the coating rate of the cellulose surface are greatly improved, the surface of the cellulose paper base which is originally chemically inert is activated, the cellulose paper base can be used as an excellent carrier loaded by carbon quantum dots, the agglomeration of the carbon quantum dots can be prevented, the carbon quantum dots can be uniformly distributed, optical annihilation is avoided, uniform and strong fluorescence is emitted, and the carbon quantum dot fluorescent paper which has the excellent fluorescence performance of the carbon quantum dots and the flexible and excellent mechanical performance of the filter paper can be prepared, and has high fluorescence intensity and excellent anti-counterfeiting performance. The prepared carbon quantum dot fluorescent paper is environment-friendly in component, wherein the fluorescent material carbon quantum dot has excellent biocompatibility, water solubility and low cytotoxicity, the base material is paper made of natural cellulose, the paper is wide in source, various in types, environment-friendly, low in price and renewable, and hydrogen bonds formed by a large number of hydroxyl groups exist between cellulose molecules or inside the cellulose molecules, so that the prepared carbon quantum dot fluorescent paper has strong mechanical stability.
The carbon quantum dot fluorescent paper prepared in example 1 was examined. By carrying out X-ray diffraction on the carbon quantum dot fluorescent anti-counterfeiting paper, as shown in figure 2, an XRD (X-ray diffraction) pattern shows that the anti-counterfeiting paper only has a carbon quantum characteristic peak of 23 degrees, and the preparation is proved to be successful. As shown in FIG. 3, the detection by the high sensitivity fluorescence spectrometer (FS5) shows that the light yellow carbon quantum dot fluorescent paper has a strong blue fluorescence emission peak at about 450nm under the irradiation of excitation light at about 350 nm. As shown in FIG. 4, the carbon quantum dot fluorescent paper and the blank cellulose paper base are compared in a dark field by a fluorescence metallographic microscope, and it is found that the blank paper sample shows the original paper color under the irradiation of the 365nm excitation light of the fluorescence metallographic microscope, and the carbon quantum dot fluorescent paper shows uniform strong blue fluorescence under the irradiation of the 365nm excitation light.
Example 2
The preparation method of the carbon quantum dot fluorescent paper comprises the following specific steps:
s1, weighing 15g of flaxseed, grinding into powder, adding the powder into 150mL of ethanol solution, uniformly stirring to prepare a flaxseed ethanol solution, measuring 20mL of diethylenetriamine (produced by Guangzhou Qing Biotechnology limited) serving as a cellulose activator into 100mL of deionized water to prepare an aqueous solution by using a dropper, slowly dripping the diethylenetriamine aqueous solution into the flaxseed ethanol solution under the condition of magnetic stirring to form a uniform mixed solution after continuously stirring for 30min, weighing 0.5g of polyethyleneimine (UN-1369 produced by Shanghai Yong En chemical engineering limited) cellulose modifier, adding 15mL of deionized water into the cellulose modifier under the condition of magnetic stirring to prepare an aqueous solution, dripping the cellulose modifier aqueous solution into the uniform mixed solution under the condition of magnetic stirring, and continuously stirring for 30min to prepare a carbon quantum dot reaction suspension;
s2, inverting the carbon quantum dot reaction suspension liquid prepared in the step S1 into a tetrafluoroethylene tank of a high-temperature high-pressure reaction kettle, soaking a cellulose dissolving regenerated paper base film into the carbon quantum dot reaction suspension liquid, and then putting the high-temperature high-pressure reaction kettle into an oil bath kettle at 180 ℃ for 10 hours;
and S3, after the reaction is finished, naturally cooling the high-temperature high-pressure reaction kettle to room temperature to obtain a middle paper pattern of the cellulose dissolving regenerated paper base film, washing the middle paper pattern for 4 times by using deionized water and absolute ethyl alcohol respectively, and then placing the middle paper pattern in an air drying oven at 40 ℃ for drying for 4 hours to obtain the carbon quantum dot fluorescent paper.
Wherein, the linseed powder is used as a natural carbon source, can be dissolved in ethanol, has no harm to the environment and human health, and is a green and environment-friendly carbon source; the method is characterized in that diethylenetriamine is used as a cellulose activator to activate the surface of filter paper fibers, so that more active position points are generated on the surface of the filter paper fibers, and after the surface of fibers in a cellulose dissolving and regenerating paper base film is modified by being matched with a cellulose modifier polyethyleneimine, active functional groups are introduced, so that the grafting rate and the coating rate of the cellulose surface are greatly improved, the surface of the cellulose paper base which is originally chemically inert is activated, the cellulose paper base film can be used as an excellent carrier for loading carbon quantum dots, the carbon quantum dots can be prevented from being agglomerated, the carbon quantum dots can be uniformly distributed, optical annihilation is avoided, uniform and strong fluorescence is emitted, the carbon quantum dot fluorescent paper which has excellent fluorescence performance of the carbon quantum dots and also has the flexibility and excellent mechanical performance of the cellulose dissolving and regenerating paper base film can be prepared, and the fluorescent paper has high fluorescence intensity and excellent anti-counterfeiting performance. The prepared carbon quantum dot fluorescent paper is environment-friendly in component, wherein the fluorescent material carbon quantum dot has excellent biocompatibility, water solubility and low cytotoxicity, the cellulose dissolving and regenerating paper base film is wide in source, various in types, environment-friendly, low in price and renewable, and hydrogen bonds formed by a large number of hydroxyl groups exist between cellulose molecules or inside the cellulose molecules, so that the prepared carbon quantum dot fluorescent paper has strong mechanical stability.
Example 3
The preparation method of the carbon quantum dot fluorescent paper comprises the following specific steps:
s1, weighing 20g of citric acid, adding the citric acid into 200mL of deionized water, uniformly stirring to prepare a citric acid aqueous solution, measuring 10mL of a urea aqueous solution with the mass concentration of 50% by using a dropper as a cellulose activator, slowly dropping the urea aqueous solution into the citric acid aqueous solution under the condition of magnetic stirring, continuously stirring for 30min to form a uniform mixed solution, weighing 2g of a polyethyleneimine (UN-1369, Shanghai Youn chemical Co., Ltd.) cellulose modifier, adding 20mL of deionized water into the cellulose modifier under the condition of magnetic stirring to prepare an aqueous solution, dropwise adding the cellulose modifier aqueous solution into the uniform mixed solution under the condition of magnetic stirring, and continuously stirring for 30min to prepare a carbon quantum dot reaction suspension;
s2, inverting the carbon quantum dot reaction suspension liquid prepared in the step S1 into a tetrafluoroethylene tank of a high-temperature high-pressure reaction kettle, dipping cellulose dissolving and regenerating composite paper into the carbon quantum dot reaction suspension liquid, and then putting the high-temperature high-pressure reaction kettle into an oil bath kettle at 180 ℃ for keeping for 10 hours;
and S3, after the reaction is finished, naturally cooling the high-temperature high-pressure reaction kettle to room temperature to obtain a cellulose-dissolved regenerated composite paper intermediate pattern, washing the intermediate pattern for 4 times by using deionized water and absolute ethyl alcohol respectively, and then placing the intermediate pattern in an air-blast drying oven at 40 ℃ for drying for 4 hours to obtain the carbon quantum dot fluorescent paper.
Wherein, the citric acid is used as a natural food additive, is soluble in water, has no harm to the environment and human health, and is a green and environment-friendly carbon source; the method is characterized in that urea is used as a cellulose activator to activate the surface of filter paper fibers, so that more active position points are generated on the surface of the filter paper fibers, and after the surface of fibers in a cellulose dissolving and regenerating paper base film is modified by matching with a cellulose modifier polyethyleneimine, active functional groups are introduced, so that the grafting rate and the coating rate of the cellulose surface are greatly improved, the surface of the cellulose paper base which is originally chemically inert is activated, the cellulose paper base can be used as an excellent carrier for loading carbon quantum dots, the carbon quantum dots can be prevented from being agglomerated, the carbon quantum dots can be uniformly distributed, optical annihilation is avoided, uniform and strong fluorescence is emitted, the carbon quantum dot fluorescent paper which has excellent fluorescence performance of the carbon quantum dots and flexibility and excellent mechanical performance of cellulose dissolving and regenerating composite paper can be prepared, and the fluorescent paper has high fluorescence intensity and excellent anti-counterfeiting performance. The prepared carbon quantum dot fluorescent paper is environment-friendly in component, wherein the fluorescent material carbon quantum dot has excellent biocompatibility, water solubility and low cytotoxicity, the cellulose dissolving and regenerating composite paper is wide in source, various in types, environment-friendly, low in price and renewable, and hydrogen bonds formed by a large number of hydroxyl groups exist between cellulose molecules or in the cellulose molecules, so that the prepared carbon quantum dot fluorescent paper has strong mechanical stability.
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.
The above description is only for the preferred embodiment of the present invention, but the present invention should not be limited to the embodiment and the disclosure of the drawings, and therefore, all equivalent or modifications that do not depart from the spirit of the present invention are intended to fall within the scope of the present invention.
Claims (6)
1. A preparation method of carbon quantum dot fluorescent paper is characterized by comprising the following steps:
s1, weighing 4-20g of carbon source substances of carbon quantum dots, dissolving the carbon source substances in 50-200mL of carbon source substance solvent, uniformly stirring to prepare a carbon source substance solution of the carbon quantum dots, weighing 10-50mL of cellulose activator by a dropper, adding 50-250mL of deionized water, magnetically stirring to prepare an aqueous solution, slowly dripping the aqueous solution of the cellulose activator into the carbon source substance solution of the carbon quantum dots, continuously stirring for 20-30min to form a uniform mixed solution, weighing 0.4-2g of cellulose modifier, adding 5-20mL of deionized water, magnetically stirring to prepare a cellulose modifier aqueous solution, dripping into the uniform mixed solution under the condition of magnetic stirring, continuously stirring for 20-30min, and preparing to obtain a carbon quantum dot reaction suspension;
s2, inverting the carbon quantum dot reaction suspension liquid prepared in the step S1 into a tetrafluoroethylene tank of a high-temperature high-pressure reaction kettle, soaking a cellulose paper base into the carbon quantum dot reaction suspension liquid, and then putting the high-temperature high-pressure reaction kettle into an oil bath kettle at the temperature of 180 ℃ for 10 hours;
and S3, after the reaction is finished, naturally cooling the high-temperature high-pressure reaction kettle to room temperature to obtain an intermediate paper sample, washing the intermediate paper sample for 3-4 times by using deionized water and absolute ethyl alcohol respectively, and then placing the intermediate paper sample in a forced air drying oven at 40 ℃ for drying for 2-8 hours to obtain the carbon quantum dot fluorescent paper.
2. The method for preparing carbon quantum dot fluorescent paper as set forth in claim 1, wherein: the carbon source substance of the carbon quantum dots is one or more of sucrose, flaxseed, citric acid, wax gourd, peanut shell, watermelon peel and orange peel.
3. The method for preparing carbon quantum dot fluorescent paper as set forth in claim 1, wherein: the carbon source substance solvent is one of water or ethanol or a water/ethanol mixed solution.
4. The method for preparing carbon quantum dot fluorescent paper as set forth in claim 1, wherein: the cellulose activator is one of diethylenetriamine and urea.
5. The method for preparing carbon quantum dot fluorescent paper as set forth in claim 1, wherein: the cellulose modifier is one of polydiallyl dimethyl amine chloride and polyethyleneimine.
6. The method for preparing carbon quantum dot fluorescent paper as set forth in claim 1, wherein: the cellulose paper base is one or more of filter paper, cellulose dissolving and regenerating paper base film and cellulose dissolving and regenerating composite paper.
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