CN106634982B - Solid red silanized carbon dots and preparation method thereof - Google Patents
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000007787 solid Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 27
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 20
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
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- 239000002245 particle Substances 0.000 claims description 7
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical group CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 3
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 4
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 4
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
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- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 125000005370 alkoxysilyl group Chemical group 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- SBVCEDLIWDSBGE-UHFFFAOYSA-N iminosilane Chemical compound [SiH2]=N SBVCEDLIWDSBGE-UHFFFAOYSA-N 0.000 description 2
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- 238000006467 substitution reaction Methods 0.000 description 2
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 2
- XRWBWOMIMCRATH-UHFFFAOYSA-N CC1(C)C2(C)C(CCC[Si](OC)(OC)OC)CC1CC2 Chemical compound CC1(C)C2(C)C(CCC[Si](OC)(OC)OC)CC1CC2 XRWBWOMIMCRATH-UHFFFAOYSA-N 0.000 description 1
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- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses solid red silanization and a preparation method and application thereof. The method is a reflux method and comprises the following steps: dissolving citric acid in acetone, uniformly mixing with a silane coupling agent, heating for reaction to obtain viscous red carbon dots, and placing the viscous red carbon dots in a 60 ℃ oven for 24 hours to obtain solid carbon dots. The method can rapidly obtain the solid carbon dots in one step by simple and rapid reflux reaction without subsequent treatment of strong acid or a surface passivator, and has the advantages of simple and easily obtained raw materials, low price and mild reaction conditions. The problem that the existing solid red carbon dots cannot be produced in a large scale due to the limitation of the preparation process and raw materials is solved, and the prepared carbon dots are good in stability and free of deliquescence.
Description
Technical Field
The invention belongs to the technical field of fluorescent nano material synthesis, and particularly relates to solid red silanized Carbon Dots (CDs) and a preparation method thereof.
Background
The fluorescent carbon nano material has better fluorescence performance and low toxicity, and has good application prospect in the fields of information safety, photocatalytic drug transmission, cell imaging, sensing, photoelectric devices, disease diagnosis and the like. Carbon dots, one of the fluorescent carbon nanomaterials, have received much attention due to their unique optical properties and environmental friendliness.
However, the solid-state carbon quantum dots are difficult to prepare at present because the carbon dots are easy to cause fluorescence quenching when in an aggregation state. Most of the work in the field so far is about the fluorescence property and application of the carbon dot aqueous solution, and few reports relate to the solid-state luminescence property and related application of the carbon dot hybrid solid-phase material and the carbon dot aggregate.
The studies on the carbon dot luminescence property in the art are mostly limited to the fluorescence of short wavelength (blue, green), and the fluorescence of long wavelength (orange, red) are rarely reported. The long wavelength fluorescence has the excellent characteristics that the short wavelength fluorescence cannot be achieved in special applications, so that the research on the red fluorescent carbon dot is particularly important. Although there are reports about red-light carbon dots, they all show liquid fluorescence, and the research on solid red-light carbon dots is very important.
In order to overcome the defects of the prior art, the invention provides a novel solid red carbon dot and a preparation method thereof. The preparation method disclosed by the invention is simple and quick in operation process, cheap and easily-obtained in raw materials, good in product stability, free of deliquescence, simple in preparation process of carbon dots, easy in post-treatment, uniform in particle size (as shown in figure 3), and remarkable in fluorescence effect, wherein the carbon dots do not have typical fluorescence excitation dependent properties (as shown in figure 8), and are different from the carbon dots with excitation dependent properties reported by most of documents.
Disclosure of Invention
The invention discloses a solid red silanized carbon dot and a preparation method and application thereof. The method can rapidly obtain the solid carbon dots in one step by simple and rapid reflux reaction without subsequent treatment of strong acid or a surface passivator, and has the advantages of simple and easily obtained raw materials, low price and mild reaction conditions. The problem that the existing solid red carbon dots cannot be produced in a large scale due to the limitation of a preparation process and raw materials is solved, the prepared carbon dots are good in stability, free of deliquescence, uniform in particle size (as shown in figure 3) and remarkable in fluorescence effect, and the carbon dots do not have typical fluorescence excitation dependence (as shown in figure 8) and are different from the carbon dots with excitation dependence reported by most of documents.
In one aspect, the invention provides a method for preparing novel solid red carbon dots. The preparation method has the advantages of simple and quick operation process, cheap and easily-obtained raw materials and good product stability.
The preparation method of the carbon dot provided by the invention has the advantages that the preparation process of the carbon dot is simple, the post-treatment is easy, the particle size is uniform (as shown in figure 3), the stability is good, the fluorescence effect is obvious, the carbon dot does not have typical fluorescence excitation dependent properties (as shown in figure 8), the excitation is changed, the emission peak position is unchanged, and the method is different from the carbon dot with the excitation dependent properties reported by most of literatures.
In one aspect, the invention relates to a preparation method of solid red silanized carbon dots, wherein the method is a reflux method and comprises the following steps: dissolving citric acid in acetone to obtain a uniformly mixed solution, adding the uniformly mixed solution into a silane coupling agent, heating for reaction to obtain a viscous carbon dot, and placing the viscous carbon dot in an oven for drying to obtain a solid carbon dot.
In some embodiments, the method of the present invention, wherein the resulting viscous state carbon dot is placed in a 60 ℃ oven for 24h to obtain a solid state carbon dot.
In some embodiments, the methods of the invention, wherein the heating reaction is performed at 150-240 ℃.
In some embodiments, the method of the invention, wherein the heating reaction has a reaction time of 5 to 60 min.
In some embodiments, the method of the present invention, wherein the amount ratio of the citric acid to the acetone to the silane coupling agent is 1-4 g: 5-10 mL: 10-20 mL.
In some embodiments, the method of the present invention, wherein the citric acid, acetone, and silane coupling agent are used in a ratio of 1g:5mL:10 mL.
In some embodiments, the method of the present invention, wherein the silane coupling agent comprises at least one of an aminosilane coupling agent comprising 2 to 3 alkoxysilyl groups, an iminosilane coupling agent, an epoxysilane coupling agent, and a mercaptosilane coupling agent.
In some embodiments, the method of the present invention, wherein the silane coupling agent comprises at least one of N- (β -aminoethyl) - γ -aminopropyl-methyldimethoxysilane, N-aminoethyl- γ -aminopropyl-trimethoxysilane, 3-aminopropyltriethoxysilane, methyltriethoxysilane, and 3-bornylpropyltrimethoxysilane.
In some embodiments, the process of the present invention, wherein the silane coupling agent is N- (β -aminoethyl) - γ -aminopropyl-methyldimethoxysilane.
In another aspect, the present invention relates to solid red silanized carbon dots prepared by the method of the present invention, wherein the carbon dots have a particle size of 5-7nm, and the transmission electron microscopy image is substantially as shown in fig. 3.
In some embodiments, the carbon dots of the present invention have a degree of graphitization structure with a high resolution transmission electron micrograph substantially as shown in figure 4.
In some embodiments, the carbon dots of the present invention comprise Si element and C element content up to about 63.42%, with the XPS spectrum substantially as shown in figure 5.
In some embodiments, the XRD pattern of the carbon dots of the present invention is substantially as shown in figure 6.
The purpose of the invention is realized by the following technical scheme: silanization of red solid carbon dots, including optimal preparation conditions and post-treatment methods.
A preparation method of solid red silanized carbon dots comprises the following steps:
the preparation method of the carbon dots is a reflux method, and comprises the following steps:
(1) dissolving citric acid in acetone, and performing ultrasonic dispersion to completely dissolve the citric acid to obtain a solution;
(2) adding the solution obtained in the step (1) into a silane coupling agent, and carrying out reflux reaction to obtain a flowing viscous red carbon dot;
(3) placing the flowing viscous carbon dots obtained in the step (2) in a 60 ℃ oven to stand for 24 hours to obtain solid red carbon dots;
the dosage ratio of the citric acid to the acetone to the silane coupling agent is 1g to 5mL to 10 mL.
The reflux reaction is preferably carried out at 150 ℃ and 240 ℃ for 5-60min, and more preferably at 150 ℃ for 5 min.
The silane coupling agent described in the present invention includes, but is not limited to, at least one of aminosilane coupling agent containing 2 to 3 alkoxysilyl groups, iminosilane coupling agent, epoxysilane coupling agent, and mercaptosilane coupling agent, such as N- (β -aminoethyl) - γ -aminopropyl-methyldimethoxysilane (AEAPMS), N-aminoethyl- γ -aminopropyl-trimethoxysilane (AEATMS), 3-Aminopropyltriethoxysilane (APTES), Methyltriethoxysilane (METS), 3-Mercaptopropyltrimethoxysilane (MPTES), and the like. More preferably N- (β -aminoethyl) - γ -aminopropyl-methyldimethoxysilane (AEAPMS).
(4) The carbon dots obtained in the step (3) have good stability, can emit bright red light under ultraviolet light, and can be compounded with various substances to obtain a composite material with excellent performance.
The term "substantially as shown" as used herein means that at least 50%, or at least 60%, or at least 70%, or at least 80%, or at least 90%, or at least 95%, or at least 99% of the features or peaks in the transmission electron micrograph, XPS spectrum, or XRD spectrum are shown in the figures.
In the context of the present invention, the word "about" or "approximately" when used or whether used, means within 10%, suitably within 5%, and especially within 1% of a given value or range. Alternatively, the term "about" or "approximately" means within an acceptable standard error of the mean, for one of ordinary skill in the art. Whenever a number is disclosed with a value of N, any number within the values of N +/-1%, N +/-2%, N +/-3%, N +/-5%, N +/-7%, N +/-8% or N +/-10% is explicitly disclosed, wherein "+/-" means plus or minus.
The principle of the invention is as follows:
the method utilizes the reflux reaction of the citric acid, the acetone and the silane coupling agent, has the advantages of simple and easily obtained raw materials, low price, mild reaction conditions, high yield of prepared carbon dots and stable fluorescence property, and can be well applied to the fields of photoelectric devices, photocatalysis, biological imaging, agriculture and the like.
Compared with the prior art, the invention has the following advantages and effects:
(1) according to the invention, citric acid, acetone and a silane coupling agent are used for reflux reaction, and subsequent strong acid or surface passivating agent treatment is not needed, so that the solid carbon dots can be simply and rapidly obtained.
(2) The method has the advantages of wide and easily available raw materials, low price, mild preparation conditions, low energy consumption, reaction at 150 ℃, high yield, capability of preparing 8mL of liquid viscous carbon dots and hopeful large-scale industrial production.
(3) The carbon dots prepared by the method have the advantages of good stability, no deliquescence, good light stability and uniform particle size (shown in figure 3), do not have typical fluorescence excitation dependence (shown in figure 8), have changed excitation and unchanged emission peak positions, are different from the carbon dots with excitation dependence reported by most of documents, and can be applied to the fields of photoelectricity, photocatalysis, gas sensing, agriculture and the like.
Drawings
Fig. 1 shows the emission spectra of carbon dots (λ ex 365nm) obtained in example 1 at different reaction temperatures.
Fig. 2 shows the emission spectra of the carbon dots obtained in example 2 at different reaction times (λ ex-365 nm).
FIG. 3 is a transmission electron micrograph of carbon dots prepared in example 3 at an optimum reaction temperature (150 ℃ C.) and an optimum reaction time (5 min).
FIG. 4 is a high resolution TEM image of carbon dots prepared in example 3 at the optimal reaction temperature (150 ℃ C.) and the optimal reaction time (5 min).
FIG. 5 is an XPS spectrum of the carbon dots obtained in example 3.
FIG. 6 is an XRD spectrum of carbon dots obtained in example 3.
FIG. 7 is an IR spectrum of a carbon dot obtained in example 3.
FIG. 8 is a graph of the emission spectra of carbon dots prepared in example 3 under different excitations.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
1g of citric acid was dissolved in 5mL of acetone, and the solution was added to 10mL of a silane coupling agent (AEAPMS, industrial grade, available from Kyork chemical Co., Ltd.) and subjected to a reflux reaction at 150 ℃ and 240 ℃ for 10 min. The carbon dots under different reaction temperatures can be prepared, and the emission spectrum is shown in figure 1 (obtained by testing with a fluorescence spectrometer F-7000 of Tianmei (China) scientific instruments, Inc.).
Example 2
1g of citric acid was dissolved in 5mL of acetone, and the solution was dissolved completely by sonication, and then the obtained solution was added to 10mL of a silane coupling agent (AEAPMS, industrial grade, available from Guangzhou Longkai chemical Co., Ltd.) to carry out a reflux reaction at 150 ℃ for 5 to 60 minutes. The carbon dots under different reaction times can be prepared, and the emission spectrum is shown in figure 2 (obtained by testing with fluorescence spectrometer F-7000 of Tian Mei (China) scientific instruments Co., Ltd.).
Example 3
Dissolving 1g of citric acid in 5mL of acetone, performing ultrasonic treatment to completely dissolve the citric acid, adding the obtained solution into 10mL of silane coupling agent (AEAPMS, industrial grade, available from Guangzhou Longkai chemical engineering Limited responsibility company), performing reflux reaction at 150 ℃ for 5min (namely, the optimal reaction temperature and reaction time), and cooling to room temperature to obtain the viscous carbon dots. The carbon dots produced were observed and tested, and the results are shown in FIGS. 3-8.
Referring to FIG. 3, it is a transmission electron microscope image of the carbon dots prepared in this example, and it is apparent from the image that the carbon dots are uniformly distributed, and have good dispersibility and particle size of 5-7 nm.
Referring to fig. 4, which is a high-resolution transmission electron microscope image of the carbon dots prepared in the present embodiment, it can be clearly seen that the carbon dots have obvious lattice fringes, which indicates that the prepared carbon dots have a certain degree of graphitization structure.
Referring to fig. 5, the XPS spectrum of the carbon dots obtained in the present example and the element content thereof are shown, and it is apparent from the figure that the material contains Si element.
Referring to fig. 6, which is an XRD spectrum of the carbon dots prepared in this embodiment and the content of the elements thereof, it is apparent from the graph that the carbon dots exhibit a broad peak with a peak position of 25 degrees, which corresponds to a characteristic peak of the graphitized structure of the carbon dots, and corresponds to the [002] crystal plane of graphite, which can further explain the graphitized lattice stripe of fig. 4. This also further confirms that the material is a graphitized carbon dot.
Referring to FIG. 7, it is an infrared spectrum of a carbon dot obtained in the present embodiment, and it can be seen that the carbon dot contains Si-O-Si, Si-O-CH, and Si-CH2The absorption of the bond indicates that the product produced is a silane functionalized carbon site.
Referring to fig. 8, which is a spectrum of emission light of carbon dots prepared in the present embodiment at different excitation wavelengths, it can be seen from the graph that as the excitation wavelength is continuously increased by 500-.
The silane coupling agents in the above examples may be replaced with other silane coupling agents such as APTES, AEATMS, or MPTES in addition to AEAPMS, and the effects are consistent.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. A preparation method of solid red silanized carbon dots is a reflux method and comprises the following steps: dissolving citric acid in acetone to obtain a uniformly mixed solution, then adding the uniformly mixed solution into a silane coupling agent, heating for reaction to obtain a viscous carbon dot, and then placing the viscous carbon dot in an oven for standing to obtain a solid carbon dot; wherein,
the silane coupling agent is N- (beta-aminoethyl) -gamma-aminopropyl-methyldimethoxysilane;
the dosage ratio of the citric acid to the acetone to the silane coupling agent is 1g:5mL:10 mL;
the heating reaction is at 150oAnd C, reacting for 5 min.
2. The method of claim 1, wherein the viscous state carbon dot is placed at 60 foAnd standing in an oven C for 24 hours to obtain solid carbon dots.
3. A solid red silanized carbon dot prepared according to the method of any one of claims 1-2, wherein the carbon dot particle size is 5-7 nm.
4. The carbon dot according to claim 3, wherein the carbon dot contains an Si element and a C element content is 63.42%.
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