CN115260723A - Preparation method of carbon-aminated quantum dot degradable fluorescent film - Google Patents
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Abstract
The invention discloses a preparation method of an aminated carbon quantum dot degradable fluorescent film, which comprises the following steps: s1: adding pentaerythrityl tetramine and oleylamine into absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the pentaerythrityl tetramine and the oleylamine, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, performing solvothermal reaction for 4-8h at 120-150 ℃, performing rotary evaporation, dissolving the dark brown product in acetone, adding a catalyst, and stirring and dissolving to obtain an aminated carbon quantum dot solution; s2: and (2) dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare 5wt% of polylactic acid solution, then dropwise adding an aminated carbon quantum dot solution into the polylactic acid solution, stirring and reacting for 1-3h, then coating the solution on a quartz chip, and naturally drying the quartz chip to obtain the aminated carbon quantum dot degradable fluorescent film. According to the invention, the aminated carbon quantum dot is prepared by taking pentamine as a carbon source and oleylamine as a stabilizer for the first time, and is grafted to the tail end of a long chain of polylactic acid, so that the composite stability of the pentamine and the oleylamine is improved, the fluorescence quenching of the carbon quantum dot is inhibited, and the fluorescence stability of the carbon quantum dot is improved.
Description
Technical Field
The invention belongs to the field of fluorescent film preparation, and particularly relates to a preparation method of a carbon-aminated quantum dot degradable fluorescent film.
Background
Carbon Quantum Dots (CQDs), also called carbon dots or carbon nanodots, are zero-dimensional carbon nanomaterials with remarkable fluorescence performance, are composed of ultrafine, dispersed and quasi-spherical carbon nanoparticles with the size of less than 10nm, and have good application prospects in various fields such as medical imaging technology, environmental monitoring, chemical analysis, catalyst preparation, energy development and the like. The existing preparation methods of the carbon quantum dots comprise two main types: the top-down method and the bottom-up method respectively comprise the following steps: arc discharge, laser ablation, electrochemical methods; the "bottom-up" method comprises: hydrothermal method, chemical oxidation method, microwave synthesis method, template method. When the carbon quantum dots are prepared by the top-down method, the carbon sources include carbon nanotubes, carbon fibers, graphite rods, carbon dust, activated carbon and the like. The CQDs have different preparation methods and different types of carbon sources, so that the carbon quantum dots have various chemical structures and optical properties, and can better meet various practical application requirements.
The CQDs fluorescent film is formed by compounding carbon quantum dots and a polymer film forming agent, but the carbon quantum dot inorganic substance and an organic polymer are poor in compatibility, so that the CQDs fluorescent film is poor in stability and mechanical property.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of an aminated carbon quantum dot degradable fluorescent film.
The technical scheme of the invention is summarized as follows:
a preparation method of a carbon-aminated quantum dot degradable fluorescent film comprises the following steps:
s1: adding pentamine and oleylamine into anhydrous ethanol, ultrasonically dispersing for 7min, mixing, transferring into a reaction kettle with polytetrafluoroethylene lining, performing solvothermal reaction at 120-150 deg.C for 4-8 hr, rotary evaporating to remove anhydrous ethanol solvent, and mixing
Dissolving the obtained dark brown product in acetone, adding a catalyst, stirring and dissolving to obtain an aminated carbon quantum dot solution;
s2: dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare 5wt% of polylactic acid solution, then dropwise adding an aminated carbon quantum dot solution, stirring and reacting for 1-3h, then coating on a quartz plate, and naturally drying to obtain the aminated carbon quantum dot degradable fluorescent film.
Preferably, the catalyst is dicyclohexylcarbodiimide.
Preferably, the dosage ratio of the pentamine, the oleylamine, the absolute ethyl alcohol, the acetone and the catalyst is (0.1-0.5) g, (0.18-0.8) g, 100mL and 10mL, and (0.01-0.02) g.
Preferably, the volume ratio of the carbon amide quantum dot solution to the 5wt% polylactic acid solution is 1: (1-4). The invention has the beneficial effects that:
according to the invention, pentaerythrite is used as a carbon source, oleylamine is used as a stabilizer for the first time, an aminated carbon quantum dot is prepared by a solvothermal method, under the catalysis of dicyclohexylcarbodiimide, an amino functional group rich on the surface of the aminated carbon quantum dot and carboxyl-terminated polylactic acid are subjected to amidation reaction, and then the fluorescent carbon quantum dot is grafted to the tail end of a long chain of the polylactic acid, and the fluorescent carbon quantum dot is stably embedded in a polylactic acid film in a chemical bond form, so that the composite stability of the fluorescent carbon quantum dot and the polylactic acid film is improved, meanwhile, the fluorescence quenching of the carbon quantum dot is effectively inhibited, the fluorescence stability of the carbon quantum dot is improved, compared with the traditional silane coupling agent modification mode, the surface modification of a non-luminescent intermediate is not needed, the fluorescent aminated carbon quantum dot is directly and covalently connected with the polylactic acid, the absorption of the non-luminescent silane coupling agent to fluorescence is avoided, and the fluorescence efficiency is greatly improved.
Drawings
FIG. 1 shows the UV-VIS absorption spectrum, excitation spectrum and emission spectrum of the aminated carbon quantum dot prepared in example 1;
FIG. 2 is a fluorescence spectrum of the carbon quantum dot degradable fluorescent thin films prepared in examples 1 to 4 and comparative example;
FIG. 3 is a flow chart of a method for preparing the carbon-amido quantum dot degradable fluorescent film of the present invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
The invention discloses a preparation method of an aminated carbon quantum dot degradable fluorescent film, which comprises the following steps:
s1: adding pentamine and oleylamine into absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the pentamine and the oleylamine, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, performing solvothermal reaction at 120-150 ℃ for 4-8h, performing rotary evaporation to remove the absolute ethyl alcohol solvent, dissolving the obtained dark brown product into acetone, adding dicyclohexylcarbodiimide serving as a catalyst, and stirring and dissolving to obtain a carbon amide quantum dot solution; the dosage ratio of the pentamine, the oleylamine, the absolute ethyl alcohol, the acetone and the catalyst is (0.1-0.5) g, (0.18-0.8) g, 100mL, (0.01-0.02) g;
s2: dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare 5wt% of polylactic acid solution, then dropwise adding an aminated carbon quantum dot solution, stirring and reacting for 1-3h, then coating on a quartz plate, and naturally drying to obtain the aminated carbon quantum dot degradable fluorescent film; the volume ratio of the aminated carbon quantum dot solution to the 5wt% polylactic acid solution is 1: (1-4).
Example 1
A preparation method of a carbon-aminated quantum dot degradable fluorescent film comprises the following steps:
s1: adding 0.1g of pentamine and 0.18g of oleylamine into 100mL of absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the pentamine and the oleylamine, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, performing solvothermal reaction at 130 ℃ for 8h, performing rotary evaporation until the absolute ethyl alcohol solvent is removed, dissolving the obtained dark brown product (which shows strong blue light under a 365nm ultraviolet lamp and shows that fluorescent aminated carbon quantum dots are formed) into 10mL of acetone, adding 0.01g of catalyst dicyclohexylcarbodiimide, and stirring and dissolving to obtain an aminated carbon quantum dot solution;
s2: 3.4737g of terminal carboxyl polylactic acid is dissolved in 50mL of dichloromethane to prepare 5wt% polylactic acid solution;
and then, dripping 10mL of carbon amide quantum dot solution into 10mL of 5wt% polylactic acid solution, stirring for reaction for 1h, coating on a quartz plate, and naturally drying to obtain the carbon amide quantum dot degradable fluorescent film.
Fig. 1 shows the uv-vis absorption spectrum, excitation spectrum and emission spectrum of the aminated carbon quantum dot prepared in example 1: as can be seen from fig. 1, the absorption peak of the ultraviolet-visible absorption spectrum of the aminated carbon quantum dot at 340nm belongs to N-pi transition of-N = N-, and is colorless and transparent under natural light, and shows intense blue light under 365nm ultraviolet light; in the fluorescence spectrum, the carbon quantum dot has a maximum emission peak at 515nm under 435nm excitation.
Example 2 is the same as example 1, except that: and S2, dripping 10mL of carbon amide quantum dot solution into 20mL of 5wt% polylactic acid solution, stirring for reacting for 1h, coating on a quartz plate, and naturally drying to obtain the carbon amide quantum dot degradable fluorescent film.
Example 3 is the same as example 1, except that: and S2, dripping 10mL of carbon amide quantum dot solution into 30mL of 5wt% polylactic acid solution, stirring for reacting for 1h, coating on a quartz plate, and naturally drying to obtain the carbon amide quantum dot degradable fluorescent film.
Example 4 is the same as example 1, except that: and S2, dripping 10mL of carbon amide quantum dot solution into 40mL of 5wt% polylactic acid solution, stirring for reacting for 1h, coating on a quartz plate, and naturally drying to obtain the carbon amide quantum dot degradable fluorescent film.
The comparative example uses ascorbic acid as a carbon source and N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane as a coupling agent to prepare the fluorescent film, and the preparation method comprises the following steps:
s1: adding 0.1g of ascorbic acid and 0.18g of oleylamine into 100mL of absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the ascorbic acid and the oleylamine, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, performing solvothermal reaction at 130 ℃ for 8h, performing rotary evaporation until the absolute ethyl alcohol solvent is removed, mixing and stirring the obtained dark brown product and 0.1g of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane for 0.5h, dissolving the obtained mixture into 10mL of acetone, adding 0.01g of catalyst dicyclohexylcarbodiimide, and stirring and dissolving to obtain a silane modified carbon quantum dot solution;
s2: 3.4737g of terminal carboxyl polylactic acid is dissolved in 50mL of dichloromethane to prepare 5wt% polylactic acid solution;
and then, dripping 10mL of silane modified carbon quantum dot solution into 10mL of 5wt% polylactic acid solution, stirring for reaction for 1h, coating on a quartz plate, and naturally drying to obtain the carbon quantum dot degradable fluorescent film.
FIG. 2 is a fluorescence spectrum of the carbon quantum dot degradable fluorescent thin films prepared in examples 1 to 4 and comparative example: as can be seen from FIG. 2, the carbon quantum dot solutions of examples 1-4 are not changed, and the fluorescence intensity is gradually decreased as the dichloromethane solution ratio of the carboxyl-terminated polylactic acid is increased under the excitation of light with a wavelength of 435nm, and the fluorescence intensity of the fluorescent film of example 1 is far higher than that of the comparative example as can be seen from the spectra of comparative example 1 and comparative example 1, because the carbon quantum dot modified by aminosilane of the comparative example has the problem of fluorescence absorption by a coupling agent, while the aminated carbon quantum dot prepared by using pentaerythrite as a carbon source in example 1 is directly combined with the carboxyl-terminated polylactic acid, so that the structural stability of the film is solved, and the fluorescence performance is also greatly ensured.
In the embodiment 1-4, pentaerythrite is used as a carbon source for the first time, oleylamine is used as a stabilizer, an aminated carbon quantum dot is prepared by a solvothermal method, under the catalysis of dicyclohexylcarbodiimide, an amino functional group rich on the surface of the aminated carbon quantum dot and carboxyl-terminated polylactic acid are subjected to amidation reaction, and then the fluorescent carbon quantum dot is grafted to the long chain end of the polylactic acid, and the fluorescent carbon quantum dot is stably embedded in a polylactic acid film in a chemical bond form, so that the composite stability of the fluorescent carbon quantum dot and the polylactic acid film is improved, meanwhile, the fluorescence quenching of the carbon quantum dot is effectively inhibited, the fluorescence stability of the carbon quantum dot is improved, compared with the traditional silane coupling agent modification mode, the surface modification of a non-luminous intermediate is not needed, the fluorescent aminated carbon quantum dot is directly and covalently connected with the polylactic acid, the absorption of the non-luminous silane coupling agent to fluorescence is avoided, and the fluorescence efficiency is greatly improved.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (4)
1. A preparation method of a carbon-aminated quantum dot degradable fluorescent film is characterized by comprising the following steps:
s1: adding pentaerythrityl tetramine and oleylamine into absolute ethyl alcohol, performing ultrasonic dispersion for 7min to uniformly mix the pentaerythrityl tetramine and the oleylamine, transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining, performing solvothermal reaction at the temperature of between 120 and 150 ℃ for 4 to 8 hours, performing rotary evaporation to remove the absolute ethyl alcohol solvent, dissolving the obtained dark brown product into acetone, adding a catalyst, and stirring and dissolving to obtain an aminated carbon quantum dot solution;
s2: dissolving carboxyl-terminated polylactic acid in dichloromethane to prepare 5wt% of polylactic acid solution, then dropwise adding an aminated carbon quantum dot solution, stirring and reacting for 1-3h, then coating on a quartz plate, and naturally drying to obtain the aminated carbon quantum dot degradable fluorescent film.
2. The method for preparing the carbon-aminated quantum dot degradable fluorescent film according to claim 1, wherein the catalyst is dicyclohexylcarbodiimide.
3. The method for preparing a carbon-aminated quantum dot degradable fluorescent film according to claim 1, wherein the dosage ratio of the pentaerythritol, the oleylamine, the absolute ethyl alcohol, the acetone and the catalyst is (0.1-0.5) g, (0.18-0.8) g, 100mL (0.01-0.02) g.
4. The method for preparing the carbon-amido quantum dot degradable fluorescent film according to claim 1, wherein the volume ratio of the carbon-amido quantum dot solution to the 5wt% polylactic acid solution is 1: (1-4).
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| CN116273117A (en) * | 2023-02-13 | 2023-06-23 | 嘉兴学院 | Microplastic-based carbon quantum dot/graphite phase carbon nitride photocatalyst, preparation method and application thereof |
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| CN116273117A (en) * | 2023-02-13 | 2023-06-23 | 嘉兴学院 | Microplastic-based carbon quantum dot/graphite phase carbon nitride photocatalyst, preparation method and application thereof |
| CN116273117B (en) * | 2023-02-13 | 2024-04-09 | 嘉兴学院 | Microplastic-based carbon quantum dot/graphite phase carbon nitride photocatalyst, preparation method and application thereof |
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