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Method for preparing supported bimetal organic framework material MIL-100(Fe-Cu) and denitration application

An organic framework and bimetal technology, applied in the field of preparation of new dual-core metal-organic framework material MIL-100, can solve the problems of high reaction temperature, narrow temperature window, vanadium toxicity, etc., and achieve high catalytic activity, regular pore structure, crystal uniform effect

Inactive Publication Date: 2017-01-04
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The SCR currently employs V 2 o 5 -WO 3 / TiO 2 It is a mature commercial catalyst, but there are also many defects such as: high reaction temperature, narrow temperature window, vanadium is toxic at high temperature, etc.

Method used

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  • Method for preparing supported bimetal organic framework material MIL-100(Fe-Cu) and denitration application
  • Method for preparing supported bimetal organic framework material MIL-100(Fe-Cu) and denitration application
  • Method for preparing supported bimetal organic framework material MIL-100(Fe-Cu) and denitration application

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Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: The preparation method of stable metal precursor solution.

[0031] Prepare 5mL, 0.7mol / LCuSO 4 ·5H 2 The O solution was dissolved in 60 mL of ultrapure water, and a mixed solution of CTAB, PVP, and citric acid (molar ratio 1:1:3) was added dropwise, and magnetically stirred for 10 min. 5mL, 1.2mol / L NaOH solution or 1.2mol / L NaBH 4The solution was dropped into the above solution at a constant speed. Ultrasonic treatment was carried out for 30 minutes while titrating, and after all the titration was completed, it was placed on a magnetic stirrer and stirred for 30 minutes.

Embodiment 2

[0032] Embodiment 2: the preparation method of MIL-100 (Fe) catalyst.

[0033] Ferric nitrate nonahydrate (3.35 mmol) and trimesic acid (3.35 mmol) were dissolved in 25 mL of ultrapure water. The uniformly mixed solution was placed in a closed glass container, and the mixed solution was heated by high-frequency electromagnetic wave oscillating microwaves. After a heating time of 25s, the temperature was increased to 160°C and maintained for 15 minutes, and a uniformly dispersed orange solid was obtained.

[0034] The product was treated in a water bath with high-purity water and absolute ethanol at 60°C (1 g of catalyst was added to about 150 mL of high-purity water or ethanol) to remove impurities. and dried in a constant temperature drying oven at 70°C. The dried samples were subjected to vacuum activation treatment to prepare catalysts.

Embodiment 3

[0035] Embodiment 3: the preparation method of MIL-100 (Fe-Cu) catalyst.

[0036] Take 5mL, 10mL, and 15mL of the above-mentioned stable metal precursors, add 0.2g of Fe-MOF material, and stir magnetically for 2h. Then move the reactant to a polyvinyl chloride liner reactor, seal it and place it in an oven for heating at 100°C for 12h. After the reaction kettle is lowered to room temperature, the product is centrifuged for 3-5 times (the solution is high-purity water), soaked in absolute ethanol solution and washed repeatedly. Finally, the product was heated overnight in a constant temperature drying oven at 70° C. to obtain a pure brown yellow powder, namely the organic framework material MIL-100 (Fe—Cu), with a yield of 78%.

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Abstract

The invention provides a method for preparing a supported bimetal organic framework material MIL-100(Fe-Cu) and denitration application, and belongs to the field of novel material design and preparation. By means of the post-synthesis modification method, the Cu element is successfully introduced into an original MOFs framework, and a novel MOFs material with bimetal active sites is constructed. The method is characterized in that the hydrothermal technology is used, a metal precursor solution is prepared by means of stabilizer to be effectively combined with Fe-MOFs, and the material MIL-100(Fe-Cu) is prepared and used for denitration reaction. Compared with an original monometal catalyst, a catalyst prepared through the method has unsaturated active sites of Fe3+ and Cu+, denitration activity is improved by about 15%, and the material is good in dispersity, high in yield and good in catalytic activity.

Description

technical field [0001] The invention relates to a preparation technology of a novel dual-core metal-organic framework material MIL-100 (Fe-Cu) with certain catalytic performance, and belongs to the field of design and preparation of novel materials. At the same time, it also involves its practical application as a catalytic material in flue gas denitrification. Background technique [0002] Nitrogen oxides (NOx) are one of the main sources of air pollution. With the advancement of my country's industrial process, industrial waste gas and vehicle exhaust emissions are increasing, and environmental problems caused by nitrogen oxides contained in waste gas are gradually emerging. Among them, acid rain and photochemical smog caused by nitrogen oxide emissions have become very serious environmental pollution problems in my country. [0003] Currently, NH 3 -SCR flue gas denitrification technology is a widely used nitrogen oxide control technology in industry, which has the adv...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01D53/90B01D53/56
CPCB01D53/8628B01D53/90B01J31/1691B01J31/2213B01D2251/2062B01J2531/842B01J2531/0238B01J35/617
Inventor 石勇张旺李春艳李新勇
Owner DALIAN UNIV OF TECH
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