CN104974750B - 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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- CN104974750B CN104974750B CN201510436822.9A CN201510436822A CN104974750B CN 104974750 B CN104974750 B CN 104974750B CN 201510436822 A CN201510436822 A CN 201510436822A CN 104974750 B CN104974750 B CN 104974750B
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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, more particularly to a kind of carbon quantum decomposed based on polyethyleneimine
Point preparation method.The method by simple operations can prepare can autofluorescence nitriding carbon quantum dot, thus be expected in photoelectricity
The fields such as material, bio-imaging, target drug-carrying obtain extensive application.
Background technology
Polyethyleneimine is a kind of high molecular weight water soluble polymer, in colourless or faint yellow viscous liquid, be dissolved in water and
Ethanol, with high tack, high adsorption, as a kind of widely used non-virus carrier, is caused in the past ten years
The concern of scholars.Polyethyleneimine is usually multiple with organic fluorescent dye or quantum dot because of " proton sponge effect " of its uniqueness
Close, as the retrospective pharmaceutical carrier of trace, to be applied to biomedical sector.But with organic fluorescent dye or quantum dot
Compound often preparation process is loaded down with trivial details, also further increases cytotoxicity, and obtained composite stability is poor.Therefore,
Develop that a kind of preparation process is simple, do not increase cytotoxicity and polyethyleneimine amine structure characteristic can be retained, be provided simultaneously with quantum dot
The method decomposed based on polyethyleneimine of spontaneous light characteristic just seems extremely important.
The content of the invention
It is an object of the invention to provide a kind of carbon quantum dot preparation method decomposed based on polyethyleneimine, existing to solve
Polyethyleneimine and organic fluorescent dye or quantum dot complex method often preparation process is loaded down with trivial details, increased cytotoxicity and
The technical problem of product stability difference.The present invention obtains what is decomposed with polyethyleneimine as raw material by ethanol high temperature reduction
Polyethyleneimine, while retaining polyethyleneimine amine structure characteristic, further increases the autofluorescence performance of uniqueness, is which is further
Biologic applications are laid a good foundation.
A kind of carbon quantum dot preparation method decomposed based on polyethyleneimine, is comprised the steps：
(1) solution that concentration is 10-50mg/10ml is made in polyethyleneimine dispersion in ethanol, will after being sufficiently stirred for
Solution is proceeded in reactor, is reacted 20 hours in 180-200 DEG C of baking oven, and natural cooling obtains carbon quantum dot stoste；
(2) stoste is further purified using Gradient column chromatography method, removes unnecessary undecomposed polyethyleneimine and obtain final product
To the carbon quantum dot of autofluorescence.
Further, a kind of carbon quantum dot preparation method decomposed based on polyethyleneimine, step（1）Described in poly- second
Alkene imines is the collateralization polyethyleneimine that extensively can be bought on market, and its molecular formula is C2X+4KH5X+10KNX+2KAnd be in glue
Body.
Further, a kind of carbon quantum dot preparation method decomposed based on polyethyleneimine, step（1）Described in ethanol
For the pure analysis absolute ethyl alcohol of ethanol mass fraction >=99.7%；Described reactor is polytetrafluoroethyllining lining reactor.
Further, a kind of carbon quantum dot preparation method decomposed based on polyethyleneimine, step（2）Described in gradient
It is fixing phase that column chromatography method uses neutral alumina or silica gel for chromatography, adopts ethanol for solvent.
The present invention is decomposed the principle for preparing carbon quantum dot by polyethyleneimine：Polyethyleneimine with height branched structure
（PEI）Substantial amounts of primary amine, tertiary amine, secondary amine are contained in surface, have more ensured abundant nitrogen source while carbon source is provided；By ethanol
Branched macromolecule polyethyleneimine is progressively decomposed into small molecule by reproducibility at high temperature, forms nitriding carbon quantum dot.Using
Product is separated with not sufficiently reactive raw material and is further purified by column chromatography method.
The present invention has advantages below compared with prior art：
1st, the present invention prepares nitriding carbon quantum dot by decomposing polyethyleneimine, using polyethyleneimine simultaneously as carbon source
And nitrogen source, raw material are simply common.
2nd, polyethyleneimine is most widely used non-virus carrier, is widely used in cell transfecting.This method increased
Unique autofluorescence performance, conveniently follows up its interaction trajectory or cell marking.
3rd, the present invention adopts ethanol solution during high temperature reduction polyethyleneimine, improves reduction efficiency, while being
Next step is provided the foundation using column chromatography for separation.
4th, the present invention carries out further separating-purifying using column chromatography method to products therefrom, effectively eliminates preparation process
In the impurity brought into and excess reactant, while having reached the purpose of isolation of purified.
5th, preparation process is simple of the present invention, a step realize the preparation of nitriding carbon quantum dot and functionalization, it is easy to operate,
Applied range, beneficial to industrialization promotion.
Description of the drawings
Fig. 1 examples 1 prepare the photoluminescence spectrum of nitriding carbon quantum dot and photoluminescence excitation.
Fig. 2 examples 1 react front polyethyleneimine（Raw PEI）With nitriding carbon quantum dot after reaction（D-PEI）Fourier
Infrared spectrum.
Under Fig. 3 difference excitation wavelengths, example 1 prepares the photoluminescence spectrum of nitriding carbon quantum dot.
Specific embodiment
Specific embodiment is chosen according to technical scheme of the present invention to be described as follows：
Embodiment 1：
The polyethyleneimine of 200mg is dispersed in the ethanol of 40ml, is sufficiently stirred for, solution is transferred in reactor,
200 DEG C of reaction 20h are warming up to, room temperature is cooled to.Using column chromatography method, separating-purifying is carried out to product, obtain purple in 365nm
Outer light excites the nitriding carbon quantum dot for issuing green-yellow light, as shown in Figure 1（Wherein, PLE is photoluminescence excitation；PL is photic
Luminous spectrum）.The FTIR spectrum of polyethyleneimine and reacted carbon quantum dot before reaction is as shown in Figure 2.Prepare institute
Obtain nitriding carbon quantum dot ethanol solution and show strong yellow-green fluorescence, the luminescence generated by light under different excitation wavelengths under ultraviolet light
Spectrum is as shown in Figure 3.Its maximum excitation wavelength is 430nm, and maximum emission wavelength now is 514nm.
Embodiment 2：
The polyethyleneimine of 50mg is dispersed in the ethanol of 40ml, is sufficiently stirred for, solution is transferred in reactor, risen
Temperature is cooled to room temperature to 200 DEG C of reaction 20h.Using column chromatography method, separating-purifying is carried out to product, obtain ultraviolet in 365nm
Light excites the nitriding carbon quantum dot for issuing green-yellow light.
Embodiment 3：
The polyethyleneimine of 100mg is dispersed in the ethanol of 40ml, is sufficiently stirred for, solution is transferred in reactor,
180 DEG C of reaction 20h are warming up to, room temperature is cooled to.Using column chromatography method, separating-purifying is carried out to product, obtain purple in 365nm
Outer light excites the nitriding carbon quantum dot for issuing green-yellow light.
The above, is only presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to the present invention
Any simple modification, change and equivalence changes that technical spirit is made to above example, still fall within the technology of the present invention side
In the protection domain of case.
Claims (4)
1. it is a kind of based on polyethyleneimine decompose carbon quantum dot preparation method, it is characterised in that comprise the steps：
（1）The solution that concentration is 10-50mg/10ml is made in polyethyleneimine dispersion in ethanol, by solution after being sufficiently stirred for
Proceed in reactor, react 20 hours in 180-200 DEG C of baking oven, natural cooling obtains carbon quantum dot stoste；
（2）Stoste is further purified using Gradient column chromatography method, remove unnecessary undecomposed polyethyleneimine and obtain certainly
The carbon quantum dot for fluorescing.
2. it is according to claim 1 it is a kind of based on polyethyleneimine decompose carbon quantum dot preparation method, it is characterised in that
Step（1）Described in polyethyleneimine for collateralization polyethyleneimine.
3. a kind of carbon quantum dot preparation method decomposed based on polyethyleneimine according to claim 1 and 2, its feature exists
In step（1）Described in ethanol for ethanol mass fraction >=99.7% pure analysis absolute ethyl alcohol；Described reactor is poly-
Tetrafluoroethene liner reactor.
4. a kind of carbon quantum dot preparation method decomposed based on polyethyleneimine according to claim 1 and 2, its feature exists
In step（2）Described in Gradient column chromatography method to use neutral alumina or silica gel for chromatography be fixing phase, adopt ethanol for
Solvent.
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| 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 |
| 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 |
| CN108493409B (en) * | 2018-03-12 | 2021-02-26 | 安徽大学 | Preparation method of nitrogen-doped carbon-coated flower-shaped nano 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 |
| 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 |
| CN112072106B (en) * | 2020-08-28 | 2022-04-08 | 浙江大学 | Conductive adhesive material, preparation method thereof, negative electrode plate and lithium ion battery |
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| US8357507B2 (en) * | 2010-03-08 | 2013-01-22 | Cromoz Inc. | Water soluble fluorescent quantum carbon dots |
| CN102675565A (en) * | 2012-05-09 | 2012-09-19 | 天津大学 | Carbon quantum dot-poly N-isopropylacrylamide composite material and preparation method thereof |
| CN103497762B (en) * | 2013-06-26 | 2015-03-25 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
| CN103756675A (en) * | 2014-01-17 | 2014-04-30 | 西安亚博生物技术有限公司 | Nitrogen doped carbon quantum dot as well as preparation method and application thereof |
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