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Calcium metal-organic coordination polymer and preparation method thereof

A technology of coordination polymers and polymers, applied in the preparation of organic compounds, organic chemical methods, organic chemistry, etc., to achieve the effects of easy-to-obtain raw materials, simple preparation methods, and uniform orientation

Inactive Publication Date: 2016-06-08
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As another important component of metal-organic coordination polymers, metal ions can be alkali metals, alkaline earth metals, transition metals, and rare earth metal ions, etc. Currently, there are relatively few studies on alkali metals and alkaline earth metals.

Method used

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  • Calcium metal-organic coordination polymer and preparation method thereof
  • Calcium metal-organic coordination polymer and preparation method thereof
  • Calcium metal-organic coordination polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh 0.2 mmol of 3,3',5,5'-biphenyltetracarboxylic acid, heat and stir with N'N-dimethylformyl or N'N-dimethylacetamide amine until completely dissolved, then add For ionized water, weigh 0.77 mmol calcium nitrate and add it to the solution. After it is completely dissolved, finally add 0.1 mol / L sodium hydroxide drop by drop to keep the solution clear. If it becomes turbid, stop adding. Add the above solution into a polytetrafluoroethylene high-pressure reactor, place it in a programmed temperature-controlled oven, heat it up to 150°C at a rate of 5°C per minute, keep the temperature constant for 84 hours, and then cool it down to 30°C. 1°C per minute. Filtration and washing afforded white crystals of the metal organic complex.

[0024] Wherein, the yield of the calcium metal-organic coordination polymer in the above preparation method is 67.2% (based on Ca).

Embodiment 2

[0026] Weigh 0.3mmol of 3,3',5,5'-biphenyltetracarboxylic acid, heat and stir with N'N-diethylformamide until completely dissolved, then add deionized water, weigh 1.21mmol of calcium nitrate and add After it is completely dissolved, add 0.1mol / L sodium hydroxide drop by drop at last to keep the solution clear, and stop adding if it becomes turbid. Add the above solution into a polytetrafluoroethylene high-pressure reactor, place it in a programmed temperature-controlled oven, heat it up to 130°C at a rate of 4°C per minute, keep the temperature constant for 96 hours, and then cool it down to 30°C. 1°C per minute. Filtration and washing afforded white crystals of the metal organic complex.

[0027] Wherein, the yield of the calcium metal-organic coordination polymer in the above preparation method is 69.0% (based on Ca).

Embodiment 3

[0029] Weigh 0.15mmol of 3,3',5,5'-biphenyltetracarboxylic acid, heat and stir with N-methylpyrrolidone or dimethyl sulfoxide until completely dissolved, then add deionized water, weigh 0.63mmol of calcium nitrate and add After it is completely dissolved, add 0.1mol / L sodium hydroxide drop by drop at last to keep the solution clear, and stop adding if it becomes turbid. Add the above solution into a polytetrafluoroethylene autoclave, place it in a programmed temperature-controlled oven, heat it up to 90°C at a rate of 2°C per minute, keep the temperature constant for 110 hours, and then cool it down to 30°C, the cooling rate 1°C per minute. Filtration and washing give calcium metal-organic coordination polymer crystals.

[0030] Wherein, the yield of the calcium metal-organic coordination polymer in the above preparation method is 66.1% (based on Ca).

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Abstract

The invention provides a calcium metal-organic coordination polymer and a preparation method thereof, belonging to the field of coordination chemistry. The chemical formula of the calcium metal-organic coordination polymer is [C22H21N2O13Ca2] which belongs to an orthorhombic system; the space group is P2[1]2[1]2[1]; and the cell parameters are as follows: a=13.883(11)A, b=13.883A, c=17.739(14)A, alpha=90.00 degrees, beta=90.00 degrees, gamma=90.00 degrees, and V=3419(4)A<3>. The metal organic coordination polymer is synthesized by a solvothermal process, thereby being beneficial to quickly obtaining the perfect crystals with fewer defects and uniform orientation. The preparation method is simple, and the metal ions preferably adopt pollution-free harmless calcium ions, so the raw material is accessible and economical. The obtained polymer has the advantages of high yield and favorable chemical stability, and has excellent application potential in the fields of gas adsorption and separation, catalysis, identification, optics and the like.

Description

technical field [0001] The invention belongs to the field of coordination chemistry, and specifically relates to an organic coordination polymer of calcium metal with a three-dimensional structure, more specifically, a single crystal structure of a metal organic coordination polymer and a preparation method thereof. Background technique [0002] In recent years, functional metal-organic coordination polymer materials not only have a variety of structural characteristics, but also have potential applications in gas adsorption and separation, ion exchange, catalysis, optics, magnetism, etc. research hotspots and frontier topics. Metal-organic coordination polymer materials are a kind of framework materials with one-dimensional, two-dimensional and three-dimensional structures, which are self-assembled by organic ligands and metal ions or ion clusters under certain conditions and connected by coordination bonds. Organic polycarboxylic acid ligands are naturally the first choic...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C63/331
CPCC07C63/331C07B2200/13C07C51/418
Inventor 王荣明张亮亮孙道峰
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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