CN103332674B - Method for hydrothermally synthesizing carbon quantum dots on basis of tartaric acid and organic amine - Google Patents
Method for hydrothermally synthesizing carbon quantum dots on basis of tartaric acid and organic amine Download PDFInfo
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Abstract
The invention discloses a method for hydrothermally synthesizing carbon quantum dots on basis of tartaric acid and organic amine. The method comprises the steps of: adding tartaric acid into water, then adding organic amine, evenly mixing the solution, adding in a hydrothermal reaction kettle, reacting at 150-220 DEG C for 18-36 hours, conducting dialysis treatment to obtain impurity-free carbon quantum dots. The invention provides a new method for synthesizing carbon quantum dots, and the carbon quantum dots which are good in controllability and uniform in particle size can be synthesized.
Description
Technical field
The present invention relates to a kind of nano material synthetic method, be specifically related to a kind of method of Hydrothermal Synthesis carbon quantum dot.
Background technology
The research of Illuminant nanometer material attracts the broad interest of the scientist in the fields such as material, physics, chemistry, as organic dye, fluorescin, gold and silver nanocluster, semiconductor-quantum-point, silicon quantum dot and carbon quantum dot etc.Relative to traditional semiconductor-quantum-point and organic dye, carbon quantum dot has lower toxicity, higher is water-soluble, excellent chemical stability and good biocompatibility, therefore carbon quantum dot has wide practical use in biomarker, fluorescence imaging and pharmaceutical carrier etc., is current study hotspot.
The synthetic method of carbon quantum dot is a lot, can be classified as two classes, method and from bottom to top method from top to bottom.Bottom-to-top method utilizes raw material widely, synthesizes luminous carbon quantum dot of different nature.More classical synthetic method mainly contains: the method (Chem.Mater.2009 of sugar nitration mixture process passivation again; 21,5563-5565.); Sugar is ultrasonic method (Carbon2011 under acid or alkaline conditions; 49,605-609.); Vanadium Pentoxide in FLAKES and acetic acid direct reaction method (ACS Nano2012; 6,400-409.); Citric acid and thanomin pyrolysis method (J.Am.Chem.Soc.2012; 134,747-750.); Amino acid hydrothermal method or carborization (Chem.Commun.2012; 48,3984-3986. and Chem.Eur.J.2013; 19,2276-2283.).Present method adopts Self-absorption Correction Factor, utilizes tartrate and organic amine Hydrothermal Synthesis carbon quantum dot.
Summary of the invention
Problem to be solved by this invention is the method adopting novel raw water thermal synthesis carbon quantum dot.
For achieving the above object, a kind of method carrying out Hydrothermal Synthesis carbon quantum dot based on tartrate and organic amine is provided.Be achieved through the following technical solutions: take a certain amount of tartrate and add in suitable quantity of water, add organic amine, solution mixes, and adds in hydrothermal reaction kettle, at 150 ~ 220 DEG C, be incubated 18 ~ 36 hours, utilize dialysis treatment to obtain pure carbon quantum dot.
Based on a method for the Hydrothermal Synthesis carbon quantum dot of tartrate and organic amine, specifically comprise the following steps:
Step 1, tartrate is added to the water, more slowly adds organic amine wherein, forms solution;
Step 2, adds in sealed reactor by above-mentioned solution, hydro-thermal reaction;
Step 3, takes out reaction solution, removes impurity, obtain pure carbon quantum dot by dialysis.
Tartrate in described step 1 and organic amine are analytical reagent, without purification process, directly use; Described a certain amount of tartaric amount is 0.5 ~ 2g; The amount of described suitable quantity of water is 20 ~ 40mL, and the amount of described a certain amount of thanomin is 0.5 ~ 2mL; Described organic amine is thanomin, diethanolamine or trolamine.Hydrothermal reaction kettle volume in described step 2 is 50mL; Described hydrothermal reaction condition is be incubated 18 ~ 36 hours at 150 ~ 220 DEG C; Described soaking time Duan Weicong temperature starts timing when being raised to temperature of reaction; Cooling adopts naturally cooling; Dialysis tubing in described step 3 adopts the dialysis tubing of 500 ~ 3000Da, is put in the beaker of 1 ~ 5L, dialysis treatment.
Hydrothermal method synthesis carbon quantum dot, can synthesize controllability good, the carbon quantum dot that size of particles is homogeneous.Tartrate and organic amine synthesis carbon quantum dot are a kind of methods of synthesizing carbon quantum dot from bottom to top of novelty.
Be described further to design of the present invention, the concrete technique effect implemented and produce, to understand object of the present invention, characteristic sum effect fully below.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the carbon quantum dot that thanomin and tartrate hydro-thermal reaction obtain
Fig. 2 is the TEM figure of the carbon quantum dot that trolamine and tartrate hydro-thermal reaction obtain
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Step 1, weighs 1g tartrate and adds in 25mL water, slowly add 1mL thanomin wherein;
Step 2, adds above-mentioned solution in 50mL sealed reactor, at 160 DEG C, be incubated 24 hours;
Step 3, takes out reaction solution, removes impurity, obtain pure carbon quantum dot by dialysis.
Embodiment 2
Step 1, the tartrate weighing 1g adds in 25mL water, slowly adds 1mL diethanolamine wherein;
Step 2, adds above-mentioned solution in 50mL sealed reactor, at 160 DEG C, be incubated 24 hours;
Step 3, takes out reaction solution, removes impurity, obtain pure carbon quantum dot by dialysis.
Embodiment 3
Step 1, the tartrate weighing 1g adds in 25mL water, slowly adds 1mL trolamine wherein;
Step 2, added above-mentioned solution in 50mL sealed reactor, 160 DEG C of insulations 24 hours;
Step 3, takes out reaction solution, removes impurity, obtain pure carbon quantum dot by dialysis.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that the ordinary skill of this area just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (2)
1., based on a method for tartrate and organic amine Hydrothermal Synthesis carbon quantum dot, it is characterized in that, the method comprises the following steps:
Step 1, first adds 0.5 ~ 2g tartrate in 20 ~ 40mL water, then adds 0.5 ~ 2mL organic amine, forms solution;
Step 2, adds in sealed reactor by above-mentioned solution, and reactor volume is 50mL, hydro-thermal reaction 18 ~ 36 hours at 150 ~ 220 DEG C, timing when the reaction times is for being raised to temperature of reaction from temperature, naturally cooling;
Step 3, takes out reaction solution, removes impurity, obtain pure carbon quantum dot by dialysis;
Described organic amine is thanomin, diethanolamine or trolamine;
The dialysis tubing of described dialysis employing 1000 ~ 3000Da, is put in the beaker of 1 ~ 5L, dialysis treatment.
2., according to a kind of method based on tartrate and organic amine Hydrothermal Synthesis carbon quantum dot described in claim 1, it is characterized in that, wherein said tartrate and described organic amine are analytical reagent.
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| CN105647526B (en) * | 2015-12-30 | 2018-01-16 | 五邑大学 | A kind of nearly full spectrum fluorescent nano-sized carbon point and preparation method thereof |
| CN105713608B (en) * | 2016-01-27 | 2018-05-18 | 太原理工大学 | A kind of preparation method of the controllable nitrogen-doped carbon quantum dot of size |
| CN105754593B (en) * | 2016-01-27 | 2018-04-24 | 山西大学 | A kind of hollow fluorescent carbon quantum dot and its preparation method and application |
| CN106634979B (en) * | 2016-11-16 | 2019-11-05 | 新疆维吾尔自治区产品质量监督检验研究院 | A kind of Nitrogen doped carbon quantum dot and preparation method and application |
| CN110343521B (en) * | 2018-04-02 | 2022-05-06 | 中国科学院宁波材料技术与工程研究所 | Thermal response phosphorescent material, preparation method and application thereof |
| CN109266340A (en) * | 2018-12-06 | 2019-01-25 | 钦州学院 | A kind of preparation method and applications of nitrogen-doped carbon quantum dot |
| CN113698928A (en) * | 2021-09-02 | 2021-11-26 | 深圳大学 | Carbon dot, preparation method thereof and application of carbon dot in preparation of mitochondrial-targeted fluorescent probe |
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| CN103086355A (en) * | 2013-02-01 | 2013-05-08 | 浙江大学 | Synthetic method of carbon quantum dot material |
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| CN102849724A (en) * | 2012-10-12 | 2013-01-02 | 上海交通大学 | Preparation method of water-soluble carbon quantum dots |
| CN103045242A (en) * | 2013-01-21 | 2013-04-17 | 吉林大学 | Preparation method of carbon dot having high fluorescent quantum yield |
| CN103086355A (en) * | 2013-02-01 | 2013-05-08 | 浙江大学 | Synthetic method of carbon quantum dot material |
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