CN106118646A - The cheap preparation method of one class yellow emission carbon quantum dot - Google Patents
The cheap preparation method of one class yellow emission carbon quantum dot Download PDFInfo
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Abstract
The invention discloses the cheap preparation method of a class yellow emission carbon quantum dot, preparation process is as follows: the charcoal with fullerene industrialized production by-product is grey as raw material, adds concentrated sulphuric acid and concentrated nitric acid, supersound process, obtains dispersion liquid；Dispersion liquid is placed in heat treated in oil bath, is cooled to room temperature, with distilled water diluting and use K2CO3It is transferred to neutrality, obtains crude product；Crude product centrifugal segregation is precipitated, then carries out dialysis, obtain carbon quantum dot.Low in raw material price selected by the present invention, steady sources, preparation process is simple, and gained carbon quantum dot can launch yellow fluorescence, and quantum yield is high, it is adaptable to the fields such as opto-electronic conversion, bio-imaging, ion sensor.
Description
Technical field
The present invention relates to the cheap preparation method of a class yellow emission carbon quantum dot, belong to nano material preparation technology neck
Territory.
Background technology
Luminescent material is widely used in opto-electronic device, biomarker and biomedicine field.For a long time, the mankind
The luminescent material obtaining extensive concern and actual application in life and production mainly has organic dyestuff, rare earth compounding, quasiconductor
Quantum dot, metal nanometer cluster etc..Although these luminescent material abundant species, quantum yield are high and emission wavelength is adjustable, but with
Time they have again its limitation, as degradable, light stability is poor, expensive, non-renewable etc., and major part is the most toxic makes
It is restricted at biomedicine field.Therefore, advanced luminescent material always chemistry and the diligent pursuit of material supply section scholar are sought
Target.
Carbon quantum dot be found because of luminous in 2004 and in 2006 by success first prepare less than 10 nanometers
Carbon granule (J. Am. Chem. Soc., 2004, 126, 12736; J. Am. Chem. Soc., 2006, 128,
7756) newcomer of nano-carbon material family after fullerene, CNT, Graphene, is become.They not only have tradition
Luminescence generated by light that semiconductor-quantum-point is had and the optical property such as light emitting region is adjustable, also overcome semiconductor-quantum-point toxicity
Big shortcoming.As a kind of advanced luminescent material, compared with traditional material, it is stable that carbon quantum dot has good biocompatibility, light
Property height, low cost, the plurality of advantages such as nontoxic, renewable.Therefore, once it has been observed that carbon quantum dot is because it is at life sciences, material
The huge applications potentiality in the field such as science, chemical science and receive much concern.In recent years, due to being continually striving to of scientist,
Carbon quantum dot achieves the most progressive in preparation, but the major part of synthesis is that short wavelength launches such as blue-light carbon quantum dot, long
The carbon quantum dot that wavelength is launched is less because of preparation difficulty, low yield report, and this limits the actual application of carbon quantum dot undoubtedly
Scope.
On the other hand, how by preferred feedstock and preparation technology, the production cost of carbon quantum dot is reduced, to promoting carbon amounts
The extensively application of son point is significant.The method of preparation carbon quantum dot is a lot of at present, is broadly divided into method from top to bottom and (swashs
Light is cleared up, proton beam radiation, electrochemical oxidation, acid oxidase, etc.) and method (pyrolysis, vapour deposition, etc.) from bottom to top.Its
In, laser is cleared up, proton beam radiation, vapour deposition etc. need more complicated equipment, and experiment condition is harsher, time and energy
Source consumes bigger；Although the carbon quantum dot quality that pyrolysis and electrochemical oxidation obtain is higher, but is not suitable for large-scale production.Compare
Under, acid oxidation demonstrates the advantage of uniqueness because it can prepare carbon quantum dot in a large number.Plurality of raw materials can be used for this side
Method, the ashes produced such as wax candle or combustion of natural gas, biomass, coal dust etc. (Angew. Chem. Int. Ed. 2007, 46,
6473; Chem. Commun. 2013, 49, 10290; Chem. Commun. 2012, 48, 8835; Chem. Commun. 2012, 48, 380; Angew. Chem. Int. Ed. 2012, 51, 9297; Angew. Chem.Int. Ed. 2013, 52, 8151.).But these raw materials or originate inadequate, or the carbon quantum dot of blue emission can only be obtained,
And the fluorescence quantum yield of prepared carbon quantum dot typically the most relatively low (< 4%).Therefore, longwave transmissions carbon quantum dot is developed
Preparation method has very important realistic meaning.
Summary of the invention
For solving the problem that the existing carbon quantum dot preparation field cheap preparation method of longwave transmissions carbon quantum dot lacks, this
The cheap preparation method of bright offer one class yellow emission carbon quantum dot.
The continuous propelling of the member being found at first along with nano-carbon material family, i.e. fullerene process of industrialization, fowler
The yield of alkene raises year by year.The by-product charcoal ash (hereinafter referred to as fullerene charcoal ash) that period produces occupies entire solid matters
More than 85%.For a long time, the resource that this part is valuable fails fully to be obtained by.In the present invention, we make use of this just
One precious resources, turns waste into wealth, and by optimizing preparation technology, has prepared the carbon quantum dot of yellow emission.The method is simple to operate,
Required low in raw material price, steady sources, it is possible to being substantially reduced cost, prepared carbon quantum dot sends out yellow fluorescence, glimmering
Quantum yield is high.
The cheap preparation method of one class yellow emission carbon quantum dot, it is characterised in that specifically comprise the following steps that
1., under condition of ice bath, concentrated nitric acid is slowly added dropwise concentrated sulphuric acid, stirring, in time there is no smog, sealed ultrasonic 1 h
~3 h；
2. in fullerene charcoal ash, add the nitration mixture that 1. step prepares, supersound process 1 h ~ 5 h, obtain dividing of fullerene charcoal ash
Dissipate liquid；
3. by the dispersion liquid of fullerene charcoal ash at 80 ~ 120 DEG C of heat treated 10 ~ 36 h, room temperature is then naturally cooled to；
4. the suspension after step 3. being cooled down is placed in frozen water, adds ultra-pure water stirring, then uses K2CO3It is adjusted to neutrality, obtains
Crude product；
5. crude product step 4. obtained is centrifugal leaches precipitation；
6. with the bag filter of PSPP, filtrate is carried out classification dialysis, the dialysate of each several part is concentrated,
Carbon quantum dot solution to different size scope.
Step 1. described in the volume ratio of concentrated sulphuric acid and concentrated nitric acid be 1:1 ~ 3:1.
Step 2. described in fullerene charcoal ash be 1:95-1:147 with the mass ratio of nitration mixture.
Step 5. described in centrifugal rotating speed be 8000 r/min, centrifugation time is 30 min.
Step 6. in the molecular cut off of selected bag filter be respectively 100 Da, 500 Da, 1000 Da, 2000 Da.
Step 6. described in the time interval of classification dialysis be 3 ~ 6 days.
After fullerene charcoal ash selected by the present invention is the fullerene purification that Suzhou great virtue carbon nanosecond science and technology company limited produces
By-product.
The outstanding characteristic of the present invention is: 1) replace tradition quantum with the charcoal ash of by-product in fullerene commercial process
Expensive reaction raw materials needed for some preparation, wide material sources, nontoxic, cheap, and achieve and turn waste into wealth, suit current
Sustainable development and green chemical concept；2) preparation method is simple and feasible, uses chemical oxidization method, simple to operate, low cost,
Productivity is high, is suitable for large-scale industrial production；3) the carbon quantum dot transmitted wave length prepared by is in yellow region, and fluorescence volume
Sub-productivity is high, good light stability.
It is an advantage of the present invention that raw material is cheap, steady sources；Preparation process is simple, and the cycle is short, and productivity is high；Preparation
Carbon quantum dot has good aqueous solubility, directly can use as aqueous solution, also can be made into powdery and use, and mean diameter is little,
Luminous intensity is high, and fluorescence quantum yield is high.
Accompanying drawing explanation
Fig. 1. embodiment 4 obtains > 2000 Da, 500 ~ 1000 Da, 1000 ~ 2000 Da carbon quantum dot aqueous solutions are in day
Light (a, c, e) He 365 nm uviol lamps (b, d, f) under photo.Photo from daylight it can be seen that > 2000 Da
Component colors is relatively deep, even and if other two kinds of component aqueous solutions concentrate after still color shallower, show product with > 2000 Da are
Main.Photo from uviol lamp is it can be seen that the main component of prepared carbon quantum dot sends out yellow fluorescence.
Fig. 2. embodiment 4 obtains > the high resolution transmission electron microscopy figure of 2000 Da carbon quantum dot solution, show institute
The carbon quantum dot even particle size distribution of preparation, averagely at about 2 nm.
Fig. 3. embodiment 4 obtains > 2000 Da carbon quantum dot and the Fourier transform infrared spectroscopy figure of raw material.From figure
It can be seen that carbon quantum dot is at 3424 cm-1With 1384 cm-1Occur in that the stretching vibration peak of-OH, at 1730 cm-1Occur in that C
The stretching vibration of=O key.Though raw material fullerene charcoal ash is at 3448 cm-1There is the stretching vibration peak of-OH, at 1696 cm-1There is C=O key
Stretching vibration, but intensity is relatively weak, thus after explanation acid oxidase, the content of carbon quantum dot surface hydroxyl and carboxyl relative to
Raw material has had large increase.
Fig. 4. embodiment 4 obtains > ultra-violet absorption spectrum of 2000 Da carbon quantum dot solution and in different excitation wavelengths
Under fluorescent emission spectrogram.It can be seen that prepared carbon quantum dot has typical excitation wavelength dependency, along with
The increase of excitation wavelength, transmitted wave length generation red shift, maximum excitation wavelength is 470 nm, and corresponding maximum emission wavelength is
528.5 nm, fluorescence quantum yield is 5.47%.
Fig. 5. the ultra-violet absorption spectrum of 500 ~ 1000 Da carbon quantum dot solution that embodiment 4 obtains and at different excitation waves
Fluorescent emission spectrogram under Chang.It can be seen that carbon quantum dot shows excitation wavelength dependency equally, along with excitation wave
Long increase, transmitted wave length generation red shift, maximum excitation wavelength is 460 nm, and corresponding maximum emission wavelength is 528.5 nm.
Fig. 6. the ultra-violet absorption spectrum of 1000 ~ 2000 Da carbon quantum dot solution that embodiment 4 obtains and exciting in difference
Fluorescent emission spectrogram under wavelength.It can be seen that carbon quantum dot also shows excitation wavelength dependency, along with excitation wave
Long increase, transmitted wave length generation red shift, maximum excitation wavelength is 460 nm, and corresponding maximum emission wavelength is 527 nm.
Detailed description of the invention
Embodiment 1
Taking 50 mg fullerene charcoals ashes in 50 mL round-bottomed flasks, put it in the beaker filling frozen water, stirring is lower will be in advance
The 8 mL concentrated nitric acids/concentrated sulphuric acid mixed liquor (volume ratio is 1:3) mixed is slowly dropped in round-bottomed flask, after acid drips,
Continue stirring 30 min.Stop stirring, ultrasonic 2 h, round-bottomed flask is placed in oil bath pan, at 100 DEG C, heats 24 h.Treat sample
After naturally cooling to room temperature, it is replaced in frozen water, is slowly added dropwise 25 mL deionized waters under stirring, uses K2CO3It is neutralized to
PH 7, centrifugal (12500 turns, 30 min), remove precipitation, supernatant be transferred in the dialysis bag of 100 Da, dialysis 3 ~ 6 days,
Discard dialysate, liquid in bag is transferred in 500 Da dialysis bags, continue dialysis 3 ~ 6 days, dialysate is retained, concentrates, then
Liquid in bag is transferred in the dialysis bag of 1000 Da and 2000 Da successively, repeats aforesaid operations.
Embodiment 2
On the basis of embodiment 1, the volume of concentrated nitric acid/concentrated sulphuric acid mixed liquor (volume ratio is 1:3) is adjusted to 4 mL, other
Condition is constant.
Embodiment 3
On the basis of embodiment 2, concentrated nitric acid and concentrated sulphuric acid volume ratio being adjusted to 1:2, other condition is constant.
Embodiment 4
On the basis of embodiment 2, concentrated nitric acid and concentrated sulphuric acid volume ratio being adjusted to 1:1, other condition is constant.
Embodiment 5
On the basis of embodiment 4, oil bath temperature changing 120 С into, other condition is constant.
Embodiment 6
On the basis of embodiment 4, oil bath temperature changing 80 С into, other condition is constant.
Embodiment 7
On the basis of embodiment 4, the time that oil bath processed changes 12 h into, and other condition is constant.
Embodiment 8
On the basis of embodiment 4, the time that oil bath processed changes 36 h into, and other condition is constant.
Embodiment 9
Take expand 5 times 250 mg fullerene charcoals ash in 100 mL round-bottomed flasks, put it in the beaker filling frozen water,
Under stirring, the 40 mL concentrated nitric acids/concentrated sulphuric acid mixed liquor (volume ratio is 1:3) mixed in advance is slowly dropped to round-bottomed flask
In, after acid drips, continue stirring 30 min.Stop stirring, ultrasonic 2 h, round-bottomed flask is placed in oil bath pan, at 100 DEG C
Heat 24 h.After sample naturally cools to room temperature, it is replaced in frozen water, under stirring, is slowly added dropwise 30 mL deionizations
Water, uses K2CO3It is neutralized to pH 7, centrifugal (12500 turns, 30 min), remove precipitation, supernatant is directly transferred to 2000 Da's
In dialysis bag, dialysis 3 ~ 6 days, discard dialysate, by liquid concentration in bag.
Claims (6)
1. the cheap preparation method of a class yellow emission carbon quantum dot, it is characterised in that specifically comprise the following steps that
1., under condition of ice bath, concentrated nitric acid is slowly added dropwise concentrated sulphuric acid, stirring, in time there is no smog, sealed ultrasonic 1 h
~3h；
2. in fullerene charcoal ash, add the nitration mixture that 1. step prepares, supersound process 1 h ~ 5 h, obtain dividing of fullerene charcoal ash
Dissipate liquid；
3. by the dispersion liquid of fullerene charcoal ash at 80 ~ 120 DEG C of heat treated 10 ~ 36 h, room temperature is then naturally cooled to；
4. the suspension after step 3. being cooled down is placed in frozen water, adds ultra-pure water stirring, then uses K2CO3It is adjusted to neutrality, obtains
Crude product；
5. crude product step 4. obtained is centrifugal leaches precipitation；
6. with the bag filter of PSPP, filtrate is carried out classification dialysis, the dialysate of each several part is concentrated,
Carbon quantum dot solution to different size scope.
2. preparation method as claimed in claim 1 cheap, it is characterised in that step 1. described in concentrated sulphuric acid and the body of concentrated nitric acid
Long-pending ratio is 1:1 ~ 3:1.
3. preparation method as claimed in claim 1 cheap, it is characterised in that step 2. described in fullerene charcoal ash and nitration mixture
Mass ratio is 1:95-1:147.
4. preparation method as claimed in claim 1 cheap, it is characterised in that step 5. described in centrifugal rotating speed be 8000 r/
Min, centrifugation time is 30 min.
5. preparation method as claimed in claim 1 cheap, it is characterised in that step 6. in the molecular cut off of selected bag filter
It is respectively 100 Da, 500 Da, 1000 Da, 2000 Da.
6. preparation method as claimed in claim 1 cheap, it is characterised in that step 6. described in the time interval of classification dialysis
It it is 3 ~ 6 days.
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Cited By (8)
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| CN107619034A (en) * | 2017-10-16 | 2018-01-23 | 赵方浩 | The preparation method of green fluorescence carbon quantum dot |
| CN107629788A (en) * | 2017-09-28 | 2018-01-26 | 苏州轻光材料科技有限公司 | The preparation method of a kind of multicolor fluorescence quantum dot and in white light LEDs application |
| CN107674674A (en) * | 2017-09-28 | 2018-02-09 | 苏州轻光材料科技有限公司 | The preparation method of a kind of gold-tinted quantum dot and in white light LEDs application |
| CN107880881A (en) * | 2017-11-27 | 2018-04-06 | 陕西科技大学 | A kind of preparation method of carbon quantum dot |
| CN108380136A (en) * | 2018-04-16 | 2018-08-10 | 中国科学院兰州化学物理研究所 | A kind of method that carbon quantum dot induction vermiculate glues is formed |
| CN109225233A (en) * | 2018-10-26 | 2019-01-18 | 陕西科技大学 | A kind of layered double hydroxide/carbon quantum dot elctro-catalyst and preparation method thereof |
| CN109225232A (en) * | 2018-10-26 | 2019-01-18 | 陕西科技大学 | A kind of elctro-catalyst and preparation method thereof |
| CN109266338A (en) * | 2018-10-26 | 2019-01-25 | 陕西科技大学 | A kind of fowler alkenyl carbon quantum dot and preparation method thereof |
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| CN104479675A (en) * | 2014-12-08 | 2015-04-01 | 上海大学 | Large-scaled industrial preparation method for fluorescent graphene quantum dot material |
| CN104650864A (en) * | 2015-03-04 | 2015-05-27 | 东华大学 | Method for preparing biomass based carbon quantum dots |
| CN104743545A (en) * | 2015-03-11 | 2015-07-01 | 中国科学院青岛生物能源与过程研究所 | Preparation method of petroleum asphalt-based carbon quantum dot and application of petroleum asphalt-based carbon quantum dot prepared by method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629788A (en) * | 2017-09-28 | 2018-01-26 | 苏州轻光材料科技有限公司 | The preparation method of a kind of multicolor fluorescence quantum dot and in white light LEDs application |
| CN107674674A (en) * | 2017-09-28 | 2018-02-09 | 苏州轻光材料科技有限公司 | The preparation method of a kind of gold-tinted quantum dot and in white light LEDs application |
| CN107619034A (en) * | 2017-10-16 | 2018-01-23 | 赵方浩 | The preparation method of green fluorescence carbon quantum dot |
| CN107880881A (en) * | 2017-11-27 | 2018-04-06 | 陕西科技大学 | A kind of preparation method of carbon quantum dot |
| CN108380136A (en) * | 2018-04-16 | 2018-08-10 | 中国科学院兰州化学物理研究所 | A kind of method that carbon quantum dot induction vermiculate glues is formed |
| CN109225233A (en) * | 2018-10-26 | 2019-01-18 | 陕西科技大学 | A kind of layered double hydroxide/carbon quantum dot elctro-catalyst and preparation method thereof |
| CN109225232A (en) * | 2018-10-26 | 2019-01-18 | 陕西科技大学 | A kind of elctro-catalyst and preparation method thereof |
| CN109266338A (en) * | 2018-10-26 | 2019-01-25 | 陕西科技大学 | A kind of fowler alkenyl carbon quantum dot and preparation method thereof |
| CN109225233B (en) * | 2018-10-26 | 2021-08-13 | 陕西科技大学 | Layered double metal hydroxide/carbon quantum dot electrocatalyst and preparation method thereof |
| CN109225232B (en) * | 2018-10-26 | 2021-11-16 | 陕西科技大学 | Electrocatalyst and preparation method thereof |
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Application publication date: 20161116 |