Sulfydryl-modified molybdenum sulfide quantum dot, preparation method of sulfydryl-modified molybdenum sulfide quantum dot and detection method of 2,4,6-trinitrotoluene

A technology of trinitrotoluene and sulfhydryl modification, which can be used in chemical instruments and methods, measuring devices, fluorescence/phosphorescence, etc., and can solve problems such as the existence of molybdenum oxide sulfide quantum dots

Active Publication Date: 2017-08-01
ANHUI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, there are still some problems in these methods. Firstly, whether it is an organic solvent or an organic molecule that provides a sulfur source, there is a possibility of carbonization under high temperature conditions, that is, there may be carbon points mixed in the product; secondly, the introduction of hydrogen peroxide is due to its oxidation. properties, so it has the possibility of oxidizing molybdenum sulfide quantum dots

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  • Sulfydryl-modified molybdenum sulfide quantum dot, preparation method of sulfydryl-modified molybdenum sulfide quantum dot and detection method of 2,4,6-trinitrotoluene
  • Sulfydryl-modified molybdenum sulfide quantum dot, preparation method of sulfydryl-modified molybdenum sulfide quantum dot and detection method of 2,4,6-trinitrotoluene
  • Sulfydryl-modified molybdenum sulfide quantum dot, preparation method of sulfydryl-modified molybdenum sulfide quantum dot and detection method of 2,4,6-trinitrotoluene

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preparation example Construction

[0031] Among the present invention, a kind of preparation method of molybdenum sulfide quantum dots modified by mercapto group is provided, wherein, the preparation method comprises:

[0032] 1) first mix hydroxylamine hydrochloride, molybdenum disulfide and an inorganic solvent, then perform heat treatment, and then carry out centrifugal purification to obtain molybdenum sulfide quantum dots;

[0033] 2) Mixing the molybdenum sulfide quantum dots, the mercapto-containing compound and an inorganic solvent, and then performing a contact reaction to prepare mercapto-modified molybdenum sulfide quantum dots.

[0034] In the above-mentioned preparation method, the amount of each component can be selected in a wide range, as long as the molybdenum disulfide is sufficiently stripped so that the heat treatment reaction can proceed; but in order to further improve the molybdenum disulfide stripping efficiency As for the production yield of quantum dots, preferably, relative to 1 part ...

Embodiment 1

[0053] First, mix hydroxylamine hydrochloride, molybdenum disulfide and water according to the weight ratio of 1:0.2:90, transfer it to a high-pressure reactor, heat it in water at 180°C for 10 hours, and then select a rotation speed of 11,000 rpm for 15 minutes to obtain molybdenum sulfide quantum dots;

[0054] Next, mix the purified molybdenum sulfide quantum dots with cysteine ​​at a weight ratio of 0.03:0.6, then add water, conduct a contact reaction at 60°C for 10 hours, and then transfer to a dialysis bag with a molecular weight of 1000 for dialysis for 12 hours , that is, the sulfhydryl-modified molybdenum sulfide quantum dots were prepared, denoted as A1.

Embodiment 2

[0056] First, mix hydroxylamine hydrochloride, molybdenum disulfide and water according to the weight ratio of 1:0.3:95, transfer to a high-pressure reactor, heat water at 190°C for 11 hours, and then select a speed of 11,000rpm for centrifugal purification for 15 minutes to obtain molybdenum sulfide quantum dots; then, The purified molybdenum sulfide quantum dots and cysteine ​​were mixed according to the weight ratio of 0.04:0.7, then water was added, and the contact reaction was carried out at 80°C for 11 hours, and then transferred to a dialysis bag with a molecular weight of 1000 for dialysis for 12 hours. The mercapto-modified molybdenum sulfide quantum dots were prepared, denoted as A2.

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Abstract

The invention discloses a sulfydryl-modified molybdenum sulfide quantum dot, a preparation method of the sulfydryl-modified molybdenum sulfide quantum dot and a detection method of 2,4,6-trinitrotoluene, wherein the method comprises the following steps of 1, firstly mixing hydroxylamine hydrochloride, molybdenum disulfide and solvents; then, performing heat treatment; next, performing centrifugal purification so as to prepare the sulfydryl-modified molybdenum sulfide quantum dot; (2) mixing the sulfydryl-modified molybdenum sulfide quantum dot, sulfydryl-containing compounds and the solvents; then, performing contact reaction so as to prepare the sulfydryl-modified molybdenum sulfide quantum dot. The sulfydryl-modified molybdenum sulfide quantum dot prepared by the method has the advantages of high quantum yield, strong anti-jamming capability and good stability. In addition, the sulfydryl-modified molybdenum sulfide quantum dot prepared by the method has the good selectivity on the detection of the 2,4,6-trinitrotoluene solution concentration.

Description

technical field [0001] The invention relates to an inorganic nanometer material, in particular to a molybdenum sulfide quantum dot modified by a mercapto group, a preparation method thereof and a detection method of 2,4,6-trinitrotoluene. Background technique [0002] In recent years, due to transition metal chalcogenides (MoS 2 ,WS 2 ,WSe 2 etc.) Similar to the two-dimensional layered structure of graphene, it has attracted extensive attention due to its special optoelectronic properties. When the size of the two-dimensional material is less than about 10nm, it becomes a quantum dot with excellent luminescence performance. Molybdenum sulfide quantum dots currently prepared are usually prepared by mixing chalcogenide bulk materials with organic solvents and ultrasonically reflowing at high temperature to prepare molybdenum sulfide quantum dots, or using sulfur-containing organic matter to provide sulfur sources and sodium molybdate to provide molybdenum sources. Either p...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/68G01N21/64
CPCC09K11/02C09K11/681G01N21/6428
Inventor 夏云生张慧
Owner ANHUI NORMAL UNIV
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