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Preparation method of zirconium-based microporous coordination polymer

A coordination polymer and microporous technology, applied in the field of synthesis and preparation, can solve problems such as difficult separation, low production efficiency, and high price, and achieve the effects of shortening reaction time, improving production efficiency, and reducing costs

Active Publication Date: 2020-05-08
长春市梅丰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis methods reported in the current literature cannot meet the requirements of industrial production, because many experimental factors have an impact on the industrial production of Zr-MOF materials.
In terms of zirconium sources, the use of organic zirconium sources is expensive, and inorganic zirconium sources will introduce inorganic ions into the reaction system, making subsequent separation difficult
ZrCl 4 It is the most widely used zirconium source at present, but its price is expensive, which will obviously increase the production cost of industrialization
[0004] Compared with the current method of synthesizing Zr-MOF, taking UIO-66 as an example, in order to obtain high-quality UIO-66, ZrCl is mostly used 4 or ZrOCl 2 As a zirconium source, the disadvantage of this method is that the zirconium source is expensive and the production efficiency is low (~5kg m -3 ·day -1 ), high cost of solvent purification, low quality, and difficulty in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0013] Firstly, the preparation method of the zirconium-based microporous coordination polymer according to the first aspect of the present invention will be described, which includes the steps of dissolving zirconium source zirconium carbonate in an organic solvent containing a scheduling agent, acid chloride, and deionized water to obtain a mixture, wherein , The organic solvent is one or two of N,N'-dimethylformamide (DMF) and N,N'-diethylformamide (DEF); then the organic carboxylic acid ligand is dissolved in The mixture is heated to react; solid-liquid separation is carried out after the reaction is completed, the separated solid is washed and activated to obtain the zirconium-based microporous coordination polymer, and the separated liquid (mainly organic solvent) can be recycled without purification.

[0014] In the preparation method of the zirconium-based microporous coordination polymer according to the present invention, by using zirconium carbonate as the zirconium sou...

Embodiment 1

[0027] First, the zirconium carbonate (with ZrO 2 The total mass content is 40%) dissolved to contain acetyl chloride CH 3 In the DMF solution of COCl and HAc acetic acid, deionized water was added to obtain a mixture, and then 1,4-terephthalic acid (BDC) was dissolved in the mixture, and the mixture was heated to 130°C for 4 hours and the reaction was completed After solid-liquid separation, the separated solids are washed and activated to obtain zirconium-based microporous coordination polymer products. The product yield is 93% and the specific surface area is 1540m. 2 / g. The amount of each substance added is shown in Table 1.

[0028] Table 1

[0029] Zirconium carbonate BDCCH 3 COCl

Embodiment 2

[0031] First, the zirconium carbonate (with ZrO 2 The total mass content is 40%) dissolved to contain benzoyl chloride C 7 H 5 ClO, benzoic acid (BA) in DEF solution, then add deionized water to obtain a mixture, then 4,4'-biphthalic acid (4,4'-BPDC) is dissolved in the mixture, and the mixture is heated React at 150°C for 2 hours. After the reaction is completed, solid-liquid separation is carried out. The separated solid is washed and activated to obtain a zirconium-based microporous coordination polymer product with a product yield of 65% and a specific surface area of ​​2755m 2 / g. The amount of each substance added is shown in Table 2.

[0032] Table 2

[0033] Zirconium carbonate 4,4’-BPDCC 7 H 5 ClO

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Abstract

The invention provides a method for preparing a zirconium-based micro-porous coordination polymer. The method comprises the following steps: dissolving a zirconium source (zirconium carbonate) in an organic solvent containing a dispatching agent, acyl chloride and deionized water so as to obtain a mixture, wherein the organic solvent is one or two of N,N'-dimethylformamide and N,N'-diethylformamide; dissolving an organic carboxylate ligand in the mixture, and heating to react; performing solid-liquid separation after reaction, washing and activating the separated solids so as to obtain the zirconium-based micro-porous coordination polymer, wherein the separated liquid can be recycled without purification. According to the preparation method of the zirconium-based micro-porous coordination polymer disclosed by the invention, the zirconium carbonate serves as a zirconium source, and any inorganic ion or organic matter residue is not remained in the reaction system, so that the organic solvent can be recycled, the utilization efficiency of the organic solvent is improved, the purification cost is reduced, the reaction time is shortened, the production efficiency is improved, and the product quality can be effectively improved by taking acyl chloride as a chlorine source.

Description

Technical field [0001] The invention relates to the field of synthetic preparation, in particular to a method for preparing a zirconium-based microporous coordination polymer. Background technique [0002] So far, there have been more than 20,000 metal-organic framework materials (MOF materials) with different structures and compositions. The designable structure and adjustable pore properties exhibited by MOF materials have attracted people’s attention. . As the application of MOF materials is explored more extensively, such as in gas storage / separation, catalysis, sensing, drug slow release, etc., the question that follows is how to industrially produce MOF materials, including large-scale, low-cost Cost, process is simple and controllable, and environmentally friendly. In recent years, among MOF materials, a class of MOF materials with a three-dimensional network structure composed of zirconium metal clusters as nodes and organic carboxylic acid ligands has attracted people'...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 李亚丰张李梅
Owner 长春市梅丰科技有限公司