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Divalent metal-base MIL-53 microporous material, and preparation method and application thereof

A microporous material and metal technology, applied in the field of +2-valent metal MIL-53 microporous material and its preparation, can solve the problems of poor adsorption selectivity and weak binding force, and achieve simple steps, good stability, and adsorption. good performance

Inactive Publication Date: 2019-02-01
DONGGUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the adsorption is carried out in the form of physical adsorption, the binding force between the adsorbent and the adsorbed substance is weak (van der Waals force or electrostatic attraction), and the selectivity of adsorption is poor.

Method used

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  • Divalent metal-base MIL-53 microporous material, and preparation method and application thereof
  • Divalent metal-base MIL-53 microporous material, and preparation method and application thereof
  • Divalent metal-base MIL-53 microporous material, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method based on +2 valent metal MIL-53 microporous material, the method is as follows:

[0035] Mn(NO 3 ) 2 solution (0.3 mmol, 0.0861g), H 2 BDC (0.1mmol, 0.0224g), bpdo (0.1mmol, 0.0188g) and DMF / H 2 O (3.0 ml: 1.0 ml) was placed in a small 25.0 ml beaker, and the resulting mixture was stirred at room temperature for one hour, and the resulting solution was transferred to a 17.0 ml stainless steel reaction vessel with a polytetrafluoroethylene liner, at 120 ° C for spontaneous pressure After heating for 10 hours under certain conditions, the reaction system was slowly cooled to room temperature to obtain red rod-shaped crystals and a very small amount of colorless block-shaped crystals. After the product was filtered and dried naturally, the colorless crystals could be removed manually. Finally, put the colorless solid product into a round-bottomed flask connected with an oil pump to evacuate, and heat in an oil bath at 150° C. for 8 hours to prepar...

Embodiment 2

[0037] A preparation method based on +2 valent metal MIL-53 microporous material, the method is as follows:

[0038] Mn(NO 3 ) 2 solution (0.1 mmol, 0.0287g), H 2 BDC (0.2 mmol, 0.0448g), bpdo (0.2mmol, 0.0376 g) and DMF / H 2 O (3.0 ml: 1.0 ml) was placed in a small 25.0 ml beaker, and the resulting mixture was stirred at room temperature for one hour, and the resulting solution was transferred to a 17.0 ml stainless steel reaction vessel with a polytetrafluoroethylene liner, at 120 ° C for spontaneous pressure After heating for 10 hours under certain conditions, the reaction system was slowly cooled to room temperature to obtain red rod-shaped crystals and a very small amount of colorless block-shaped crystals. After the product was filtered and dried naturally, the colorless crystals could be removed manually. Finally, put the colorless solid product into a round-bottomed flask connected with an oil pump to evacuate, and heat in an oil bath at 150° C. for 8 hours to prep...

Embodiment 3

[0040] A preparation method based on +2 valent metal MIL-53 microporous material, the method is as follows:

[0041] Mn(NO 3 ) 2 solution (0.5 mmol, 0.1435g), H 2 BDC (0.25mmol, 0.0560g), bpdo (0.25mmol, 0.0470g) and DMF / H 2 O (3.0 ml: 1.0 ml) was placed in a small 25.0 ml beaker, and the resulting mixture was stirred at room temperature for one hour, and the resulting solution was transferred to a 17.0 ml stainless steel reaction vessel with a polytetrafluoroethylene liner, at 120 ° C for spontaneous pressure After heating for 10 hours under certain conditions, the reaction system was slowly cooled to room temperature to obtain red rod-shaped crystals and a very small amount of colorless block-shaped crystals. After the product was filtered and dried naturally, the colorless crystals could be removed manually. Finally, put the colorless solid product into a round-bottomed flask connected with an oil pump to evacuate, and heat in an oil bath at 150° C. for 8 hours to prep...

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Abstract

The invention relates to a divalent metal-base MIL-53 microporous material, and a preparation method and application thereof. The chemical composition of the microporous material is [Mn2(BDC)2(bpdo).(DMF)2]infinity, wherein, the BDC is terephthalic acid, the bpdo is 4,4'-bipyridine nitrogen oxide, and the DMF is N,N'-dimethylformamide. The preparation method of the microporous material comprises the following steps: S1, dissolving an Mn(NO3)2 solution, the terephthalic acid H2BDC and the bpdo in a solvent by mixing and stirring, carrying out heating for a reaction for 10-12 hours at a temperature of 120-150 DEG C in a closed environment, and carrying out cooling, filtering and drying; and S2, heating the reaction product obtained in the step S1 at an oil bath temperature of 150-160 DEG C under a vacuum condition for 6-8 hours to obtain the divalent metal-base MIL-53 microporous material. The microporous material provided by the invention is suitable for adsorbing a small amount or trace amount of benzene, toluene, ethylbenzene, and xylene (BTEX) residues in water and air in the environment. The preparation method provided by the invention is simple in steps, low in raw material cost and high in repeatability, and can be used to realize batch preparation.

Description

technical field [0001] The invention relates to the field of microporous materials, in particular to a +2-valent metal MIL-53 microporous material and a preparation method thereof. Background technique [0002] Benzene (benzene), toluene (toluene), ethylbenzene (ethylbenzene, EB) and three isomers of xylene (including ortho-ortho-xylene, OX; meta-xylene, MX and para -xylene, PX) are collectively referred to as BTEX. BTEX are some of the most common aromatic compounds in petroleum, and they constitute the most soluble and mobile part of crude oil and petroleum products. Their concentration in petroleum determines the physical and chemical properties of petroleum such as density, viscosity, flash point, dispersibility, emulsification stability, and solubility. In BTEX, benzene is one of the basic raw materials of petrochemical industry. The chemical products based on benzene mainly include styrene, cyclohexane, phenol, chlorinated benzene, nitrobenzene, alkylbenzene, maleic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01D53/02B01J20/22C02F1/28
CPCB01D53/02B01D2257/7027B01J20/226C02F1/285C02F2101/32C02F2101/322C08G83/008
Inventor 刘丹张新民王严杰
Owner DONGGUAN UNIV OF TECH
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