Method for regulating ZIF-8 crystal morphology by utilizing surfactant

A surfactant, ZIF-8 technology, used in organic chemistry methods, 2/12 groups of organic compounds without C-metal bonds, zinc organic compounds, etc., can solve the problem of difficult to control morphology, ZIF-8 crystal size Uneven distribution and other problems, to achieve the effect of simple and easy to operate synthesis method, uniform size and high yield

Inactive Publication Date: 2018-02-23
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems of uneven distribution of ZIF-8 crystal particle size and difficulty in controlling the morphology, the present invention provides a method for regulating the morphology of ZIF-8 crystals by using a surfactant. The method is simple to operate and has obvious effects

Method used

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  • Method for regulating ZIF-8 crystal morphology by utilizing surfactant
  • Method for regulating ZIF-8 crystal morphology by utilizing surfactant
  • Method for regulating ZIF-8 crystal morphology by utilizing surfactant

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 24283g of 2-methylimidazole was dissolved in 28mL of water, 027g of CTAC solution was dissolved in 1mL of water, and 0.134g of zinc chlorate was dissolved in 4mL of water. First, add CTAC solution to imidazole solution, stir for 10 minutes, and let it stand at room temperature for 2 hours, then add zinc chloride solution to the above mixed solution, and stir for 5 minutes, Zn 2+ / CTAC / 2-Hmim / H 2 The molar ratio of O is 1:0.08:30:1800. Subsequently, the solution was transferred into a reaction kettle and reacted at 100° C. for 24 h. After the reaction, cool to room temperature, centrifuge (rotate at 10000r / min, centrifuge for 15min), wash with methanol for 5 times, and finally dry in an oven at 80°C for 24h to obtain ZIF-8 crystals.

[0030] Such as figure 1 As shown in (c), the product identified by X-ray diffraction is indeed a ZIF-8 crystal. Such as image 3 Scanning electron microscope pictures show that the crystals are cubic, and the particle size is about 200...

Embodiment 2

[0032] Dissolve 2.4283g of 2-methylimidazole in 20mL of water, 0.54g of CTAB solution in 1mL of water, and 0.216g of zinc acetate dihydrate in 3mL of water. Firstly, CTAB solution was added to the imidazole solution, stirred for 10 minutes, and allowed to stand at room temperature for 12 hours, then the dihydrate zinc acetate solution was added to the above mixed solution, stirred for 5 minutes, Zn 2+ / CTAB / 2-Hmim / H 2 The molar ratio of O is 1:0.16:30:1600. Subsequently, the solution was transferred into a reaction kettle and reacted at 120° C. for 24 h. After the reaction, cool to room temperature, centrifuge (8000r / min, centrifuge 10min), wash with methanol 3 times, and finally put it into a 100°C oven and dry for 24h to obtain ZIF-8 crystals.

[0033] Such as figure 1 As shown in (d), the product identified by X-ray diffraction is indeed a ZIF-8 crystal. Such as Figure 4 Scanning electron microscope pictures show that the crystals are flaky, with a length of about 1.2...

Embodiment 3

[0035] 4.0379g of 2-methylimidazole was dissolved in 28mL of water, 1.26g of TTAB solution was dissolved in 1mL of water, and 0.216g of zinc acetate dihydrate was dissolved in 4mL of water. First add the TTAB solution to the imidazole solution, stir for 10 minutes, let it stand at room temperature for 5 hours, then add the dihydrate zinc acetate solution to the above mixed solution, stir for 5 minutes, Zn 2+ / TTAB / 2-Hmim / H 2 The molar ratio of O is 1:0.28:50:1800. Subsequently, the solution was transferred into a reaction kettle and reacted at 120° C. for 18 h. After the reaction, cool to room temperature, centrifuge (5000r / min, centrifuge 8min), wash with methanol 4 times, and finally put into 120°C oven and dry for 12h to obtain ZIF-8 crystal.

[0036]Such as figure 1 As shown in (e), the product identified by X-ray diffraction is indeed a ZIF-8 crystal. Such as Figure 5 Scanning electron microscope pictures show that the crystal morphology is interspersed twin crystal...

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Abstract

The invention provides a method for regulating ZIF-8 crystal morphology by utilizing a surfactant and belongs to the technical field of synthesis of porous materials. The method disclosed by the invention is mainly characterized in that the morphology and size of the ZIF-8 crystal are controlled by adding a certain amount of a surfactant. The specific preparation method comprises the following steps: respectively dissolving a zinc salt, a surfactant and dimethyl imidazole into a certain amount of water, stirring to enable the components to be fully dissolved, and preparing a solution; mixing adimethyl imidazole solution and a surfactant solution, fully stirring, finally adding a zinc salt solution, and mixing and stirring for 10 minutes; then transferring the mixed solution into a high temperature reactor, and reacting at a constant temperature for several hours; cooling, centrifuging, washing and drying, thereby obtaining the ZIF-8 crystal. The ZIF-8 crystal prepared by the method has excellent crystallinity and has five morphologies such as rhombic dodecahedron, cube, sheet, interpenetration twin and rod. The invention provides a novel method for controlling the morphology and size of MOFs materials.

Description

technical field [0001] The invention belongs to the technical field of porous material synthesis, and relates to a method for regulating the crystal morphology of ZIF-8 by using a surfactant. Background technique [0002] Zeolitic imidazolate frameworks (ZIFs) are a new class of metal-organic frameworks (MOFs) with a zeolite topology formed by the coordination of metal ions and imidazole derivatives, which have excellent thermal and hydrothermal stability. In recent years, most studies have focused on the stability of ZIFs materials, the diversity of framework structures, and their applications in gas separation and storage, catalysis, and biomedicine. The morphology and size of ZIFs crystals have a great influence on their applications. For example, reducing the size of the crystals from micron to nanoscale can improve the physical properties of the crystals, such as increasing the surface area and reducing the diffusion resistance. As another example, changing the shape o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06C07D233/58
CPCC07F3/003C07B2200/13C07D233/58
Inventor 潘宜昌杨帆盛露倩许凯王重庆
Owner NANJING UNIV OF TECH
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