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Preparation method and application of RHO zeolite type 2-ethylimidazole zinc porous material

A technology of ethylimidazole zinc and porous materials, applied in chemical instruments and methods, other chemical processes, organic chemistry, etc., can solve the problems of cases without porous materials, MAF-6 cannot be obtained, reaction conditions are sensitive, etc., to achieve The effects of high resolution and selectivity factors, cheap and easy-to-obtain raw materials and solvents, and short reaction times

Inactive Publication Date: 2015-04-29
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although Friscic's group found that MAF-5 and MAF-6 could be obtained by the reaction of ZnO and Heim by ball milling, the product was impure (containing ZnO) and easily converted into the close-packed isomer MAF-32 in a relatively short period of time (Angew . Chem. Int. Ed., 2010, 49, 9640)
In addition, so far there is no case of practical application of this porous material
[0005] A large amount of zinc methylimidazole (code MAF-4) (CN 103635463 A) can be conveniently synthesized by directly mixing the water-based solution of metal salt and imidazole ligand and adding lye, but this method cannot synthesize pure phase MAF- 6. Using the rapid mixing acid-base neutralization method, the alcohol solution of the ligand and the zinc ammonia solution are simply mixed and stirred, and MAF-5 and MAF-32 have been successfully synthesized respectively (ZL201010169244.4)
However, the direct use of this traditional method has always been unable to obtain pure phase MAF-6, which may be due to its large pores and is more sensitive to reaction conditions.

Method used

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  • Preparation method and application of RHO zeolite type 2-ethylimidazole zinc porous material
  • Preparation method and application of RHO zeolite type 2-ethylimidazole zinc porous material
  • Preparation method and application of RHO zeolite type 2-ethylimidazole zinc porous material

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Experimental program
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Effect test

Embodiment 1

[0048]Example 1 Preparation of Porous Coordination Polymer MAF-6

[0049] 2-Ethylimidazole (4.0 mmol, 0.384 g) was dissolved in methanol solution (30 mL) to obtain a colorless clear solution, and 5 mL of cyclohexane was added. At room temperature, add Zn(OH) dropwise at a constant speed within 40 min 2 (2.0 mmol, 0.198 g) in concentrated aqueous ammonia (25%, 40 mL), followed by stirring for another 1 h, and the obtained white precipitate was filtered, washed with water and methanol and dried to obtain 0.40 g sample (yield 78%). The resulting powder was placed under a nitrogen atmosphere at 120 o C heated for 30 min to remove the guest molecules, and the pure phase MAF-6 without the guest can be obtained. The X-ray diffraction pattern of the product is shown in figure 1 .

Embodiment 2

[0050] The thermal stability characterization of embodiment 2 embodiment 1 gained MAF-6

[0051] The thermal stability of MAF-6 obtained in Example 1 was obtained by thermogravimetric analysis. For thermogravimetric curves, see figure 2 .

Embodiment 3

[0052] Example 3 Porosity Characterization of MAF-6 Gained in Example 2

[0053] The MAF-6 obtained in Example 1 was put into a glass sample tube after the guest was removed, and then its nitrogen adsorption isotherm was measured on an ASAP 2020M adsorption instrument at 77 K. N 2 The adsorption isotherm is type I adsorption, and the Langmuir specific surface area is 1695 m 2 g -1 , the BET specific surface area is 1343 m 2 g -1 , and its adsorption isotherm diagram is shown in image 3 .

[0054] Put the MAF-6 obtained in Example 1 into a glass sample tube after removing the guest, and then measure the vapor adsorption isotherms of benzene, ethanol, methanol and water in a BELSORP-max adsorption instrument at room temperature. The saturated adsorption capacity of benzene, ethanol and methanol (at P / P 0 = 0.83 values) were 6.3 mmol g -1 , 9.2 mmol g -1 and 13.2 mmol g -1 , basically no adsorption to water, the adsorption isotherm diagram is shown in Figure 4...

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Abstract

The invention discloses a preparation method of an RHO zeolite type 2-ethylimidazole zinc porous material and an application of the material in gas chromatography. The porous coordination polymer provided by the invention has the structural formula of RHO-[Zn(eim)2] (the code number is MAF-6), wherein eim represents anions with removal of protons in organic ligand 2-ethylimidazole (Heim), and RHO represents a topological structure with RHO zeolite. The preparation method disclosed by the invention has the advantages that the traditional fast-mixing acid-alkaline neutralization reaction is improved; the parameters such as the reactant concentration, the used amount of a template agent and the reaction time are optimized, and especially the feeding sequence, i.e., different concentration proportions of the reactants when a reaction system is started is changed, so that finally MAF-6 with larger amount and high quality is prepared; the obtained sample has good thermal stability and chemical stability, the porosity is 55.4%, and the Langmuir specific surface is larger than 1650m<2>g<-1>. The porous material MAF-6 can be used for preparing a capillary column, has good gas chromatographic separation capability and reproducibility and better thermal / chemical stability, and can be used for separating and detecting organic compounds with similar boiling points or sizes.

Description

technical field [0001] The invention relates to the field of complex porous materials and the field of gas chromatography, more specifically, to a preparation method and application of a RHO zeolite type 2-ethylimidazolium zinc porous material. Background technique [0002] Porous coordination polymer is a crystalline material composed of metal ions and organic ligands. It has the advantages of large specific surface area, low density, adjustable pore size and strong modification of pore surface. It can be widely used in gas adsorption and storage. , separation and catalysis. And in analytical chemistry, such as on-site sampling, solid phase extraction, high performance liquid chromatography and gas chromatography, etc. have also attracted the attention of scientific researchers. [0003] For example, Gas Chromatography (GC for short) has been widely used in scientific research and industrial production as a common separation and analysis method due to its fast analysis...

Claims

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Application Information

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IPC IPC(8): C07D233/58B01J20/22B01J20/282B01J20/30
CPCB01J20/282B01J20/3057B01J2220/46B01J2220/62B01J2220/86C07D233/58
Inventor 张杰鹏何纯挺蒋露洪惠玲陈小明
Owner SUN YAT SEN UNIV
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