XRD分析CuZnAl催化剂中活性组分的晶粒组成
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摘要
利用X射线衍射(XRD)分析了合成气制甲醇CuZnAl催化剂的物相,结果表明:主要为单斜相的CuO,未见ZnO和Al_2O_3的衍射峰。单斜相CuO的衍射峰可以分峰为较窄的衍射峰和弥散衍射峰。利用Bruker的XRD数据分析软件EVA、TOPAS计算这两部分对应的晶粒尺寸和含量,分别为5～9nm、含量20%～30%的大晶粒和1～2nm、含量70%～80%的微细晶粒。把样品中的活性组分区分为微细晶粒和大晶粒,而不是把微细晶粒作为非晶相,这更能准确反映催化剂的组成特点。催化剂性能评价的结果表明:合成气制备甲醇时,微细晶粒含量越高、大晶粒尺寸相对较小的样品,其催化性能更好。
The crystal phase of CuZnAl catalyst for methanol synthesis is characterized by x-ray diffraction(XRD). The result indicates that the main phase is monoclinic phase CuO, and the diffraction peaks of ZnO and Al_2O_3 are not found. The diffraction peaks of CuO can be divided into narrow peaks and broad peak. The crystallite size and content of the two parts are respectively calculated by EVA and TOPAS softwares of Bruker. The crystallite size calculated from narrow peaks is 5-9nm and its content is 20%-30% while the size calculated from broad peaks is 1-2nm and its content is 70%-80%, which indicates that the active compositions in the sample include two kinds of crystalline in nature. On the basis of the relationship established between XRD result and the catalyst evaluation data, it is suggested that the catalyst, which has smaller crystallite with higher content and bigger crystallite with relatively small size, perform better.
The crystal phase of CuZnAl catalyst for methanol synthesis is characterized by x-ray diffraction(XRD). The result indicates that the main phase is monoclinic phase CuO, and the diffraction peaks of ZnO and Al_2O_3 are not found. The diffraction peaks of CuO can be divided into narrow peaks and broad peak. The crystallite size and content of the two parts are respectively calculated by EVA and TOPAS softwares of Bruker. The crystallite size calculated from narrow peaks is 5-9nm and its content is 20%-30% while the size calculated from broad peaks is 1-2nm and its content is 70%-80%, which indicates that the active compositions in the sample include two kinds of crystalline in nature. On the basis of the relationship established between XRD result and the catalyst evaluation data, it is suggested that the catalyst, which has smaller crystallite with higher content and bigger crystallite with relatively small size, perform better.
引文
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[2]宋志强,秦金良,李红良,等.Cu O/Zn O/Al2O3应用于合成气催化合成甲醇[J].辽宁化工,2015,44(9):1049-1051.
[3]陈文瑞,李虎强,冯媛.合成气制甲醇催化剂研究进展(Ⅰ)-铜基催化剂[J].广州化工,2017,45(9):3-5.
[4]于杨.Cu/Zn O/Zn-Al水滑石催化剂的制备及在富CO2合成气制甲醇反应中的催化性能[J].工业催化,2015,23(12):991-995.
[5]Flores J H,Maia da Costa M E H,Pais da Silva M I.Effect of Cu-Zn O-Al2O3supported on H-ferrierite on hydrocarbons formation from CO hydrogenation[J].Chin JCatal,2016,37:378-388.
[6]Günter M M,Ressler T,Bems B,et al.Implication of the microstructure of binary Cu/Zn O catalysts for their catalytic activity in methanol synthesis[J].Catal Lett,2001,71:37-44.
[7]张鑫,刘静,李光强.XRD与TEM技术在分析纳米金属晶粒尺寸中的应用[J].南方金属,2006,(3):15-17.
[8]李忠,刘岩,范辉,等.Zr对Cu O/Zn O/Al2O3前驱体物相、催化剂结构及其合成甲醇性能的影响[J].无机化学学报,2010,26(7):1245-1251.
[9]覃丽禄.透射式电子背散射衍射技术(t-EBSD)在材料学中的应用研究进展世界科技研究与发展[J].世界科技研究与发展,2017,39(2):134-138.
[10]刘紫微,华佳捷,林初城,等.透射模式电子背散射衍射技术在纳米材料研究中的应用[J].无机材料学报,2015,(8):833-837.
[11]刘存业,李建,刘荣泰,等.超微粒子Ag和Ag2O的TEM和XRD分析[J].分析测试学报,1996,(4):69-73.
[12]王晓叶,郑斌,冯志海.X射线衍射全谱拟合定量分析方法研究[J].宇航材料工艺,2012,(2):108-110。
[13]烟卫,刘昱,李艳苹,等.X射线衍射法钾混盐无标样定量相分析[J].理化检验,2014,50(4):413-416.
[14]赵伟,封亚辉,李建军.X射线衍射法快速测定矿产品中的主要物相和主元素含量[J].理化检验,2015,51(4)523-527.
[15]Zhang F,Zhang Y L,Liu Y,et al.Synthesis of Cu/Zn/Al/Mg catalysts on methanol production by different precipitation methods[J].Mol Catal,2017,441:190-198
[16]郭宪吉,齐化多,徐三魁,等.铜基甲醇合成催化剂的表征及铜、锌组分间的相互作用[J].天然气化工-C1化学与化工,2000,25(5):36-39.
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