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Controllable preparation of MIL material, and application of MIL material in separation enrichment of furan compounds

A technology for separation and enrichment of compounds, applied in other chemical processes, organic chemistry, chemical instruments and methods, etc., can solve the problems of low concentration and difficult separation, and achieve the effect of simple process, low energy consumption, and easy operation.

Inactive Publication Date: 2020-06-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, furan compounds are organic oxygen-rich compounds with high boiling points, which are produced in the aqueous phase system with low concentration and difficult separation

Method used

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  • Controllable preparation of MIL material, and application of MIL material in separation enrichment of furan compounds
  • Controllable preparation of MIL material, and application of MIL material in separation enrichment of furan compounds
  • Controllable preparation of MIL material, and application of MIL material in separation enrichment of furan compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Controllable Preparation of micro MIL-53(Al)

[0047] Uniformly disperse 13g of aluminum nitrate nonahydrate and 2.88g of terephthalic acid in 50ml of ultrapure water to obtain a mixed precursor solution, transfer it to a fully enclosed stainless steel reactor, set the reaction temperature to 220°C, and in a stable reaction environment Keep for 72h. After the reaction was completed, the heating was stopped and cooled to room temperature naturally to obtain a white powder sample. The samples were centrifuged and washed 3 times with ultrapure water, and the centrifugation conditions were: 15000r / min, 5min, 25°C. The samples were placed in an air atmosphere, and the drying temperature was set at 85°C for drying. The fully dried powder sample was fully ground to obtain the material micro MIL-53(Al)as. figure 1 The X-ray diffraction spectrum of micro MIL-53(Al)as is given, figure 2 The scanning electron microscope image of micro MIL-53(Al)as is given, and the scale bar ...

Embodiment 2

[0049] micro MIL-53(Al) for separation and enrichment of furan compound-furfural

[0050] The adsorption performance of biomass furfural on micro MIL-53(Al)lt was tested by loss method. At room temperature, uniformly disperse 0.050g micro MIL-53(Al)lt in 0.50ml furfural aqueous solution, and absorb for 0-20min under continuous mixing. Obtain the supernatant after adsorption equilibrium by centrifugation, and analyze the concentration of furfural in the supernatant by liquid chromatography. In order to correct the adsorption data, the blank comparison experiment was carried out under the same conditions. Experiments show that the adsorption reaches equilibrium within 20 minutes. Equilibrium adsorption capacity Q(mg g -1 ) can be calculated by the following formula:

[0051] Q=V·(C 0 –C e )·m -1

[0052] Wherein V is the volume (mL) of furfural aqueous solution used, C 0 is the concentration of furfural in the aqueous solution before adsorption (g L -1 ), C e is the c...

Embodiment 3

[0054] NH 2 - Controlled preparation of MIL-53(Fe)

[0055] Dissolve 0.96g of ferric chloride hexahydrate, 0.58g of 2-aminoterephthalic acid, and 0.05g of benzoic acid in 30ml of solvent to obtain a precursor mixed solution. The solvent is N,N-dimethylformamide (DMF) and water (The volume ratio of DMF and water is 3:1). The precursor solution was transferred to a fully-sealed stainless steel reactor, and the constant temperature was set at 150°C for 24 hours. After the reaction was completed, the heating was stopped, and it was naturally cooled to room temperature to obtain a powder sample. The sample was centrifuged and washed once with the solvent DMF, and the centrifugation conditions were: 15000r / min, 5min, 25°C. Take 30ml of DMF and transfer the sample to a stainless steel reaction kettle, and keep the temperature at 150°C for 5.5h again. After the reaction was completed, the heating was stopped and cooled to room temperature naturally. Without changing the centrifug...

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Abstract

The invention discloses controllable preparation of an MIL material, and separation and enrichment application of a furan compound, wherein the structural characteristics of the MIL material comprisedesignable hydrophilicity and hydrophobicity, a one-dimensional pore channel structure and a good respiratory effect. Based on the advantages of the material body, the MIL material preparation methodwhich is low in energy consumption, easy and convenient to operate and simple in process is developed. In view of wide industrial application of the furan compound, application of the MIL material inseparation and enrichment of the furan compound has far-reaching significance for large-scale industrial production of biomass-based industrial products and energy structure optimization.

Description

technical field [0001] The invention belongs to the field of chemical separation of materials, and in particular relates to the controllable preparation of MIL materials and the application of separation and enrichment of furan compounds. Background technique [0002] MIL (Materials of Institute Lavoisier) materials are MOFs materials composed of carboxylic acid ligands and SBU (Secondary Building Units) of trivalent metals. It has programmable hydrophilicity and hydrophobicity and a unique one-dimensional pore structure, and has a good breathing effect. MIL materials achieve the separation of mixtures by modulating their own pore size through stress response. Therefore, under adjustable external conditions (such as mixture concentration, temperature, whether there is light, whether there is an electric field or whether there is a magnetic field, etc.), the use of MIL materials to separate mixtures will surely become a breakthrough in the field of separation. [0003] Fura...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/48C08G83/00B01J20/22B01J20/30
CPCB01J20/226C07D307/48C08G83/008
Inventor 杨维慎曹娜班宇杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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