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Metal-organic framework material and synthetic method thereof

A metal-organic framework and synthesis method technology, applied in the field of metal-organic framework materials and their synthesis, can solve the problems of difficult preparation and poor crystallinity, and achieve the effects of good thermal stability, good crystallinity and strong coordination ability

Inactive Publication Date: 2015-09-09
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the metal-organic framework compounds of the UiO series often have poor crystallinity and are difficult to prepare.

Method used

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  • Metal-organic framework material and synthetic method thereof
  • Metal-organic framework material and synthetic method thereof

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Experimental program
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Embodiment 1

[0055] A metal-organic framework material of this embodiment has the chemical formula Zr 6 C 168 H 182 N 4 O 40 S 24 , and the chemical structural formula shown in formula I:

[0056]

[0057] formula I;

[0058] Wherein, formula I contains five Zr-O clusters, and the chemical structural formula represented by the Zr-O clusters is as follows:

[0059]

[0060] Zr-O clusters.

[0061] The metal organic framework material has a cubic crystal structure, and the space group of the cubic crystal system is: Pm-3m ; The unit cell parameters of the cubic crystal system are: a=32.7399(16) ?, b=32.7399(16) ?, c=32.7399(16) ?, a = b = g = 90°; V=35094(5) ? 3 .

[0062] Wherein, in the chemical structural formula represented by the above formula I, the zirconium atom adopts the classical UiO-68 configuration, and each zirconium oxygen cluster Zr 6 O 4 (OH) 4 is connected to twelve ligands, each of which is connected to two zirconium-oxygen clusters Zr 6 O 4 (OH)...

Embodiment 2

[0064] A method for synthesizing a metal-organic framework material of the present embodiment, which comprises the following steps:

[0065] Step 1, the synthesis of the first intermediate product 2',5'-dimercapto-p-terphenyl-4,4'-dicarboxylate methyl ester

[0066] 2',5'-dimercapto-p-terphenyl-4,4'-dicarboxylic acid and catalyst concentrated sulfuric acid were added to methanol, and then refluxed at 90°C for 20h to obtain the first reactant, and the first reactant was cooled After reaching room temperature, add excess water to the first reactant, then carry out suction filtration, and then naturally air dry to obtain a white solid, which is the first intermediate product 2',5'-dimercapto-p-terphenyl-4,4' - methyl diformate;

[0067] In this embodiment, the molar ratio between the first intermediate product 2',5'-dimercapto-p-terphenyl-4,4'-dicarboxylate methyl ester, methanol and the catalyst concentrated sulfuric acid is 1:3:0.2.

[0068] Step 2, the synthesis of the secon...

Embodiment 3

[0080] A method for synthesizing a metal-organic framework material of the present embodiment, which comprises the following steps:

[0081] Step 1, the synthesis of the first intermediate product 2',5'-dimercapto-p-terphenyl-4,4'-dicarboxylate methyl ester

[0082] 2',5'-dimercapto-p-terphenyl-4,4'-dicarboxylic acid and catalyst concentrated sulfuric acid were added to methanol, and then refluxed at 85°C for 25h to obtain the first reactant, and the first reactant was cooled After reaching room temperature, add excess water to the first reactant, then carry out suction filtration, and then naturally air dry to obtain a white solid, which is the first intermediate product 2',5'-dimercapto-p-terphenyl-4,4' - methyl diformate;

[0083] In this embodiment, the molar ratio between the first intermediate product 2',5'-dimercapto-p-terphenyl-4,4'-dicarboxylate, methanol and the catalyst concentrated sulfuric acid is 1:2:0.1.

[0084] Step 2, the synthesis of the second intermediat...

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Abstract

The invention relates to the technical field of light engineering and chemical engineering materials, in particular to a metal-organic framework material and a synthetic method thereof. The chemical formula of the metal-organic framework material is Zr6C168H182N4O40S24, and the metal-organic framework material adopts a cubic system crystal structure. The synthetic method of Zr6C168H182N4O40S24 comprises the following steps: step 1, synthesizing 2'5'-dimercapto-p-terphenyl-4,4'-dicarboxylic methanoate; step 2, synthesizing 2'5'-diethyl sulfide-s-methyl-p-terphenyl-4-4'-dicarboxylic methanoate; step 3, synthesizing a ligand, namely 2'5'-diethyl sulfide-s-methyl-p-terphenyl-4-4'-dicarboxylic acid; step 4, carrying out reaction between the ligand and zirconium tetrachloride to finally synthesize the colorless octahedronlike crystalline metal-organic framework material. The metal-organic framework material can be used for loading nobel metallic ions and heavy metal ions.

Description

technical field [0001] The invention relates to the technical field of light industry and chemical materials, in particular to a metal organic framework material and a synthesis method thereof. Background technique [0002] In recent years, Metal-Organic framework (MOF) has developed rapidly as an emerging porous material. The advantage of this type of porous material is that the function of the porous material can be tailored through the design of organic functional molecules. However, the difficulty lies in the design and synthesis of organic functional molecules. Based on a large number of previous works, it was found that thioether aromatic carboxylic acid compounds have merged soft and hard atoms (the theory of soft and hard acids and bases). The S on the thioether acts as a soft base, and the O on the carboxyl acts as a hard base. This type of compound has obvious advantages when forming metal-organic framework materials. When choosing hard acid metal ions such as (Z...

Claims

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Application Information

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IPC IPC(8): C07F7/00B01J20/22B01J20/28B01J20/30
Inventor 何军吴超黄建何永和吴娟黄家鸿
Owner GUANGDONG UNIV OF TECH
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