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Di(polyoxometallate)-organic chain-cage silsesquioxane hybrid cluster compound and preparation method thereof

A polyoxometalate and silsesquioxane technology, which is applied in the preparation of hybrid clusters and the field of preparation of di-organic chain-cage silsesquioxane hybrid clusters, can solve the problem of no Problems such as self-assembly behavior, poor solubility, poor thermal stability, etc., to achieve the effect of large application value and regular structure period

Inactive Publication Date: 2019-09-13
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Due to their own structure and properties, polyoxometalates also have disadvantages, such as mostly inorganic crystals or powders, poor thermal stability, poor solubility, etc.
But so far, there is no research on the connection of two polyoxometalates with a cage silsesquioxane, let alone the related self-assembly behavior.

Method used

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  • Di(polyoxometallate)-organic chain-cage silsesquioxane hybrid cluster compound and preparation method thereof
  • Di(polyoxometallate)-organic chain-cage silsesquioxane hybrid cluster compound and preparation method thereof
  • Di(polyoxometallate)-organic chain-cage silsesquioxane hybrid cluster compound and preparation method thereof

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Embodiment 1

[0041] A hybrid compound of bis(polyoxometalate)-organic chain-cage silsesquioxane, which is composed of two polyoxometalates and a cage silsesquioxane through an organic chain to covalently A hybrid compound formed by means of bonds, the formed compound has an accurate molecular weight of 12079.43, and its chemical formula is {[(n-Bu) 4 N] 6 P 2 W 15 V 3 o 59 (OCH 2 ) 3 CNHCO} 2 C 6 h 3 CONHCH 2 CH 2 CONH(C 31 h 69 Si 8 o 12 ), the chemical structural formula of two (polyoxometalates)-organic chain-cage silsesquioxane (2POM-POSS) is as follows:

[0042]

[0043] Its preparation method is that the tert-butyl 5-nitroisophthalate is passed through zinc powder to reduce the nitro group to the amino group to obtain (2-t-BuO-NH 2 ), the amino group is connected with succinic anhydride to obtain (2-t-BuO-COOH), and the exposed carboxyl group is dehydrated and condensed with the reactive group amino group on the cage silsesquioxane to obtain (2-t-BuO-POSS ), and t...

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Abstract

The invention provides a di(polyoxometallate)-organic chain-cage silsesquioxane hybrid cluster compound and a preparation method thereof. The hybrid cluster compound is formed by covalent bonding of two polyoxometallates and one cage silsesquioxane through an organic chain. According to the preparation method, two polyoxometallates (Bu4N)6[H3P2W15V3O62] and one cage silsesquioxane (POSS-NH2) are connected through a six-step reaction to obtain the organic-inorganic hybrid material. The hybrid cluster compound is formed through connection via the organic chain by the means of covalent bonds andhas a precisely fixed molecular weight and molecular shape; and in solution self-assembly studies, the hybrid cluster compound is dissolved in acetone, n-decane is added, and volatilization at 25 DEGC is performed. During the volatilization of acetone, di(polyoxometallate)-organic chain-cage silsesquioxane molecules undergo self-assembling; and with a high-power transmission microscope, a stripedsheet structure is observed in a high-angle annular dark field image-scanning transmission mode.

Description

technical field [0001] The invention belongs to the technical field of preparation of bis(polyoxometalate)-organic chain-cage silsesquioxane hybrid clusters, in particular to a bis(Wells-Dawson type polyoxometalate)-organic Method for preparing hybrid clusters of chain-cage silsesquioxanes. Background technique [0002] Polyoxometalates (Polyoxometalates, POMs) are a class of clusters formed by early transition metal atoms (such as vanadium, molybdenum, tungsten, etc.) and central atoms (such as phosphorus, silicon, etc.) through oxygen coordination bridges. Polyoxometalates can be divided into isopolyacids and heteropolyacids according to the type of oxoacids they contain. A polyoxometalate synthesized from one oxo-acid is called an isopolyacid, while a polyoxometalate synthesized from two or more oxo-acids is called a heteropolyacid. Isopolyacids can be considered to be formed by the condensation of two or more simple oxyacid molecules of the same kind. Isopolyacids can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/06
CPCC08G77/045C08G77/06
Inventor 王维张兰兰刘洪开
Owner NANKAI UNIV
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