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Order mesoporous hollow zeolite material and one-step hydro-thermal synthesis method thereof
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A zeolite material and mesoporous technology, applied in the field of ordered mesoporous hollow zeolite materials and one-step hydrothermal synthesis, can solve unseen problems and achieve the effects of high hydrothermal stability, reduced synthesis cost and simple process
Inactive Publication Date: 2011-06-01
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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However, there are no related patents and literature reports on the synthesis of hollow structure materials containing ordered mesoporous zeolites.
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Embodiment 1
[0025] Synthesis of ordered mesoporous channel zeolite hollow structure material: aluminum isopropoxide, water, ethyl orthosilicate, tetrapropyl ammonium hydroxide, mixed and stirred evenly to obtain zeolite mother liquor, and then sodium hydroxide solution was added dropwise to the mother liquor After stirring for 2 hours, aging for 20 hours, the above steps were carried out in a constant temperature and humidity box at 15°C; then, at room temperature, the above solution was added dropwise to the hexadecyltrimethylammonium bromide solution and stirred for 2 hours , aging for 4 hours. The molar ratio of the reactants is
[0026] 100SiO 2 / 1Al 2 o 3 / 18TPAOH / 16600H 2 O / 44NaOH / 5.6CTAB. Put the above solution into a stainless steel reactor and heat it with water at 150°C, crystallize for 14 hours, wash, filter and dry, and roast at 600°C for 10 hours to obtain an ordered mesoporous MFI hollow zeolite. Typical XRD spectrum (attached Figure 4 ), SEM( figure 2 ), TEM( im...
Embodiment 2
[0028] According to the content of each component in Example 1, put it into a stainless steel reactor and heat it at 150°C, crystallize for 6 hours, wash, filter and dry, and roast at 600°C for 10 hours. According to the XRD data, it can be found that the product is ordered mesoporous Aluminosilicate (see image 3 A), no zeolite is formed, i.e. an amorphous material (see Figure 4 B).
Embodiment 3
[0030] According to the content of each component in Example 1, put it into a stainless steel reactor and heat it with water at 180°C, crystallize for 10 hours, wash, filter and dry, and roast at 600°C for 10 hours, zeolite begins to form, but the crystallization of zeolite is not complete, while maintaining a certain mesoporous order.
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Abstract
The invention provides an order mesoporous hollow zeolite material and a one-step hydro-thermal synthesis method thereof, belonging to the inorganic material field. The order mesoporous hollow zeolitematerial of the invention is characterized in that the hollow zeolite is provided with an inorganic crystal framework with micropore and mesoporous structure simultaneously, the particle diameter ofthe hollow mesoporous zeolite is 0.1-50 microns, the wall thickness of the hollow particle is 0.01-0.5 micron, pore canal size of the micropore and mesoporous is 0.4-50nm, and the order pore canals are communicated in three dimensions. In the invention, zeolite molecular sieve mother liquor is selected and added with surface active agent to obtain an order mesoporous zeolite molecular sieve by hydrothermal method. The invention reduces material synthesis cost with simple technique, and the prepared material has high hydrothermal stability and order mesoporous hollow structure.
Description
technical field [0001] The invention relates to an ordered mesoporous hollow zeolite material and a one-step hydrothermal synthesis method thereof, belonging to the field of inorganic materials. Background technique [0002] Microporous zeolite molecular sieve is an important shape-selective catalyst in the modern petroleum industry. It has the characteristics of uniform and well-developed microporous structure, strong acidity and good hydrothermal stability, and has been widely used in many fields. However, due to its small pore size, it is difficult for large-diameter molecules to enter the pores, and at the same time, the diffusion resistance is large, so that the macromolecules formed in the pores cannot escape quickly, which greatly limits its application in the field of macromolecular catalysis. The mesoporous zeolite molecular sieve has the advantages of microporous zeolite molecular sieve and mesoporous material at the same time, which can make up for the deficiency ...
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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/06C01B39/02C01B39/04
Inventor 赵晋津陈航榕施剑林
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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