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Coordination framework materials of copper-cyclotriphosphazene hexacarboxylic acid derivatives and their preparation and application

A technology of cyclotriphosphazene hexacarboxylic acid and framework materials, which is applied in the direction of copper organic compounds, other chemical processes, alkali metal compounds, etc., and can solve the application occasions that do not have specific requirements for molecular arrangement and cannot form specific structures. Derivatives, structural arrangement random problems, etc., to achieve excellent adsorption performance, novel topology, and strong repeatability

Inactive Publication Date: 2017-06-13
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, further studies have shown that although derivatives based on hexachlorocyclotriphosphazene have the above-mentioned characteristics, these derivatives often have random internal molecular structures and cannot form derivatives with specific structures. Applications with specific requirements
In addition, using hexachlorocyclotriphosphazene to generate derivatives, the yield of the reaction is often not high, which affects practical application

Method used

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  • Coordination framework materials of copper-cyclotriphosphazene hexacarboxylic acid derivatives and their preparation and application
  • Coordination framework materials of copper-cyclotriphosphazene hexacarboxylic acid derivatives and their preparation and application
  • Coordination framework materials of copper-cyclotriphosphazene hexacarboxylic acid derivatives and their preparation and application

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Experimental program
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Embodiment 1

[0044] The preparation of embodiment 1 complex 1

[0045] Six-(4-carboxylic acid phenoxy group) cyclotriphosphazene preparation method is as follows:

[0046] First synthesize methyl p-hydroxybenzoate, weigh 6g of p-hydroxybenzoic acid with electronic balance, add in 100ml round bottom flask, then add about 50ml of methanol, drop about 15 drops of concentrated sulfuric acid (mass percentage concentration is 98%) , after refluxing at 70°C for 4h, a colorless transparent solution was obtained, the reaction device was removed, methanol was evaporated to dryness, and finally washed with distilled water to obtain 7g of white product (ie, methyl p-hydroxybenzoate), which was dried for later use, and the yield was about 93 %. Next, add 1.5g (0.0043mol) sublimated hexachlorocyclotriphosphazene (baked at 50°C for 5h), 6.5g (0.043mol) methyl p-hydroxybenzoate (dried), about 1g under Ar atmosphere Potassium carbonate (can be baked at 120°C for about 1-2 hours to ensure dryness), then a...

Embodiment 2

[0054] The preparation of embodiment 2 complex 2

[0055] The preparation method of hexa-(4-carboxylic acid phenoxy)cyclotriphosphazene is the same as in Example 1.

[0056] The synthetic preparation method of complex 2 is as follows:

[0057] First weigh 20mg of hexa-(4-carboxyphenoxy)cyclotriphosphazene, 10mg of copper nitrate and 10mg of 4,4'-bipyridine, add 1.5mL of deionized water and 10mL of N,N'-dimethylformaldehyde Amide, after ultrasonic reaction for 5 minutes, add 5 drops of 2mol L -1 nitric acid aqueous solution to obtain a solvothermal reaction precursor solution; put the precursor solution into a hydrothermal reaction kettle, and place the reaction kettle in a 100°C oven to react for 4 days, and then cool down at a rate of 5°C / h to obtain blue rod-shaped crystals , filtered and washed with appropriate deionized water to obtain the final product complex 2 (complex 2 is the framework material 2); the complex 2 has the following structure:

[0058]

[0059] The...

Embodiment 3

[0065] The preparation of embodiment 3 complex 1

[0066](1) Ligand synthesis: In an argon atmosphere, add 1.5g of hexachlorocyclotriphosphazene, 6.5g of methyl p-hydroxybenzoate and 1g of potassium carbonate to 50ml of acetone, then stir for 5min, and heat to 60°C for reaction A mixed solution was formed in 20 hours; then, the acetone in the mixed solution was evaporated to dryness to obtain a white solid; then, the white solid was washed with distilled water, then filtered, and then the filter residue obtained by filtering was added to 40ml of ethyl acetate, stirred Spin dry after dissolving, promptly obtain six (4-formic acid methyl ester-phenoxy) cyclotriphosphazene; In 30mL methanol, add 5g six (4-formic acid methyl ester-phenoxy) cyclotriphosphazene, and 6g Sodium hydroxide was stirred and heated to reflux at 65° C. for at least 12 hours, and then the methanol was dried under reduced pressure to obtain solid I; then, 150 mL of distilled water was added to the solid I to ...

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Abstract

The invention discloses a copper-cyclotriphosphazene hexacarboxylic acid derivative coordination framework material and a preparation method and application thereof. The coordination framework material is formed by adopting raw materials comprising copper ions and a ligand L through reaction, wherein the ligand L is hexa-(4-carboxylate benzoxy) cyclotriphosphazene and the chemical formula is C42H30O18N3P3; in addition, the coordination framework material is a three-dimensional framework material and has one-dimensional linear pore passages. By improving the composition and structure of the coordination framework material, various parameters in the preparation method and the like, the structurally ordered copper-cyclotriphosphazene hexacarboxylic acid derivative coordination framework materials can be obtained, the preparation method of the series of materials can effectively guarantee the reaction yield and the actual application is facilitated.

Description

technical field [0001] The invention belongs to the field of self-assembly of transition metal coordination framework materials, and more specifically relates to a coordination framework material prepared by using cyclotriphosphazene derived hexacarboxylic acid ligands to prepare copper-cyclotriphosphazene hexacarboxylic acid derivatives, and its Preparation method and application; the frame material is a network frame material with a void structure, has very special adsorption properties, and has a good application prospect. Background technique [0002] Due to its specific pore structure, coordination framework materials have shown excellent application prospects in various application fields. However, how to effectively construct materials with specific framework structures and properties is still the research focus of coordination materials researchers. At present, the methods for effectively constructing framework materials still focus on the rational selection and con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/08C07F9/6593B01J20/22B01J20/30B01J20/28
Inventor 李宝陈熙李钊张天乐
Owner HUAZHONG UNIV OF SCI & TECH
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