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Cluster-base crystalline material, and preparation method and application thereof

A technology for base crystals and adsorption materials, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of thermal stability frame disadvantage, limited application, frame shrinkage, etc., and achieve easy mass preparation, mild conditions, and good resistance. The effect of high temperature performance

Inactive Publication Date: 2016-06-29
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with the previous porous materials, the thermal stability of many MOFs materials and the rigidity of the framework are at a disadvantage. After the solvent molecules are removed, the framework will shrink or even partially collapse, which limits its application in gas storage and separation. Applications

Method used

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  • Cluster-base crystalline material, and preparation method and application thereof
  • Cluster-base crystalline material, and preparation method and application thereof
  • Cluster-base crystalline material, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: Preparation of cluster-based crystalline material

[0032] Mix 30mg of cobalt chloride hexahydrate and 6mg of isonicotinic acid ligand in a beaker to obtain a mixture, then add 2mL of DMA, stir at room temperature for 30min to obtain a mixture; transfer the above mixture into a 10mL vial with a screw stopper, add 0.5 mL tetrafluoroboric acid aqueous solution, baked at 120°C for 36 hours, filtered and separated to obtain the product after cooling down to room temperature; washed the above solid with DMA for 3 times to obtain red strip-shaped hybrid material crystals, based on organic ligands The calculated yield is 68%. The main infrared absorption peaks are: 3388m, 3116w, 1615s, 1558s, 1401s, 1317m, 1185s, 1077s, 835m, 775s, 632s.

Embodiment 2

[0033] Embodiment 2: Preparation of cluster-based crystalline material

[0034] Mix 28mg of cobalt chloride hexahydrate and 8mg of isonicotinic acid ligand in a beaker to obtain a mixture, then add 5mL of DMA, stir at room temperature for 30min to obtain a mixture; transfer the above mixture into a 10mL vial with a screw stopper, add 1.5 mL tetrafluoroboric acid aqueous solution, baked at 120°C for 36 hours, filtered and separated to obtain the product after cooling down to room temperature; washed the above solid with DMA for 3 times to obtain red strip-shaped hybrid material crystals, based on organic ligands The calculated yield is 65%. The main infrared absorption peaks are: 3388m, 3116w, 1615s, 1558s, 1401s, 1317m, 1185s, 1077s, 835m, 775s, 632s.

Embodiment 3

[0035] Embodiment 3: the preparation of cluster-based crystalline material

[0036] Mix 31mg of cobalt chloride hexahydrate and 5mg of isonicotinic acid ligand in a beaker to obtain a mixture, then add 2mL of DMA, stir at room temperature for 30min to obtain a mixture; transfer the above mixture into a 10mL vial with a screw stopper, add 3mL The aqueous solution of tetrafluoroboric acid was baked at 120°C for 36 hours, then filtered and separated to obtain the product after cooling down to room temperature; the above solid was washed 3 times with DMA to obtain a red striped hybrid material crystal, calculated based on organic ligands The yield was 60%. The main infrared absorption peaks are: 3388m, 3116w, 1615s, 1558s, 1401s, 1317m, 1185s, 1077s, 835m, 775s, 632s.

[0037] Get the further characterization of the obtained carboxy-based crystalline material in Example 1, and its process is as follows:

[0038] (1) Determination of crystal structure

[0039] Under a polarizing...

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Abstract

The invention discloses a cluster-base crystalline material, and a preparation method and application thereof. The chemical formula of the cluster-base crystalline material is [Co6(mu3-OH)4(Ina)8](H2O)10(DMA)2, wherein Ina is an isonicotinic acid anion ligand, and DMA is N,N-dimethylacetamide. The cluster-base crystalline material is crystallized in the monoclinic system, the space group is P2[1] / c, a=9.2607(2)A, b=12.0677(3)A, c=31.0183(7)A, beta=97.604(3) degrees, and V=3435.98(15)A<3>. The cluster-base crystalline material has the advantages of favorable stability for organic solvents and higher heat stability; and the gas adsorption test result indicates that the material has favorable selective adsorptivity for C2H2 and CH4.

Description

technical field [0001] The invention relates to the preparation of crystalline materials, in particular to a cluster-based crystalline material and its preparation method and application. Background technique [0002] As a new type of organic-inorganic hybrid materials, metal-organic frameworks (MOFs) materials have shown good application prospects in the field of gas storage and separation due to their structural design and pore environment adjustability ( Zhou, H.-C.; Kitagawa, S. Chem. Soc. Rev., 2014, 43, 5415; Cui, Y.; Li, B.; He, H.; Zhou, W.; Chen, B.; Qian, G.; Acc.Chem.Res., 2016, 49, 483; Du, M.; Li, C.-P.; Chen, M.; .; Liu, C.-S.J.Am.Chem.Soc., 2014, 136, 10906; Zhao, X.; Bu, X.; Zhai, Q.-G.; TranH.; Feng, P.J.Am.Chem.Soc ., 2015, 137, 1396). Scientists can enhance the interaction between gas molecules and the framework by introducing unsaturated metal vacancies and organic linkers containing polar functional groups, thereby achieving storage capacity and selec...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/32B01J20/22
CPCB01J20/226B01J20/32C08G83/008
Inventor 陈迪明刘春森杜淼田稼越
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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