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A method for preparing porous organic-inorganic hybrid materials, hybrid materials obtained by the method and catalytic uses of the materials

A technology of hybrid materials and organic compounds, the application of which also includes the use of non-porous organic-inorganic hybrid materials and the preparation of the materials and organic compounds in the field to achieve energy-saving, economically and environmentally beneficial effects

Active Publication Date: 2013-02-06
KOREA RES INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organic-inorganic hybrid materials in which the chromium component in the metal-organic framework structure is replaced by another metal have not been reported

Method used

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  • A method for preparing porous organic-inorganic hybrid materials, hybrid materials obtained by the method and catalytic uses of the materials
  • A method for preparing porous organic-inorganic hybrid materials, hybrid materials obtained by the method and catalytic uses of the materials
  • A method for preparing porous organic-inorganic hybrid materials, hybrid materials obtained by the method and catalytic uses of the materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Example 1: Preparation of porous organic-inorganic hybrid material (Fe-BTC) using mixed acids

[0080] Add 1mmol of metallic iron and 1M HNO to the Teflon reactor 3 60ml, 40ml of 5M HF (aqueous solution) and 7mmol of 1,3,5-benzenetricarboxylic acid (BTCA), and then distilled water was added. The final molar ratio of the reaction materials is Fe:HF:HNO 3 :BTCA:H 2 O=1:2:0.6:0.7:278.

[0081] The mixed reaction mass was stirred at room temperature at 500 rpm for 20 minutes to make the reaction mass as homogeneous as possible.

[0082] The Teflon reactor containing the pretreated reaction material was installed on a microwave reactor (CEM company, Mars-5 type), and then heated up to 200 ° C by microwave irradiation (2.54GHz), and the reaction material was heated at 200 C for 2 minutes for crystallization. Subsequently, the reaction mass was cooled to room temperature, centrifuged, washed with distilled water and dried to obtain a porous organic-inorganic hybrid mat...

Embodiment 2

[0088] Example 2 (Cr-BDC-1)

[0089] After adding Cr(NO 3 ) 3 9H 2 After O and 1,4-phthalic acid (BDCA), distilled water was added so that the molar ratio of the final reaction mass was Cr:HNO 3 :BDCA:H 2 O=1:0.1:1:272. Basically, if Cr(NO 3 ) 3 Soluble in water, will hydrate to generate strong acid. Therefore, it has with the addition of HNO 3 same effect. After putting the Teflon reactor containing the reaction materials into an electric oven and reacting at 210°C for 11 hours, it was cooled to room temperature, centrifuged, washed with distilled water and dried to obtain a porous organic-inorganic hybrid Material Chromium phthalate (Cr-BDC). The results of X-ray diffraction analysis of the Cr-BDC thus prepared showed characteristic diffraction peaks at about 3.3, 5.2, 5.9, 8.5 and 9.1 for 2θ values, and it is known that chromium phthalate having cubic crystallinity ( Figure 4 ). It has been confirmed that the X-ray diffraction pattern of the chromium phthalat...

Embodiment 3

[0090] Example 3 (Cr-BDC-2)

[0091] 1g of the porous organic-inorganic hybrid material prepared in Example 2 was added to 50ml of 1M NH 4 F, with stirring at 70 °C, prepared an organic-inorganic hybrid material with increased surface area by removing impurities present in the pores of the porous material. From the X-ray diffraction spectrum ( Figure 5 ), it was confirmed that the crystallinity was maintained without being destroyed after treatment with ammonium fluoride. In addition, from the measurement results of nitrogen adsorption of the porous organic-inorganic hybrid material before and after treatment with ammonium fluoride, it can be shown that an organic-inorganic hybrid material having the following characteristics can be obtained: the surface area is increased by 700 m due to the ammonium fluoride treatment 2 / g (3373m before treatment with ammonium fluoride 2 / g, 4074m after processing 2 / g), and, when P / P 0 When =0.5, the adsorption capacity has increased...

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Abstract

A method of preparing an iron-containing porous organic / inorganic hybrid material is provided to prepare an organic / inorganic hybrid material through a batch or continuous reaction process for a short reaction time and prepare an organic / inorganic hybrid material having a special crystal structure within a short time, and an iron-containing porous organic / inorganic hybrid material prepared by the method is provided. In a method of preparing a porous organic / inorganic hybrid material using metal material and coordination compound as reaction raw materials, a method of preparing an iron-containing porous organic / inorganic hybrid material comprises: a pretreatment step of stirring iron or an iron salt as the metal material, and benzene tricarboxylic acid as the coordination compound at a rotation speed of 50 to 2000 revolutions per minute for 5 to 600 minutes in the presence of a solvent, and a mixed acid as a reaction promoter in which nitric acid is mixed with hydrofluoric acid at a molar ratio of 0.1 to 1:1 to 0.1, or irradiating ultrasonic waves of 15000 Hz to 30 MHz onto the iron or an iron salt and the benzene tricarboxylic acid for 1 to 600 minutes to form a crystal nucleus; and a step of irradiating a microwave of 1 to 30 GHz onto the crystal nucleus-formed reaction solution to prepare an organic / inorganic hybrid material in a temperature range of 100 to 250 deg.C. The solvent is an alcohol having 1 to 10 carbon atoms, a ketone having 2 to 10 carbon atoms, a hydrocarbon having 5 to 20 carbon atoms, or mixtures thereof. Further, the iron-containing porous organic / inorganic hybrid material has a structure of Materials of Institut Lavoisier-100.

Description

technical field [0001] The invention relates to a method for preparing a porous organic-inorganic hybrid material and its catalytic application. More specifically, the present invention relates to porous metal-containing organic-inorganic hybrid materials and methods of making the same. That is, it relates to a new method for the preparation of iron-containing porous organic-inorganic hybrid materials, which can be used not only as adsorbents, gas storage materials, sensors, catalysts, and catalyst supports, etc., Also useful for inclusion of guest molecules smaller than the pore size or separation of molecules larger than the pore size due to the large surface area of ​​these porous organic-inorganic hybrid materials with molecular or nanometer sized pores. Among them, the organic compound ligand is bound to the central metal through the prepared iron-containing porous organic-inorganic hybrid material. The preparation is to form a crystal nucleus by pretreating the metal or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J35/10
CPCY02C10/08B01J31/16B01J31/28B82Y30/00
Inventor 张钟山黄璄圭郑成和洪度荣徐有境杰勒德·费雷克里斯蒂安·塞尔
Owner KOREA RES INST OF CHEM TECH