核壳结构复合催化材料AC@ZSM-5的构建及其费—托合成应用初探
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摘要
核壳结构催化材料(记作“核@壳”)可以解决因活性纳米粒子团聚、活性中心中毒、流失等而导致催化剂活性下降的问题,同时又给不同催化过程之间的耦合开启了全新途径。由于分子筛膜在分离和催化上的独特作用,在传统催化剂颗粒外表面包覆一层分子筛膜可将核催化剂的催化作用和分子筛膜的分离、催化过程结合起来以提高催化剂的整体性能。活性炭(AC)是重要的催化剂／催化剂载体,随着对AC孔结构和其表面物理化学性质认识的深入,活性炭材料在催化领域必将获得更多应用。由于AC颗粒表面的不平整性和憎水性,采用直接水热法很难在其表面生长分子筛膜。因此,在AC表面包覆一层分子筛膜有理论和现实意义。本文采用改进的晶种法和凝胶过渡层法在不规则AC颗粒表面得到连续致密的MFI型分子筛膜壳层,发现了此类材料独特的开裂机理。在成功制备分子筛膜包覆AC复合材料AC@MFI的基础上,在AC中引入Co、Zr活性组分,得到分子筛膜包覆的新型催化材料CoZr/AC@ZSM-5。以费-托合成为模型反应,对催化材料的反应性能进行了初步研究。论文的主要研究内容如下：
AC直接用于水热合成,多数颗粒表面只有零星的分子筛晶粒附着。为了增加AC表面官能团以增加可供分子筛成核的中心,分别对AC进行空气氧化、硝酸处理、尿素水溶液水热处理和阳离子聚合物修饰等改性处理,处理之后分子筛晶粒在AC表面附着密度有所增加,但不足以成膜。有机物结焦和氧化铝过渡层辅助晶种二次生长法均能得到分子筛膜覆盖度比较高的AC颗粒。实验表明在无晶种条件下勃姆石凝胶层包覆的AC颗粒(AC@Gel)经水热后也能得到分子筛膜包覆比较完整的AC颗粒。
以勃姆石凝胶为过渡层,在动态水热条件下可制备出均匀、致密分子筛膜包覆AC的复合材料AC@ZSM-5,产物中几乎不含分子筛粉末。Zeta电位测试表明凝胶层表面可以比AC表面吸附更多的分子筛前驱物。不同晶化时间样品的SEM结果表明凝胶层的使用消除了AC颗粒表面物理化学性质不均匀的影响,增加了AC表面可供分子筛晶粒成核的中心数目,使分子筛的结晶过程均发生在凝胶层／溶液界面。此外,考察了凝胶层使用量对成膜覆盖度、重复合成对膜厚及分子筛膜取向的影响。
在用焙烧法去除分子筛膜中的模板剂时,AC@ZSM-5产生了严重的开裂和剥落。不同温度下的焙烧实验表明开裂发生在200～250℃。在AC@ZSM-5外表面二次涂覆凝胶有效地阻止了分子筛膜的开裂。热分析(TA)和程序升温脱附-质谱联用(TPD-MS)结果均表明在分子筛膜合成过程中AC吸附了大量的模板剂。在焙烧升温过程中AC内吸附的模板剂率先分解,此时分子筛膜壳层中的模板剂尚未开始分解,致密的分子筛壳层使得AC内产生的部分分解产物不能及时逸出发生爆破而导致分子筛膜开裂。二次涂覆凝胶层的方法增强了分子筛壳层的机械强度,使得在低升温速率下开裂现象极大缓和。三异丙苯吸附实验表明焙烧后无开裂的样品尚存有一些缺陷,经正硅酸四乙酯(TEOS)修饰和二次无模板剂水热合成之后缺陷明显减少。
为了考察分子筛膜包覆型核壳结构材料的催化性能,论文选择了费-托合成为模型反应。首先分别以Co(NO3)2·6H2O和Zr(NO3)4·5H2O为前驱体,采用等体积浸渍法在AC颗粒中引入Co、Zr活性组分制备CoZr/AC催化剂,然后采用凝胶过渡层法合成分子筛膜包覆的CoZr/AC@ZSM-5催化材料；进而分别实验考察了CoZr/AC、CoZr/AC@ZSM-5以及CoZr/AC和分子筛混合装填CoZr/AC-ZSM-5催化剂上的反应效果,表明包覆分子筛膜后的催化剂能明显改变产物分布；最后,结合产物组成和对反应前后的催化剂表征结果,对CoZr/AC@ZSM-5催化剂上低的CO转化率、高的甲烷和低碳烃选择性做出了合理的解释。
To develop the catalytic materials with core-shell structure (denoted as "core@shell") can avoid the catalysts deactivation due to the coalescence, poison or loss of active species. It also provides a new way to couple different catalytic processes. Owing to the catalytic and separate properties of zeolite membrane, encapsulating solid catalyst particles by zeolite membrane can realize the integration of catalysis and separation process and improve their overall performance. Activated carbon (AC) is a typical catalyst or supports. And with the further understanding of its pore structure and surface physicochemical properties, AC will obtain increasing attention in chemical industry. As mentioned above, coating a zeolite membrane shell on AC can be expected to maintain the stabilities of AC-based catalysts. But for the roughness and hydrophobic property of AC surface, it is difficult to coat zeolite membranes on AC particles with direct hydrothermal synthesis. The objectives of this work are to develop a method to coat continuous and dense MFI-type zeolite membrane on the surface of irregular AC particles. Based on successfully fabricated composite material AC@ZSM-5, active species of Co and Zr are introduced into AC and the prepared catalysts (CoZr/AC@ZSM-5) are investigated in Fischer-Tropsch synthesis (FTS). The effects of the zeolite membrane shell on the reaction will be discussed. The main contents of the dissertation are as follows.
After the direct hydrothermal synthesis, the zeolite crystals were loosely spread on AC particles with much of the surface uncoated. To increase the functional groups of AC surface, AC particles were pre-treated by air oxidation, concentrated nitric acid, urea solution and cationic polymer. Although the pretreatment enhanced the crystals coverage on AC, the attached zeolite crystals were still not sufficient to form a membrane. Secondary growth with the help of organics coking and intermediate alumina layer could obtain a better zeolite encapsulated AC particle. An important discovery was zeolite membrane fully covered AC particle could be prepared on the surface of boehmite gel/alumina coated AC particles, even no seeds deposited.
Continuous and dense ZSM-5membranes encapsulated AC particles (AC@ZSM-5) were obtained by using intermediate boehmite gel layer with dynamic hydrothermal treatment. No powder mixed with final products was observed. Zeta potential tests indicated that there were more TPA-silicate precursors exist on the surface of boehmite gel coated AC (AC/Gel) than that on AC. In order to study the growth of membrane, a series of samples under different hydrothermal durations were synthesized and then examined with SEM. Results show that zeolite crystals nucleate at the support/solution interface rather than in solution with the help of the intermediate layer. Optimum conditions for synthesis of AC@ZSM-5were identified through synthesis and characterization of these core-shell structured particles prepared with varying the mass ratio of gel to AC and the times of coating.
Template removal process of as-synthesized AC@ZSM-5was investigated. Serious cracking and peelings occurred during calcinations. Calcined tests indicated some cracks of membrane shell appeared with the temperatures in the range of200～250℃. By coating a secondary beohmite gel layer onto AC@ZSM-5, crack free samples were obtained. Combined the thermal gravity analyses (TG) with the temperature-programmed desorption/mass spectrum (TPD/MS) techniques, it was indicated that template contained in AC core and membrane shell decomposed in different way. For as-synthesized AC@ZSM-5, AC particles are wrapped by a compact membrane shells. As the temperatures increase, the template adsorbed in AC pyrolyzed first and the decomposed products like tripropylamine would accumulate in AC core. Subsequently, the inner pressure of the composite is strong enough to break through the membrane shell. An additional outer gel layer could increase the strength of the zeolite shell significantly and made crack free after calcination.1,3,5-Triisopropylbenzene (T/PB) adsorption tests suggested that defects like inter-crystalline gaps exist in shell membrane due to the shrink of crystals after template removal. Part of defects could be modified by using tetraethylorthosilicate (TEOS) or template-free secondary growth.
In order to test the potential use of core-shell structured AC@ZSM-5in Fischer-Tropsch synthesis, the active metals of cobalt and zirconium were introduced by incipient impregnating AC particles with Co(NO3)2-6H2O and solution. The obtained particles were denoted as CoZr/AC. Following the membrane synthesis using the intermediate layer as mentioned previously, the particles, named as CoZr/AC@ZSM-5, were obtained. For comparison, ZSM-5powders with the same Si/Al atomic ratio as the membrane shell were shaped to20～40mesh and used to mix with the CoZr/AC catalysts. The weight ratio of ZSM-5to CoZr/AC was1:10, which was identical with the mass ratio of membrane contained in CoZr/AC@ZSM-5. The FTS results of bare CoZr/AC, mixed CoZr/AC-ZSM-5and encapsuled CoZr/AC@ZSM-5were summarized. On the basis of the reaction results, the effects of the zeolite membrane shell on the reaction were illustrated.
AC直接用于水热合成,多数颗粒表面只有零星的分子筛晶粒附着。为了增加AC表面官能团以增加可供分子筛成核的中心,分别对AC进行空气氧化、硝酸处理、尿素水溶液水热处理和阳离子聚合物修饰等改性处理,处理之后分子筛晶粒在AC表面附着密度有所增加,但不足以成膜。有机物结焦和氧化铝过渡层辅助晶种二次生长法均能得到分子筛膜覆盖度比较高的AC颗粒。实验表明在无晶种条件下勃姆石凝胶层包覆的AC颗粒(AC@Gel)经水热后也能得到分子筛膜包覆比较完整的AC颗粒。
以勃姆石凝胶为过渡层,在动态水热条件下可制备出均匀、致密分子筛膜包覆AC的复合材料AC@ZSM-5,产物中几乎不含分子筛粉末。Zeta电位测试表明凝胶层表面可以比AC表面吸附更多的分子筛前驱物。不同晶化时间样品的SEM结果表明凝胶层的使用消除了AC颗粒表面物理化学性质不均匀的影响,增加了AC表面可供分子筛晶粒成核的中心数目,使分子筛的结晶过程均发生在凝胶层／溶液界面。此外,考察了凝胶层使用量对成膜覆盖度、重复合成对膜厚及分子筛膜取向的影响。
在用焙烧法去除分子筛膜中的模板剂时,AC@ZSM-5产生了严重的开裂和剥落。不同温度下的焙烧实验表明开裂发生在200～250℃。在AC@ZSM-5外表面二次涂覆凝胶有效地阻止了分子筛膜的开裂。热分析(TA)和程序升温脱附-质谱联用(TPD-MS)结果均表明在分子筛膜合成过程中AC吸附了大量的模板剂。在焙烧升温过程中AC内吸附的模板剂率先分解,此时分子筛膜壳层中的模板剂尚未开始分解,致密的分子筛壳层使得AC内产生的部分分解产物不能及时逸出发生爆破而导致分子筛膜开裂。二次涂覆凝胶层的方法增强了分子筛壳层的机械强度,使得在低升温速率下开裂现象极大缓和。三异丙苯吸附实验表明焙烧后无开裂的样品尚存有一些缺陷,经正硅酸四乙酯(TEOS)修饰和二次无模板剂水热合成之后缺陷明显减少。
为了考察分子筛膜包覆型核壳结构材料的催化性能,论文选择了费-托合成为模型反应。首先分别以Co(NO3)2·6H2O和Zr(NO3)4·5H2O为前驱体,采用等体积浸渍法在AC颗粒中引入Co、Zr活性组分制备CoZr/AC催化剂,然后采用凝胶过渡层法合成分子筛膜包覆的CoZr/AC@ZSM-5催化材料；进而分别实验考察了CoZr/AC、CoZr/AC@ZSM-5以及CoZr/AC和分子筛混合装填CoZr/AC-ZSM-5催化剂上的反应效果,表明包覆分子筛膜后的催化剂能明显改变产物分布；最后,结合产物组成和对反应前后的催化剂表征结果,对CoZr/AC@ZSM-5催化剂上低的CO转化率、高的甲烷和低碳烃选择性做出了合理的解释。
To develop the catalytic materials with core-shell structure (denoted as "core@shell") can avoid the catalysts deactivation due to the coalescence, poison or loss of active species. It also provides a new way to couple different catalytic processes. Owing to the catalytic and separate properties of zeolite membrane, encapsulating solid catalyst particles by zeolite membrane can realize the integration of catalysis and separation process and improve their overall performance. Activated carbon (AC) is a typical catalyst or supports. And with the further understanding of its pore structure and surface physicochemical properties, AC will obtain increasing attention in chemical industry. As mentioned above, coating a zeolite membrane shell on AC can be expected to maintain the stabilities of AC-based catalysts. But for the roughness and hydrophobic property of AC surface, it is difficult to coat zeolite membranes on AC particles with direct hydrothermal synthesis. The objectives of this work are to develop a method to coat continuous and dense MFI-type zeolite membrane on the surface of irregular AC particles. Based on successfully fabricated composite material AC@ZSM-5, active species of Co and Zr are introduced into AC and the prepared catalysts (CoZr/AC@ZSM-5) are investigated in Fischer-Tropsch synthesis (FTS). The effects of the zeolite membrane shell on the reaction will be discussed. The main contents of the dissertation are as follows.
After the direct hydrothermal synthesis, the zeolite crystals were loosely spread on AC particles with much of the surface uncoated. To increase the functional groups of AC surface, AC particles were pre-treated by air oxidation, concentrated nitric acid, urea solution and cationic polymer. Although the pretreatment enhanced the crystals coverage on AC, the attached zeolite crystals were still not sufficient to form a membrane. Secondary growth with the help of organics coking and intermediate alumina layer could obtain a better zeolite encapsulated AC particle. An important discovery was zeolite membrane fully covered AC particle could be prepared on the surface of boehmite gel/alumina coated AC particles, even no seeds deposited.
Continuous and dense ZSM-5membranes encapsulated AC particles (AC@ZSM-5) were obtained by using intermediate boehmite gel layer with dynamic hydrothermal treatment. No powder mixed with final products was observed. Zeta potential tests indicated that there were more TPA-silicate precursors exist on the surface of boehmite gel coated AC (AC/Gel) than that on AC. In order to study the growth of membrane, a series of samples under different hydrothermal durations were synthesized and then examined with SEM. Results show that zeolite crystals nucleate at the support/solution interface rather than in solution with the help of the intermediate layer. Optimum conditions for synthesis of AC@ZSM-5were identified through synthesis and characterization of these core-shell structured particles prepared with varying the mass ratio of gel to AC and the times of coating.
Template removal process of as-synthesized AC@ZSM-5was investigated. Serious cracking and peelings occurred during calcinations. Calcined tests indicated some cracks of membrane shell appeared with the temperatures in the range of200～250℃. By coating a secondary beohmite gel layer onto AC@ZSM-5, crack free samples were obtained. Combined the thermal gravity analyses (TG) with the temperature-programmed desorption/mass spectrum (TPD/MS) techniques, it was indicated that template contained in AC core and membrane shell decomposed in different way. For as-synthesized AC@ZSM-5, AC particles are wrapped by a compact membrane shells. As the temperatures increase, the template adsorbed in AC pyrolyzed first and the decomposed products like tripropylamine would accumulate in AC core. Subsequently, the inner pressure of the composite is strong enough to break through the membrane shell. An additional outer gel layer could increase the strength of the zeolite shell significantly and made crack free after calcination.1,3,5-Triisopropylbenzene (T/PB) adsorption tests suggested that defects like inter-crystalline gaps exist in shell membrane due to the shrink of crystals after template removal. Part of defects could be modified by using tetraethylorthosilicate (TEOS) or template-free secondary growth.
In order to test the potential use of core-shell structured AC@ZSM-5in Fischer-Tropsch synthesis, the active metals of cobalt and zirconium were introduced by incipient impregnating AC particles with Co(NO3)2-6H2O and solution. The obtained particles were denoted as CoZr/AC. Following the membrane synthesis using the intermediate layer as mentioned previously, the particles, named as CoZr/AC@ZSM-5, were obtained. For comparison, ZSM-5powders with the same Si/Al atomic ratio as the membrane shell were shaped to20～40mesh and used to mix with the CoZr/AC catalysts. The weight ratio of ZSM-5to CoZr/AC was1:10, which was identical with the mass ratio of membrane contained in CoZr/AC@ZSM-5. The FTS results of bare CoZr/AC, mixed CoZr/AC-ZSM-5and encapsuled CoZr/AC@ZSM-5were summarized. On the basis of the reaction results, the effects of the zeolite membrane shell on the reaction were illustrated.
引文
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