水滑石类化合物及其多级核壳结构复合材料负载金催化剂的制备及催化性能研究
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摘要
负载型纳米金催化剂在不饱和醛/酮化合物选择性加氢、选择性醇氧化等许多重要的化学反应中表现出独特的催化特性，使其成为当前催化研究领域的热点。载体除了具有固载纳米金粒子的作用外，由于金属-载体相互作用使其对纳米金颗粒的粒径分布、氧化态、形貌等具有重要的影响，并且在反应过程中表现出与金粒子之间的协同效应。水滑石类化合物，又称层状双羟基复合金属氧化物（LayeredDouble Hydroxide，简写为LDH），由于其具有层板金属元素的可调控性及本征碱性，近年来作为一种新型催化剂载体受到人们的广泛关注。本论文以提高纳米金催化剂的催化性能、实现纳米金催化剂的方便回收及循环再利用的绿色催化为目标，首次设计合成了三种独特的LDH基功能化载体，继而负载纳米金粒子制得系列尺寸、形貌可控的高性能纳米金催化剂。采用XRD、SEM/TEM/HRTEM/STEM、ICP、BET、H_2-TPR及XPS等方法系统研究了催化剂的晶体结构、组成和形貌，考察催化剂在,-不饱和醛加氢以及醇氧化反应中的催化性能，探讨金与载体之间的相互作用机制及催化剂结构与催化性能之间的协同关联。论文的主要结果和创新点如下：
（1）以共沉淀法制备了系列具有可还原过渡金属Fe原子级高分散的三元LDH载体Mg_2Fe_xAl_(1-x)-LDH。采用修饰的沉积-沉淀法将纳米金粒子负载于该三元LDH载体上制得了系列粒子尺寸为40~100nm的Au/Mg_2Fe_xAl_(1-x)-LDH催化剂。研究发现，载体尺寸变化对负载金粒子尺寸分布无明显影响。然而，载体层板中高分散的Fe对Au粒子尺寸表现出限域效应，随着Fe含量增加，Au粒子尺寸逐渐由9nm减至5nm。与载体Mg_2Fe_xAl_(1-x)-LDH相比，催化剂中的Fe~(3+)还原成Fe~(2+)及Fe0的温度分别降低的了280℃和100℃，表明存在强的金-载体电子相互作用，使得负载金催化剂载体上的Fe~(3+)被部分还原，并且使催化剂表面具有更多的Au~(3+)。将该催化剂直接应用于肉桂醛加氢反应中，表现出较高的催化加氢活性和肉桂醇选择性，其中Au/Mg_2Fe_(0.8)Al_(0.2)-LDH显示出最高的加氢活性和肉桂醇选择性，与其较小的金粒子尺寸（5nm）和最强的金-载体相互作用吻合。同时，较低的催化剂预处理温度因有利于保持较高的Au~(3+)/Au~0比而显示更高的活性。可以确认Au~(3+)为该催化体系加氢的活性中心，Fe~(2+)的存在很可能稳定了催化剂中的Au~(3+)活性中心。
（2）利用γ-Al_2O_3表面Al源，以硝酸镁和硝酸铁为Mg源和Fe源，在550μm的球形γ-Al_2O_3成型载体表面原位取向生长Mg(Fe)Al-LDH纳米晶壳层薄膜对其修饰，首次得到一种结构化的微米级球形多级核壳结构复合载体γ-Al_2O_3@Mg(Fe)Al-LDH。通过沉积-沉淀法在该载体上负载纳米金粒子，首次得到直径为550μm的多级结构微球型负载金催化剂γ-Al_2O_3@Mg(Fe)Al-LDH@Au。金粒子与Mg(Fe)Al-LDH壳层薄膜修饰层中Fe~(3+)的电子相互作用使得Fe~(3+)被部分还原为Fe~(2+)，并且金粒子中的活性组分Au~(3+)的含量随壳层中Fe含量的增加逐渐增加，该催化剂的肉桂醛加氢活性和不饱和醇的选择性明显增高。反应时间的延长和压力的升高有利于加氢活性的提高，但不饱和醇选择性基本保持不变。温度升高有利于肉桂醛转化率的增大，但使得C=C（C~(δ+)–C~(δ-)）键与金粒子间较弱的相互作用进一步减弱，导致肉桂醇的选择性增加。该结构化多级核壳微球型催化剂仅通过沉降即可实现方便有效的分离回收。
（3）通过一步共沉淀法首次在具有超顺磁特性、尺寸均一的Fe_3O_4纳米球（450nm）表面取向生长MgAl-LDH壳层，得到一种蜂巢状形貌的多级核壳结构磁性复合物载体Fe_3O_4@MgAl-LDH。通过沉积-沉淀法在该Fe_3O_4@MgAl-LDH复合物壳层MgAl-LDH纳米晶上负载纳米金颗粒，得到直径约为650nm的球形多级核壳结构磁性纳米金催化剂Fe_3O_4@MgAl-LDH@Au。其壳层MgAl-LDH的含量为64wt%，厚约20nm、宽约100nm的MgAl-LDH纳米晶片垂直于Fe_3O_4表面由内而外交错生长。活性组分纳米金粒子主要分布于交错的MgAl-LDH纳米晶的边位和交接位，其平均粒径为7nm。催化剂经还原处理后，以分子O_2为氧化剂，无需添加碱助剂条件下，苯乙酮的收率高于99%。该催化剂良好的催化性能归因于载体壳层MgAl-LDH上碱性位与活性组分零价纳米金的协同作用。同时该催化剂较强的比饱和磁化强度（49.2emu·g~(-1)）使其在反应结束后可通过外加磁场方便回收，重复使用5次后活性没有明显降低，是一种高效绿色催化剂。
（4）调变壳层LDH层板组成，首次得到系列含有过渡金属Ni、Cu的多级核壳结构磁性纳米金催化剂Fe_3O_4@MAl-LDH@Au (M=Ni、CuMg)。垂直于Fe_3O_4表面交错取向生长的NiAl-LDH纳米晶片厚约20nm、宽约60nm，其晶粒尺寸明显小于MgAl-LDH（100nm）和CuMgAl-LDH（100nm），因而其比表面积最大（98.1m~2·g~(-1)）。Fe_3O_4@NiAl-LDH@Au催化剂具有较Fe_3O_4@MgAl-LDH@Au和Fe_3O_4@CuMgAl-LDH@Au体系更为致密的LDH壳层，导致其比饱和磁化强度（41.8emu·g~(-1)）与Fe_3O_4@CuMgAl-LDH@Au（52.2emu·g~(-1)）相比稍低。平均粒径为7nm的金粒子多分布于LDH纳米晶的边位和角位。Fe_3O_4@NiAl-LDH@Au催化剂壳层中Ni-OH与纳米金粒子的协同作用使其醇氧化性能明显高于Fe_3O_4@MgAl-LDH@Au和Fe_3O_4@CuMgAl-LDH@Au体系。该催化剂在无溶剂条件下表现出较高的1-苯乙醇氧化活性（TOF:2,760h~(-1)），并且适用于多种底物的一级醇和二级醇类化合物的催化选择性氧化。
In the last few years, supported gold particles have attracted growinginterest owing to their unusual and somewhat unexpected catalyticproperties in many important reactions, such as hydrogenation of α, β-unsaturated carbonyl compounds and selective oxidation of alcohols. Thenature of the support, the size and chemical state of Au particles arebelieved to be pivotal in determining the catalytic behavior of thesupported Au catalysts. Collaborative effect between gold and supportinduces the high catalytic activity. Hydrotalcite-like compounds, alsoknown as layered double hydroxides (LDH), have recently reattractedprofound interest as a unique support due to cationic tunability andintrinsic basicity of the brucite-like layer. In the present thesis, threespecial kind of LDH-based functionalized support materials have beendesigned and assembled for loading Au catalysts with controlled size,morphology and catalytic activities aiming at enhancing catalyticproperty and realizing green catalysis of nanogold catalysts in terms of facile recovery and efficiently recycling. The crystal structure,composition and morphology of the catalysts are systematically studiedusing XRD, SEM/TEM/HRTEM/STEM, ICP, BET, H_2-TPR and XPSmethods. The catalysts were evaluated in the liquid-phase hydrogenationof cinnamaldehyde and aerobic oxidation of alcohols. The gold-supportinteraction mechanism and structure-property relationship were discussed.The main results and innovations are shown as follows.
(1) A series of ternary LDH support materials Mg_2Fe_xAl_(1-x)-LDH withhighly dispersed reducible Fe~(3+)cations have been prepared by acoprecipitation step. Then using a modified deposition-precipitation (DP)method, a series of gold nanocatalysts Au/Mg_2Fe_xAl_(1-x)-LDH were obtaiedwith diameter from40to100nm. The characterization results illustratethat the dimension of the support show less influence on the average Auparticle size, however, the average Au particle size decreased from9nmto5nm with increasing Fe contents, ascribing to the confinement effectof the highly dispersed iron cations in ternary LDH supports. Upon theH_2-TPD results, the peak temperatures related to the reduction of Fe~(3+)toFe~(2+)and Fe~0, respectively, downshift by280oC and100oC comparedwith the corresponding supports, implying a strong gold–supportelectronic effect. The highest hydrogenation activity of Au/Mg_2Fe_(0.8)Al_(0.2)-LDH can be linked with its smallest Au particles (5nm) and the strongestAu-support electronic effect. Meanwhile, high activity was observed on the catalyst pretreated at low temperature because of holding highAu~(3+)/Au0ratio over the LDH support with proper amount of iron highlydispersed. The interaction between gold and Mg_2Fe_xAl_(1-x)-LDH causes animportant population of positively charged Au~(3+)probably stablized byreduced iron species Fe~(2+).
(2) A novel microsized hierarchical core-shell type gold nanocatalystγ-Al_2O_3@Mg(Fe)Al-LDH@Au was firstly fabricated via a facilesynthesis method. Firstly, a microsized core-shell composite support hasbeen prepared by in situ growing Mg(Fe)Al-LDH on the surface ofspherical γ-Al_2O_3(550μm) using urea as precipitant. Then the Aunanoparticles were effectively supported on thus-formed supportγ-Al_2O_3@Mg(Fe)Al-LDH by a DP method. A detailed analysis of thecatalyst structure is provided. Particular attention is paid to thegold-support interaction effect and percentage of Au~(3+)species in gold,which play vital roles in the hydrogenation activity and selectivity ofunsaturated alcohol. The increase of reaction time, temperature andpressure led to high catalytic activity but the unchanged selectivity of theunsaturated alcohol. The novel hierarchical core-shell gold nanocatalystscan be easily recovered by simple sedimentation.
(3) A novel hierarchical core-shell structured magnetic goldnanocatalyst Fe_3O_4@MgAl-LDH@Au was firstly assembled via a facilesynthesis route. The direct coating of LDH plateletlike nanocrystals vertically oriented to the Fe_3O_4particles (450nm) surface leads to ahoneycomb like core-shell Fe_3O_4@MgAl-LDH nanosphere. By a DPmethod, a gold-supported magnetic catalyst Fe_3O_4@MgAl-LDH@Au hasbeen obtained. The MgAl-LDH coating shell (68wt%) is composed ofedge-curving lamella with a thickness of ca.20nm and a width of ca.100nm, growing from the magnetite core to the outer surface andperpendicular to the Fe_3O_4surface. Au nanoparticles are evenlydistributed on the edge and junction sites of the interlaced MgAl-LDHnanocrystals with a mean diameter of7.0nm. After pre-reduction, thecatalyst exhibited excellent activity for the oxidation of1-phenylethanol,due to both the intrinsic basicity of the support and synergetic effectbetween Au and support. The catalyst (49.2emu·g~(-1)) can be effectivelyrecovered by using an external magnetic field. Five runs have been testedfor the Au nanocatalysts after easy magnetic separation by using a magnet,and no deactivation of the catalyst has been observed.
(4) Upon the synergetic effect of transition metal on gold catalystand the LDH composition tunability, a series of hierarchical core-shellstructured magnetic gold nanocatalyst Fe_3O_4@MAl-LDH@Au (M=Ni,CuMg) containing transition metal cations was firstly fabricated. Thelower saturation magnetization (Ms) of Fe_3O_4@NiAl-LDH@Au (41.8emu·g~(-1)) than the Fe_3O_4@CuMgAl-LDH@Au (52.2emu·g~(-1)) is mainlydue to the denser shell with a thickness of ca.60nm. The synergy between metallic Au nanoparticles and hydrotalcite supports does notonly involve the surface basic sites of the hydrotalcites but also includesNi-OH involved in alcohol dehydrogenation. Furthermore, we found thatthe Fe_3O_4@NiAl-LDH@Au via pre-reduction shows high activity for thesolvent-free oxidation of1-phenylethanol (TOF:2,760h~(-1)). The generalapplicability of Fe_3O_4@NiAl-LDH@Au for aerobic oxidation of alcoholswas further evaluated with extended substrate scope. The Fe_3O_4@NiAl-LDH@Au catalyst is not only effective for the oxidation of benzylicalcohols but also for less reactive cyclohexanol and linear aliphaticalcohols.
（1）以共沉淀法制备了系列具有可还原过渡金属Fe原子级高分散的三元LDH载体Mg_2Fe_xAl_(1-x)-LDH。采用修饰的沉积-沉淀法将纳米金粒子负载于该三元LDH载体上制得了系列粒子尺寸为40~100nm的Au/Mg_2Fe_xAl_(1-x)-LDH催化剂。研究发现，载体尺寸变化对负载金粒子尺寸分布无明显影响。然而，载体层板中高分散的Fe对Au粒子尺寸表现出限域效应，随着Fe含量增加，Au粒子尺寸逐渐由9nm减至5nm。与载体Mg_2Fe_xAl_(1-x)-LDH相比，催化剂中的Fe~(3+)还原成Fe~(2+)及Fe0的温度分别降低的了280℃和100℃，表明存在强的金-载体电子相互作用，使得负载金催化剂载体上的Fe~(3+)被部分还原，并且使催化剂表面具有更多的Au~(3+)。将该催化剂直接应用于肉桂醛加氢反应中，表现出较高的催化加氢活性和肉桂醇选择性，其中Au/Mg_2Fe_(0.8)Al_(0.2)-LDH显示出最高的加氢活性和肉桂醇选择性，与其较小的金粒子尺寸（5nm）和最强的金-载体相互作用吻合。同时，较低的催化剂预处理温度因有利于保持较高的Au~(3+)/Au~0比而显示更高的活性。可以确认Au~(3+)为该催化体系加氢的活性中心，Fe~(2+)的存在很可能稳定了催化剂中的Au~(3+)活性中心。
（2）利用γ-Al_2O_3表面Al源，以硝酸镁和硝酸铁为Mg源和Fe源，在550μm的球形γ-Al_2O_3成型载体表面原位取向生长Mg(Fe)Al-LDH纳米晶壳层薄膜对其修饰，首次得到一种结构化的微米级球形多级核壳结构复合载体γ-Al_2O_3@Mg(Fe)Al-LDH。通过沉积-沉淀法在该载体上负载纳米金粒子，首次得到直径为550μm的多级结构微球型负载金催化剂γ-Al_2O_3@Mg(Fe)Al-LDH@Au。金粒子与Mg(Fe)Al-LDH壳层薄膜修饰层中Fe~(3+)的电子相互作用使得Fe~(3+)被部分还原为Fe~(2+)，并且金粒子中的活性组分Au~(3+)的含量随壳层中Fe含量的增加逐渐增加，该催化剂的肉桂醛加氢活性和不饱和醇的选择性明显增高。反应时间的延长和压力的升高有利于加氢活性的提高，但不饱和醇选择性基本保持不变。温度升高有利于肉桂醛转化率的增大，但使得C=C（C~(δ+)–C~(δ-)）键与金粒子间较弱的相互作用进一步减弱，导致肉桂醇的选择性增加。该结构化多级核壳微球型催化剂仅通过沉降即可实现方便有效的分离回收。
（3）通过一步共沉淀法首次在具有超顺磁特性、尺寸均一的Fe_3O_4纳米球（450nm）表面取向生长MgAl-LDH壳层，得到一种蜂巢状形貌的多级核壳结构磁性复合物载体Fe_3O_4@MgAl-LDH。通过沉积-沉淀法在该Fe_3O_4@MgAl-LDH复合物壳层MgAl-LDH纳米晶上负载纳米金颗粒，得到直径约为650nm的球形多级核壳结构磁性纳米金催化剂Fe_3O_4@MgAl-LDH@Au。其壳层MgAl-LDH的含量为64wt%，厚约20nm、宽约100nm的MgAl-LDH纳米晶片垂直于Fe_3O_4表面由内而外交错生长。活性组分纳米金粒子主要分布于交错的MgAl-LDH纳米晶的边位和交接位，其平均粒径为7nm。催化剂经还原处理后，以分子O_2为氧化剂，无需添加碱助剂条件下，苯乙酮的收率高于99%。该催化剂良好的催化性能归因于载体壳层MgAl-LDH上碱性位与活性组分零价纳米金的协同作用。同时该催化剂较强的比饱和磁化强度（49.2emu·g~(-1)）使其在反应结束后可通过外加磁场方便回收，重复使用5次后活性没有明显降低，是一种高效绿色催化剂。
（4）调变壳层LDH层板组成，首次得到系列含有过渡金属Ni、Cu的多级核壳结构磁性纳米金催化剂Fe_3O_4@MAl-LDH@Au (M=Ni、CuMg)。垂直于Fe_3O_4表面交错取向生长的NiAl-LDH纳米晶片厚约20nm、宽约60nm，其晶粒尺寸明显小于MgAl-LDH（100nm）和CuMgAl-LDH（100nm），因而其比表面积最大（98.1m~2·g~(-1)）。Fe_3O_4@NiAl-LDH@Au催化剂具有较Fe_3O_4@MgAl-LDH@Au和Fe_3O_4@CuMgAl-LDH@Au体系更为致密的LDH壳层，导致其比饱和磁化强度（41.8emu·g~(-1)）与Fe_3O_4@CuMgAl-LDH@Au（52.2emu·g~(-1)）相比稍低。平均粒径为7nm的金粒子多分布于LDH纳米晶的边位和角位。Fe_3O_4@NiAl-LDH@Au催化剂壳层中Ni-OH与纳米金粒子的协同作用使其醇氧化性能明显高于Fe_3O_4@MgAl-LDH@Au和Fe_3O_4@CuMgAl-LDH@Au体系。该催化剂在无溶剂条件下表现出较高的1-苯乙醇氧化活性（TOF:2,760h~(-1)），并且适用于多种底物的一级醇和二级醇类化合物的催化选择性氧化。
In the last few years, supported gold particles have attracted growinginterest owing to their unusual and somewhat unexpected catalyticproperties in many important reactions, such as hydrogenation of α, β-unsaturated carbonyl compounds and selective oxidation of alcohols. Thenature of the support, the size and chemical state of Au particles arebelieved to be pivotal in determining the catalytic behavior of thesupported Au catalysts. Collaborative effect between gold and supportinduces the high catalytic activity. Hydrotalcite-like compounds, alsoknown as layered double hydroxides (LDH), have recently reattractedprofound interest as a unique support due to cationic tunability andintrinsic basicity of the brucite-like layer. In the present thesis, threespecial kind of LDH-based functionalized support materials have beendesigned and assembled for loading Au catalysts with controlled size,morphology and catalytic activities aiming at enhancing catalyticproperty and realizing green catalysis of nanogold catalysts in terms of facile recovery and efficiently recycling. The crystal structure,composition and morphology of the catalysts are systematically studiedusing XRD, SEM/TEM/HRTEM/STEM, ICP, BET, H_2-TPR and XPSmethods. The catalysts were evaluated in the liquid-phase hydrogenationof cinnamaldehyde and aerobic oxidation of alcohols. The gold-supportinteraction mechanism and structure-property relationship were discussed.The main results and innovations are shown as follows.
(1) A series of ternary LDH support materials Mg_2Fe_xAl_(1-x)-LDH withhighly dispersed reducible Fe~(3+)cations have been prepared by acoprecipitation step. Then using a modified deposition-precipitation (DP)method, a series of gold nanocatalysts Au/Mg_2Fe_xAl_(1-x)-LDH were obtaiedwith diameter from40to100nm. The characterization results illustratethat the dimension of the support show less influence on the average Auparticle size, however, the average Au particle size decreased from9nmto5nm with increasing Fe contents, ascribing to the confinement effectof the highly dispersed iron cations in ternary LDH supports. Upon theH_2-TPD results, the peak temperatures related to the reduction of Fe~(3+)toFe~(2+)and Fe~0, respectively, downshift by280oC and100oC comparedwith the corresponding supports, implying a strong gold–supportelectronic effect. The highest hydrogenation activity of Au/Mg_2Fe_(0.8)Al_(0.2)-LDH can be linked with its smallest Au particles (5nm) and the strongestAu-support electronic effect. Meanwhile, high activity was observed on the catalyst pretreated at low temperature because of holding highAu~(3+)/Au0ratio over the LDH support with proper amount of iron highlydispersed. The interaction between gold and Mg_2Fe_xAl_(1-x)-LDH causes animportant population of positively charged Au~(3+)probably stablized byreduced iron species Fe~(2+).
(2) A novel microsized hierarchical core-shell type gold nanocatalystγ-Al_2O_3@Mg(Fe)Al-LDH@Au was firstly fabricated via a facilesynthesis method. Firstly, a microsized core-shell composite support hasbeen prepared by in situ growing Mg(Fe)Al-LDH on the surface ofspherical γ-Al_2O_3(550μm) using urea as precipitant. Then the Aunanoparticles were effectively supported on thus-formed supportγ-Al_2O_3@Mg(Fe)Al-LDH by a DP method. A detailed analysis of thecatalyst structure is provided. Particular attention is paid to thegold-support interaction effect and percentage of Au~(3+)species in gold,which play vital roles in the hydrogenation activity and selectivity ofunsaturated alcohol. The increase of reaction time, temperature andpressure led to high catalytic activity but the unchanged selectivity of theunsaturated alcohol. The novel hierarchical core-shell gold nanocatalystscan be easily recovered by simple sedimentation.
(3) A novel hierarchical core-shell structured magnetic goldnanocatalyst Fe_3O_4@MgAl-LDH@Au was firstly assembled via a facilesynthesis route. The direct coating of LDH plateletlike nanocrystals vertically oriented to the Fe_3O_4particles (450nm) surface leads to ahoneycomb like core-shell Fe_3O_4@MgAl-LDH nanosphere. By a DPmethod, a gold-supported magnetic catalyst Fe_3O_4@MgAl-LDH@Au hasbeen obtained. The MgAl-LDH coating shell (68wt%) is composed ofedge-curving lamella with a thickness of ca.20nm and a width of ca.100nm, growing from the magnetite core to the outer surface andperpendicular to the Fe_3O_4surface. Au nanoparticles are evenlydistributed on the edge and junction sites of the interlaced MgAl-LDHnanocrystals with a mean diameter of7.0nm. After pre-reduction, thecatalyst exhibited excellent activity for the oxidation of1-phenylethanol,due to both the intrinsic basicity of the support and synergetic effectbetween Au and support. The catalyst (49.2emu·g~(-1)) can be effectivelyrecovered by using an external magnetic field. Five runs have been testedfor the Au nanocatalysts after easy magnetic separation by using a magnet,and no deactivation of the catalyst has been observed.
(4) Upon the synergetic effect of transition metal on gold catalystand the LDH composition tunability, a series of hierarchical core-shellstructured magnetic gold nanocatalyst Fe_3O_4@MAl-LDH@Au (M=Ni,CuMg) containing transition metal cations was firstly fabricated. Thelower saturation magnetization (Ms) of Fe_3O_4@NiAl-LDH@Au (41.8emu·g~(-1)) than the Fe_3O_4@CuMgAl-LDH@Au (52.2emu·g~(-1)) is mainlydue to the denser shell with a thickness of ca.60nm. The synergy between metallic Au nanoparticles and hydrotalcite supports does notonly involve the surface basic sites of the hydrotalcites but also includesNi-OH involved in alcohol dehydrogenation. Furthermore, we found thatthe Fe_3O_4@NiAl-LDH@Au via pre-reduction shows high activity for thesolvent-free oxidation of1-phenylethanol (TOF:2,760h~(-1)). The generalapplicability of Fe_3O_4@NiAl-LDH@Au for aerobic oxidation of alcoholswas further evaluated with extended substrate scope. The Fe_3O_4@NiAl-LDH@Au catalyst is not only effective for the oxidation of benzylicalcohols but also for less reactive cyclohexanol and linear aliphaticalcohols.
引文
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