CN104974750A - Method for preparing carbon quantum dots by virtue of polyethyleneimine decomposition - Google Patents
Method for preparing carbon quantum dots by virtue of polyethyleneimine decomposition Download PDFInfo
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- CN104974750A CN104974750A CN201510436822.9A CN201510436822A CN104974750A CN 104974750 A CN104974750 A CN 104974750A CN 201510436822 A CN201510436822 A CN 201510436822A CN 104974750 A CN104974750 A CN 104974750A
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- polymine
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Abstract
The invention discloses a method for preparing carbon quantum dots by virtue of polyethyleneimine decomposition, belonging to the technical field of preparation of nanometer materials. The method comprises the steps of dispersing polyethyleneimine as a raw material into an ethanol solvent, adequately stirring, carrying out heat treatment at 180-200 DEG C for 20 hours in a reaction kettle, and naturally cooling, so as to obtain decomposed auto-fluorescent polyethyleneimine. The method disclosed by the invention has the advantages that the synthetic process is simple and convenient and high in efficiency; polyethyleneimine simultaneously servers as a carbon source and a nitrogen source, so that obtained carbon quantum dots have high impurity and moderate particle sizes, are monodisperse and water soluble and are expected to be applied to the LED membrane materials, fluorescent marks, DNA carriers and targeted drug delivery particles.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly a kind of carbon quantum dot preparation method decomposed based on polymine.The method can be prepared by simple operations can the nitriding carbon quantum dot of autofluorescence, and be thus expected at photoelectric material, bio-imaging, the fields such as target drug-carrying obtain widespread use.
Background technology
Polymine is a kind of high molecular weight water soluble polymer, and in colourless or faint yellow viscous liquid, water-soluble and ethanol, has high tack, high absorbability, as the widely used non-virus carrier of one, causes the concern of scholars in the past ten years.Polymine because of its uniqueness " proton sponge effect " usually with organic fluorescent dye or quantum dot compound, using as the retrospective pharmaceutical carrier of trace, be applied to biomedical sector.But with the compound of organic fluorescent dye or quantum dot, often preparation process is loaded down with trivial details, also further increases cytotoxicity, and obtained matrix material poor stability.Therefore, developing a kind of preparation process simply, does not increase cytotoxicity and can retain polymine structural performance, and the method based on polymine decomposition simultaneously possessing quantum dot luminous characteristic just seems extremely important.
Summary of the invention
The object of this invention is to provide a kind of carbon quantum dot preparation method decomposed based on polymine, with the complex method solving existing polymine and organic fluorescent dye or quantum dot often preparation process loaded down with trivial details, add cytotoxicity and the technical problem of product stability difference.The present invention take polymine as starting material, is obtained the polymine decomposed by ethanol high temperature reduction, while retaining polymine structural performance, further increases unique autofluorescence performance, for its further biologic applications is laid a good foundation.
Based on the carbon quantum dot preparation method that polymine decomposes, comprise the steps:
(1) solution that concentration is 10-50mg/10ml is made in polymine dispersion in ethanol, proceed in reactor after fully stirring by solution, react 20 hours in 180-200 DEG C of baking oven, naturally cooling, namely obtains carbon quantum dot stoste;
(2) adopt Gradient column chromatography method to purify further to stoste, remove the carbon quantum dot that namely unnecessary undecomposed polymine obtains autofluorescence.
Further, a kind of carbon quantum dot preparation method decomposed based on polymine, the polymine described in step (1) is the collateralization polymine that market can extensively buy, and its molecular formula is C
2X+4Kh
5X+10Kn
x+2Kand in colloid.
Further, a kind of carbon quantum dot preparation method decomposed based on polymine, the ethanol described in step (1) is the analytical pure dehydrated alcohol of ethanol massfraction >=99.7%; Described reactor is polytetrafluoroethyllining lining reactor.
Further, a kind of carbon quantum dot preparation method decomposed based on polymine, the Gradient column chromatography method described in step (2) uses neutral alumina or silica gel for chromatography to be stationary phase, and employing ethanol is developping agent.
The present invention decomposes the principle of preparation carbon quantum dot by polymine: polymine (PEI) surface with height branched structure, containing a large amount of primary amine, tertiary amine, secondary amine, has more ensured abundant nitrogenous source while providing carbon source; By ethanol reductibility at high temperature, branched macromolecule polymine is progressively decomposed into small molecules, forms nitriding carbon quantum dot.Adopt column chromatography method that product is separated further purification with the starting material fully do not reacted.
The present invention compared with prior art has the following advantages:
1, the present invention prepares nitriding carbon quantum dot by decomposing polymine, and adopt polymine simultaneously as Carbon and nitrogen sources, starting material are simply common.
2, polymine is most widely used non-virus carrier, is widely used in cell transfecting.Present method adds unique autofluorescence performance, conveniently follows up its interaction trajectory or cell marking.
3, the present invention adopts ethanolic soln in high temperature reduction polymine process, improves reduction efficiency, simultaneously for next step adopts column chromatography for separation to provide the foundation.
4, the present invention adopts column chromatography method to carry out further separating-purifying to products therefrom, effectively eliminates the impurity and excess reactant brought in preparation process, reaches the object of isolation of purified simultaneously.
5, preparation technology of the present invention is simple, and namely a step achieves preparation and the functionalization of nitriding carbon quantum dot, easy handling, and applied range, is beneficial to industrialization promotion.
Accompanying drawing explanation
Fig. 1 example 1 prepares photoluminescence spectrum and the photoluminescence excitation of nitriding carbon quantum dot.
Fig. 2 example 1 reacts the FTIR spectrum of front polymine (Raw PEI) and the rear nitriding carbon quantum dot (D-PEI) of reaction.
Under the different excitation wavelength of Fig. 3, example 1 prepares the photoluminescence spectrum of nitriding carbon quantum dot.
Embodiment
Choose specific embodiment according to technical scheme of the present invention to be described as follows:
Embodiment 1:
The polymine of 200mg is dispersed in the ethanol of 40ml, fully stirs, solution is transferred in reactor, be warming up to 200 DEG C of reaction 20h, cool to room temperature.Adopt column chromatography method, carry out separating-purifying to product, obtain the nitriding carbon quantum dot issuing yellow green light at 365nm ultraviolet excitation, (wherein, PLE is photoluminescence excitation as shown in Figure 1; PL is photoluminescence spectrum).The FTIR spectrum of the polymine before reaction and reacted carbon quantum dot as shown in Figure 2.Prepare gained nitriding carbon quantum dot ethanolic soln and demonstrate strong yellow-green fluorescence under ultraviolet light, the photoluminescence spectrum under different excitation wavelength as shown in Figure 3.Its maximum excitation wavelength is 430nm, and maximum emission wavelength is now 514nm.
Embodiment 2:
The polymine of 50mg is dispersed in the ethanol of 40ml, fully stirs, solution is transferred in reactor, be warming up to 200 DEG C of reaction 20h, cool to room temperature.Adopt column chromatography method, separating-purifying is carried out to product, obtains the nitriding carbon quantum dot issuing yellow green light at 365nm ultraviolet excitation.
Embodiment 3:
The polymine of 100mg is dispersed in the ethanol of 40ml, fully stirs, solution is transferred in reactor, be warming up to 180 DEG C of reaction 20h, cool to room temperature.Adopt column chromatography method, separating-purifying is carried out to product, obtains the nitriding carbon quantum dot issuing yellow green light at 365nm ultraviolet excitation.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (4)
1., based on the carbon quantum dot preparation method that polymine decomposes, it is characterized in that, comprise the steps:
The solution that concentration is 10-50mg/10ml is made in polymine dispersion in ethanol, proceeds in reactor after fully stirring by solution, react 20 hours in 180-200 DEG C of baking oven, naturally cooling, namely obtains carbon quantum dot stoste;
Adopt Gradient column chromatography method to purify further to stoste, remove the carbon quantum dot that namely unnecessary undecomposed polymine obtains autofluorescence.
2. a kind of carbon quantum dot preparation method decomposed based on polymine according to claim 1, it is characterized in that, the polymine described in step (1) is collateralization polymine, and its molecular formula is C
2X+4Kh
5X+10Kn
x+2Kand in colloid.
3. a kind of carbon quantum dot preparation method decomposed based on polymine according to claim 1 and 2, it is characterized in that, the ethanol described in step (1) is the analytical pure dehydrated alcohol of ethanol massfraction >=99.7%; Described reactor is polytetrafluoroethyllining lining reactor.
4. a kind of carbon quantum dot preparation method decomposed based on polymine according to claim 1 and 2, it is characterized in that, Gradient column chromatography method described in step (2) uses neutral alumina or silica gel for chromatography to be stationary phase, and employing ethanol is developping agent.
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Cited By (9)
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| CN106398693A (en) * | 2016-08-31 | 2017-02-15 | 山西大学 | Preparation method and application of nitrogen doped yellow fluorescent carbon dots |
| CN107474831A (en) * | 2017-06-28 | 2017-12-15 | 昆明理工大学 | A kind of post separation prepares sulphur, the method for nitrogen-doped carbon quantum dot and application |
| CN108493409A (en) * | 2018-03-12 | 2018-09-04 | 安徽大学 | A kind of preparation method of nitrogen-doped carbon cladding flower-like nanometer molybdenum disulfide |
| CN108659830A (en) * | 2018-06-01 | 2018-10-16 | 盐城师范学院 | A method of fluorescent carbon point is prepared based on chalina |
| CN109135737A (en) * | 2018-08-18 | 2019-01-04 | 南京慧基生物技术有限公司 | A kind of nitrogen-doped carbon quantum dot and its preparation method and application |
| CN109423282A (en) * | 2017-09-05 | 2019-03-05 | 中国林业科学研究院林产化学工业研究所 | A kind of synthetic method and application of N doping water-solubility fluorescent carbon quantum dot |
| CN109796973A (en) * | 2019-02-21 | 2019-05-24 | 中国科学院长春光学精密机械与物理研究所 | Solid luminescent carbon nano dot and preparation method and application |
| CN110484248A (en) * | 2019-07-25 | 2019-11-22 | 太原理工大学 | A kind of preparation method of flexibility carbon quantum dot film |
| CN112072106A (en) * | 2020-08-28 | 2020-12-11 | 浙江大学 | Conductive adhesive material, preparation method thereof, negative electrode plate and lithium ion battery |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398693A (en) * | 2016-08-31 | 2017-02-15 | 山西大学 | Preparation method and application of nitrogen doped yellow fluorescent carbon dots |
| CN106398693B (en) * | 2016-08-31 | 2018-04-03 | 山西大学 | A kind of preparation method and application of N doping yellow fluorescence carbon point |
| CN107474831A (en) * | 2017-06-28 | 2017-12-15 | 昆明理工大学 | A kind of post separation prepares sulphur, the method for nitrogen-doped carbon quantum dot and application |
| CN107474831B (en) * | 2017-06-28 | 2020-02-07 | 昆明理工大学 | Method for preparing sulfur and nitrogen doped carbon quantum dots by column separation and application |
| CN109423282A (en) * | 2017-09-05 | 2019-03-05 | 中国林业科学研究院林产化学工业研究所 | A kind of synthetic method and application of N doping water-solubility fluorescent carbon quantum dot |
| CN108493409A (en) * | 2018-03-12 | 2018-09-04 | 安徽大学 | A kind of preparation method of nitrogen-doped carbon cladding flower-like nanometer molybdenum disulfide |
| CN108659830A (en) * | 2018-06-01 | 2018-10-16 | 盐城师范学院 | A method of fluorescent carbon point is prepared based on chalina |
| CN109135737A (en) * | 2018-08-18 | 2019-01-04 | 南京慧基生物技术有限公司 | A kind of nitrogen-doped carbon quantum dot and its preparation method and application |
| CN109796973A (en) * | 2019-02-21 | 2019-05-24 | 中国科学院长春光学精密机械与物理研究所 | Solid luminescent carbon nano dot and preparation method and application |
| CN109796973B (en) * | 2019-02-21 | 2020-11-03 | 中国科学院长春光学精密机械与物理研究所 | Solid luminescent carbon nanodot and preparation method and application thereof |
| CN110484248A (en) * | 2019-07-25 | 2019-11-22 | 太原理工大学 | A kind of preparation method of flexibility carbon quantum dot film |
| CN112072106A (en) * | 2020-08-28 | 2020-12-11 | 浙江大学 | Conductive adhesive material, preparation method thereof, negative electrode plate and lithium ion battery |
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