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Preparation method of poly 2,5-dimercapto-1,3,4-thiadiazole nanosheets

A technology of thiadiazole and dimercapto, which is applied in the field of preparation of poly 2,5-dimercapto-1,3,4-thiadiazole nanosheets, can solve the problem of low polymer molecular weight and low yield that have not been found yet. Low problems, to achieve the effect of good self-stabilization, high yield, high molecular weight and yield

Inactive Publication Date: 2020-08-11
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the chemical oxidative polymerization of 2,5-dimercapto-1,3,4-thiadiazole, methanol, water-methanol (volume ratio 1:1), water-ethanol (volume ratio 1:2), or 0.1 mol L -1 Acetic acid-sodium acetate aqueous solution is the reaction medium, iodine, hydrogen peroxide, or ammonium persulfate is the oxidant, the product is light yellow, but the general yield is low, and the molecular weight of the polymer is not high
Moreover, so far, there has been no report on the preparation of poly-2,5-dimercapto-1,3,4-thiadiazole nanosheets by chemical oxidative polymerization.

Method used

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  • Preparation method of poly 2,5-dimercapto-1,3,4-thiadiazole nanosheets
  • Preparation method of poly 2,5-dimercapto-1,3,4-thiadiazole nanosheets
  • Preparation method of poly 2,5-dimercapto-1,3,4-thiadiazole nanosheets

Examples

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Embodiment 1

[0035] Example 1: A method for preparing poly-2,5-dimercapto-1,3,4-thiadiazole nanosheets by chemical oxidative polymerization, the specific operation is as follows:

[0036] (1) Accurately weigh 2.33mmol (0.3497g) of 2,5-dimercapto-1,3,4-thiadiazole monomer, add it to 10mL of absolute ethanol and ultrasonically dissolve it completely, and prepare 2, The organic solution of 5-dimercapto-1,3,4-thiadiazole; Accurately weigh 6.99mmol (0.8861g) I 2 Simple substance, it was added to 30mL of absolute ethanol and ultrasonically dissolved until it was completely dissolved, and it was formulated as I 2 organic solution;

[0037] (2) will I 2 The organic solution of 2,5-dimercapto-1,3,4-thiadiazole and the organic solution of 2,5-dimercapto-1,3,4-thiadiazole were respectively placed in a constant temperature water bath at 25°C for 20 minutes, and then the oxidant solution was added dropwise to 2,5 -dimercapto-1,3,4-thiadiazole organic solution, the whole process was carried out under...

Embodiment 2

[0038] Example 2: A method for synthesizing poly-2,5-dimercapto-1,3,4-thiadiazole nanosheets by chemical oxidation, the specific operation is as follows:

[0039] Present embodiment method is the same as example 1, and difference is that oxidizing agent is by I 2 The organic solution was replaced by H 2 o 2 organic solution, the yield of the resulting poly 2,5-dimercapto-1,3,4-thiadiazole nanosheets was 82.13%, and its transmission electron microscope showed Figure 4 As shown, it can be seen that the polymer is in the form of a sheet, and its scanning electron microscope is shown as Figure 5 , and its flake thickness is 133-666nm.

[0040] Figure 6 It is the infrared spectrum of poly 2,5-dimercapto-1,3,4-thiadiazole (PBT) and BT monomer, which shows that PBT is at 1045, 1385, 1643 and 3447cm -1 There is a strong absorption peak at 713, 1045, 1255 and 1498cm -1 There is a strong absorption peak.

[0041] Figure 7 It is a wide-angle X-ray diffraction pattern of poly ...

Embodiment 3

[0042] Example 3: A method for synthesizing poly-2,5-dimercapto-1,3,4-thiadiazole nanosheets by chemical oxidation, the specific operation is as follows:

[0043] The method of this example is the same as Example 1, except that the solvent for dissolving 2,5-dimercapto-1,3,4-thiadiazole monomer is replaced by DMF, methanol, and 80% ethanol, and the obtained poly-2,5-di The yields of mercapto-1,3,4-thiadiazole nanosheets were 38.75%, 92.23% and 73.71%, respectively.

[0044] The UV-Vis spectra of PBT and monomer BT synthesized in different media are shown in Figure 8 , it can be seen that the monomer BT has strong absorption peaks at 267 and 358nm respectively; while PBT has strong absorption peaks at 259 and 358nm, and the polymer prepared with ethanol as the reaction medium has obvious absorption peaks at 421nm .

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Abstract

The invention discloses a preparation method of poly 2,5-dimercapto-1,3,4-thiadiazole nanometer sheets, and belongs to the field of organic function high polymer materials. The method comprises the following steps of respectively dissolving 2,5-dimercapto-1,3,4-thiadiazole monomers and oxidizing agents into an organic solvent; then, dripping the oxidizing agent solution into the monomer solution; under the stirring condition, enabling the oxidizing agents and monomers to perform sufficient contact reaction. The method provided by the invention has the advantages that the addition of any additive stabilizing agents is not needed; the self-stabilizing polymer nanometer sheets with the thickness being 30 to 700nm can be synthesized only by controlling the polymerization reaction conditions; the synthesis is completed in one step. The method has the advantages that the synthesis method and the post-treatment work procedures are simple; no stabilizing agents and no surfactants are involved; the product is pure; the molecular weight of the obtained product is high; the synthesis cost is low; the general applicability can be realized, and the like.

Description

technical field [0001] The invention belongs to the field of organic functional polymer materials, and in particular relates to a preparation method of poly 2,5-dimercapto-1,3,4-thiadiazole nanosheets. Background technique [0002] 2,5-dimercapto-1,3,4-thiadiazole polymer is a heterocyclic aromatic polymer containing S and N atoms, which can be used as a high-energy storage cathode material for secondary lithium-ion batteries, and can also be used as an electrode The modified material is used for high-sensitivity and high-selectivity electrochemical detection of lead ions, cadmium ions, morin, etc., and is also an excellent heavy metal ion adsorbent and antibacterial and disinfectant. [0003] In previous studies, the preparation method of 2,5-dimercapto-1,3,4-thiadiazole polymer was mainly electrochemical polymerization, which was prepared by cyclic voltammetry. American scholar Shouji et al. (Shouji E, Buttry D A, An investigation of the effect of pyridine derivatives on ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G61/12
CPCC08G61/12C08G2261/11C08G2261/3229
Inventor 黄绍军李超马成章杜萍黄秋玲朱艳琴
Owner KUNMING UNIV OF SCI & TECH