强化介孔分子筛酸中心及水热稳定性的研究
摘要
本论文致力于合成具有强酸位的介孔分子筛及提高介孔分子筛的水热稳定性。
第一章为绪论,主要介绍介孔分子筛的合成机理,模板剂类型,介孔分子筛类型,及介孔分子筛应用等方面的信息;第二章是实验试剂及各种测试仪器型号及测试条件;在第三章中,以沸石MCM-22前驱物为原料,合成了相对于常规介孔分子筛MCM-41具有更强酸性的介孔分子筛MM-22,并将其应用到苯酚叔丁基化反应中,结果表明,MM-22表现了比Al-MCM-41,ZSM-5,MCM-22更好的催化性能;在第四章中,以沸石MCM-22为起始原料,通过碱处理打破沸石结构得到沸石次级结构单元,然后介孔化得到了具有强酸性的介孔分子筛M-MCM-22,测试结果表明,M-MCM-22具有规则的六方介孔结构,沸石MCM-22中的铝状态在M-MCM-22中得到延续;在第五章中,使用与第四章相同的方法对沸石MCM-49和MCM-56进行处理,得到了强酸性的介孔分子筛M-MCM-49和M-MCM-56;第六章中,我们以新颖的方法提高了介孔分子筛的水热稳定性:碳填充后高温处理。将此方法应用到介孔材料KIT-6上,使得材料的水热稳定性得到了大幅度提高。以小孔径的介孔分子筛MCM-41和MCM-48为起始材料,通过碳填充后高温处理的方法得到了具有高水热稳定性的超微孔材料。
According to the IUPAC, porous materials can be classified into three types by pore size: microprous materials are characterized by pore sizes of < 2 nm, mesoporous materials are characterized by pore size in the range of 2–50 nm, and the pore size > 50 nm can vest in macroporous materials. The microporous materials have been widely used in many fields such as adsorption and separation, ion-exchange, and industrial catalysis, because of their unique pore structures and characters. However, microporous materials can only be applied in the area related to small molecules; it can not effectively deal with large molecules due to the limitation of the pore size. Therefore, investigating porous materials with larger pores becomes very necessary.
Mesoporous materials have large surface area, uniform pore channels, high thermal stability and ability to be recycled, and thus they are widely used as catalysts or catalyst supports for many catalytic reactions. Since the discovery of M41S molecular sieves, varied kinds of mesoporous materials have been synthesized. Because conventional mesoporous aluminosilicates commonly possess weak acidity and poor hydrothermal stability due to amorphous pore walls, their catalytic applications are limited. Therefore, the preparation of new mesoporous aluminosilicates with strong acidity and high hydrothermal stability becomes very important. Based on this background, this paper carries out research of improving acidity and hydrothermal stability of mesoporous materials.
The acid strength of zeolites materials is higher than conventional mesoporous aluminosilicates. According to literatures, making the secondary structure units of zeolites into the framework can enhance the acid strength of mesoporous materials. In the third chapter, using zeolite MCM-22 precursor as silica and aluminium sources, through two-step crystallization procedure in the presence of cetyltrimethylammonium bromide (CTAB), a KIT-1-like structural mesoporous aluminosilicate (denoted as MM-22) has been synthesized under basic conditions. The characterized results show that MM-22 is pure mesoporous phase, and constructed of secondary structure units of zeolite MCM-22. Compared with classic Al-MCM-41 and ZSM-5, MM-22 has stronger acidity and higher hydrothermal stability. In the alkylation reaction of phenol with tert-butanol, MM-22 shows higher catalytic activity than Al-MCM-41, MCM-22 and ZSM-5.
In addition, destroying the crystal structure of zeolites also can obtain the secondary structure units of zeolites. All of the MCM-22 zeolite family is samdwich structure. Their crystal structure can be destroyed easily in the alkaline solution, producing large numbers of secondary structure units. In the chapter four, zeolite MCM-22 is treated by sodium hydroxide solution firstly, then cetyltrimethylammonium bromide (CTAB) is combined as mesoporous template to synthesize mesoporous material denoted as M-MCM-22 with enhanced acidity. Analytic results show that M-MCM-22 has ordered hexagonal p6mm mesostructure and its framework contains the secondary structure of zeolites MCM-22, which makes the acid sites of M-MCM-22 stronger in comparison with conventional Al-MCM-41. 27Al MAS NMR study confirms that aluminum in M-MCM-22 is exclusively in tetrahedral coordination. The catalytic performance of M-MCM-22 is tested in alkylation of phenol with tert-butanol and M-MCM-22 shows highly steady catalytic properties. The highest conversion of phenol can be achieved at 418 K, while the highest selectivity to 2, 4-di-TBP is obtained at 398 K. It is found that high temperature is advantageous to form 4-TBP, whereas low weight hourly space velocity (WHSV/h-1) is helpful for both conversion of phenol and selectivity to 2,4-DTBP. It is also shown that high ratio of tert-butanol/phenol is beneficial for obtaining high conversion of phenol and selectivity to 2,4-di-TBP.
In chapter five, by treating zeolite MCM-56 and MCM-49 with a sodium hydroxide solution for obtaining secondary structure units of zeolite as silicon and aluminum sources, using cetyltrimethylammonium bromide (CTAB) as template and adjusting the pH value to neutral, mesoporous aluminosilicat with hexagonal structure denoted as MM-56 and MM-49 are synthesized. Compared with conventional mesoporous aluminosilicates materials, MM-56 and MM-49 have enhanced acid sites and show higher catalytic activity for the alkylation of phenol with tert-butanol.
Less Si–OH groups can reduce mesoporous structure damage conducted by hydrolysis in hot water, thus the hydrothermal stability can be enhanced. It is well known that high temperature can make the number of Si–OH groups decreased, and the hydrothermal stability can be correspondingly reinforced. However under the high temperature condition, the mesoporous structure is easily destroyed. In chapter six, super-microporous materials with enhanced hydrothermal stability are synthesized by a novel method. We make sucrose dip into the pore of pure silica MCM-41 and MCM-48 to keep the pore structure firstly. Afterwards, by treating the materials at high temperature under nitrogen condition and then removing the carbon filled in pore channel, super-microporous silica with high hydrothermal stability denoted as MCM-41-T and MCM-48-T were obtained. Up to now, less attention has been developed to the synthesis of materials in the super-microporous (pore size 1–2 nm) range. The materials in this pore size range are very important since they may bridge the gap between microporous zeolites and mesoporous materials. Such materials exhibit the potential of size and shape selectivity for those organic molecules which are too large to access into the pores of microporous zeolites and zeolite-like materials. Analytic results show that after treatment by high temperature, the pore sizes of MCM-41 and MCM-48 decrease from mesoporous area to super-microporous range. MCM-41-T and MCM-48-T have high Q4/Q3 ratio and enhanced hydrothermal stability. Refluxed in boiled water for 96 h, the pore structure still remains. Making the furfural dip into the pore of mesoporous aluminosilicates and then treating at high temperature do not induce aluminium out from the mesoporous framework, and therefore the Bronsted acid sites only slightly decreases. We also apply this method to synthesize lager pore size mesoporous materials KIT-6 and it is found that hydrothermal stability of the material is considerably enhanced after high temperature treatment.
第一章为绪论,主要介绍介孔分子筛的合成机理,模板剂类型,介孔分子筛类型,及介孔分子筛应用等方面的信息;第二章是实验试剂及各种测试仪器型号及测试条件;在第三章中,以沸石MCM-22前驱物为原料,合成了相对于常规介孔分子筛MCM-41具有更强酸性的介孔分子筛MM-22,并将其应用到苯酚叔丁基化反应中,结果表明,MM-22表现了比Al-MCM-41,ZSM-5,MCM-22更好的催化性能;在第四章中,以沸石MCM-22为起始原料,通过碱处理打破沸石结构得到沸石次级结构单元,然后介孔化得到了具有强酸性的介孔分子筛M-MCM-22,测试结果表明,M-MCM-22具有规则的六方介孔结构,沸石MCM-22中的铝状态在M-MCM-22中得到延续;在第五章中,使用与第四章相同的方法对沸石MCM-49和MCM-56进行处理,得到了强酸性的介孔分子筛M-MCM-49和M-MCM-56;第六章中,我们以新颖的方法提高了介孔分子筛的水热稳定性:碳填充后高温处理。将此方法应用到介孔材料KIT-6上,使得材料的水热稳定性得到了大幅度提高。以小孔径的介孔分子筛MCM-41和MCM-48为起始材料,通过碳填充后高温处理的方法得到了具有高水热稳定性的超微孔材料。
According to the IUPAC, porous materials can be classified into three types by pore size: microprous materials are characterized by pore sizes of < 2 nm, mesoporous materials are characterized by pore size in the range of 2–50 nm, and the pore size > 50 nm can vest in macroporous materials. The microporous materials have been widely used in many fields such as adsorption and separation, ion-exchange, and industrial catalysis, because of their unique pore structures and characters. However, microporous materials can only be applied in the area related to small molecules; it can not effectively deal with large molecules due to the limitation of the pore size. Therefore, investigating porous materials with larger pores becomes very necessary.
Mesoporous materials have large surface area, uniform pore channels, high thermal stability and ability to be recycled, and thus they are widely used as catalysts or catalyst supports for many catalytic reactions. Since the discovery of M41S molecular sieves, varied kinds of mesoporous materials have been synthesized. Because conventional mesoporous aluminosilicates commonly possess weak acidity and poor hydrothermal stability due to amorphous pore walls, their catalytic applications are limited. Therefore, the preparation of new mesoporous aluminosilicates with strong acidity and high hydrothermal stability becomes very important. Based on this background, this paper carries out research of improving acidity and hydrothermal stability of mesoporous materials.
The acid strength of zeolites materials is higher than conventional mesoporous aluminosilicates. According to literatures, making the secondary structure units of zeolites into the framework can enhance the acid strength of mesoporous materials. In the third chapter, using zeolite MCM-22 precursor as silica and aluminium sources, through two-step crystallization procedure in the presence of cetyltrimethylammonium bromide (CTAB), a KIT-1-like structural mesoporous aluminosilicate (denoted as MM-22) has been synthesized under basic conditions. The characterized results show that MM-22 is pure mesoporous phase, and constructed of secondary structure units of zeolite MCM-22. Compared with classic Al-MCM-41 and ZSM-5, MM-22 has stronger acidity and higher hydrothermal stability. In the alkylation reaction of phenol with tert-butanol, MM-22 shows higher catalytic activity than Al-MCM-41, MCM-22 and ZSM-5.
In addition, destroying the crystal structure of zeolites also can obtain the secondary structure units of zeolites. All of the MCM-22 zeolite family is samdwich structure. Their crystal structure can be destroyed easily in the alkaline solution, producing large numbers of secondary structure units. In the chapter four, zeolite MCM-22 is treated by sodium hydroxide solution firstly, then cetyltrimethylammonium bromide (CTAB) is combined as mesoporous template to synthesize mesoporous material denoted as M-MCM-22 with enhanced acidity. Analytic results show that M-MCM-22 has ordered hexagonal p6mm mesostructure and its framework contains the secondary structure of zeolites MCM-22, which makes the acid sites of M-MCM-22 stronger in comparison with conventional Al-MCM-41. 27Al MAS NMR study confirms that aluminum in M-MCM-22 is exclusively in tetrahedral coordination. The catalytic performance of M-MCM-22 is tested in alkylation of phenol with tert-butanol and M-MCM-22 shows highly steady catalytic properties. The highest conversion of phenol can be achieved at 418 K, while the highest selectivity to 2, 4-di-TBP is obtained at 398 K. It is found that high temperature is advantageous to form 4-TBP, whereas low weight hourly space velocity (WHSV/h-1) is helpful for both conversion of phenol and selectivity to 2,4-DTBP. It is also shown that high ratio of tert-butanol/phenol is beneficial for obtaining high conversion of phenol and selectivity to 2,4-di-TBP.
In chapter five, by treating zeolite MCM-56 and MCM-49 with a sodium hydroxide solution for obtaining secondary structure units of zeolite as silicon and aluminum sources, using cetyltrimethylammonium bromide (CTAB) as template and adjusting the pH value to neutral, mesoporous aluminosilicat with hexagonal structure denoted as MM-56 and MM-49 are synthesized. Compared with conventional mesoporous aluminosilicates materials, MM-56 and MM-49 have enhanced acid sites and show higher catalytic activity for the alkylation of phenol with tert-butanol.
Less Si–OH groups can reduce mesoporous structure damage conducted by hydrolysis in hot water, thus the hydrothermal stability can be enhanced. It is well known that high temperature can make the number of Si–OH groups decreased, and the hydrothermal stability can be correspondingly reinforced. However under the high temperature condition, the mesoporous structure is easily destroyed. In chapter six, super-microporous materials with enhanced hydrothermal stability are synthesized by a novel method. We make sucrose dip into the pore of pure silica MCM-41 and MCM-48 to keep the pore structure firstly. Afterwards, by treating the materials at high temperature under nitrogen condition and then removing the carbon filled in pore channel, super-microporous silica with high hydrothermal stability denoted as MCM-41-T and MCM-48-T were obtained. Up to now, less attention has been developed to the synthesis of materials in the super-microporous (pore size 1–2 nm) range. The materials in this pore size range are very important since they may bridge the gap between microporous zeolites and mesoporous materials. Such materials exhibit the potential of size and shape selectivity for those organic molecules which are too large to access into the pores of microporous zeolites and zeolite-like materials. Analytic results show that after treatment by high temperature, the pore sizes of MCM-41 and MCM-48 decrease from mesoporous area to super-microporous range. MCM-41-T and MCM-48-T have high Q4/Q3 ratio and enhanced hydrothermal stability. Refluxed in boiled water for 96 h, the pore structure still remains. Making the furfural dip into the pore of mesoporous aluminosilicates and then treating at high temperature do not induce aluminium out from the mesoporous framework, and therefore the Bronsted acid sites only slightly decreases. We also apply this method to synthesize lager pore size mesoporous materials KIT-6 and it is found that hydrothermal stability of the material is considerably enhanced after high temperature treatment.
引文
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