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Hierarchical porous zeolite imidazate skeletal material, and preparation method thereof

A technology of zeolite imidazolate and framework materials, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., and can solve the problems of easy collapse of mesopores, long reaction time, and non-environmental protection , to achieve good catalytic activity, mild conditions, and short time-consuming effects

Active Publication Date: 2019-08-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many problems in the current method, such as long reaction time, use of special additives (triethylamine or ammonium hydroxide), etc.
In addition, the high cost and backbone instability of long ligands is almost unavoidable, since their mesopores are extremely prone to collapse upon guest removal.
Moreover, the use of organic solvents in large quantities is not economical and environmentally friendly

Method used

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  • Hierarchical porous zeolite imidazate skeletal material, and preparation method thereof
  • Hierarchical porous zeolite imidazate skeletal material, and preparation method thereof
  • Hierarchical porous zeolite imidazate skeletal material, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of a hierarchical porous zeolite imidazolate framework material, comprising the following steps:

[0034] (1) Add 0.44g Zn(NO 3 ) 2 ·6H 2 O and 0.13g Sodium Dodecyl Sulfate (SDS), stirred at 60°C until the solid was dissolved to obtain a clear and transparent homogeneous solution;

[0035] (2) Add 0.49g of 2-methylimidazole (2-Mim) to the homogeneous solution, and stir at 60°C for 30min to obtain a suspension;

[0036] (3) Centrifuge the suspension, wash with 50% ethanol aqueous solution and absolute ethanol, and dry at 110° C. for 12 hours to obtain the zeolite imidazolate framework material (ZIF8). Table 1 shows the structural characterization test data of the zeolite-like imidazolate framework material prepared in this example.

[0037] The X-ray diffraction pattern of the hierarchically porous zeolite imidazolate framework material (ZIF-8) prepared in Example 1 is as follows figure 1 As shown, the scanning electron microscope image is shown...

Embodiment 2

[0039] A preparation method of a hierarchical porous zeolite imidazolate framework material, comprising the following steps:

[0040] (1) With 4.75g deep eutectic solvent (ChCl / urea-DES, the molar ratio of choline chloride and urea is 1:2) and 0.25g deionized water, stir and mix evenly, obtain mixed solvent;

[0041] (2) Add 0.44g Zn(NO 3 ) 2 ·6H 2 O and 0.13g Sodium Dodecyl Sulfate (SDS), stirred at 60°C until the solid was dissolved to obtain a clear and transparent homogeneous solution;

[0042] (3) Add 0.49g of 2-methylimidazole (2-Mim) to the homogeneous solution and stir at 60°C for 30min to obtain a suspension;

[0043] (4) Centrifuge the suspension, wash with 50% ethanol aqueous solution and absolute ethanol, and dry at 110° C. for 12 hours to obtain the zeolite imidazolate framework material. Table 1 shows the structural characterization test data of the zeolite-like imidazolate framework material prepared in this example.

[0044] The X-ray diffraction pattern o...

Embodiment 3

[0046] A preparation method of a hierarchical porous zeolite imidazolate framework material, comprising the following steps:

[0047] (1) With 4.25g deep eutectic solvent (ChCl / urea-DES, the molar ratio of choline chloride and urea is 1:2) and 0.75g deionized water, stir and mix evenly, obtain mixed solvent;

[0048] (2) Add 0.44g Zn(NO 3 ) 2 ·6H 2 O and 0.13g Sodium Dodecyl Sulfate (SDS), stirred at 60°C until the solid was dissolved to obtain a clear and transparent homogeneous solution;

[0049] (3) Add 0.49g of 2-methylimidazole (2-Mim) to the homogeneous solution and stir at 60°C for 30min to obtain a suspension;

[0050](4) Centrifuge the suspension, wash with 50% ethanol aqueous solution and absolute ethanol, and dry at 110° C. for 12 hours to obtain the zeolite imidazolate framework material. Table 1 shows the structural characterization test data of the zeolite-like imidazolate framework material prepared in this example.

[0051] The X-ray diffraction pattern of...

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Abstract

The invention belongs to the technical field of metal organic skeletal material, and discloses a hierarchical porous zeolite imidazate skeletal material, and a preparation method thereof. The preparation method comprises following steps: 1, a deep eutectic solvent and water are mixed so as to obtain a mixed solvent; 2, a metal salt, and a surfactant are dissolved in the mixed solvent so as to obtain a homogeneous solution, wherein the metal salt is one or a mixture of more than one components selected from zinc salts or cobalt salts; 3, an imidazole derivative is added into the homogeneous solution, and heating stirring is carried out so as to obtain a suspension solution; and 4, the suspension solution is subjected to centrifugation, washing, and drying so as to obtain the hierarchical porous zeolite imidazate skeletal material. The preparation method is simple; the reaction conditions are mild; preparation process is rapid; no environment pollution is caused; the prepared material ishigh in specific surface area and porosity, and possesses a hierarchical porous structure. The obtained hierarchical porous zeolite imidazate skeletal material possesses excellent catalytic activityin CO2 and epoxide cycloaddition reaction.

Description

technical field [0001] The invention belongs to the technical field of metal organic framework materials, and relates to a hierarchical porous zeolite imidazolate framework material and a preparation method thereof. Background technique [0002] Metal-organic frameworks (MOFs) are a class of inorganic-organic hybrid porous materials with regular pore structures constructed by interconnecting metal centers and organic ligands through covalent bonds or ionic covalent bonds. With the research and development of MOFs materials, a kind of zeolitic imidazolate frameworks (ZIFs) has been synthesized. ZIFs is a kind of MOFs materials with zeolite framework structure, which is composed of transition metal ions Zn or Co and imidazole organic compounds. It has the advantages of both zeolite and MOFs: large specific surface area, high crystallinity, high thermal and chemical stability. ZIFs also have the characteristics of tunable pore size and structure. Therefore, ZIFs are often use...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/06B01J35/10C07D317/36
CPCC08G83/008B01J31/063C07D317/36B01J35/618B01J35/617B01J35/638B01J35/635B01J35/633B01J35/651B01J35/647
Inventor 陈砺胡丽华严宗诚磨晓虹
Owner SOUTH CHINA UNIV OF TECH
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