公开(公告)号：KR100816547B1

公开(公告)日：2008-03-25

申请号：KR1020060117549

申请日：2006-11-27

Applicant: 한국화학연구원

Inventor： 장종산 ,  황영규 ,  정성화 ,  서유경 ,  세레 ,  페레이

IPC: B01J31/28 ,  B01J31/16 ,  B82Y30/00

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.

Abstract translation: 提供一种制备含铁多孔有机/无机混合材料的方法，通过间歇或连续反应方法制备有机/无机混合材料，反应时间短，并制备具有特殊晶体结构的有机/无机混合材料 提供了通过该方法制备的含铁多孔有机/无机混合材料。 在使用金属材料和配位化合物作为反应原料制备多孔有机/无机混合材料的方法中，制备含铁多孔有机/无机混合材料的方法包括：将铁或铁盐搅拌的预处理步骤 金属材料和苯三羧酸作为配位化合物，在溶剂存在下，以旋转速度为50〜2000转每分钟5〜600分钟，作为反应促进剂，将硝酸与 氢氟酸的摩尔比为0.1-1:1至0.1，或将15000Hz至30MHz的超声波照射到铁或铁盐和苯三羧酸上1至600分钟以形成晶核; 以及将1〜30GHz的微波照射到晶核形成的反应溶液上以在100〜250℃的温度范围内制备有机/无机混合材料的工序。 溶剂是具有1至10个碳原子的醇，具有2至10个碳原子的酮，具有5至20个碳原子的烃或其混合物。 此外，含铁多孔有机/无机混合材料具有Institut Lavoisier-100的材料结构。

公开(公告)号：KR100680767B1

公开(公告)日：2007-02-09

申请号：KR1020060011481

申请日：2006-02-07

Applicant: 한국화학연구원

Inventor： 정성화 ,  장종산 ,  황영규 ,  세레 ,  페레이

IPC: C07F11/00 ,  C07F9/00 ,  B82B3/00

Abstract: A method for preparing a porous organic-inorganic hybrid material is provided to be able to obtain the nano-sized porous organic-inorganic hybrid material through microwave heating within short reaction time, thereby reducing energy consumption and being environmentally useful. The method for preparing a porous organic-inorganic hybrid material having an average particle diameter of less than 500 nm comprises the steps of: (a) mixing a metal precursor which is at least one selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Hg, Mg, Ca, Sr, Ba, Sc, Y, Al, Ga, In, Tl, Si, Ge, Sn, Pb, As, Sb and Bi, an organic matter able to act as a ligand such as carboxyl group, carboxyl anion group, NH2, NH, CONH2, SO3H, SO3^-, CS2H, CS2^-, pyridine and pyrazine, and a solvent to prepare a reactant mixture solution; and (b) applying microwave having frequency of 0.3-300 GHz into the reactant mixture solution and then heating it at a temperature of more than 100 deg.C.

Abstract translation: 提供一种制备多孔有机 - 无机混合材料的方法，以便能够在短的反应时间内通过微波加热获得纳米尺寸的多孔有机 - 无机混合材料，由此减少能量消耗并且对环境有用。 用于制备平均粒径小于500nm的多孔有机 - 无机混合材料的方法包括以下步骤：（a）混合至少一种选自Ti，Zr，Hf， V，Nb，Ta，Cr，Mo，W，Mn，Re，Fe，Ru，Os，Co，Rh，Ir，Ni，Pd，Pt，Cu，Ag，Au，Zn，Cd，Hg，Mg，Ca， Sr，Ba，Sc，Y，Al，Ga，In，Tl，Si，Ge，Sn，Pb，As，Sb和Bi中的一种或两种以上作为配位体发挥作用的有机物质如羧基，羧基阴离子基团， NH，CONH 2，SO 3 H，SO 3 - ， - CS 2 H，CS 2 - ， - 吡啶和吡嗪和溶剂以制备反应混合物溶液; 和（b）将频率为0.3-300GHz的微波施加到反应混合物溶液中，然后在高于100℃的温度下加热。