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Preparation and application of novel dual-core organic skeleton material MIL-100(Fe-Mn)

An organic framework, fe-mn technology, applied in the field of preparation of new binuclear metal-organic framework material MIL-100, can solve the problem of few reports related to the synthesis of binuclear MOFs crystal, achieve excellent surface adsorption and chemical reactivity, and cheap source. , the effect of improving the production yield

Inactive Publication Date: 2016-01-13
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are few reports on the synthesis of binuclear MOFs crystals

Method used

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  • Preparation and application of novel dual-core organic skeleton material MIL-100(Fe-Mn)
  • Preparation and application of novel dual-core organic skeleton material MIL-100(Fe-Mn)
  • Preparation and application of novel dual-core organic skeleton material MIL-100(Fe-Mn)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Preparation method of stable zero-valent nano-iron suspension.

[0035] Prepare 100mL, 2.5mol / LFe (NO 3 ) 3 ·9H 2 O solution will be 100mL, 5mol / LNaBH 4 The solution was dripped into the above Fe(NO) at a uniform speed of 5mL / min. 3 ) 3 ·9H 2 O solution. Vibrate while titrating. After all the titration is completed, continue to shake for 15 min until all the hydrogen is dissipated. The supernatant is removed by centrifugation at a centrifugation rate of 6000 r / min. The product was washed 3 times with deionized water, and finally the product was adjusted to 50 mL suspension solution with deionized water, and 0.3M (molar ratio 1:1) ethylenediaminetetraacetic acid (EDTA) and polyethylene glycol ( PEG) and ultrasonic dispersion to obtain a stable zero-valent nano-iron suspension with a concentration of about 28 mg / mL.

Embodiment 2

[0036] Example 2: Preparation method of MIL-100 (Fe-Mn) catalyst.

[0037] Add 5 ml of Mn (NO 3 ) 2 ·4H 2 O solution (1mol / L), H 3BTC (12.5 mmol) was ultrasonically dispersed at 80° C. for 2 h, and at the same time, HF (wt>40%) was slowly added dropwise, and the pH value of the solution was adjusted to 3-6. Then, the reactant was moved to a stainless steel reaction kettle with a polytetrafluoroethylene liner, sealed and placed in an oven to be heated, heated at 120°C for 8 hours and then heated to 150°C for 8 hours. After the reaction kettle was lowered to room temperature, the product was vacuum filtered, soaked in fresh absolute ethanol solution for about 24 hours, and then repeatedly washed with ethanol for several times. Finally, the product was heated in a vacuum drying oven at 80° C. overnight to obtain a pure orange powder, namely the organic framework material MIL-100 (Fe-Mn), with a yield of 89%.

Embodiment 3

[0039] According to the reactant Mn (NO 3 ) 2 ·4H 2 O solution (1mol / L) was increased to 10mL, H 3 The amount of BTC was increased to 25 mmol, and the amount of other raw materials and experimental procedures remained unchanged, and an orange-yellow MIL-100 (Fe-Mn) material was obtained.

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Abstract

The invention relates to preparation and application of a novel dual-core organic skeleton material MIL-100(Fe-Mn), and belongs to the technical field of novel material preparation. Firstly, a high-dispersion zero-price nanometer iron suspension with spherical or elliptical particles and average granularity of 60-100 nm is prepared; manganese salt and organic ligand are added to the zero-price nanometer iron suspension, and the organic skeleton material MIL-100(Fe-Mn) with yield of 89% is prepared. According to the testing conditions of denitration activity, 500 ppm NO, 500 ppm NH3, 5% O2 and N2 serve as balancing gas, the total flow of smoke is 100 ml / min, and the denitration catalytic efficiency at a temperature of 290 DEG C to 300 DEG C reaches 80% or higher. The prepared catalyst is novel in crystal structure, high in dispersibility and high in yield; meanwhile, Fe3+ and Mn3+ unsaturated active sites are obtained, and excellent catalytic activity is expressed.

Description

technical field [0001] The invention relates to a preparation method of a novel dual-core metal-organic framework material MIL-100 (Fe-Mn) with certain catalytic performance, and belongs to the technical field of novel material preparation. At the same time, it also involves its application as a catalytic material in flue gas denitration. Background technique [0002] Metal-Organic Frameworks (MOFs) have received extensive attention in the fields of gas storage, drug delivery, gas separation, and catalysis. Especially in the past five years, research reports on MOFs as excellent catalysts have increased rapidly. MOFs not only have rich structures, controllable pore size, high specific surface area, electronic effects and multifunctional metal centers, but also contain special organic functional groups and unsaturated metals. In terms of its metal content, it can reach 20-40 wt%. Metallic unsaturated coordination is numerous and has high dispersibility. The metal ions are ...

Claims

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Application Information

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IPC IPC(8): C07F19/00B01J31/22B01D53/86B01D53/56
Inventor 李春艳石勇高晓霞侯晓多
Owner DALIAN UNIV OF TECH
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