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Middle hole ZSM-5 zeolite microsphere and preparation method thereof

A technology of ZSM-5 and microspheres, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of increased cost and complicated preparation process, and achieve the reduction of preparation cost and simplification Preparation process, overcome the effect of not easy to separate

Inactive Publication Date: 2012-03-28
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
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  • Claims
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Problems solved by technology

Chinese patent 200510025272.8 discloses the use of urea-formaldehyde resin as a template to induce colloidal nano-zeolite polymerization to prepare the method for zeolite microspheres with hierarchical pores; Chemical Materials (2009, 21, 2344-2348) and Journal of Material Chemistry (2009, 19, 7614- 7616) respectively reported the addition of F127 and polymethyl methacrylate ball-forming templates in the zeolite synthesis system to prepare mesoporous ZSM-5 zeolite microspheres in one step, wherein the mesoporous and hierarchical pores are made of nano-sized zeolite particles The intercrystalline pores formed by the aggregation of the crystals, and no mesopores in the crystals, must use polymer balling agents to form balls in the preparation process, so the preparation process is complicated and the cost increases

Method used

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  • Middle hole ZSM-5 zeolite microsphere and preparation method thereof
  • Middle hole ZSM-5 zeolite microsphere and preparation method thereof

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Experimental program
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Effect test

Embodiment approach 1

[0021] Take 0.1mol of anilinopropyltrimethoxysilane and dissolve it in 670mL of alcoholic aqueous solution containing 60% (w / w) of methanol. After the dissolution is complete, add 30g (0.5mol) with a specific surface area of ​​200m 2 / g, silicon dioxide with a particle size of 12nm, poured into a 1500mL three-necked flask, refluxed and stirred at 100°C for 8h, separated from solid and liquid, washed with ethanol at room temperature, and dried at 100°C to obtain a solid surface silanized silica powder. Take 4.3 g of the above-mentioned silanized silica, add 1.33 g of tetrapropylammonium bromide (TPABr) and 72 mL of deionized water, stir in a three-necked flask at room temperature for 10 h, then add 0.1 g of aluminum isopropoxide, 0.2 g of hydroxide Sodium, reflux and stir at 90°C for 20h; put it into a sealed reaction kettle, crystallize at 180°C for 3 days; centrifuge the crystallized product from solid and liquid, wash at room temperature, dry at 100°C, and roast in air at 600...

Embodiment approach 2

[0024] Change the amount of anilinopropyltrimethoxysilane in embodiment 1 to 0.0625mol, and keep the other conditions unchanged, carry out silanization to silica; then take 3.9g of the silanized silica to synthesize mesoporous ZSM-5 Zeolite microspheres. The X-ray diffraction spectrum shows that the product is ZSM-5 zeolite with high crystallinity; the scanning electron microscope photos show that the diameter of the microspheres is about 5-7 μm; The size of the mesopores in the small crystal grains is 3-4nm; the external specific surface area is 205m 2 / g, the mesopore volume is 0.19mL / g.

Embodiment approach 3

[0026] Change the amount of anilinopropyltrimethoxysilane in Embodiment 1 to 0.025mol, and keep other conditions unchanged, carry out silanization to silicon dioxide; take 3.3g of the silanized silicon dioxide to synthesize mesoporous ZSM-5 zeolite Microspheres. The results show that the diameter of the microspheres is about 5-7μm; the size of the small grains is 15-30nm; the size of the inner and middle pores in the small grains is 3-4nm; 2 / g, the mesopore volume is 0.14mL / g.

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Abstract

The invention relates to a middle hole ZSM-5 zeolite microsphere and a preparation method thereof, which belong to the field of inorganic nonmetallic materials and catalyst preparation. The middle hole ZSM-5 zeolite microsphere is characterized by belonging to a microsphere with intracrystalline middle holes and intercrystalline middle holes and being formed by nanometer zeolites with the intracrystalline middle holes through self aggregation; the diameter of the microspheres is between 4mum and 8mum, the diameter of the nanometer zeolite grain is between 15nm and 50nm, and the diameter of the intracrystalline middle holes is between 3nm and 8nm. The microsphere is synthesized in the hydrothermal crystallization system by using nanometer silicon dioxide with the silanized surface as raw materials. The zeolite microsphere combines the advantages of the nanometer zeolite and the middle hole zeolite, overcomes the defect of difficult separation of the nanometer zeolite in the synthesis and use process and has uniform size, good sphericity degree, high hydrothermal stability and mechanical strength. The porosity of the middle holes can be regulated through changing the mol proportioning ratio of the organic silane coupling agents and silicon dioxide. The use of spherulization agents is avoided, the preparation process is simplified, and the preparation cost is reduced.

Description

technical field [0001] The invention relates to a mesoporous ZSM-5 zeolite microsphere and a preparation method thereof, which belong to the field of preparation of inorganic non-metallic materials and catalysts. Specifically, it relates to a ZSM-5 zeolite microsphere formed by the self-aggregation of nano zeolite grains and a preparation method thereof. Background technique [0002] ZSM-5 zeolite molecular sieve is a high-silica zeolite developed by Mobil Corporation of the United States. Its pore arrangement is characterized by the intersection of straight cylindrical channels and transverse sinusoidal channels. , The cross-section of the sinusoidal channel is approximately circular, with a diameter of 0.55nm. The structural characteristics of ZSM-5 and the corresponding strong acidity and excellent hydrothermal stability endow it with unique catalytic and adsorption properties, and are widely used in petrochemical and other fields. [0003] However, limited by the small...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38
Inventor 马静红李瑞丰薛招腾张拓崔丽萍
Owner TAIYUAN UNIV OF TECH
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