CN104017576B - A kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot - Google Patents
A kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot Download PDFInfo
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- CN104017576B CN104017576B CN201410280811.1A CN201410280811A CN104017576B CN 104017576 B CN104017576 B CN 104017576B CN 201410280811 A CN201410280811 A CN 201410280811A CN 104017576 B CN104017576 B CN 104017576B
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Abstract
The invention discloses a kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot.Concrete steps are, take a certain amount of citrate of lime and urea adds in suitable quantity of water, stir and obtain suspension, in microwave oven, rotate 3 ~ 10min under 400 ~ 800W, reaction products therefrom are put into drying 0.5 ~ 5h at vacuum drying oven 40 ~ 80 DEG C.With methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution evaporation is done, and utilize silicagel column to carry out column chromatography to obtain nitrogen-doped carbon quantum dot.This heterogeneous procedures is compared with previous method, and the reaction times is short, reaction instrument is simple, preparation process convenient, and expands the range of choice of carbon source, is a kind of method of green syt nitrogen-doped carbon quantum dot.
Description
Technical field
The invention belongs to technical field prepared by nitrogen-doped carbon quantum dot, relate to a kind of method of microwave reaction synthetic nitrogen doping carbon quantum dot.
Background technology
Carbon quantum dot is the Novel Carbon Nanomaterials received much concern recent years, and the characteristics such as preparation is simple, environmental friendliness, bio-toxicity are low, good stability that it has, have potential application prospect in fields such as solar cell, cell imaging, pharmaceutical carrier, LED.
Microwave carborization, because the reaction times is short, productive rate is high, is widely used in the synthesis of carbon quantum dot.Through retrieval, publication number is the Chinese invention patent of CN102604629A, discloses " preparation method of amino-carbon quantum dot and application thereof ".It is characterized in that comprising the following steps: with the aqueous phosphatic of glucosamine for raw material, take microwave oven as reaction platform, the carbon quantum dot of fluorescence property is prepared in heating, by going out residue and moisture after dialysis and rotary evaporation, simple to operate, cost is low, yield is high, preparation technology's device simple, and can in very short time complete operation, be easy to promote.The carbon quantum dot rich surface obtained is containing amino, and soluble in water, fluorescence quantum yield improves greatly, and is used successfully to viable cell labelling, has broad application prospects.
Publication number is the Chinese invention patent of CN103771390A, discloses " a kind of method of bioactive enzyme assisted microwave synthesis method synthesis carbon quantum dot, the carbon quantum dot prepared thus and application thereof ".It is characterized in that comprising the following steps: carbon matrix precursor and bioactive enzyme ultrasonic disperse in deionized water, are made the transparent aqueous solution by (1); (2) solution obtained in step (1) is placed in household microwave oven and carries out microwave heating, after reaction, obtain the carbon quantum dot that brown color liquid is biological activity enzyme modification; (3) the carbon quantum dot solution dialysis tubing be obtained by reacting in step (2) is dialysed, remove unreacted carbon matrix precursor and bioactive enzyme.The method productive rate is high, and the fluorescent carbon quantum dot of preparation is that bioactive enzyme is modified, and can enter in nucleus, thus have the diagnosis and treatment function to cancer; Adopt bioactive enzyme as the promoting agent reacted and passivation agents, with citric acid, Citrate trianion, glucose, fructose or amylose starch for carbon precursor, make fluorescent carbon quantum dot biological safety in preparation and use procedure good; Employing microwave process for synthesizing is with low cost.
Those skilled in the art is devoted to develop that a kind of reaction times is short, reaction instrument is simple, raw material is easy to get, preparation process facilitates easy carbon quantum dot synthetic method.
Summary of the invention
Technical problem to be solved by this invention is: adopt citrate of lime and urea are reaction raw materials and provide a kind of method based on Microwave synthesize nitrogen-doped carbon quantum dot.
Object of the present invention can be achieved through the following technical solutions: take a certain amount of citrate of lime and urea adds in suitable quantity of water, solution stirring is even, in microwave oven, after rotating for some time with certain power microwave, product is put into vacuum drying oven dry for some time, with methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution evaporation is done, and utilize silicagel column to carry out column chromatography to obtain nitrogen-doped carbon quantum dot.
Concrete scheme of the present invention is, a kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprises the following steps:
A. in beaker, add pure water, then add citrate of lime and urea;
B. react in microwave oven, reacted beaker is taken out, put into vacuum drying oven dry;
C. use methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution evaporation is done, and utilize silicagel column to carry out column chromatography to obtain nitrogen-doped carbon quantum dot.
Preferably, in above-mentioned steps a, the amount of pure water is 5 ~ 20ml, and the quality of citrate of lime is 1 ~ 10g, and the quality of urea is 1 ~ 10g.
Preferably, the microwave power of above-mentioned steps b is 400 ~ 800W, and the time of reacting in microwave is 3 ~ 10min, and time of drying is 0.5 ~ 5h, and drying temperature is 40 ~ 80 DEG C.
Preferably, the height of the silicagel column in above-mentioned steps c is 1/3 ~ 2/3 of chromatography column, the mixed solution that elutriant is selected from methylene dichloride or is formed by methylene dichloride and methanol mixed.
More preferably, above-mentioned elutriant by methylene dichloride and methyl alcohol according to volume ratio methylene dichloride: methyl alcohol=1:0 ~ 1:1 is mixed to form.
Compared to prior art, heterogeneous procedures of the present invention is compared with previous method, and the reaction times is short, reaction instrument is simple, preparation process convenient, and expands the range of choice of carbon source, is a kind of method of green syt nitrogen-doped carbon quantum dot.
Accompanying drawing explanation
Fig. 1 is schematic diagram of the present invention;
Fig. 2 is the ultraviolet-visible absorption spectra figure of the nitrogen-doped carbon quantum dot that the embodiment of the present invention 1 is synthesized;
Fig. 3 is the transmission electron microscopy figure of the nitrogen-doped carbon quantum dot that the embodiment of the present invention 1 is synthesized.
Embodiment
Embodiment 1
Based on a method for citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprise the following steps:
A. get the beaker of 25ml, add 10ml pure water, then add 3g citrate of lime and 3g urea;
B. reaction 3min in the household microwave oven (800W), takes out reacted beaker, puts into dry 2h at vacuum drying oven 60 DEG C;
C. use methanol extraction nitrogen-doped carbon quantum dot, be spin-dried for by solution in Rotary Evaporators, and utilize silica gel chromatographic column column chromatography, wherein the height of silicagel column is at 1/3 place of chromatography column, and elutriant is methylene dichloride, obtains nitrogen-doped carbon quantum dot.
Embodiment 2
Based on a method for citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprise the following steps:
A. get the beaker of 25ml, add 10ml pure water, then add 1g citrate of lime and 3g urea;
B. reaction 8min in the household microwave oven (600W), takes out reacted beaker, puts into dry 5h at vacuum drying oven 40 DEG C;
C. methanol extraction nitrogen-doped carbon quantum dot is used, in Rotary Evaporators, solution is spin-dried for, wherein the height of silicagel column is at 1/2 place of chromatography column, and elutriant is methylene dichloride and the methyl alcohol mixed liquor of volume ratio 2:1, and utilizes silica gel chromatographic column column chromatography to obtain nitrogen-doped carbon quantum dot.
Embodiment 3
Based on a method for citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprise the following steps:
A. get the beaker of 25ml, add 10ml pure water, then add 2g citrate of lime and 3g urea;
B. reaction 10min in the household microwave oven (400W), takes out reacted beaker, puts into dry 0.5h at vacuum drying oven 80 DEG C;
C. methanol extraction nitrogen-doped carbon quantum dot is used, be spin-dried for by solution in Rotary Evaporators, and utilize silica gel chromatographic column column chromatography, wherein the height of silicagel column is at 2/3 place of chromatography column, methylene dichloride and the methyl alcohol mixed liquor of elutriant to be volume ratio be 1:1, obtain nitrogen-doped carbon quantum dot.
Embodiment 4
Based on a method for citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprise the following steps:
A. get the beaker of 50ml, add 20ml pure water, then add 10g citrate of lime and 10g urea;
B. reaction 10min in the household microwave oven (400W), takes out reacted beaker, puts into dry 0.5h at vacuum drying oven 80 DEG C;
C. methanol extraction nitrogen-doped carbon quantum dot is used, be spin-dried for by solution in Rotary Evaporators, and utilize silica gel chromatographic column column chromatography, wherein the height of silicagel column is at 2/3 place of chromatography column, methylene dichloride and the methyl alcohol mixed liquor of elutriant to be volume ratio be 1:1, obtain nitrogen-doped carbon quantum dot.
Embodiment 5
Based on a method for citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprise the following steps:
A. get the beaker of 25ml, add 5ml pure water, then add 1g citrate of lime and 1g urea;
B. reaction 10min in the household microwave oven (400W), takes out reacted beaker, puts into dry 0.5h at vacuum drying oven 80 DEG C;
C. methanol extraction nitrogen-doped carbon quantum dot is used, be spin-dried for by solution in Rotary Evaporators, and utilize silica gel chromatographic column column chromatography, wherein the height of silicagel column is at 2/3 place of chromatography column, methylene dichloride and the methyl alcohol mixed liquor of elutriant to be volume ratio be 1:1, obtain nitrogen-doped carbon quantum dot.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art 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 (5)
1., based on a method for citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, it is characterized in that, comprise the following steps:
A. in beaker, add 5 ~ 20ml pure water, then add 1 ~ 10g citrate of lime and 1 ~ 10g urea;
B. be react 3 ~ 10min in the microwave oven of 400 ~ 800W at power, after having reacted, beaker taken out, put into vacuum drying oven dry;
C. use methanol extraction nitrogen-doped carbon quantum dot, done by solution evaporation in Rotary Evaporators, recycling silicagel column carries out column chromatography and obtains nitrogen-doped carbon quantum dot.
2., according to a kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, the time of drying in step b is 0.5 ~ 5h, and drying temperature is 40 ~ 80 DEG C.
3. according to a kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, the height of the silicagel column in step c is 1/3 ~ 2/3 of chromatography column, the mixed solution that elutriant is selected from methylene dichloride or is formed by methylene dichloride and methanol mixed.
4., according to a kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot described in claim 3, it is characterized in that, described elutriant by methylene dichloride and methyl alcohol according to volume ratio methylene dichloride: methyl alcohol=1:0 ~ 1:1 is mixed to form.
5. the nitrogen-doped carbon quantum dot that according to claim arbitrary in Claims 1-4 prepared by method.
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| CN105018081B (en) * | 2015-06-30 | 2017-08-25 | 中国科学院理化技术研究所 | A kind of carbon quantum dot laccase model of supported copper and its production and use |
| CN105176528B (en) * | 2015-08-24 | 2018-02-23 | 中物院成都科学技术发展中心 | A kind of preparation method of nitrogen-doped carbon based quantum dot |
| CN105419793A (en) * | 2015-12-28 | 2016-03-23 | 江南大学 | Method for microwave synthesis of carbon quantum dots on basis of citric acid and hexamethylene tetramine |
| CN108328607B (en) * | 2018-02-12 | 2021-05-11 | 吉林师范大学 | Ultra-small blue-green light dual-emission nitrogen and chlorine co-doped graphene quantum dot and preparation method thereof |
| CN108767117B (en) * | 2018-06-07 | 2020-04-07 | 吉林大学 | Perovskite solar cell based on carbon quantum dot doped anti-solvent passivated grain boundary defects and preparation method thereof |
| CN108844935B (en) * | 2018-07-06 | 2020-07-24 | 山西大同大学 | Preparation method and application of boron-nitrogen co-doped carbon dots |
| CN109853068B (en) * | 2019-01-30 | 2021-08-10 | 东华大学 | Carbon quantum dot/fibroin composite nanofiber and preparation method and application thereof |
| CN111229286B (en) * | 2020-03-24 | 2021-03-23 | 吉林大学 | Catalytic material, preparation method thereof and photocatalyst |
| CN114835105B (en) * | 2022-05-20 | 2023-11-28 | 中国石油大学(华东) | Method for preparing carbon dots with temperature resistance, salt resistance and drag reduction performance, product and application thereof |
| CN116376642B (en) * | 2023-04-10 | 2024-03-22 | 北京中铁科新材料技术有限公司 | Environment-friendly nano insulator cleaning agent and preparation method thereof |
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| CN103045242A (en) * | 2013-01-21 | 2013-04-17 | 吉林大学 | Preparation method of carbon dot having high fluorescent quantum yield |
| CN103663412A (en) * | 2013-12-05 | 2014-03-26 | 中国科学院大学 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
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