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Preparation method and application of zeolite imidazate framework material ANA-[Co (eIm) 2]

A technology of zeolite imidazolate and framework materials, which is applied in chemical instruments and methods, chemical/physical processes, ion exchange, etc., can solve the problem of no literature reports on the crystal structure of MAF-5, the product is easily mixed with heterogeneous MAF-32, and the synthesis The process is affected by operating conditions and other issues, and achieves the effect of no impurity phase, high crystallinity, and simple method

Active Publication Date: 2020-09-04
TAIYUAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method not only has high cost of raw materials, but also the synthesis process is affected by operating conditions, and the obtained product is easily mixed with heterogeneous MAF-32(Co)
In addition, there is no literature report on the crystal structure of MAF-5(Co)

Method used

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  • Preparation method and application of zeolite imidazate framework material ANA-[Co (eIm) 2]
  • Preparation method and application of zeolite imidazate framework material ANA-[Co (eIm) 2]
  • Preparation method and application of zeolite imidazate framework material ANA-[Co (eIm) 2]

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] ANA-[Co(eIm) 2 ] Synthetic ratio one:

[0028] ANA-[Co(eIm) 2 ] The synthesis steps are: according to cobalt acetate tetrahydrate (99.5%, Aladdin Reagent (Shanghai) Co., Ltd.): 2-ethylimidazole (98.0%, Aladdin Reagent (Shanghai) Co., Ltd.): ethanol (99.5%, Sinopharm Group Chemical Reagent Co., Ltd.) = 1:7.5:257.3 molar ratio of raw materials. First, cobalt acetate tetrahydrate (1 mmol, 0.249 g), 2-ethylimidazole (7.5 mmol, 0.721 g) and ethanol (257 mmol, 15 mL) were sequentially mixed at room temperature, and then the mixture was transferred to a 30 mL hydrothermal In the reactor, react at 150 ºC for 24 h. After the reaction, it was naturally cooled to room temperature, and the obtained sample was washed several times with ethanol, filtered and dried at room temperature, and finally the phase structure was determined by PXRD. figure 1 For the synthetic ANA-[Co(eIm) 2 ] Diffraction pattern. By comparison, it was found that the synthesized ANA-[Co(eIm) 2 ]’s diffr...

Embodiment 2

[0030] ANA-[Co(eIm) 2 ] Synthetic ratio two:

[0031] ANA-[Co(eIm) 2 ] The synthesis steps are: according to cobalt acetate tetrahydrate (99.5%, Aladdin Reagent (Shanghai) Co., Ltd.): 2-ethylimidazole (98.0%, Aladdin Reagent (Shanghai) Co., Ltd.): ethanol (99.5%, Sinopharm Group Chemical Reagent Co., Ltd.) = 1:10:137.2 molar ratio of raw materials. First, cobalt acetate tetrahydrate (10 mmol, 2.491 g), 2-ethylimidazole (100 mmol, 9.612 g) and ethanol (1372 mmol, 80 mL) were sequentially mixed at room temperature, and then the mixture was transferred to a hydrothermal reaction vessel , reacted at 150 ºC for 24 h. After the reaction, it was naturally cooled to room temperature, and the obtained sample was washed several times with ethanol, filtered and dried at room temperature, and finally the phase structure was determined by PXRD. figure 2 For the synthetic ANA-[Co(eIm) 2 ] Diffraction pattern. By comparison, it was found that the synthesized ANA-[Co(eIm) 2 ]’s diffra...

Embodiment 3

[0039] Embodiment 3: Static competitive adsorption experiment

[0040] This embodiment adopts the ANA-[Co(eIm) prepared in Example 2 2 ] for static competitive adsorption experiments. ANA-[Co(eIm) 2 ] Activated with methanol at room temperature for 36 h, then prepared into particles of 500-600 μm, and then activated in vacuum at 150 ºC for 12 h to remove solvent molecules. The two-component furfural / 5-hydroxymethylfurfural static competitive adsorption experiment was performed as follows: Weigh 0.1 g of adsorbent particles into a 10 mL centrifuge tube, add 5 mL of different concentrations of furfural / 5-hydroxymethylfurfural (0.5-50 g L -1 / 0.5-50 g L -1 ) mixture, then sealed and placed in a 25 ºC environment for 36 h to ensure adsorption equilibrium. After the adsorption was completed, the sample was centrifuged, and the supernatant was taken to filter the membrane, and the concentration was quantitatively analyzed. Figure 6 for ANA-[Co(eIm) 2 ] Static competitive ads...

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Abstract

The invention discloses a preparation method and application of a zeolite imidazate framework material ANA-[Co (eIm) 2]. The preparation method comprises the following steps: sequentially mixing cobalt acetate tetrahydrate, 2-ethylimidazole and solvent ethanol according to a molar ratio of divalent metal Co salt to 2-ethylimidazole to ethanol of 1: (6-12): (120-270) at room temperature, and reacting at 120-150 DEG C for 1-2 days; and after the reaction is finished, cooling, washing the obtained sample with ethanol for multiple times, filtering at room temperature, and drying to obtain the product ANA-[Co (eIm) 2]. The invention also provides application of the zeolite imidazate framework material ANA-[Co (eIm) 2] in adsorption separation of a mixed aqueous solution of low-concentrating furfural and 5-hydroxymethylfurfural.

Description

technical field [0001] The invention relates to a zeolite imidazolate framework material ANA-[Co(eIm) 2 ] preparation method and application, specifically relate to a kind of utilization ANA-[Co(eIm) 2 The method for realizing the separation of furfural and 5-hydroxymethylfurfural with the elliptical pore structure of ] belongs to the application field of inorganic functional materials. Background technique [0002] Furfural and 5-hydroxymethylfurfural are two important platform compounds obtained from lignocellulose-rich biomass resources, which can be derived from a series of high value-added chemicals. However, low concentrations (10-50 g L -1 ) furfural and 5-hydroxymethylfurfural mixed aqueous solution, in order to obtain the finished furfural and 5-hydroxymethylfurfural, the two need to be separated. Given the low concentrations of furfural and 5-hydroxymethylfurfural and their heat-sensitivity, traditional separation methods are difficult. The adsorption separatio...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01D15/08
CPCB01J20/226B01D15/08
Inventor 石琪赵宇王静徐红董晋湘
Owner TAIYUAN UNIV OF TECH
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