CN105502338A - Method for microwave preparation of fluorescent carbon dots with green onion as raw material - Google Patents
Method for microwave preparation of fluorescent carbon dots with green onion as raw material Download PDFInfo
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- CN105502338A CN105502338A CN201511004642.XA CN201511004642A CN105502338A CN 105502338 A CN105502338 A CN 105502338A CN 201511004642 A CN201511004642 A CN 201511004642A CN 105502338 A CN105502338 A CN 105502338A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a method for microwave preparation of fluorescent carbon dots with a green onion as a raw material, and relates to the field of preparation of fluorescent nano materials. One green onion is taken and smashed through a smashing machine, a certain quantity of the smashed green onion is weighed out and put into a beaker, a microwave reaction is carried out for a period of time in a microwave oven, and 50 mL to 300 mL of deionized water is added to the obtained product for magnetic stirring for 8 min; then ultrasonic treatment is carried out, evenly-dispersed suspension liquid is obtained and is centrifuged, and supernate is extracted; the obtained supernate is dialyzed, filtering is carried out through a filter membrane, rotary evaporation and concentration are carried out to obtain a concentrated carbon quantum dot solution, then the carbon quantum dot solution is subjected to freeze drying at the temperature of -50 DEG C, and finally carbon quantum dot solid powder is obtained. No chemical reagent needs to be added to the reaction raw material, only the green onion is adopted as the raw material, the raw material is wide and easy to obtain, the preparation method is simple, and the prepared fluorescent carbon dots are good in water solubility and high in stability and can be applied to the field of bioimaging, analysis and detection and the like.
Description
Technical field
The present invention relates to a kind of preparation of fluorescent nano material, particularly relating to a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point.
Background technology
Carbon point (CarbonDots, CDs) is a kind of novel fluorescence carbon nano-particles occurred in recent years.2004, Xu (JAm.Chem.Soc, 2004, Late Cambrian sends the material of fluorescence under ultra violet lamp when Single Walled Carbon Nanotube prepared by cigarette ash 126:12736) etc. produced at purification arc-over, obtains three groups of different fluorescent carbon nano-particles of molecular weight through further electrophoretic separation.Traditional semiconductor-quantum-point is due to defects such as the toxicity problem that self exists and optical flare phenomenons, and the HUMAN HEALTH brought thus and the impacts such as the potential harm of environment are constrained to its application widely.Fluorescent carbon point has good fluorescent stability, unglazed scintillation, excellent water-soluble and biocompatibility, hypotoxicity, excitation wavelength and emission wavelength controllable, and there is the performance of a series of excellences such as fluorescence changes, making fluorescent carbon point replace the status of quantum dot in biomedicine becomes possibility.
The synthetic method of carbon point mainly contains Electrochemical preparation method, strong acid oxidation style, laser assisted preparation method; arc discharge method, ultrasonic method, but due to these preparation method's processing steps above-mentioned loaded down with trivial details; the more high factor of raw materials cost, causes the synthesis of fluorescent carbon point to be difficult to accomplish scale production.Therefore, explore simple, the eco-friendly preparation method of a kind of material equipment, the research of carbon point is significant undoubtedly.At present, utilize green material to synthesize the focus that carbon point is current research, the document about green syt carbon quantum dot of nearest report has: VaibhavkumarNM, SanjayJ, HirakenduB, RakeshKS, SureshKK.SensorsandActuatorsB.2015,213,434-443 (hydrothermal treatment consists of Sucus Mali pumilae); RuanSB, ZhuBY, ZhangHJ, ChenJT, ShenS, QianJ, HeQ, GaoHL.JournalofColloidandInterfaceScience.2014,422,25-29 (hydro-thermal Spider Web); WeiJM, ZhangX, ShengYZ, ShenJM, HuangP, GuoSK, PanJQ, FengBX.MaterialsLetters.2014,123,107-111 (hydrothermal treatment consists of Semen Maydis powder).Current most methods all lays particular emphasis on hydrothermal treatment consists, although the starting material in these methods are cheap and easy to get, and length consuming time.
Summary of the invention
The object of the invention is to for above-mentioned technological deficiency, provide a kind of carbon source green and wide material sources, fast and convenient mass-producing can prepare the method for carbon quantum dot.
For achieving the above object, the invention provides a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point, the present invention is achieved through the following technical solutions: get a green onion, pulverized with pulverizer, the green onion taking a certain amount of pulverizing is placed in beaker, microwave reaction for some time in microwave oven, the product obtained adds 50-300mL deionized water magnetic agitation 8min, then supersound process is carried out, obtain finely dispersed suspension liquid, suspension liquid is through centrifugal extraction supernatant liquor, by the supernatant liquor dialysis obtained, with membrane filtration, rotary evaporation is concentrated obtains concentrated carbon quantum dot solution, then at-50 DEG C, lyophilize finally obtains carbon quantum dot pressed powder.
Take green onion as the method that raw material microwave prepares fluorescent carbon point, specifically comprise the following steps:
Step 1, gets a green onion, is pulverized with pulverizer;
Step 2, the green onion taking a certain amount of pulverizing is placed in 50-250mL beaker, in microwave oven after microwave reaction for some time, cooling;
Step 3, adds 50-300mL deionized water magnetic agitation 8min, then carries out supersound process, obtain finely dispersed suspension liquid by the product of acquisition, suspension liquid is through centrifugal extraction supernatant liquor;
Step 4, by the supernatant liquor dialysis obtained, with filtering with microporous membrane, rotary evaporation is concentrated obtains concentrated carbon quantum dot solution, and then at-50 DEG C, lyophilize finally obtains carbon quantum dot pressed powder.
Of the present invention a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point, further technical scheme is, in described step 2, microwave power is 500-800w, and the microwave reaction time is 3-6min.
Of the present invention a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point, further technical scheme is, in described step 2, is cooled to naturally cooling.
Of the present invention a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point, further technical scheme is, in described step 3, ultrasonic power is 100w, and ultrasonic frequency is 53kHz, and ultrasonic time is 60-180min.
Of the present invention a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point, further technical scheme is, in described step 3, centrifugal speed is 8000-10000r/min, and centrifugation time is 8-10min.
Of the present invention a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point, further technical scheme is, in described step 4, dialysis adopts the dialysis tubing of 1000-3000Da, and be put in the beaker of 2-5L and dialyse, dialysis time is 36-48h.
Of the present invention a kind of take green onion as the method that raw material microwave prepares fluorescent carbon point, further technical scheme is, in described step 4 process adopt aperture be the millipore filtration of 0.22um, rotary evaporation bath temperature is 60 DEG C, and lyophilize temperature is-50 DEG C.
The present invention has following beneficial effect: be raw material with green onion, and raw material is extensively easy to get, environmental protection, and microwave method prepares fluorescent carbon point, fast simply, with low cost; And the fluorescent carbon point good water solubility of preparation, stability is high, can be widely used in biological detection and analysis as fluorescent marker.
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 transmission electron microscope picture of carbon point prepared by the embodiment of the present invention 1.
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, gets a green onion, is pulverized with pulverizer.Step 2, the green onion taking 5g pulverizing is placed in 100mL beaker, with after the power microwave of 800w reaction 6min in microwave oven, naturally cooling.Step 3, adds 150mL deionized water magnetic agitation 8min by the product of acquisition, ultrasonic 180min under be 100w frequency being then 53kHz condition at power, obtains finely dispersed suspension liquid, and suspension liquid extracts supernatant liquor through the centrifugal 8min of 10000r/min.Step 4, by the supernatant liquor splendid attire of acquisition in the dialysis tubing of 3000Da, the beaker being placed in 4L is dialysed 36h, then the filtering with microporous membrane of 0.22um is used, obtain concentrated carbon quantum dot solution in 60 DEG C of water-bath rotary evaporations are concentrated, then at-50 DEG C, lyophilize finally obtains carbon quantum dot pressed powder.
Embodiment 2
Step 1, gets a green onion, is pulverized with pulverizer.Step 2, the green onion taking 2g pulverizing is placed in 50mL beaker, with after the power microwave of 500w reaction 3min in microwave oven, naturally cooling.Step 3, adds 50mL deionized water magnetic agitation 8min by the product of acquisition, ultrasonic 60min under be 100w frequency being then 53kHz condition at power, obtains finely dispersed suspension liquid.Suspension liquid extracts supernatant liquor through the centrifugal 9min of 10000r/min.Step 4, by the supernatant liquor splendid attire of acquisition in the dialysis tubing of 2000Da, the beaker being placed in 2L is dialysed 36h, then the filtering with microporous membrane of 0.22um is used, obtain concentrated carbon quantum dot solution in 60 DEG C of water-bath rotary evaporations are concentrated, then at-50 DEG C, lyophilize finally obtains carbon quantum dot pressed powder.
Embodiment 3
Step 1, gets a green onion, is pulverized with pulverizer.Step 2, the green onion taking 8g pulverizing is placed in 250mL beaker, with after the power microwave of 700w reaction 6min in microwave oven, naturally cooling.Step 3, adds 300mL deionized water magnetic agitation 8min by the product of acquisition, ultrasonic 160min under be 100w frequency being then 53kHz condition at power, obtains finely dispersed suspension liquid.Suspension liquid extracts supernatant liquor through the centrifugal 10min of 8000r/min.Step 4, by the supernatant liquor splendid attire of acquisition in the dialysis tubing of 2000Da, the beaker being placed in 5L is dialysed 48h, then the filtering with microporous membrane of 0.22um is used, obtain concentrated carbon quantum dot solution in 60 DEG C of water-bath rotary evaporations are concentrated, then at-50 DEG C, lyophilize finally obtains carbon quantum dot pressed powder.
Embodiment 4
Step 1, gets a green onion, is pulverized with pulverizer.Step 2, the green onion taking 4g pulverizing is placed in 200mL beaker, with after the power microwave of 600w reaction 5min in microwave oven, naturally cooling.Step 3, adds 200mL deionized water magnetic agitation 8min by the product of acquisition, ultrasonic 100min under be 100w frequency being then 53kHz condition at power, obtains finely dispersed suspension liquid.Suspension liquid extracts supernatant liquor through the centrifugal 10min of 9000r/min.Step 4, by the supernatant liquor splendid attire of acquisition in the dialysis tubing of 1000Da, the beaker being placed in 3L is dialysed 48h, then the filtering with microporous membrane of 0.22um is used, obtain concentrated carbon quantum dot solution in 60 DEG C of water-bath rotary evaporations are concentrated, then at-50 DEG C, lyophilize finally obtains carbon quantum dot pressed powder.
Claims (7)
1. be the method that raw material microwave prepares fluorescent carbon point with green onion, it is characterized in that, comprise the following steps:
Step 1, gets a green onion, is pulverized with pulverizer;
Step 2, the green onion taking a certain amount of pulverizing is placed in 50-250mL beaker, in microwave oven after microwave reaction for some time, cooling;
Step 3, adds 50-300mL deionized water magnetic agitation 8min, then carries out supersound process, obtain finely dispersed suspension liquid by the product of acquisition, suspension liquid is through centrifugal extraction supernatant liquor;
Step 4, by the supernatant liquor dialysis obtained, with filtering with microporous membrane, rotary evaporation is concentrated obtains concentrated carbon quantum dot solution, and then at-50 DEG C, lyophilize finally obtains carbon quantum dot pressed powder.
2. be the method that raw material microwave prepares fluorescent carbon point according to a kind of described in claim 1 with green onion, it is characterized in that, in described step 2, microwave power is 500-800w, and the microwave reaction time is 3-6min.
3. be the method that raw material microwave prepares fluorescent carbon point according to a kind of described in claim 1 with green onion, it is characterized in that, in described step 2, be cooled to naturally cooling.
4. be the method that raw material microwave prepares fluorescent carbon point according to a kind of described in claim 1 with green onion, it is characterized in that, in described step 3, ultrasonic power is 100w, and ultrasonic frequency is 53kHz, and ultrasonic time is 60-180min.
5. be the method that raw material microwave prepares fluorescent carbon point according to a kind of described in claim 1 with green onion, it is characterized in that, in described step 3, centrifugal speed is 8000-10000r/min, and centrifugation time is 8-10min.
6. be the method that raw material microwave prepares fluorescent carbon point according to a kind of described in claim 1 with green onion, it is characterized in that, in described step 4, dialysis adopts the dialysis tubing of 1000-3000Da, and be put in the beaker of 2-5L and dialyse, dialysis time is 36-48h.
7. be the method that raw material microwave prepares fluorescent carbon point according to a kind of described in claim 1 with green onion, it is characterized in that, in described step 4, process adopts aperture to be the millipore filtration of 0.22um, and rotary evaporation bath temperature is 60 DEG C, and lyophilize temperature is-50 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395789A (en) * | 2016-09-27 | 2017-02-15 | 安徽师范大学 | Method for synthesizing carbon dots |
| CN106744808A (en) * | 2016-11-30 | 2017-05-31 | 辽宁大学 | A kind of carbon quantum dot with fish scale as raw material and its preparation method and application |
| CN107311145A (en) * | 2017-08-29 | 2017-11-03 | 湖南农业大学 | A kind of fluorescent carbon point for the method and its preparation that fluorescent carbon point is prepared by raw material of silkworm excrement |
| CN110051879A (en) * | 2019-05-29 | 2019-07-26 | 哈尔滨工业大学 | A kind of preparation method of the compound hemostatic material of fluorescent carbon point modification |
| CN114304249A (en) * | 2021-12-13 | 2022-04-12 | 大连工业大学 | Preparation of onion-source bacteriostatic carbon dots and application of onion-source bacteriostatic carbon dots in aquatic product preservation |
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| CN103387219A (en) * | 2013-07-22 | 2013-11-13 | 苏州大学 | A preparation method for water-soluble multicolor carbon quantum points by microwave radiation |
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| CN105038781A (en) * | 2015-04-01 | 2015-11-11 | 河南师范大学 | Method of one-step synthesizing fluorescent carbon dots with corncob as carbon source |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395789A (en) * | 2016-09-27 | 2017-02-15 | 安徽师范大学 | Method for synthesizing carbon dots |
| CN106395789B (en) * | 2016-09-27 | 2019-02-12 | 安徽师范大学 | A kind of synthetic method of carbon dots |
| CN106744808A (en) * | 2016-11-30 | 2017-05-31 | 辽宁大学 | A kind of carbon quantum dot with fish scale as raw material and its preparation method and application |
| CN106744808B (en) * | 2016-11-30 | 2019-09-13 | 辽宁大学 | It is a kind of using fish scale as carbon quantum dot of raw material and its preparation method and application |
| CN107311145A (en) * | 2017-08-29 | 2017-11-03 | 湖南农业大学 | A kind of fluorescent carbon point for the method and its preparation that fluorescent carbon point is prepared by raw material of silkworm excrement |
| CN110051879A (en) * | 2019-05-29 | 2019-07-26 | 哈尔滨工业大学 | A kind of preparation method of the compound hemostatic material of fluorescent carbon point modification |
| CN110051879B (en) * | 2019-05-29 | 2021-08-03 | 哈尔滨工业大学 | Preparation method of composite hemostatic material modified by fluorescent carbon dots |
| CN114304249A (en) * | 2021-12-13 | 2022-04-12 | 大连工业大学 | Preparation of onion-source bacteriostatic carbon dots and application of onion-source bacteriostatic carbon dots in aquatic product preservation |
| CN114304249B (en) * | 2021-12-13 | 2023-11-07 | 大连工业大学 | Preparation of onion source antibacterial carbon dots and application of onion source antibacterial carbon dots in preservation of aquatic products |
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Application publication date: 20160420 |