CN103911151A - Sulfur phosphorus nitrogen co-doped carbon point with adjustable fluorescence property and preparation method of sulfur phosphorus nitrogen co-doped carbon point - Google Patents
Sulfur phosphorus nitrogen co-doped carbon point with adjustable fluorescence property and preparation method of sulfur phosphorus nitrogen co-doped carbon point Download PDFInfo
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Abstract
The invention discloses a sulfur phosphorus nitrogen co-doped carbon point with adjustable fluorescence property and a preparation method of the of sulfur phosphorus nitrogen co-doped carbon point. According to the technical scheme, the carbon point is prepared by processing cucumber juice as a precursor by virtue of a hydrothermal method in one step, has the particle size of 2-8nm, and is an amorphous fluorescent carbon point with the average particle sizes of 5.6nm, 3.5nm and 2.7nm respectively; the wavelengths of corresponding fluorescent spectrums are 450nm, 505nm and 571nm respectively. According to the preparation method, no chemical reagent is added, only the cucumber juice is taken as a unique raw material, a reaction is carried out in a hydrothermal reaction kettle, so that the preparation method is environmental friendly and is convenient, quick and good in repeatability.
Description
Technical field
The invention belongs to carbon nanomaterial technical field, be specifically related to adjustable nitrogen co-doped carbon point of sulphur phosphorus of a kind of fluorescence property and preparation method thereof.
Background technology
A kind of novel nano-material that carbon point is mainly made up of carbon, their size is less than 10 nanometers conventionally.Since within 2004, being isolated and purified with carbon point by the method for electrophoresis from Single Walled Carbon Nanotube first, become gradually a up-and-coming youngster of carbon nanomaterial family [referring to (a) Xu XY; Ray R; Gu Y; Ploehn HJ; Gearheart L; Raker K, et al. J. Am. Chem. Soc 2004; 126 (40): 12736-7. (b) Baker SN, Baker GA, Angew. Chem. Int. Ed 2010; 49 (38): 6726-44].Compare with fluorescence dye with traditional semiconductor-quantum-point, water-soluble, the good unreactiveness that had due to fluorescent carbon point, be easy to functionalization, high bleach-resistant, the low advantage such as toxicity and good biocompatibility, caused scientific worker's extensive concern.Its superior performance makes fluorescent carbon nano material in many Application Areass such as bio-imaging, biosensor, drug release and opto-electronic device, substitute traditional quantum dot based on toxic metal [referring to (c) Michalet X; Pinaud FF; Bentolila LA; Tsay JM; Doose S; Li JJ, et al. Science 2005; 307 (5709): 538-44. (d) Sanderson K, Nature 2009; 459 (7248): 760-1].Many carbon back fluorescent nano materials are reported at present, as soccerballene, carbon nanotube, Nano diamond and carbon point etc.Because the pattern of carbon point is controlled, size and fluorescence property are adjustable, and its abundant raw material is cheap and synthetic route easily, has caused domestic and international scientist's research boom.
Up to the present, investigator is devoted to study the different synthetic methods of carbon point, and these methods roughly can be summarized as two main types, and one is the synthesis method of (top-down) from top to bottom, and another kind is the synthesis method of (bottom-up) from bottom to top.Common top-down synthetic method comprises that arc discharge method, laser ablation method and electrochemical synthesis etc. are [referring to (e) Shen JH, Zhu YH, Yang XL, Li CZ, Chem. Commun 2012; 48 (31): 3686-99. (f) Cao L, Wang X, Meziani MJ, Lu FS, Wang HF, Luo PJG, et al. J. Am. Chem. Soc 2007; 129 (37): 11318-9. (g) Zheng L, Y Chi, Dong Y, Lin J, Wang B, J. Am. Chem. Soc 2009; 131 (13): 4564-5], and top-down synthesis method normally obtains undersized carbon point the graphite material of bulk by oxidation or the method such as ablation.Synthesis method from bottom to top comprises that combustion method or hydrothermal synthesis method, template and microwave process for synthesizing etc. are [referring to (h) Liu HP, Ye T, Mao CD, Angew. Chem. Int. Ed 2007; 46 (34): 6473-75. (i) Liu RL, Wu DQ, Liu SH, Koynov K, Knoll W, Li Q, Angew. Chem. Int. Ed 2009; 48 (25): 4598-601. (j) Zhu H, Wang XL, Li YL, Wang ZJ, Yang F, Yang XR. Chem. Commun 2009; 0 (34): 5118 – 20], common synthesis method is from bottom to top using small molecules as precursor synthesis carbon point.Recently; containing heteroatomic carbon point has become the focus of research; its reason is can effectively change by the caused structural changes of heteroatomic doping the intrinsic propesties of carbon point; comprise that Electronic Performance, surface and local chemical reactivity etc. are [referring to (k) Stephan O, Ajayan PM, Colliex C; Redlich P; Lambet JM, Bernier P, et al. Science 1994; 266 (5191): 1683-85. (l) Bourlinos BB, Bakandritsos A, Kouloumpis A, Gournis D, Krysmann M, Giannelis EP, et al. J. Mater. Chem 2012; 22 (44): 23327-30.].In the carbon point of doping, current research mainly concentrates on preparation and the optical property research thereof of nitrogen-doped carbon point.The preparation of nitrogen-doped carbon point adopts electrochemical synthesis, ultrasonic and hydrothermal treatment consists synthesis method etc. [referring to (m) Ma Z, Ming H, Huang H, Liu Y, Kang ZH, New J. Chem 2012 conventionally; 36 (4): 861-64. (n) Zhang YQ, Ma DK, Zhuang Y, Zhang X, Chen W, Hong LL, et al. J. Mater. Chem 2012; 22 (33): 16714-18. (o) Bao L, Zhang ZL, Tian ZQ, Zhang L, Liu C, Lin Y, et al. Adv. Mater 2011; 23 (48): 5801-6. (p) Sun D, Ban R, Zhang PH, Wu GH, Zhang JR, Zhu JJ. Carbon, 2013; 64:424-34].And the preparation of other Heteroatom doping carbon point, character and applied research thereof, bibliographical information is less, particularly, in preparation, character and the applied research thereof of heteroatoms codoped carbon point, substantially belongs to blank.At present, utilize hydrothermal method, take Sucus Cucumidis sativi as presoma, single stage method is prepared the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property and be have not been reported.
Summary of the invention
The technical problem that the present invention solves has been to provide adjustable nitrogen co-doped carbon point of sulphur phosphorus of a kind of fluorescence property and preparation method thereof, and this preparation method, take Sucus Cucumidis sativi as precursor, adopts the adjustable nitrogen co-doped carbon point of sulphur phosphorus of hydrothermal method one-step synthesis fluorescence property.
Technical scheme of the present invention is: the nitrogen co-doped carbon point of sulphur phosphorus that a kind of fluorescence property is adjustable, it is characterized in that utilizing take Sucus Cucumidis sativi as precursor hydrothermal method one step to be prepared from, its particle size range is 2-8nm, the nitrogen co-doped carbon point of this sulphur phosphorus is the unformed fluorescent carbon point that median size is respectively 5.6nm, 3.5nm and 2.7nm, and the wavelength of corresponding fluorescence spectrum is respectively 450nm, 505nm and 571nm.
The preparation method of the nitrogen co-doped carbon point of sulphur phosphorus that fluorescence property of the present invention is adjustable, it is characterized in that comprising the following steps: (1) utilizes juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; (2) Sucus Cucumidis sativi step (1) being obtained is transferred to the temperature confined reaction 6-36h in 100-150 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, take out the sample filtering membrane that aperture is 0.22 μ m and filter, remove macrobead and obtain the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; (3) the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus concentrated by rotary evaporation step (2) being obtained, then utilizes Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
Preparation method of the present invention is without adding any chemical reagent, and only using Sucus Cucumidis sativi as unique raw material, reaction is carried out in hydrothermal reaction kettle, and environmental protection, has advantages of convenient, fast and favorable reproducibility.
Accompanying drawing explanation
fig. 1 is the x-ray photoelectron energy spectrogram of the nitrogen co-doped carbon point of sulphur phosphorus prepared of embodiment of the present invention 1-3, Fig. 2 is the X-ray powder diffraction collection of illustrative plates of the nitrogen co-doped carbon point of sulphur phosphorus prepared of embodiment of the present invention 1-3, Fig. 3 is the uv absorption spectra of the nitrogen co-doped carbon point of sulphur phosphorus prepared of embodiment of the present invention 1-3, Fig. 4 is the fluorescence spectrum figure of the nitrogen co-doped carbon point of sulphur phosphorus prepared of embodiment of the present invention 1-3, and Fig. 5 is the transmission electron microscope picture of the nitrogen co-doped carbon point of sulphur phosphorus prepared of embodiment of the present invention 1-3.
Embodiment
By the following examples foregoing of the present invention is described in further details, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
First utilize juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; Get the Sucus Cucumidis sativi that 40mL makes and be transferred to the temperature confined reaction 6h in 100 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, taking out sample is the filtering membrane filtration of 0.22 μ m with aperture, removes macrobead and obtains the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; By the nitrogen co-doped carbon point aqueous solution of the sulphur phosphorus concentrated by rotary evaporation making, then utilize Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
Embodiment 2
First utilize juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; Get the Sucus Cucumidis sativi that 40mL makes and be transferred to the temperature confined reaction 6h in 120 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, taking out sample is the filtering membrane filtration of 0.22 μ m with aperture, removes macrobead and obtains the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; By the nitrogen co-doped carbon point aqueous solution of the sulphur phosphorus concentrated by rotary evaporation making, then utilize Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
Embodiment 3
First utilize juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; Get the Sucus Cucumidis sativi that 40mL makes and be transferred to the temperature confined reaction 6h in 150 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, taking out sample is the filtering membrane filtration of 0.22 μ m with aperture, removes macrobead and obtains the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; By the nitrogen co-doped carbon point aqueous solution of the sulphur phosphorus concentrated by rotary evaporation making, then utilize Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
Can be obtained the constituent content (atom number per-cent) of the nitrogen co-doped carbon point of sulphur phosphorus prepared by embodiment 1-3 by Fig. 1 analysis, in table 1.
The nitrogen co-doped carbon point of sulphur phosphorus that as shown in Figure 2 prepared by embodiment 1-3 is agraphitic carbon point, by Fig. 3 and the known raising along with temperature of reaction of Fig. 4, ultra-violet absorption spectrum and fluorescence spectrum generation red shift, the particle size range of the nitrogen co-doped carbon point of sulphur phosphorus that as shown in Figure 5 prepared by embodiment 1-3 is 2-8nm, median size is respectively 5.6nm, 3.5nm and 2.7nm, and its particle diameter reduces gradually along with the raising of temperature of reaction.
The constituent content of the nitrogen co-doped carbon point of table 1 sulphur phosphorus
| Example | C% (atom %) | O% (atom %) | N% (atom %) | S% (atom %) | P% (atom %) |
| Example 1 | 62.79 | 32.53 | 4.27 | 0.19 | 0.22 |
| Example 2 | 63.14 | 32.37 | 4.04 | 0.21 | 0.24 |
| Example 3 | 63.89 | 31.76 | 3.83 | 0.24 | 0.28 |
Embodiment 4
First utilize juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; Get the Sucus Cucumidis sativi that 40mL makes and be transferred to the temperature confined reaction 12h in 100 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, taking out sample is the filtering membrane filtration of 0.22 μ m with aperture, removes macrobead and obtains the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; By the nitrogen co-doped carbon point aqueous solution of the sulphur phosphorus concentrated by rotary evaporation making, then utilize Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
Embodiment 5
First utilize juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; Get the Sucus Cucumidis sativi that 40mL makes and be transferred to the temperature confined reaction 24h in 120 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, taking out sample is the filtering membrane filtration of 0.22 μ m with aperture, removes macrobead and obtains the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; By the nitrogen co-doped carbon point aqueous solution of the sulphur phosphorus concentrated by rotary evaporation making, then utilize Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
Embodiment 6
First utilize juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; Get the Sucus Cucumidis sativi that 40mL makes and be transferred to the temperature confined reaction 36h in 150 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, taking out sample is the filtering membrane filtration of 0.22 μ m with aperture, removes macrobead and obtains the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; By the nitrogen co-doped carbon point aqueous solution of the sulphur phosphorus concentrated by rotary evaporation making, then utilize Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
Above embodiment has described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; do not departing under the scope of the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (2)
1. the nitrogen co-doped carbon point of sulphur phosphorus that fluorescence property is adjustable, it is characterized in that utilizing take Sucus Cucumidis sativi as precursor hydrothermal method one step to be prepared from, its particle size range is 2-8nm, the nitrogen co-doped carbon point of this sulphur phosphorus is the unformed fluorescent carbon point that median size is respectively 5.6nm, 3.5nm and 2.7nm, and the wavelength of corresponding fluorescence spectrum is respectively 450nm, 505nm and 571nm.
2. the preparation method of the adjustable nitrogen co-doped carbon point of sulphur phosphorus of a fluorescence property claimed in claim 1, it is characterized in that comprising the following steps: (1) utilizes juice extractor that new fresh cucumbers is squeezed to Sucus Cucumidis sativi, then filter with the filtering membrane that aperture is 0.45 μ m and 0.22 μ m successively, removing macrobead, to obtain the Sucus Cucumidis sativi of stable homogeneous for subsequent use; (2) Sucus Cucumidis sativi step (1) being obtained is transferred to the temperature confined reaction 6-36h in 100-150 ℃ in hydrothermal reaction kettle, then naturally cool to room temperature, take out the sample filtering membrane that aperture is 0.22 μ m and filter, remove macrobead and obtain the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus; (3) the nitrogen co-doped carbon point aqueous solution of sulphur phosphorus concentrated by rotary evaporation step (2) being obtained, then utilizes Freeze Drying Equipment freeze-drying to make the nitrogen co-doped carbon point of the adjustable sulphur phosphorus of fluorescence property.
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| CN104987863A (en) * | 2015-06-25 | 2015-10-21 | 西安交通大学 | Nitrogen, phosphorus and sulphur doping or co-doping carbon dot and batch controllable preparing method and application thereof |
| CN105502339A (en) * | 2015-12-28 | 2016-04-20 | 江南大学 | Method for hydro-thermal synthesis of carbon quantum dots with fresh ginger as raw material |
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