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Preparation method and application of zirconium based metal-organic frameworks

An organic framework and metal-based technology, which is applied in the field of adsorption and separation of nicotinamide and nicotinic acid, can solve the problems of elution of template molecules, reduction of adsorption rate and adsorption capacity of target molecules, and separation difficulties, and achieve high-efficiency separation.

Active Publication Date: 2019-10-18
TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the physical properties of niacin and niacinamide are very similar, such as solubility, molecular size, molecular mass, etc., it is difficult to separate the two
Current separation techniques include molecular imprinting methods, recrystallization, extraction, etc. However, these methods face great challenges
For example, traditional molecularly imprinted polymers have a high degree of cross-linking, which may lead to the elution of different template molecules, and at the same time, the adsorption rate and adsorption capacity of target molecules are reduced, which limits the molecular imprinting method in homologues or Applications in the separation of isomers

Method used

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  • Preparation method and application of zirconium based metal-organic frameworks
  • Preparation method and application of zirconium based metal-organic frameworks
  • Preparation method and application of zirconium based metal-organic frameworks

Examples

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Embodiment 1

[0031] Example 1 Synthesis of zirconium-based metal-organic framework material DUT-67

[0032] A method for preparing a zirconium-based metal-organic framework material (DUT-67), comprising the following steps:

[0033] S1. Mix dimethylformamide and N-methyl-2-pyrrolidone at a volume ratio of 1:1 to obtain 150mL mixed solution A; weigh 1.38g of zirconium chloride with a substance amount of 6mmol and a substance amount of 4mmol 0.66g of thiophenedicarboxylic acid, the zirconium chloride and thiophenedicarboxylic acid were added into the mixed solution A prepared together, and then 26.8mL of formic acid solution was added to the mixed solution to obtain the mixed solution B;

[0034] S2, the mixed solution B prepared in step S1 was stirred for 5 minutes, then transferred to a 100mL polytetrafluoroethylene-lined stainless steel autoclave, and heated at 120°C for 48 hours; after the reaction, the white solid was collected and used Washing with dimethylformamide and methanol, and ...

Embodiment 2

[0037] Example 2 Zirconium-based metal-organic framework material DUT-67 is used for adsorption and separation of niacin in a mixed solution of niacinamide and niacin

[0038] The zirconium-based metal-organic framework material DUT-67 prepared in Example 1 is used to adsorb nicotinamide and nicotinic acid at a pH value of 4.26 and 303K. The specific method is as follows:

[0039] Weigh 5 mg of sample DUT-67 and add it to 10 mL of a mixed solution of nicotinamide and nicotinic acid with an initial concentration of 5-500 mg / g. After ultrasonication for 10 seconds, transfer the mixed system to a constant temperature shaker for adsorption at 303K for 12 hours , the shaker speed is set to 155rpm. After the adsorption separation, filter with a microporous membrane with a pore size of 0.22 μm, collect the clear filtrate and use ultra-high performance liquid chromatography to determine the content of nicotinic acid and nicotinamide. The adsorption capacity is calculated using the eq...

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Abstract

Belonging to the technical field of adsorption separation of nicotinamide and nicotinic acid, the invention provides a preparation method and application of zirconium based metal-organic frameworks, and solves the technical problem of difficult adsorption separation of nicotinamide and nicotinic acid by existing conventional separation method. The zirconium based metal-organic frameworks DUT-67 disclosed by the invention is synthesized by solvothermal method, the chemical formula of the zirconium based metal-organic frameworks DUT-67 is Zr6O6(OH)2(tdc)4.3.1H2O.0.6DMF, with certain pore structure and unique binding site, the zirconium based metal-organic frameworks DUT-67 can achieve rapid selective adsorption separation of nicotinamide and nicotinic acid, the separation effect is obvious and the operation process is simple, the utilization rate of nicotinamide and nicotinic acid can be effectively enhanced, and the economic benefits can be improved.

Description

technical field [0001] The invention belongs to the technical field of adsorption and separation of nicotinamide and nicotinic acid, and relates to a zirconium-based metal-organic framework material for efficient and selective adsorption and separation of nicotinamide and nicotinic acid, in particular to a preparation method of a zirconium-based metal-organic framework material and its application. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOFs), as a porous material, is a crystalline material with a regular pore structure composed of metal centers bridged by organic ligands. Compared with other porous materials, metal-organic framework materials have excellent characteristics such as large specific surface area, adjustable pore structure, abundant binding sites, and good thermal stability, making them ideal for adsorption and separation, drug delivery, and biosensing. It has important application value in research fields such as imag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C07D213/80C07D213/803C07D213/82
CPCB01J20/226B01J20/28064C07D213/80C07D213/803C07D213/82
Inventor 高新丽赵旭东赵雨炜郑美琪杜国华刘双学高竹青
Owner TAIYUAN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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