Preparation method and application of MIL-100(Fe) nanometer catalyst

A nano-catalyst, stirring reaction technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as high price and easy emission of large organic pollutants , to achieve the effect of simple operation, ultra-high photodegradation performance, and mild reaction conditions

Inactive Publication Date: 2018-02-23
GUIZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the organic solvent package is not only expensive, but also requires high-pressure reactors and other equipment, and it is easy to emit a large amount of organic pollutants during large-scale synthesis.

Method used

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  • Preparation method and application of MIL-100(Fe) nanometer catalyst
  • Preparation method and application of MIL-100(Fe) nanometer catalyst
  • Preparation method and application of MIL-100(Fe) nanometer catalyst

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[0024] The preparation method of MIL-100 (Fe) nano-catalyst of the present invention, it comprises the following steps: (a) trimesic acid and inorganic base are dissolved in water to form the first solution; (b) iron source is dissolved in water to form Fe containing 2+ or / and Fe 3+ the second solution; (c) drop the first solution into the second solution, filter after stirring and reacting, rinse with ethanol, dry, and collect the filter cake; the trimesic acid, the The molar ratio of the inorganic base to the iron element is 1:2-3.5:1-1.5. The preparation method of MIL-100 (Fe) nano-catalyst of the present invention, by making trimesic acid and inorganic base react to form trimesic acid radical ion and can cooperate with iron ion or ferrous ion to form MIL- with high crystallinity 100(Fe), the reaction can quickly synthesize highly crystalline MIL-100(Fe) at room temperature, the reaction solvent is water, avoiding the use of a large amount of organic solvents, and no corro...

Embodiment 1

[0029] The present embodiment provides a kind of preparation method of MIL-100 (Fe) nano-catalyst, it comprises the following steps:

[0030] (a) Add NaOH (10.0g) into a round bottom flask, add 250mL of water to dissolve, and dissolve trimesic acid (H 3 btc, 16.7g) was added in portions, stirred to obtain a clear solution (i.e. the first solution);

[0031] (b) FeSO 4 ·7H 2 O (31.7g) was dissolved in 1000mL of water to obtain the second solution;

[0032] (c) Add the first solution dropwise to the second solution (dropping with a conventional dropper, about 1-5 drops / second, the same below) under stirring at room temperature (25°C), and stir for 12 hours; Filter, rinse the filter cake with water and ethanol, dry, and collect the filter cake. Carry out SEM, XRD and infrared test to the obtained product, the results are as follows Figure 1 to Figure 3 Shown; It can be seen that the obtained MIL-100 (Fe) particles have a particle size of 500-1000nm and a high degree of crysta...

Embodiment 2

[0034] The present embodiment provides a kind of preparation method of MIL-100 (Fe) nano-catalyst, it comprises the following steps:

[0035] (a) Add NaOH (10.0g) into a round bottom flask, add 250mL of water to dissolve, and dissolve trimesic acid (H 3 btc, 16.7g) was added in portions, stirred to obtain a clear solution (i.e. the first solution);

[0036] (b) FeCl 2 4H 2 O (22.6g) was dissolved in 1000mL of water to obtain the second solution;

[0037] (c) Add the first solution dropwise to the second solution (using a conventional dropper, about 1-5 drops / second, the same below) under stirring at room temperature (25°C), and stir for 10 hours; the above filtrate Filter, rinse the filter cake with water and ethanol, dry, and collect the filter cake.

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Abstract

The invention relates to a preparation method and application of an MIL-100(Fe) nanometer catalyst. The preparation method comprises the following steps: (a) dissolving trimesic acid and an inorganicalkali into water to form a first solution; (b) dissolving an iron source in water to form a second solution containing Fe<2+> or / and Fe<3+>; and (c) dropwise adding the first solution into the secondsolution, performing a reaction under stirring, performing filtering, performing rinsing with ethanol, performing drying, and collecting the filter cake, wherein the molar ratio of the trimesic acidto the inorganic alkali to the iron element is 1:(2-3.5):(1-1.5). The MIL-100(Fe) with high crystallinity can be synthesized at room temperature. The reaction solvent is water and avoids use of a large amount of organic solvents, highly corrosive additives such as HF are not needed, the reaction conditions are mild, high-pressure reaction kettles are not required, and the preparation method is easy to operate, easy for industrial large-scale synthesis, and greatly reduces the MIL-100(Fe) synthesis conditions.

Description

technical field [0001] The invention belongs to the field of nanometer catalysts and relates to a MIL-100(Fe) nanometer catalyst, in particular to a preparation method of the MIL-100(Fe) nanometer catalyst and its application in photodegradation of organic dyes. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOFs) are a class of organic-inorganic hybrid porous crystalline materials formed by organic multi-coordinate ligands linking metal ion nodes or clusters. , Molecular recognition, chemical sensors and other fields have achieved remarkable results. In recent years, the intersection of MOFs and nanoscience has brought MOFs research into the nanometer field, that is, metal-organic framework nanomaterials (nano-scale metal-organic frameworks, NMOFs) have become a new research hotspot. Compared with traditional large-scale MOFs, NMOFs not only have the structural advantages of traditional MOFs, such as rich pore structure, functionalized fr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C02F1/32
CPCB01J31/1691B01J31/2213B01J35/004B01J35/023B01J35/1028B01J2531/842C02F1/32C02F2101/308C02F2305/10
Inventor 庄金亮刘湘粤
Owner GUIZHOU NORMAL UNIVERSITY
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