CN109266338A - A kind of fowler alkenyl carbon quantum dot and preparation method thereof - Google Patents
A kind of fowler alkenyl carbon quantum dot and preparation method thereof Download PDFInfo
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- CN109266338A CN109266338A CN201811258054.2A CN201811258054A CN109266338A CN 109266338 A CN109266338 A CN 109266338A CN 201811258054 A CN201811258054 A CN 201811258054A CN 109266338 A CN109266338 A CN 109266338A
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Abstract
The present invention provides a kind of fowler alkenyl carbon quantum dot and preparation method thereof, comprising: S1: by Fullerene Carbon ash, heating stirring is aoxidized in concentrated acid；S2: after the reaction mixture of step S1 is cooled to room temperature, the inorganic salts and small molecular weight impurity of bulky grain, molecular weight greater than 3500Da in mixture are removed；S3: by step S2, treated that reaction solution is concentrated by evaporation and is freeze-dried as powder to get fowler alkenyl carbon quantum dot of the present invention.The present invention uses Fullerene Carbon ash, concentrated acid for raw material, and by being heated to reflux to obtain carbon quantum dot, this method, which is reacted, to be heated evenly, easy to control, carbon quantum dot that is low using cost of material, being easy to get to target product, acquisition be evenly distributed, it is easy to operate.Gained carbon quantum dot good dispersion in water, size uniformity.
Description
Technical field
The present invention relates to carbon material fields, and in particular to a kind of high-performance fowler alkenyl fluorescent carbon quantum dot and its preparation side
Method.
Background technique
Carbon quantum dot (CQD) is a kind of carbon nanomaterial that diameter is novel in 10nm or less, and 2004, Xu et al. was from electricity
In arc discharge ash when purified single-wall carbon nanotube, a kind of isolated for the first time new fluorescence carbon nanomaterial.2006, Sun
Et al. propose the new strategy-surface passivation method for improving fluorescent carbon nanodot fluorescence quantum yield, and fluorescent carbon nano dot is ordered
Entitled " carbon quantum dot ".Common carbon usually shines weak, poorly water-soluble, however carbon quantum dot but have it is good water-soluble and glimmering
Light characteristic, and have it is nontoxic, it is small to the harm of environment, it is at low cost the advantages that.In the past few years, in the synthesis of CQDs, property, answer
With etc. all achieve huge progress.Compared with traditional semiconductor-quantum-point, the CQDs that shines has highly-water-soluble, stabilization
Property is easy to functionalization and good biocompatibility, has potential application prospect in biomedical aspect.Meanwhile CQDs has
Have excellent photoelectric property, not only can be used as electron donor but also can be used as electron acceptor, this make it photoelectron, catalysis and
The fields such as sensing have a wide range of applications.The method for preparing CQD at present mainly has microwave method, electrochemical process, pyrolysismethod etc., this
A little methods have the unfavorable factors such as at high cost, energy consumption is high for large-scale batch production.Therefore, it develops easy, inexpensive
CQD preparation method for push its application be of great significance.
Summary of the invention
A kind of that it is an object of that present invention to provide exploitations is easy, preparation cost is cheap fowler alkenyl fluorescent carbon quantum dot and its
Preparation method.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of fowler alkenyl carbon quantum dot, comprising the following steps:
S1: by Fullerene Carbon ash, heating stirring is aoxidized in concentrated acid；
S2: after the reaction mixture of step S1 is cooled to room temperature, the bulky grain in mixture is removed, molecular weight is greater than
The inorganic salts and small molecular weight impurity of 3500Da；
S3: by step S2, treated that reaction solution is concentrated by evaporation and is freeze-dried as powder to get fowler alkenyl of the present invention
Carbon quantum dot.
Further, the preparation method of fowler alkenyl carbon quantum dot as described above, concentrated acid described in step S1 are concentration
Mass fraction is all larger than one or more of 95% concentrated nitric acid, the concentrated sulfuric acid, concentrated phosphoric acid.
Further, the preparation method of fowler alkenyl carbon quantum dot as described above, heating stirring in step S1 specifically:
100-120 DEG C stirring 12-15 hours.
Further, the preparation method of fowler alkenyl carbon quantum dot as described above removes arranging for bulky grain in step S2
It applies are as follows: be centrifuged with the centrifugal speed of 5000-20000rpm.
Further, the preparation method of fowler alkenyl carbon quantum dot as described above removes inorganic salts and small in step S2
The measure of molecular impurity are as follows: dialysis 3-5 days is carried out to the supernatant after centrifugation using bag filter.
Further, the preparation method of fowler alkenyl carbon quantum dot as described above, the revolving speed stirred in step S1 are
100-1000rpm。
The fowler alkenyl carbon quantum dot being prepared according to either method as above.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention uses Fullerene Carbon ash, concentrated acid for raw material, by being heated to reflux to obtain carbon quantum dot, this method react by
It is hot uniformly, easy to control, institute's carbon quantum dot that is low using cost of material, being easy to get to target product, acquisition is evenly distributed, and operation is simple
It is single.Gained carbon quantum dot good dispersion in water, size uniformity.
Detailed description of the invention
Fig. 1 (a) is TEM phenogram of the carbon quantum dot that is prepared of embodiment 1 at 200nm；
Fig. 1 (b) is TEM phenogram of the carbon quantum dot that is prepared of embodiment 1 at 100nm；
Fig. 2 is the PL fluorescence spectra for the carbon quantum dot that embodiment 1 is prepared.
Fig. 3 is the Raman spectrogram of carbon quantum dot and its synthesis material Fullerene Carbon ash that embodiment 1 is prepared.
Specific embodiment
The present invention provides a kind of method using concentrated acid processing Fullerene Carbon ash preparation carbon quantum dot, to make mesh of the invention
, technical solution and effect it is clearer, clear, the present invention is described in more detail below.Specific reality described herein
It applies example to be only used to explain the present invention, be not intended to limit the present invention.
Specific step is as follows:
The Fullerene Carbon ash of 100-300mg is added to the dense HNO of 10-30ml3In.It is heated to 100-120 DEG C under stiring
And react it 12-15 hours.After reaction mixture is cooled to room temperature, 30 minutes are centrifuged to remove with the rate of 5000r/min
Bulky grain is removed, dialysis 3-5 days then is carried out to supernatant using the bag filter that molecular cut off is 3500Da, is present in removing
Inorganic salts and small molecular weight impurity therein.After the completion of dialysis, dialyzate rotary evaporation is concentrated into about 5ml, then pour into culture
It is freezed in ware, is finally putting into freeze drier and dries to powder.
Below by specific embodiment, the present invention will be described in more detail:
Embodiment 1
The Fullerene Carbon ash of 100mg is added to the dense HNO of 10ml3In.It is heated to 100 DEG C under stiring and it is made to react 12
Hour.After reaction mixture is cooled to room temperature, then mixture is centrifuged with the rate of 5000r/min 30 minutes big to remove
Particle is then carried out dialysis 3 days to supernatant using the bag filter that molecular cut off is 3500Da, is contained therein with removing
Inorganic salts and small molecular weight impurity.After the completion of dialysis, dialyzate rotary evaporation is concentrated into about 5ml, then is poured into cold in culture dish
Freeze, is finally putting into freeze drier and dries to powder.
Embodiment 2
The Fullerene Carbon ash of 100mg is added to the dense HNO of 20ml3In.It is heated to 100 DEG C under stiring and it is made to react 12
Hour.After reaction mixture is cooled to room temperature, then mixture is centrifuged with the rate of 5000r/min 30 minutes big to remove
Particle is then carried out dialysis 3 days to supernatant using the bag filter that molecular cut off is 3500Da, is contained therein with removing
Inorganic salts and small molecular weight impurity.After the completion of dialysis, dialyzate rotary evaporation is concentrated into about 5ml, then is poured into cold in culture dish
Freeze, is finally putting into freeze drier and dries to powder.
Embodiment 3
The Fullerene Carbon ash of 200mg is added to the dense HNO of 30ml3In.It is heated to 100 DEG C under stiring and it is made to react 12
Hour.After reaction mixture is cooled to room temperature, then mixture is centrifuged with the rate of 5000r/min 30 minutes big to remove
Particle is then carried out dialysis 3 days to supernatant using the bag filter that molecular cut off is 3500Da, is contained therein with removing
Inorganic salts and small molecular weight impurity.After the completion of dialysis, dialyzate rotary evaporation is concentrated into about 5ml, then is poured into cold in culture dish
Freeze, is finally putting into freeze drier and dries to powder.
Embodiment 4
The Fullerene Carbon ash of 100mg is added to the dense HNO of 10ml3In.It is heated to 110 DEG C under stiring and it is made to react 15
Hour.After reaction mixture is cooled to room temperature, mixture is then centrifuged 30-60 minutes with the rate of 8000r/min to remove
Bulky grain is removed, dialysis 3-5 days then is carried out to supernatant using the bag filter that molecular cut off is 3500Da, is present in removing
Inorganic salts and small molecular weight impurity therein.After the completion of dialysis, dialyzate rotary evaporation is concentrated into about 5ml, then pour into culture
It is freezed in ware, is finally putting into freeze drier and dries to powder.
Table 1 is the carbon quantum dot that embodiment is prepared and the elemental analysis result of its synthesis material Fullerene Carbon ash.
Table 1
Table 1 is the elemental analysis of prepared carbon quantum dot and its raw material Fullerene Carbon ash, elemental analysis carbon as the result is shown
Content reduce, while H content increase, illustrate the surface FCS since acidification is oxidized, form hydroxyl, carboxyl (OH,
COOH), y is it is possible thereby to can be clearly seen that carbon content is substantially reduced after acid reaction.
Fig. 1 a, 1b are respectively TEM figure of the carbon quantum dot under different amplification, it can be seen that obtain favorable dispersibility
Carbon quantum dot, size is distributed in 10nm hereinafter, and size uniformity.
Fig. 2 is influence of the excitation wavelength to carbon quantum dot fluorescence spectrum, with the increase of excitation wavelength, fluorescence intensity by
Cumulative strong, when excitation wavelength reaches 520nm, fluorescence intensity reaches maximum value, and as excitation wavelength continues growing, fluorescence is strong
Degree reduces instead, and reason may be the increase with excitation wavelength, and the energy of material absorbing reduces, so emitted energy is also corresponding
It reduces, it is also possible to caused by the emission sites on the surface CQD are different.The figure, which demonstrates synthesized CQD, has fluorescent characteristic.
Fig. 3 is the Raman spectrogram of prepared carbon quantum dot and its raw material Fullerene Carbon ash, is observed in figure
1320-1340cm-1And 1560-1590cm-1Two peaks be respectively the peak D and the peak G, correspond respectively to that there is unordered carbon structure sp3
And sp2Carbon atom vibration.
Preparing gained carbon quantum dot luminescence feature using the method for the present invention is excitation wavelength 400-600nm, and launch wavelength is
500-750nm, it can be seen that, there is typical fluorescent characteristic, carbon quantum dot size using the CQD that the method for the present invention is prepared
It is distributed in 2-20nm.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (7)
1. a kind of preparation method of fowler alkenyl carbon quantum dot, which comprises the following steps:
S1: by Fullerene Carbon ash, heating stirring is aoxidized in concentrated acid；
S2: after the reaction mixture of step S1 is cooled to room temperature, the bulky grain in mixture is removed, molecular weight is greater than 3500Da
Inorganic salts and small molecular weight impurity；
S3: by step S2, treated that reaction solution is concentrated by evaporation and is freeze-dried as powder to get fowler alkenyl carbon amounts of the present invention
Sub- point.
2. the preparation method of fowler alkenyl carbon quantum dot according to claim 1, which is characterized in that dense described in step S1
Acid is that concentration mass fraction is all larger than one or more of 95% concentrated nitric acid, the concentrated sulfuric acid, concentrated phosphoric acid.
3. the preparation method of fowler alkenyl carbon quantum dot according to claim 1, which is characterized in that heating is stirred in step S1
Mix specifically: 100-120 DEG C stirring 12-15 hours.
4. the preparation method of fowler alkenyl carbon quantum dot according to claim 1, which is characterized in that removed in step S2 big
The measure of particle are as follows: be centrifuged with the centrifugal speed of 5000-20000rpm.
5. the preparation method of fowler alkenyl carbon quantum dot according to claim 4, which is characterized in that remove nothing in step S2
The measure of machine salt and small molecular weight impurity are as follows: dialysis 3-5 days is carried out to the supernatant after centrifugation using bag filter.
6. the preparation method of fowler alkenyl carbon quantum dot according to claim 1, which is characterized in that stirred in step S1
Revolving speed is 100-1000rpm.
7. the fowler alkenyl carbon quantum dot that any one of -6 methods are prepared according to claim 1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112322089A (en) * | 2020-10-30 | 2021-02-05 | 吴志强 | Environment-friendly latex paint and preparation method thereof |
| CN113876807A (en) * | 2021-10-18 | 2022-01-04 | 物生生物科技(北京)有限公司 | Spray composition for treating eye diseases and application thereof |
| CN114843538A (en) * | 2022-05-11 | 2022-08-02 | 陕西科技大学 | Non-noble metal catalyst based on carbon quantum dots and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642494A (en) * | 2013-12-27 | 2014-03-19 | 中国科学院上海微系统与信息技术研究所 | Preparation method for fluorescence carbon-based quantum dot |
| CN105197911A (en) * | 2015-09-06 | 2015-12-30 | 福州大学 | Preparation method of fullerene-like structure carbon-based quantum dot |
| CN106118646A (en) * | 2016-07-04 | 2016-11-16 | 中国科学院兰州化学物理研究所 | The cheap preparation method of one class yellow emission carbon quantum dot |
| CN106573778A (en) * | 2014-06-19 | 2017-04-19 | 威廉马歇莱思大学 | Bandgap engineering of carbon quantum dots |
-
2018
- 2018-10-26 CN CN201811258054.2A patent/CN109266338A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103642494A (en) * | 2013-12-27 | 2014-03-19 | 中国科学院上海微系统与信息技术研究所 | Preparation method for fluorescence carbon-based quantum dot |
| CN106573778A (en) * | 2014-06-19 | 2017-04-19 | 威廉马歇莱思大学 | Bandgap engineering of carbon quantum dots |
| CN105197911A (en) * | 2015-09-06 | 2015-12-30 | 福州大学 | Preparation method of fullerene-like structure carbon-based quantum dot |
| CN106118646A (en) * | 2016-07-04 | 2016-11-16 | 中国科学院兰州化学物理研究所 | The cheap preparation method of one class yellow emission carbon quantum dot |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112322089A (en) * | 2020-10-30 | 2021-02-05 | 吴志强 | Environment-friendly latex paint and preparation method thereof |
| CN113876807A (en) * | 2021-10-18 | 2022-01-04 | 物生生物科技(北京)有限公司 | Spray composition for treating eye diseases and application thereof |
| CN113876807B (en) * | 2021-10-18 | 2023-10-27 | 物生生物科技(北京)有限公司 | Spray composition for treating eye diseases and application thereof |
| CN114843538A (en) * | 2022-05-11 | 2022-08-02 | 陕西科技大学 | Non-noble metal catalyst based on carbon quantum dots and preparation method thereof |
| CN114843538B (en) * | 2022-05-11 | 2024-04-02 | 陕西科技大学 | Non-noble metal catalyst based on carbon quantum dots and preparation method thereof |
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Application publication date: 20190125 |