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Triazole derivative, preparation method thereof, nano particles thereof and application of nano particles

A technology for derivatives and triazoles, which is applied to triazole derivatives, their preparation and the application fields of nanoparticles and nanoparticles, can solve the problems of low detection sensitivity, environmental pollution, complexity and the like, and achieve simplified operation steps. , the effect of high sensitivity

Inactive Publication Date: 2015-01-28
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The titration method cannot directly detect the content of ferric ions, the detection sensitivity is not high, the error is large, and the use of potassium dichromate in the titration process will pollute the environment
Spectrophotometry is complicated to operate and the detection sensitivity is not high

Method used

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  • Triazole derivative, preparation method thereof, nano particles thereof and application of nano particles
  • Triazole derivative, preparation method thereof, nano particles thereof and application of nano particles
  • Triazole derivative, preparation method thereof, nano particles thereof and application of nano particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Synthesis of formula 1 derivative TAZ-BTTC6:

[0050] The structural formula, synthesis method and characterization results of TAZ-BTTC6 are as follows:

[0051]

[0052] Add 3,4,5-tris(4-bromobenzene)-4H-1,2,4-triazole (280mg, 0.52mmol), 4-(5-n-hexylthiophene)-7 -(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)benzo[c][1,2,5-thiadiazole](1.22g, 2.85mmol) (The synthesis of reactants refers to ACS Appl.Mater.Inter.2010,2,2679.), tetrakis(triphenylphosphine)palladium (164mg, 0.13mmol), tetra-n-butylammonium bromide (40mg, 0.13mmol), Argon protection for 10 minutes, add degassed toluene 12ml and 2mol / L degassed Na 2 CO 3 Solution 5ml, after repeated vacuum pumping / argon filling three times, raised to 85°C for 42 hours, cooled, added water and extracted three times with chloroform, the organic layer was washed with anhydrous Na 2 SO 4 After drying, the solvent was removed, and the obtained solid was purified by column chromatography to obtain 400 mg of compound TAZ-BTTC6 a...

Embodiment 2

[0054] Preparation of TAZ-BTTC6 nanoparticles

[0055] Dissolve compound TAZ-BTTC6 in tetrahydrofuran solution at a concentration of 2mg / ml, take 0.25ml of this solution, inject it into 10ml of deionized water under ultrasonication, continue ultrasonication for 10min, and use a 0.22μm polytetrafluoroethylene filter head The TAZ-BTTC6 nanoparticles of the compound were obtained by filtration. The average particle diameter of the particles was 175 nanometers, and the zate potential was -26.1mV. Since the particles had the same charge and repelled each other, the nanoparticles could exist stably in the solution. The particle size distribution of nanoparticles see figure 2 , the scanning electron micrograph (platinum spraying) measured by dropping the nanoparticle solution onto the silicon wafer and evaporating the solvent is shown in Figure 3.

Embodiment 3

[0057] Measure the normalized UV-visible absorption spectrum and the normalized fluorescence spectrum in the TAZ-BTTC6 nanoparticle aqueous solution, and measure the fluorescent emission spectrum of the nanoparticle aqueous solution at different pH values, the results are as follows Figure 4-6 shown.

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Abstract

The invention relates to synthesis of a dendritic molecule taking a 1,2,4-triazole derivative as a kernel and a benzothiophene or pyridinothiazole derivative as an arm, a preparation method of the derivative and detection of ferric ions in a lithium iron phosphate anode material by the nano particles of the compound. The triazole derivative is shown by formula 1; the fluorescence emission of the compound can be quenched by the ferric ions without suffering influence of other ions; and when measuring ferric ions in the lithium iron phosphate anode material, the triazole derivative has the advantages of high sensitivity, high speed, accuracy and simplicity and convenience in operation.

Description

technical field [0001] The present invention relates to a class of 1,2,4-triazole derivatives as the core, benzothiophene or pyrimidothiazole derivatives as the synthesis of dendritic molecules, and the preparation method of the derivatives, and the compound nano Particles for the detection of ferric ions in lithium iron phosphate cathode materials. Background technique [0002] Lithium iron phosphate (LiFePO 4 ) battery materials have attracted enough attention since they were first reported in 1997 (A.K.Padhi, K.S. Nanjundaswamy, J.B. Goodenough, J. Electrochem. Soc. 1997, 144, 1188). Compared with traditional cathode materials such as LiCoO 2 ,LiNiO 2 and LiMn 2 o 4 For example, LiFePO 4 There are many advantages, such as its theoretical capacity of 170mAhg -1 , lithium ion extraction and insertion voltage is 3.5V, good cycle stability and thermal stability (K.Tang, J.Sun, X.Yu, H.Li, X.Huang, Electrochimica Acta.2009,54,6565) . In addition, the preparation of Li...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D417/14B82Y40/00G01N21/64
Inventor 李立东徐新军王金山
Owner UNIV OF SCI & TECH BEIJING
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