CN111218285B - Preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed solution - Google Patents
Preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed solution Download PDFInfo
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- CN111218285B CN111218285B CN202010081228.3A CN202010081228A CN111218285B CN 111218285 B CN111218285 B CN 111218285B CN 202010081228 A CN202010081228 A CN 202010081228A CN 111218285 B CN111218285 B CN 111218285B
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Abstract
The invention discloses a preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed liquor. Mixing 1 part by weight of selenium powder and 20-80 parts by weight of ethylenediamine, and stirring at 20-30 ℃ for 0.5 hour to obtain a selenium-amine mixed solution; and pouring the obtained selenium-amine mixed solution into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 170-240 ℃ for 3-10 hours to obtain the fluorescent selenium nanoparticles. The fluorescent selenium nanoparticles prepared by the method disclosed by the invention are narrow in size distribution, 2-5 nm in size, excellent in water dispersibility and fluorescence property, simple in preparation process, short in preparation period and low in preparation cost. The fluorescent selenium nano-particles have good application prospects in the aspects of biological imaging, biological detection, functional medicines, photoelectric devices and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of fluorescent selenium nano particles based on selenium-amine mixed liquor.
Background
Fluorescent nanomaterials have shown great potential for applications in a number of fields such as optoelectronic devices, sensors, cellular imaging, etc., due to their unique optical properties. Compared with the fluorescent nano material containing metal elements, the fluorescent nano material without metal elements has good biocompatibility, so that the fluorescent nano material is more suitable for being applied to the fields of biological detection and biological imaging. In recent years, a plurality of fluorescent nano materials containing no metal elements, such as conjugated polymer nanoparticles, carbon quantum dots, silicon nanoparticles, sulfur quantum dots, and the like, have been synthesized, but the synthesis of fluorescent selenium nanoparticles is rarely reported. Selenium is a typical non-metallic element, selenium resources in China are rich, but high-added-value selenium-containing products are few. On the other hand, selenium is widely used in the medical field as one of the essential elements for human body, and the preparation of nanoparticles containing selenium to improve the absorption of selenium by human body has also received much attention. Therefore, the simple preparation method of the fluorescent selenium nano-particles has profound theoretical significance and application value, and not only can promote research and application of fluorescent selenium nano-materials, but also can promote development and utilization of selenium resources.
Disclosure of Invention
The invention aims to provide a preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed liquor, which has two key points, namely, the selenium-amine mixed liquor is used as a raw material and a hydrothermal reaction kettle is used for carrying out solvothermal reaction.
The method comprises the following specific steps:
(1) mixing 1 part by weight of selenium powder and 20-80 parts by weight of ethylenediamine, and stirring at 20-30 ℃ for 0.5 hour to obtain a selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at the temperature of 170-240 ℃ for 3-10 hours to obtain the fluorescent selenium nanoparticles.
The chemical reagents are all chemically pure or above.
The invention has the advantages of simple preparation process, short preparation period, low preparation cost and the like; the shape and size of the prepared fluorescent selenium nano-particles are tested by a transmission electron microscope, and the result shows that the fluorescent selenium nano-particles are spherical particles, the particle size distribution is narrow, and the size is 2-5 nanometers; the structure of the selenium nanoparticle is tested by a Raman spectrometer, and the selenium nanoparticle is proved to be the selenium nanoparticle; the optical performance of the aqueous dispersion is further tested by an ultraviolet-visible spectrophotometer and a fluorescence spectrometer, and the result proves that the aqueous dispersion has excellent water dispersibility and excellent fluorescence performance; in addition, the fluorescent selenium nanoparticles have good application prospects in the aspects of biological imaging, biological detection, functional medicines, photoelectric devices and the like.
Drawings
Fig. 1 is a transmission electron microscope photograph of fluorescent selenium nanoparticles prepared in example 1 of the present invention.
Fig. 2 is a raman spectrum of the fluorescent selenium nanoparticle prepared in example 1 of the present invention.
Fig. 3 is a uv-vis absorption spectrum of an aqueous dispersion of fluorescent selenium nanoparticles prepared in example 1 of the present invention.
FIG. 4 is a fluorescence spectrum of an aqueous dispersion of fluorescent selenium nanoparticles prepared in example 1 of the present invention (excitation wavelength of 340 nm).
Detailed Description
Example 1:
(1) 1 g of selenium powder and 30 g of ethylenediamine are mixed and stirred for 0.5 hour at the temperature of 30 ℃ to obtain selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 200 ℃ for 6 hours to obtain the fluorescent selenium nanoparticles.
Example 2:
(1) 1 g of selenium powder and 20 g of ethylenediamine are mixed and stirred for 0.5 hour at 25 ℃ to obtain selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 170 ℃ for 10 hours to obtain the fluorescent selenium nanoparticles.
Example 3:
(1) 2 g of selenium powder and 160 g of ethylenediamine are mixed and stirred for 0.5 hour at the temperature of 20 ℃ to obtain selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 220 ℃ for 5 hours to obtain the fluorescent selenium nanoparticles.
Example 4:
(1) 1 g of selenium powder and 50 g of ethylenediamine are mixed and stirred for 0.5 hour at the temperature of 20 ℃ to obtain selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 230 ℃ for 5.5 hours to obtain the fluorescent selenium nanoparticles.
Example 5:
(1) 1.5 g of selenium powder and 60 g of ethylenediamine are mixed and stirred for 0.5 hour at the temperature of 28 ℃ to obtain selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 210 ℃ for 4.5 hours to obtain the fluorescent selenium nanoparticles.
Example 6:
(1) 1 g of selenium powder and 25 g of ethylenediamine are mixed and stirred for 0.5 hour at the temperature of 22 ℃ to obtain selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 240 ℃ for 3 hours to obtain the fluorescent selenium nanoparticles.
Example 7:
(1) 1 g of selenium powder and 60 g of ethylenediamine are mixed and stirred for 0.5 hour at 26 ℃ to obtain selenium-amine mixed solution.
(2) And (2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 190 ℃ for 8 hours to obtain the fluorescent selenium nanoparticles.
The above-described embodiments are merely preferred embodiments of the present invention, and it should be noted that, for those skilled in the art, various modifications can be made without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (1)
1. A preparation method of fluorescent selenium nanoparticles based on selenium-amine mixed solution is characterized by comprising the following specific steps:
(1) mixing 1 part by weight of selenium powder and 20-80 parts by weight of ethylenediamine, and stirring at 20-30 ℃ for 0.5 hour to obtain a selenium-amine mixed solution;
(2) pouring the selenium-amine mixed solution obtained in the step (1) into a hydrothermal reaction kettle, and then reacting the hydrothermal reaction kettle at 170-240 ℃ for 3-10 hours to obtain fluorescent selenium nanoparticles;
the chemical reagents are all chemically pure or above.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276985A (en) * | 2016-12-08 | 2018-07-13 | 西安科技大学 | It is a kind of with the sulphur quantum dot of fluorescent characteristic, preparation method and applications |
| CN109810553A (en) * | 2019-01-07 | 2019-05-28 | 湖北大学 | A kind of graphene oxide composite hydroxylapatite sulfur loaded quantum dot antimicrobial coating and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276985A (en) * | 2016-12-08 | 2018-07-13 | 西安科技大学 | It is a kind of with the sulphur quantum dot of fluorescent characteristic, preparation method and applications |
| CN109810553A (en) * | 2019-01-07 | 2019-05-28 | 湖北大学 | A kind of graphene oxide composite hydroxylapatite sulfur loaded quantum dot antimicrobial coating and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| FACILE SYNTHESIS AND CHARACTERIZATION OF SELENIUM NANOPARTICLES BY THE HYDROTHERMAL APPROACH;Shar, AH 等;《DIGEST JOURNAL OF NANOMATERIALS AND BIOSTRUCTURES》;20191231;第14卷(第4期);867-872 * |
| Oxygen accelerated scalable synthesis of highly fluorescent sulfur quantum dots;Song, YH;等;《CHEMICAL SCIENCE》;20200121;第11卷(第3期);772-777 * |
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Application publication date: 20200602 Assignee: Changsha Houcheng Nanomaterial Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000493 Denomination of invention: A Preparation Method of Fluorescent Selenium Nanoparticles Based on Selenium amine Mixture Granted publication date: 20220211 License type: Common License Record date: 20221229 |
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