CN104017576A - Method for synthesizing nitrogen-doped carbon quantum dots based on calcium citrate and urea microwave reaction - Google Patents
Method for synthesizing nitrogen-doped carbon quantum dots based on calcium citrate and urea microwave reaction Download PDFInfo
- Publication number
- CN104017576A CN104017576A CN201410280811.1A CN201410280811A CN104017576A CN 104017576 A CN104017576 A CN 104017576A CN 201410280811 A CN201410280811 A CN 201410280811A CN 104017576 A CN104017576 A CN 104017576A
- Authority
- CN
- China
- Prior art keywords
- carbon quantum
- quantum dot
- urea
- citrate
- lime
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Luminescent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for synthesizing nitrogen-doped carbon quantum dots based on calcium citrate and urea microwave reaction. The method comprises the steps of weighing a certain amount of calcium citrate and urea, adding calcium citrate and urea into a proper amount of water, stirring uniformly to obtain a suspension, rotating for 3-10min in a microwave oven at 400-800W, and drying the reaction product in a vacuum drying oven at 40-80 DEG C for 0.5-5h; extracting nitrogen-doped carbon quantum dots by using methanol, evaporating the solution in a rotary evaporator, and performing column chromatography by using a silica gel column to obtain the nitrogen-doped carbon quantum dots. Compared with the conventional method, the heterogeneous method has the advantages that the reaction time is short, reaction instruments are simple, the preparation process is convenient, and the selection range of a carbon source is enlarged, so that the method is a green method for synthesizing nitrogen-doped carbon quantum dots.
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 receiving much concern recent years, and the characteristics such as it has, and preparation is simple, environmental friendliness, bio-toxicity are low, good stability, 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 synthetic of carbon quantum dot.Through retrieval, the Chinese invention patent that publication number is CN102604629A, discloses " preparation method of amino-carbon quantum dot and application thereof ".It is characterized in that comprising the following steps: the aqueous phosphatic of glucosamine of take is 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, at utmost point complete operation in the short period of time, be easy to promote.The carbon quantum dot rich surface obtaining is containing amino, and soluble in water, fluorescence quantum yield improves greatly, and successfully for viable cell labelling, has broad application prospects.
Publication number is the Chinese invention patent of CN103771390A, discloses " method of the synthetic carbon quantum dot of a kind of bioactive enzyme assisted microwave synthesis method, carbon quantum dot and the application thereof of preparation thus ".It is characterized in that comprising the following steps: (1) is by carbon matrix precursor and bioactive enzyme is ultrasonic is scattered in deionized water, makes the transparent aqueous solution; (2) solution obtaining in step (1) is placed in to 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) carbon quantum dot solution reaction in step (2) being obtained is dialysed with dialysis tubing, removes 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, thereby have the diagnosis and treatment function to cancer; Adopt bioactive enzyme as promoting agent and the passivation agents of reaction, take citric acid, Citrate trianion, glucose, fructose or amylose starch as 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 for reaction raw materials and a kind of method based on microwave synthetic nitrogen doping carbon quantum dot is provided.
Object of the present invention can be achieved through the following technical solutions: take a certain amount of citrate of lime and urea and add in suitable quantity of water, solution stirring is even, in microwave oven, with certain power microwave, after rotation for some time, product is put into dry for some time of vacuum drying oven, with methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution evaporation is dry, and utilize silicagel column to carry out column chromatography to obtain nitrogen-doped carbon quantum dot.
Concrete scheme of the present invention is that 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. in microwave oven, react, 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 dry, 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 be 0.5～5h time of drying, and drying temperature is 40～80 ℃.
Preferably, the height of the silicagel column in above-mentioned steps c is chromatography column 1/3～2/3, 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.
Than prior art, heterogeneous method of the present invention is compared with previous method, and the reaction times is short, reaction instrument is simple, preparation process convenient, and has expanded the range of choice of carbon source, is a kind of method of green synthetic nitrogen doping carbon quantum dot.
Accompanying drawing explanation
Fig. 1 is schematic diagram of the present invention;
Fig. 2 is that the UV, visible light of the synthetic nitrogen-doped carbon quantum dot of the embodiment of the present invention 1 absorbs spectrogram;
Fig. 3 is the transmission electron microscopy figure of the synthetic nitrogen-doped carbon quantum dot of the embodiment of the present invention 1.
Embodiment
Embodiment 1
A method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprises 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 household microwave oven (800W), takes out reacted beaker, puts into dry 2h at 60 ℃ of vacuum drying ovens;
C. use methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution is spin-dried for, 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
A method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprises 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 household microwave oven (600W), takes out reacted beaker, puts into dry 5h at 40 ℃ of vacuum drying ovens;
C. use methanol extraction nitrogen-doped carbon quantum dot, 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
A method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprises 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 household microwave oven (400W), takes out reacted beaker, puts into dry 0.5h at 80 ℃ of vacuum drying ovens;
C. use methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution is spin-dried for, and utilizes silica gel chromatographic column column chromatography, wherein the height of silicagel column is at 2/3 place of chromatography column, elutriant is that volume ratio is methylene dichloride and the methyl alcohol mixed liquor of 1:1, obtains nitrogen-doped carbon quantum dot.
Embodiment 4
A method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprises 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 household microwave oven (400W), takes out reacted beaker, puts into dry 0.5h at 80 ℃ of vacuum drying ovens;
C. use methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution is spin-dried for, and utilizes silica gel chromatographic column column chromatography, wherein the height of silicagel column is at 2/3 place of chromatography column, elutriant is that volume ratio is methylene dichloride and the methyl alcohol mixed liquor of 1:1, obtains nitrogen-doped carbon quantum dot.
Embodiment 5
A method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, specifically comprises 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 household microwave oven (400W), takes out reacted beaker, puts into dry 0.5h at 80 ℃ of vacuum drying ovens;
C. use methanol extraction nitrogen-doped carbon quantum dot, in Rotary Evaporators, solution is spin-dried for, and utilizes silica gel chromatographic column column chromatography, wherein the height of silicagel column is at 2/3 place of chromatography column, elutriant is that volume ratio is methylene dichloride and the methyl alcohol mixed liquor of 1:1, obtains 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 can design according to the present invention make many modifications and variations without creative work.Therefore, all technician in the art, all should be in the determined protection domain by 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 (10)
1. the method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot, is characterized in that, comprises the following steps:
A. in beaker, add pure water, then add citrate of lime and urea;
B. in microwave oven, react, after having 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 dry, 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 synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, the amount of pure water described in step a is 5～20ml.
3. according to a kind of method based on citrate of lime and urea microwave synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, the quality of citrate of lime described in step a is 1～10g.
4. according to a kind of method based on citrate of lime and urea microwave synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, the quality of urea described in step a is 1～10g.
5. according to a kind of method based on citrate of lime and urea microwave synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, the power of microwave oven described in step b is 400～800W.
6. according to a kind of method based on citrate of lime and urea microwave synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, the time of reacting in described microwave oven in step b is 3～10min.
7. according to a kind of method based on citrate of lime and urea microwave synthetic nitrogen doping carbon quantum dot described in claim 1, it is characterized in that, be 0.5～5h the time of drying in step b, and drying temperature is 40～80 ℃.
8. according to a kind of method based on citrate of lime and urea microwave 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.
9. a kind of method based on citrate of lime and urea microwave synthetic nitrogen doping carbon quantum dot described according to Claim 8, 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.
10. the nitrogen-doped carbon quantum dot of preparing according to method described in arbitrary claim in claim 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410280811.1A CN104017576B (en) | 2014-06-20 | 2014-06-20 | A kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410280811.1A CN104017576B (en) | 2014-06-20 | 2014-06-20 | A kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104017576A true CN104017576A (en) | 2014-09-03 |
| CN104017576B CN104017576B (en) | 2016-01-13 |
Family
ID=51434588
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410280811.1A Active CN104017576B (en) | 2014-06-20 | 2014-06-20 | A kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104017576B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018081A (en) * | 2015-06-30 | 2015-11-04 | 中国科学院理化技术研究所 | Copper-loaded carbon quantum dot simulation laccase and preparation method and application thereof |
| CN105176528A (en) * | 2015-08-24 | 2015-12-23 | 中物院成都科学技术发展中心 | 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 |
| CN108328607A (en) * | 2018-02-12 | 2018-07-27 | 吉林师范大学 | Nitrogen, the chlorine of a kind of double transmittings of super-small blue green light are co-doped with graphene quantum dot and preparation method thereof |
| CN108767117A (en) * | 2018-06-07 | 2018-11-06 | 吉林大学 | A kind of perovskite solar cell and preparation method thereof being passivated grain boundary defects based on carbon quantum dot doping anti-solvent |
| CN108844935A (en) * | 2018-07-06 | 2018-11-20 | 山西大同大学 | A kind of preparation method and application of the nitrogen co-doped carbon dots of boron |
| CN109853068A (en) * | 2019-01-30 | 2019-06-07 | 东华大学 | A kind of carbon quantum dot/fibroin composite nano fiber and its preparation method and application |
| CN111229286A (en) * | 2020-03-24 | 2020-06-05 | 吉林大学 | Catalytic material, preparation method thereof and photocatalyst |
| CN114835105A (en) * | 2022-05-20 | 2022-08-02 | 中国石油大学(华东) | Method for preparing temperature-resistant salt-tolerant and resistance-reducing carbon dots, product and application thereof |
| CN116376642A (en) * | 2023-04-10 | 2023-07-04 | 北京中铁科新材料技术有限公司 | Environment-friendly nano insulator cleaning agent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103834397A (en) * | 2014-03-11 | 2014-06-04 | 太原理工大学 | Method for preparing water-soluble fluorescent carbon dots |
-
2014
- 2014-06-20 CN CN201410280811.1A patent/CN104017576B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103834397A (en) * | 2014-03-11 | 2014-06-04 | 太原理工大学 | Method for preparing water-soluble fluorescent carbon dots |
Non-Patent Citations (1)
| Title |
|---|
| XINYUN ZHAI ET. AL.: "Highly luminescent carbon nanodots by microwave-assisted pyrolysis", 《CHEM. COMMUN.》 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018081A (en) * | 2015-06-30 | 2015-11-04 | 中国科学院理化技术研究所 | Copper-loaded carbon quantum dot simulation laccase and preparation method and application thereof |
| CN105176528A (en) * | 2015-08-24 | 2015-12-23 | 中物院成都科学技术发展中心 | 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 |
| CN108328607A (en) * | 2018-02-12 | 2018-07-27 | 吉林师范大学 | Nitrogen, the chlorine of a kind of double transmittings of super-small blue green light are co-doped with graphene quantum dot and preparation method thereof |
| CN108767117A (en) * | 2018-06-07 | 2018-11-06 | 吉林大学 | A kind of perovskite solar cell and preparation method thereof being passivated grain boundary defects based on carbon quantum dot doping anti-solvent |
| CN108844935A (en) * | 2018-07-06 | 2018-11-20 | 山西大同大学 | A kind of preparation method and application of the nitrogen co-doped carbon dots of boron |
| 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 |
| CN109853068A (en) * | 2019-01-30 | 2019-06-07 | 东华大学 | A kind of carbon quantum dot/fibroin composite nano fiber and its preparation method and application |
| CN109853068B (en) * | 2019-01-30 | 2021-08-10 | 东华大学 | Carbon quantum dot/fibroin composite nanofiber and preparation method and application thereof |
| CN111229286A (en) * | 2020-03-24 | 2020-06-05 | 吉林大学 | Catalytic material, preparation method thereof and photocatalyst |
| CN114835105A (en) * | 2022-05-20 | 2022-08-02 | 中国石油大学(华东) | Method for preparing temperature-resistant salt-tolerant and resistance-reducing carbon dots, product and application thereof |
| 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 |
| CN116376642A (en) * | 2023-04-10 | 2023-07-04 | 北京中铁科新材料技术有限公司 | Environment-friendly nano insulator cleaning agent and preparation method 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104017576B (en) | 2016-01-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104017576B (en) | A kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot | |
| CN104192827A (en) | Method for synthesizing carbon quantum dots on basis of organic micromolecule microwave solid-phase reaction | |
| CN100473630C (en) | Carrier type slow-release fertilizer and preparing method thereof | |
| CN103693633B (en) | The method of the synthetic fluorescence chiral carbon point of a kind of green | |
| CN101864036B (en) | Method for synthesizing super absorbent resin by plant straw | |
| CN103965372B (en) | The preparation method of a kind of chitosan-gallic acid graft copolymer | |
| CN103408346B (en) | Polymerization amino acid synergistic sustained-release composite fertilizer and preparation method thereof | |
| CN106222218A (en) | A kind of enzyme process prepares the method for rhodioside | |
| CN107382718B (en) | The method of the mesoporous alkaline molecular sieve catalyzed alcoholysis polylactic acid of CaO/MCF | |
| CN104710983A (en) | Method for preparing nitrogen-doped graphene quantum dots through metal ion coordination catalysis | |
| CN112522339B (en) | Method for preparing 3-acetamido-5-acetylfuran by degrading N-acetyl-D-glucosamine by using chitin | |
| CN104017577B (en) | A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia | |
| CN109956987A (en) | Ammonolysis method and ammonolysis composition | |
| CN105797688A (en) | Preparation method and application of gel particle adsorbent | |
| CN106631709B (en) | Method for extracting and nitrating hydroxytyrosol | |
| CN106010517B (en) | Using coke powder as carbon quantum dot fluorescence labeling material of carbon source and preparation method thereof | |
| CN111995794B (en) | Cyclodextrin porous liquid material and application thereof | |
| CN108774290A (en) | Resveratrol-carboxyalkyl type ring dextrin derivative and preparation method thereof | |
| CN115043727A (en) | Method for preparing 3-bromobutyrate compound and 3-hydroxybutyrate compound by degrading poly-3-hydroxybutyrate | |
| CN105439880A (en) | Preparation method of calcium glycinate | |
| CN102329286A (en) | Novel method for synthesizing 3-oxetanone | |
| CN105080527A (en) | Composite catalyst and preparation method thereof and lignin depolymerization method | |
| CN102584534A (en) | Method for producing mannite through adopting Raney's nickel and Raney's copper in coordination with catalytic hydrogenation | |
| CN107602623B (en) | Transition metal cobalt complex containing multi-coordination sites and preparation method thereof | |
| CN1899336A (en) | Method for preparing ginseng anti-cancer active component by immobilized enzyme |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |