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Dawson type polyacid-based metal-BBPTZ organic framework material as well as preparation method and application of Dawson type polyacid-based metal-BBPTZ organic framework material

An organic framework and metal-based technology, which is applied in the field of Dawson-type polyacid-based metal-BBPTZ organic framework materials and the preparation thereof, can solve the problems of masking of polyacids, reduction of catalytic activity, reduction of active sites, etc., and achieves simple process, The effect of stable crystal structure, improved life and efficiency

Active Publication Date: 2021-05-11
TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problem that the active site of the polyacid is easily covered when the polyacid-based metal organic framework material is used, resulting in the reduction of the active site and the reduction of the catalytic activity when contacting with the substrate, a Dawson Type polyacid-based metal-BBPTZ organic framework material and its preparation method and use

Method used

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  • Dawson type polyacid-based metal-BBPTZ organic framework material as well as preparation method and application of Dawson type polyacid-based metal-BBPTZ organic framework material
  • Dawson type polyacid-based metal-BBPTZ organic framework material as well as preparation method and application of Dawson type polyacid-based metal-BBPTZ organic framework material
  • Dawson type polyacid-based metal-BBPTZ organic framework material as well as preparation method and application of Dawson type polyacid-based metal-BBPTZ organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: a kind of Dawson type multi-acid group-BBPTZ organic framework material, the molecular formula of described Dawson type multi-acid group-BBPTZ organic framework material is: [H 2 BBPTZ] 2 Co(BBPTZ) 2 [P 2 W 18 o 62 ]·3H 2 O; ie: ie C 72 h 74 N 24 o 65 P 2 W 18 Co, monoclinic, C 2 / c Space group, the basic unit contains a [P 2 W 18 o 62 ] 6- Polyanion, one Co(II) cation, two BBPTZ ligands, two protonated BBPTZ ligands and three crystal water molecules; its unit cell parameters are: a = 26.675(2)Å, b = 16.1311(12)Å, c =30.321(2)Å, α=90°, β=104.396(8)°, γ=90°, V =12637.4(16)Å 3 , Z=4, μ=16.557mm -1 , F (000) = 10332.

[0038] The method for preparing the Dawson type polyacid-based metal-BBPTZ organic framework material, the specific steps are as follows:

[0039] (1) Synthesis of 4,4'-bis(1,2,4-triazole-1-methylene)biphenyl or BBPTZ: Weigh 1.38g (ie 20mmol) of 1,2,4-triazole , dissolve it in 50ml acetone, then add 4g PEG-400, 5g anhyd...

Embodiment 2

[0044] Example 2: Analysis of the crystal structure of the prepared Dawson-type polyacid-based metal-BBPTZ organic framework material compound: the structure of the prepared yellow blocky crystal compound was obtained using a Bruker D8 Aventura photon 100CMOS diffractometer at a temperature of 298K with Mo Kα Radiation (λ=0.71073ĩ) collected the single crystal X-ray diffraction data of the as-prepared compound, and then solved it using the ShelXT structure solving program (using the intrinsic phase method), and using the least squares method F 2 The law is refined. All non-hydrogen atoms in this compound are anisotropic, hydrogen atoms on organic carbon atoms are fixed at the calculated positions, and hydrogen atoms on water molecules, protonated BBPTZ and polyoxoanions cannot be assigned by weak reflection peaks, Instead, it is directly included in the final molecular formula.

[0045] Finally determine the molecular formula of this crystal material is [H 2 BBPTZ] 2 Co(BBP...

Embodiment 3

[0054] Example 3: Infrared spectroscopy (IR) analysis of the prepared compound crystals: the compound was pressed into tablets using KBr, at 400-4000cm -1 In the wavenumber range, use Alpha Centauri FT-IR infrared spectrometer to measure.

[0055] Infrared spectra of compounds such as Figure 6 As shown, it has four characteristic peaks in the range of 1100-700cm-1, about 1089cm -1 , 968cm -1 , 914cm -1 and 785cm -1 , and attribute them to {P 2 W 18 o 62} 6− The vibrations of ν(P–O), ν(W=Od) and ν(W–Ob / c–W). In addition, approximately at 3122cm -1 The peaks are assigned to the benzene and pyridine rings of the BBPTZ ligand v (C-H) vibration, benzene ring and triazole ring of BBPTZ ligand v (C=C), v (C=N) and v The vibration peak of (C=N) is reflected in 1610-1435 cm -1 scope, v (H 2 O) The characteristic vibration peak is about 3567cm -1 reflect.

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Abstract

The invention belongs to the technical field of metal organic framework materials, and provides a Dawson type polyacid-based metal-BBPTZ organic framework material as well as a preparation method and application thereof in order to solve the problem that the catalytic activity is reduced due to the fact that active sites of polyacid are easily covered in a polyacid-based metal organic framework material. The molecular formula of the material is [H2BBPTZ] 2Co (BBPTZ) 2 [P2W18O62]. 3H2O, the material has a monoclinic system and a C2 / c space group, and the basic unit comprises a [P2W18O62] 6-polyanion, a Co (II) cation, two protonated BBPTZ ligands and three crystal water molecules; AND the process is simple, high-quality single crystals are easy to obtain, structural analysis is simple, convenient and feasible, materials are easy to repeat, and the yield is high. The crystal structure is stable, the catalyst is a heterogeneous catalyst, synergistic catalysis is realized, and a composite functional catalyst of ''1 + 1>2'' is obtained; and the service life and efficiency of the catalyst are improved.

Description

technical field [0001] The invention belongs to the technical field of metal organic framework materials, and in particular relates to a Dawson type polyacid-based metal-BBPTZ organic framework material and its preparation method and application. The organic framework material is used as a heterogeneous desulfurization catalyst in fuel oxidation desulfurization. Background technique [0002] As a unique class of early transition metals (including Mo, W, V, Nb and Ta, etc.), polyacids have adjustable composition, charge, acidity, stability, redox and oxidation resistance. field has been extensively studied. However, as a homogeneous catalyst, polyacids are not suitable for recovery in the reaction system, and some polyacids are easily hydrolyzed in different pH solutions, which has become a problem that must be overcome in the polyacid homogeneous system. [0003] When used as heterogeneous catalysts, polyacids exhibit low specific surface areas (<10 m 2 g -1 ), and onl...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/22
CPCC08G83/008B01J31/1691B01J31/2217B01J2531/845B01J2531/0238Y02P20/584
Inventor 郝秀丽贾士芳温艳珍
Owner TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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