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Isopolymolybdate organic-inorganic hybrid compound and preparation method thereof

A technology of polymolybdic acid and compounds, applied in copper organic compounds, chemical instruments and methods, luminescent materials, etc., can solve the problems of entangled network, loss, and smaller pores, and achieve stable crystal structure, high yield, and process The effect of mild conditions

Inactive Publication Date: 2015-12-16
TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem that entangled networks are prone to occur when building microporous materials, resulting in smaller or completely lost pores, the present invention provides an organic-inorganic hybrid compound of isopolymolybdates and a preparation method thereof

Method used

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  • Isopolymolybdate organic-inorganic hybrid compound and preparation method thereof
  • Isopolymolybdate organic-inorganic hybrid compound and preparation method thereof
  • Isopolymolybdate organic-inorganic hybrid compound and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0025] A kind of organic-inorganic hybrid compound of isopolymolybdate, the molecular formula of the organic-inorganic hybrid compound of isopolymolybdate is [Bmim] 2 [Cu II (BBTZ) 2 ][β-Mo 8 o 26 ]·H 2 O is C 36 h 48 N 16 o 27 Mo 8 Cu, monoclinic, C 2 / c Space group, the basic unit contains a [β-Mo 8 o 26 ] 4? Polyanion, one Cu(II) cation, two BBTZ ligands, two Bmim cations and one crystalline water molecule; its unit cell parameters are: a = 21.680(4)?, b = 12.541(3)?, c / =23.360(5)°, α=90°, β=102.04(3)°, γ=90°, V / =6212(2)? 3 , Z=4, μ=1.984mm -1 , F (000)=3828.

[0026] The preparation method comprises the following steps:

[0027] (1) Synthesis of 1,4-bis(1,2,4-triazole-1-methylene)benzene, namely BBTZ: According to the literature [X.R.Meng, Y.L.Song, H.W.Hou, H.Y.Han, B.Xiao, Y.T. Fan, Y.Zhu, Inorg.Chem.2004, 43, 3528-3536.] synthesized, the synthesis method is: in a 100ml round bottom flask, 1,2,4-triazole (20mmol is 1.38g) dissolved In 30ml of ace...

experiment example 1

[0031] Experimental Example 1: Analysis of the crystal structure of the prepared compound:

[0032] The structure of the prepared blue blocky crystal compound was determined by using the SMART-CCD X-ray diffractometer of German Bruker Company or the IP plate single crystal diffractometer of Rigaku Company of Japan. All crystal structures were solved using the SHELXL-97 software package, using the direct method, and using the least squares method F 2 The law is refined. Finally determine the molecular formula of this crystal material is [Bmim] 2 [Cu II (BBTZ) 2 ][β-Mo 8 o 26 ]·H 2 O(1). In addition, the Perkin-Elmer2400CHN analyzer was used to measure C, H and N elements, and the ICP plasma chromatographic analyzer was used to measure metal elements, thus further proving the correctness of the molecular formula of this compound. The results are as follows.

[0033] C 36 h 48 N 16 o 27 Mo 8 Theoretical value (%) of Cu element analysis: C21.95, H2.44, N11.38, Cu3.25, ...

experiment example 2

[0038] Experimental Example 2: Thermogravimetric (TG) analysis of prepared compound crystals:

[0039] The compound uses a Perkin-Elmer TGA7 analyzer to determine the temperature range and percentage of its weight loss, and the test is at N 2 protection, the heating rate is 10℃·min -1 under the conditions.

[0040] According to the data analysis of its determination, it is found that the TG curve of the compound shows a one-step weight loss (such as Figure 7 ). The entire weight loss occurred in the temperature range from 255 °C to 560 °C, and lost 35.90%, which was attributed to the decomposition and loss of countercation Bmim and BBTZ ligands, which was consistent with the theoretical value of 35.67%. And the weight loss of about 11.74% at around 255°C to 320°C can be attributed to the loss of the counter cation Bmim, after which the BBTZ ligand begins to decompose and lose, resulting in the collapse of the framework. This property proves the stability of the compound, ...

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Abstract

The invention belongs to the technical field of macromolecular cellular materials, provides an isopolymolybdate organic-inorganic hybrid compound and a preparation method thereof and aims to solve the problem of diminishing or complete losing of porous channels due to proneness to entanglement networks in construction of cellular materials. The isopolymolybdate organic-inorganic hybrid compound with a molecular formula being C36H48N16O27Mo8Cu belongs to a monoclinic crystal system. The preparation method includes: synthesizing BBTZ; synthesizing ionic liquid [Bmin]Br; mixing (NH4)6Mo7O24.4H2O, CuCl2.2H2O, BBTZ and the ionic liquid [Bmin]Br at the room temperature, regulating pH with HCl, transferring to a reaction kettle with a polytetrafluoroethylene liner, keeping for 5 days at 160 DEG C, and cooling to the room temperature at a speed of 10 DEG C.h<-1> to obtain the compound. The isopolymolybdate organic-inorganic hybrid compound and the preparation method thereof have the advantages of technical simplicity, high repeatability, high yield, mild process conditions, stable crystal structure, availability for cation exchange, excellent thermal stability and chemical stability and applicability as high-temperature materials.

Description

technical field [0001] The invention belongs to the technical field of polymer microporous materials, and in particular relates to an organic-inorganic hybrid compound of isopolymolybdates and a preparation method thereof. Background technique [0002] Materials are one of the important material bases for human beings to improve their quality of life, and they are listed as the three pillars of modern science and technology along with energy and information. In the field of chemistry, more and more disciplines are closely related to the research and application of materials. The current development trend of material science is to use molecular engineering and molecular design ideas to hybridize, compound, and assemble multi-component building blocks with various functional properties to construct multifunctional or functionally enhanced composite materials. . In this research field, microporous materials are a hot sub-discipline that develops rapidly and is closely followe...

Claims

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Application Information

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IPC IPC(8): C07F1/08C09K11/06
Inventor 郝秀丽贾士芳温艳珍
Owner TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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