Sn-Beta分子筛的合成、表征及催化性能研究
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摘要
Sn-Beta分子筛对以低浓度H202为氧化剂、温和条件下进行的有机物分子选择氧化反应具有优异的催化性能,受到国内外研究者的广泛关注。目前Sn-Beta分子筛的合成主要是Corma等报道的以正硅酸乙酯(TEOS)为硅源、脱铝纳米Beta沸石作为晶种诱导、HF为矿化剂的水热晶化法；该方法存在合成时间长(10天以上)、环境污染严重、设备要求高、生产过程可操作性及重现性差等问题；难以规模化生产和工业化应用。
本论文致力于研究成本低廉、合成步骤相对简单、快速、环境友好和易于工业化的Sn-Beta分子筛合成新方法。分别运用白炭黑为硅源的水热合成法、脱铝补锡两步后合成法、水蒸汽辅助法和两步水热法研究了Sn-Beta分子筛的形成。采用XRD、SEM、FT-IR、 UV-Vis、UV Raman、SEM、ICP-AES和N：吸附等分析手段表征了样品的结构和性能。论文的主要内容如下：
1.以白炭黑为硅源,SnCl4·H2O为锡源,NH4F为矿化剂,水热晶化法合成Sn-Beta分子筛,考察了n(H2O)/n(SiO2)摩尔比,晶化温度,无水乙醇加入量等对Sn-Beta形成的影响。与TEOS为硅源相比,白炭黑为硅源,避免了TEOS水解蒸醇过程,简化了合成步骤,并且能够精确控制最终凝胶中n(H2O)/n(SiO2)的比例；加入无水乙醇可以改善机械搅拌性能,有利于工业化生产。所制备的Sn-Beta样品对环己酮Baeyer-Villiger(B-V)氧化反应的催化活性与常规水热晶化合成法所制备的样品相当。
2.采用酸处理Al-Beta脱铝以产生T“空位”、再高温焙烧插入Sn,即脱铝补位两步后合成法制备了Sn-Beta分子筛。对脱铝次数及焙烧温度等关键参数进行了优化考察。随着脱铝次数的增加,母体中T“空位”数量增多,进入分子筛骨架的Sn量增加；高温焙烧有利于Sn进入分子筛骨架,但过高的焙烧温度能够造成分子筛骨架坍塌,对Sn进入分子筛骨架不利。最佳合成条件为：Si/Al比为21的Al-Beta沸石,无机酸(6M HNO3)脱铝处理2次,焙烧温度为773K。Sn-Beta样品中最高Sn含量可达3.92wt%(SnO2)。所合成的Sn-Beta样品在催化环己酮转化率23.4%,选择性为70%。
3.采用干胶水蒸汽辅助法(SAC)能够快速合成Sn-Beta分子筛。对晶化时间,温度,凝胶烘干温度,釜底水量等关键因素进行了考察。结果表明：含有结构导向剂(SDA)的无定形硅锡干胶,在水蒸汽的作用下,453K时,反应3-12h就可完全转化为高结晶度的Sn-Beta分子筛晶体。从前采用SAC法合成分子筛的文献均认为：“釜底水量的多少严重影响分子筛的形成”。而本研究发现,SAC法合成釜内部结构,是导致水量多少严重影响分子筛形成的主要原因。水蒸汽在釜内顶部冷凝后,回滴到干胶合成体系中,进而改变了各物质的组成比例,导致干胶无法晶化。利用改进的合成釜,研究了釜底过量水对Sn-Beta合成的影响表明,水量对Sn-Beta的形成不敏感,可在高水量范围制备。高温有利于晶体生成；Sn含量高,所需晶化时间长,当n(Si02)/n(Sn02)≤75时,即使延长晶化时间至200h,仍然无法得到Sn-Beta;硅锡凝胶烘干温度在333～373K之间时,样品结晶度高。最佳合成条件为：硅锡凝胶烘干温度为333～373K,晶化温度为433～473K。
4.以脱铝Beta沸石为硅源,十六烷基三甲基溴化铵(CTAB)为介孔模板剂,两步水热法合成多级孔Sn-Beta分子筛。首先,溶于有机碱四乙基氢氧化铵(TEAOH)溶液中的硅源与锡源(SnCl4·5H2O),在水热条件下进行预晶化,生成Sn-Beta晶体初级结构单元。在第2步水热晶化过程中,Sn-Beta初晶在介孔模板剂CTAB的辅助下,自组装成具有多级孔结构的Sn-Beta分子筛。与常规Sn-Beta相比,多级孔Sn-Beta兼有微孔和介孑L的孔道结构,应用于环己酮B-V氧化反应,表现出较强抗失活能力和水热稳定性。
Sn-Beta has attracted much attention for its excellent catalytic performances in selective oxidation of various organic compounds with dilute H2O2as the oxidant under mild conditions. Up to date, the synthesis of Sn-Beta still relies on the traditional fluoride method which reported by corma et al. using TEOS as the silica sources. Seeds are often required and are prepared by dealumination of nano-sized Al-Beta zeolites with concentrated nitric acid. The zeolite crystallization is time-consuming (at least ten days), and the use of hydrofluoric acid as mineralizer brings unwanted pollution and health hazard, that lead to poor synthesis reproducibility and high production costs. Thus, the process is energy intensive and difficult to scale-up.
The dissertation was focused on developing facile, rapid and efficient synthesis Sn-Beta method, which is expected to provide an economical and scalable for the industrial application. A series of new strategies and methods has been used, such as hydrothermal crystallization, two-step post synthesis, steam assisted conversion (SAC) and two-step hydrothermal crystallization method. The properties of the as-prepared samples were characterized by XRD, SEM, FT-IR. UV-Vis. UV Raman. ICP and N2adsorptions. The main contents of the dissertation are as follows:
1. Sn-Beta zeolite was successfully synthesized by hydrothermal crystallization method, using fumed silica as the silica source, SnCl4·H2O as the tin source and NH4F as the assisting agent. The effects of the molar ratio of n (H2O)/n (SiO2), the crystallization temperature and the amount of ethanol on the formation of the Sn-Beta zeolite frameworks, were investigated in detail. It is shown that using fumed silica as the silica source, can avoid the hydrolysis of the TEOS process and keep the molar ratio of n (H2O)/n (SiO2) in the final gel precisely, which simplify the synthesis process effectively. With the increase of n (H2O)/n (SiO2) molar ratio in the gel. the crystalline is decreased. The addition of ethanol into the prepared gel was helpful for improving the viscosity and fluidity of the initial gel. The as-synthesized sample exhibits no better, but comparable activity compares with Sn-Beta prepared by conventional hydrothermal method using TEOS as the silica source in cyclohexanone B-V oxidation reaction.
2. Sn-Beta zeolite was prepared by a two-step post synthesis method. The procedure consists of first dealumination of Al-Beta zeolite with nitric acid and then incorporation tin into the framworks by calcination at varying temperatures. The effect factors such as the number times of dealumination and calcination temperature in the preparation Sn-Beta was optimization. The results show that, tin content is increased with the amount of vacant T-sites in the precursor. The higher calcination temperature is benefited for incorporation of tin into the zeolite framework. However, when the calcination temperature is too high, the framework will collapse; Optimal synthesis conditions:Dealumination Al-Beta (Si/Al=21) with nitric acid (6M HNO3) two times, calcination temperature of773K. the highest Sn content in the as-prepared samples is3.92wt%(SnO2). The Cyclohexanone conversion is23.4%, the Lactone Selectivity is70%。
3. Sn-Beta zeolite was prepared by a rapid and clean SAC method from the dry stannosilicate gel. The effects of the crystallization temperature and time, the gel drying temperature and the amount of water in the bottom of autoclave on the formation of the Sn-Beta zeolite frameworks, were investigated in detail. The results show that, the amorphous gel was converted to highly crystalline Sn-Beta within3-12h at mild reaction temperature of453K. Compared with the researchers, we have get a different results on the synthesize parameter of water content. In the previous literatures, all the researchers agreed that" the amount of water in the bottom of the autoclave seriously affects the formation of zeolite"; we found that the inferior design of the internal structure of the conventional SAC synthesis autoclave is the real reason. When the amount of water in the bottom of the autoclave is enough, the vapor-liquid balance could be kept in the autoclave all the time during the crystallization. The condensation of steam into water inside the autoclave would take place and the condensed water can drop back into the gel. This leads to the change of the synthesis composition. In order to avoid this phenomenon, an improved SAC autoclave was designed and used in this study; it is shown that, the amount of water in the bottom of the autoclave cannot significantly affect the formation of Sn-Beta zeolites. The higher crystallization temperature is benefited for crystal formation; Higher Sn content required longer crystallization time; the dry gel with SiO2/SnO2ratio less than75,could not be transformed into zeolite phase even after200h of crystallization. Optimized synthesis conditions of high quality of Sn-Beta zeolites are the gel drying temperature of333-373K and the crystallization temperature of433-473K. The prepared Sn-Beta zeolites are active and selective for cyclohexanone B-V oxidation reaction.
4. A novel strategy, CTAB-assisted two-step hydrothermal crystallization method, has been designed for the synthesis of hierarchical Sn-Beta. In the first step, dealuminated Al-Beta and the Sn (IV) precursor were dissolved in TEAOH (40%aqueous solution) and formed a mixture. Then, the mixture formed Sn-Beta zeolite primary structural unit by hydrothermal synthesis. In second step, primary crystal of Sn-Beta will be converted to be a hierarchical Sn-Beta by CTAB-assisted through self-assembled. The material shows greatly increased catalytic activity and a strongly prolonged lifetime in the Baeyer-Villiger oxidation cyclohexanone, as compared to conventional zeolite Sn-Beta. This excellent catalytic performance of mesoporous Sn-Beta is closely related to its hierarchical micro/meso-structure, and high hydrothermal stability against mesostructural collapse and Sn leaching during reactions.
本论文致力于研究成本低廉、合成步骤相对简单、快速、环境友好和易于工业化的Sn-Beta分子筛合成新方法。分别运用白炭黑为硅源的水热合成法、脱铝补锡两步后合成法、水蒸汽辅助法和两步水热法研究了Sn-Beta分子筛的形成。采用XRD、SEM、FT-IR、 UV-Vis、UV Raman、SEM、ICP-AES和N：吸附等分析手段表征了样品的结构和性能。论文的主要内容如下：
1.以白炭黑为硅源,SnCl4·H2O为锡源,NH4F为矿化剂,水热晶化法合成Sn-Beta分子筛,考察了n(H2O)/n(SiO2)摩尔比,晶化温度,无水乙醇加入量等对Sn-Beta形成的影响。与TEOS为硅源相比,白炭黑为硅源,避免了TEOS水解蒸醇过程,简化了合成步骤,并且能够精确控制最终凝胶中n(H2O)/n(SiO2)的比例；加入无水乙醇可以改善机械搅拌性能,有利于工业化生产。所制备的Sn-Beta样品对环己酮Baeyer-Villiger(B-V)氧化反应的催化活性与常规水热晶化合成法所制备的样品相当。
2.采用酸处理Al-Beta脱铝以产生T“空位”、再高温焙烧插入Sn,即脱铝补位两步后合成法制备了Sn-Beta分子筛。对脱铝次数及焙烧温度等关键参数进行了优化考察。随着脱铝次数的增加,母体中T“空位”数量增多,进入分子筛骨架的Sn量增加；高温焙烧有利于Sn进入分子筛骨架,但过高的焙烧温度能够造成分子筛骨架坍塌,对Sn进入分子筛骨架不利。最佳合成条件为：Si/Al比为21的Al-Beta沸石,无机酸(6M HNO3)脱铝处理2次,焙烧温度为773K。Sn-Beta样品中最高Sn含量可达3.92wt%(SnO2)。所合成的Sn-Beta样品在催化环己酮转化率23.4%,选择性为70%。
3.采用干胶水蒸汽辅助法(SAC)能够快速合成Sn-Beta分子筛。对晶化时间,温度,凝胶烘干温度,釜底水量等关键因素进行了考察。结果表明：含有结构导向剂(SDA)的无定形硅锡干胶,在水蒸汽的作用下,453K时,反应3-12h就可完全转化为高结晶度的Sn-Beta分子筛晶体。从前采用SAC法合成分子筛的文献均认为：“釜底水量的多少严重影响分子筛的形成”。而本研究发现,SAC法合成釜内部结构,是导致水量多少严重影响分子筛形成的主要原因。水蒸汽在釜内顶部冷凝后,回滴到干胶合成体系中,进而改变了各物质的组成比例,导致干胶无法晶化。利用改进的合成釜,研究了釜底过量水对Sn-Beta合成的影响表明,水量对Sn-Beta的形成不敏感,可在高水量范围制备。高温有利于晶体生成；Sn含量高,所需晶化时间长,当n(Si02)/n(Sn02)≤75时,即使延长晶化时间至200h,仍然无法得到Sn-Beta;硅锡凝胶烘干温度在333～373K之间时,样品结晶度高。最佳合成条件为：硅锡凝胶烘干温度为333～373K,晶化温度为433～473K。
4.以脱铝Beta沸石为硅源,十六烷基三甲基溴化铵(CTAB)为介孔模板剂,两步水热法合成多级孔Sn-Beta分子筛。首先,溶于有机碱四乙基氢氧化铵(TEAOH)溶液中的硅源与锡源(SnCl4·5H2O),在水热条件下进行预晶化,生成Sn-Beta晶体初级结构单元。在第2步水热晶化过程中,Sn-Beta初晶在介孔模板剂CTAB的辅助下,自组装成具有多级孔结构的Sn-Beta分子筛。与常规Sn-Beta相比,多级孔Sn-Beta兼有微孔和介孑L的孔道结构,应用于环己酮B-V氧化反应,表现出较强抗失活能力和水热稳定性。
Sn-Beta has attracted much attention for its excellent catalytic performances in selective oxidation of various organic compounds with dilute H2O2as the oxidant under mild conditions. Up to date, the synthesis of Sn-Beta still relies on the traditional fluoride method which reported by corma et al. using TEOS as the silica sources. Seeds are often required and are prepared by dealumination of nano-sized Al-Beta zeolites with concentrated nitric acid. The zeolite crystallization is time-consuming (at least ten days), and the use of hydrofluoric acid as mineralizer brings unwanted pollution and health hazard, that lead to poor synthesis reproducibility and high production costs. Thus, the process is energy intensive and difficult to scale-up.
The dissertation was focused on developing facile, rapid and efficient synthesis Sn-Beta method, which is expected to provide an economical and scalable for the industrial application. A series of new strategies and methods has been used, such as hydrothermal crystallization, two-step post synthesis, steam assisted conversion (SAC) and two-step hydrothermal crystallization method. The properties of the as-prepared samples were characterized by XRD, SEM, FT-IR. UV-Vis. UV Raman. ICP and N2adsorptions. The main contents of the dissertation are as follows:
1. Sn-Beta zeolite was successfully synthesized by hydrothermal crystallization method, using fumed silica as the silica source, SnCl4·H2O as the tin source and NH4F as the assisting agent. The effects of the molar ratio of n (H2O)/n (SiO2), the crystallization temperature and the amount of ethanol on the formation of the Sn-Beta zeolite frameworks, were investigated in detail. It is shown that using fumed silica as the silica source, can avoid the hydrolysis of the TEOS process and keep the molar ratio of n (H2O)/n (SiO2) in the final gel precisely, which simplify the synthesis process effectively. With the increase of n (H2O)/n (SiO2) molar ratio in the gel. the crystalline is decreased. The addition of ethanol into the prepared gel was helpful for improving the viscosity and fluidity of the initial gel. The as-synthesized sample exhibits no better, but comparable activity compares with Sn-Beta prepared by conventional hydrothermal method using TEOS as the silica source in cyclohexanone B-V oxidation reaction.
2. Sn-Beta zeolite was prepared by a two-step post synthesis method. The procedure consists of first dealumination of Al-Beta zeolite with nitric acid and then incorporation tin into the framworks by calcination at varying temperatures. The effect factors such as the number times of dealumination and calcination temperature in the preparation Sn-Beta was optimization. The results show that, tin content is increased with the amount of vacant T-sites in the precursor. The higher calcination temperature is benefited for incorporation of tin into the zeolite framework. However, when the calcination temperature is too high, the framework will collapse; Optimal synthesis conditions:Dealumination Al-Beta (Si/Al=21) with nitric acid (6M HNO3) two times, calcination temperature of773K. the highest Sn content in the as-prepared samples is3.92wt%(SnO2). The Cyclohexanone conversion is23.4%, the Lactone Selectivity is70%。
3. Sn-Beta zeolite was prepared by a rapid and clean SAC method from the dry stannosilicate gel. The effects of the crystallization temperature and time, the gel drying temperature and the amount of water in the bottom of autoclave on the formation of the Sn-Beta zeolite frameworks, were investigated in detail. The results show that, the amorphous gel was converted to highly crystalline Sn-Beta within3-12h at mild reaction temperature of453K. Compared with the researchers, we have get a different results on the synthesize parameter of water content. In the previous literatures, all the researchers agreed that" the amount of water in the bottom of the autoclave seriously affects the formation of zeolite"; we found that the inferior design of the internal structure of the conventional SAC synthesis autoclave is the real reason. When the amount of water in the bottom of the autoclave is enough, the vapor-liquid balance could be kept in the autoclave all the time during the crystallization. The condensation of steam into water inside the autoclave would take place and the condensed water can drop back into the gel. This leads to the change of the synthesis composition. In order to avoid this phenomenon, an improved SAC autoclave was designed and used in this study; it is shown that, the amount of water in the bottom of the autoclave cannot significantly affect the formation of Sn-Beta zeolites. The higher crystallization temperature is benefited for crystal formation; Higher Sn content required longer crystallization time; the dry gel with SiO2/SnO2ratio less than75,could not be transformed into zeolite phase even after200h of crystallization. Optimized synthesis conditions of high quality of Sn-Beta zeolites are the gel drying temperature of333-373K and the crystallization temperature of433-473K. The prepared Sn-Beta zeolites are active and selective for cyclohexanone B-V oxidation reaction.
4. A novel strategy, CTAB-assisted two-step hydrothermal crystallization method, has been designed for the synthesis of hierarchical Sn-Beta. In the first step, dealuminated Al-Beta and the Sn (IV) precursor were dissolved in TEAOH (40%aqueous solution) and formed a mixture. Then, the mixture formed Sn-Beta zeolite primary structural unit by hydrothermal synthesis. In second step, primary crystal of Sn-Beta will be converted to be a hierarchical Sn-Beta by CTAB-assisted through self-assembled. The material shows greatly increased catalytic activity and a strongly prolonged lifetime in the Baeyer-Villiger oxidation cyclohexanone, as compared to conventional zeolite Sn-Beta. This excellent catalytic performance of mesoporous Sn-Beta is closely related to its hierarchical micro/meso-structure, and high hydrothermal stability against mesostructural collapse and Sn leaching during reactions.
引文
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