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Method for photochemically preparing nano selenium

A nano-selenium and photochemical technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of inhomogeneity of nano-selenium particles, complex phase separation in the later stage, and strict reaction conditions, etc., to achieve Easy-to-master control, high industrial application prospects, easy-to-implement effects

Active Publication Date: 2019-11-01
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Based on the problems of inhomogeneous nano-selenium particles prepared in the existing preparation method, non-directional growth, strict reaction conditions and complex phase separation in the later stage, the object of the present invention is to Provides a method for photochemically preparing nano-selenium, which has the advantages of rapidity, high efficiency, mildness, controllability, and uniformity

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  • Method for photochemically preparing nano selenium
  • Method for photochemically preparing nano selenium
  • Method for photochemically preparing nano selenium

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1 photochemical reaction prepares nano selenium

[0038] Set the molar ratio of sodium selenite to AA (or BD) at 1:5, take 0.5mL of 10mM sodium selenite and 5mL of 5mM AA (or BD) solution, and add them to a glass colorimetric tube with a volume of 25mL , add ultrapure water to dilute to the mark, shake evenly, that is, 0.2mM selenite, 1.0mM AA or BD.

[0039] Then pour into a 25mL quartz photoreaction tube, and finally put the reaction tubes into the photoreactor one by one. The light intensity of the reaction is 13.5mW / cm 2 , and respectively illuminate the corresponding AA-containing solution for 70 minutes, and the solution of BD for 40 minutes to obtain a uniform red elemental selenium colloidal mixture.

[0040] Centrifuge the red colloid mixture (10000rpm, centrifuge for 30min), remove the supernatant, add ultrapure water to wash and then centrifuge, after repeating this three times, freeze-dry the obtained colloidal nano-selenium (-50°C, 0.120mBar, d...

Embodiment 2

[0044] Example 2 The influence of selenite concentration on the preparation of nano-selenium by UV / AA method reduction of selenite

[0045] Set the molar concentration of AA to 1.0mM, and the molar ratios of sodium selenite and AA to 1:10 and 1:5, respectively. Take 0.25 and 0.5mL of 10mM sodium selenite solution, 5mL of 5mM Add the AA solution into a glass colorimetric tube with a volume of 25mL, add ultrapure water to dilute to the mark, and oscillate evenly to obtain 0.1 and 0.2mM selenite solutions and 1.0mMAA respectively. Then pour into a 25mL quartz photoreaction tube, and finally put the reaction tubes into the photoreactor one by one. The light intensity of the reaction is 13.5mW / cm 2 , light reaction for 120min, sampling once every 5min to detect the concentration of selenite.

[0046] Figure 4 It is a schematic diagram of the change of selenite concentration in this embodiment. When the concentration of AA is constant and the concentration of selenite is 0.1mM,...

Embodiment 3

[0047] Example 3 Effect of Diketone Concentration on the Preparation of Nano-Selenium by UV / Diketone Method Reduction of Selenite

[0048] The molar concentration of sodium selenite is set to 0.2mM, the molar ratio of sodium selenite and AA or BD is set at 1:5, 1:10 and 1:15, take 0.5mL of 10mM sodium selenite solution, 5. Add 10 or 15mL of 5mM AA (or BD) solution into a glass colorimetric tube with a volume of 25mL, add ultrapure water to dilute to the mark, and oscillate evenly to obtain 0.2mM selenite, 1.0, 2.0 and 3.0 mM AA or BD. Then pour into a 25mL quartz photoreaction tube, and finally put the reaction tubes into the photoreactor one by one. The light intensity of the reaction is 13.5mW / cm 2 , light reaction for 80min, sampling once every 10min to detect the concentration of selenite.

[0049] Figure 5 It is a schematic diagram of the change of selenite concentration in this embodiment. Under the same conditions, the sequence of conversion effects of different p...

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Abstract

The invention discloses a method for photochemically preparing nano selenium. The method comprises the following steps: (1) uniformly mixing a selenite solution and a small-molecular diketone, and performing irradiation under an ultraviolet (UV) light source to prepare a nano selenium colloidal mixed liquid, wherein a molar concentration ratio of the selenite to the diketone is 1:(5-15); and (2) performing centrifugation on the colloidal mixed liquid, removing the supernatant, performing washing by using ultrapure water, performing centrifugation, and repeating the operation for three times toobtain colloidal nano selenium; and performing freeze drying to obtain the finished-product nano selenium. According to the method provided by the invention, the nano selenium obtained by the above method has a particle size range from 30 to 120 nm, shows better-dispersed nano-spherical particles, and has a stronger photocurrent signal and larger application value in the field of optoelectronics;and in the preparation method provided by the present application, the UV / diketone method is a homogeneous reaction, does not need a surfactant, and is simple and convenient to operate; compared witha UV / sulfite (SO3<2->) method, the method provided by the invention has higher efficiency and a wider pH applicable range (3.0 to 8.0); and compared with heterogeneous methods such as a UV / TiO2 heterogeneous method, the method provided by the invention does not need complicated phase separation.

Description

technical field [0001] The invention relates to the preparation of nanometer materials, in particular to a method for photochemically preparing nanometer selenium. Background technique [0002] Nano-selenium mainly has two forms, amorphous and crystalline, and is an important element semiconductor other than silicon and germanium. Due to its good biological activity, amorphous nano-selenium can play an important role in antagonizing harmful heavy metals, regulating immunity, anti-cancer, and anti-oxidation. Crystalline nanoselenium has a low melting point (~490K) and high optical conductivity (~8×10 4 S / cm), high chemical activity and other advantages, it is widely used in the fields of sensors, rectifiers, exposure components, photocells, electrostatic copying and so on. Due to the wide application of nano-selenium, its preparation method has attracted wide attention. Chinese patent CN1184776A discloses a preparation method of active red elemental selenium, and the nano-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/02B82Y30/00
CPCC01B19/02B82Y30/00
Inventor 张淑娟张丽任杰张驰吴兵党甘永海陈志豪
Owner NANJING UNIV
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