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Organic-inorganic hybrid supermicroporous iron(III) phosphonate nanoparticles as an efficient catalyst for the synthesis of biofuels

机译:有机-无机杂化超微孔铁(III)膦酸酯纳米颗粒作为合成生物燃料的有效催化剂

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摘要

Here we report a novel family of crystalline, supermicroporous iron(III) phosphonate nanomaterials (HFeP-1-3, HFeP-1-2, and HFeP-1-4) with different Fe~(III)-to-organophosphonate ligand mole ratios. The materials were synthesized by using a hydrothermal reaction between benzene-1,3,5-triphosphonic acid and iron(III) chloride under acidic conditions (pH≈4.0). Powder X-ray diffraction, N_2 sorption, transmission and scanning electron microscopy (TEM and SEM) image analysis, thermogravimetric and differential thermal analysis (TGA-DTA), and FTIR spectroscopic tools were used to characterize the materials. The triclinic crystal phase [P1(2) space group] of the hybrid iron phosphonate was established by a Rietveld refinement of the PXRD analysis of HFeP-1-3 by using the MAUD program. The unit cell parameters are a=8.749(1), b=8.578(1), c=17.725(3) ?; α=104.47(3), β=97.64(1), γ=113.56(3)°; and V=1013.41 ?~3. With these crystal parameters, we proposed an 24-membered-ring open framework structure for HFeP-1. Compound HFeP-1-3, with an starting Fe/ligand molar ratio of 3.0, shows the highest Brunauer-Emmett-Telller (BET) surface area of 556 m~2g ~(-1) and uniform supermicropores of approximately 1.1 nm. The acidic surface of the porous iron(III) phosphonate nanoparticles was used in a highly efficient and recyclable catalytic transesterification reaction for the synthesis of biofuels under mild reaction conditions. Iron brews biofuels: Highly crystalline, supermicroporous iron(III) phosphonate nanoparticles have been synthesized through a hydrothermal reaction between benzene-1,3,5- triphosphonic acid and FeCl_3. The resulting material was used as an efficient and recyclable catalyst for the synthesis of biofuels under mild reaction conditions (see scheme).
机译:在这里,我们报告了具有不同的Fe〜(III)-有机膦酸酯配体摩尔比的新型晶体超微孔膦酸铁(III)纳米材料(HFeP-1-3,HFeP-1-2和HFeP-1-4)。 。在酸性条件下(pH≈4.0),通过苯-1,3,5-三膦酸与氯化铁(III)的水热反应合成了材料。粉末X射线衍射,N_2吸附,透射和扫描电子显微镜(TEM和SEM)图像分析,热重和差热分析(​​TGA-DTA)以及FTIR光谱工具被用来表征材料。通过使用MAUD程序对HFeP-1-3进行PXRD分析的Rietveld改进,建立了杂膦酸铁的三斜晶相[P1(2)空间群]。晶胞参数为a = 8.749(1),b = 8.578(1),c = 17.725(3)?; α= 104.47(3),β= 97.64(1),γ= 113.56(3)°;并且V =1013.41≤3。利用这些晶体参数,我们为HFeP-1提出了24元环的开放框架结构。起始Fe /配体摩尔比为3.0的化合物HFeP-1-3显示出最高的Brunauer-Emmett-Telller(BET)表面积为556 m〜2g〜(-1),且均匀的超微孔约为1.1 nm。多孔膦酸铁(III)纳米颗粒的酸性表面用于高效且可回收的催化酯交换反应,用于在温和的反应条件下合成生物燃料。铁酿造生物燃料:高度结晶的超微孔膦酸铁(III)纳米颗粒通过苯-1,3,5-三膦酸与FeCl_3之间的水热反应合成。所得材料用作在温和的反应条件下合成生物燃料的有效且可循环使用的催化剂(请参见方案)。

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