Preparation method of micropore hollow ball molecular sieve

A molecular sieve and hollow sphere technology, used in molecular sieve catalysts, chemical instruments and methods, refining to remove heteroatoms, etc., can solve the problems of spherical structure collapse, easy fracture of silicon oxide connections, and inability to make hollow molecular sieve spheres. The effect of reduced losses

Active Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method adopts the method of hydrothermal crystallization, and the hollow ZSM-5 molecular sieve ball can be made by using the weaker basic isopropylamine as the structure directing agent, and it is also pointed out in the article that the

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  • Preparation method of micropore hollow ball molecular sieve
  • Preparation method of micropore hollow ball molecular sieve
  • Preparation method of micropore hollow ball molecular sieve

Examples

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Example Embodiment

[0020] Example 1

[0021] Put 10.5 g NaAlO 2 Dissolve 56 mL TPAOH in 100 mL deionized water to obtain a solution. The pH of the solution is about 9, and then weigh the raw mesoporous silica solid spherical molecular sieve (Properties: particle size is 400nm, average pore diameter is 2.9nm , The specific surface area is 1080m 2 / g, the pore volume is greater than 0.35cm 3 / g) 100 grams, transfer to a Buchner funnel with filter paper, and add the previously prepared solution dropwise to the raw material on the filter paper under vacuum filtration. After suction filtration and wetting, it was transferred to a crystallization kettle and crystallized at 170°C for 48 hours. The crystallization slurry was cooled to room temperature, and the powder obtained was filtered under reduced pressure until the pH value of the washing solution was close to neutral; drying was performed at 70°C for 10 hours; and then calcined at 540°C6 Hours, the obtained molecular sieve is labeled HS-1, and the ...

Example Embodiment

[0022] Example 2

[0023] Put 2.1 g NaAlO 2 Dissolve 28mL TPAOH in 50mL deionized water to obtain a solution. The pH value of the solution is about 9, and then weigh the raw materials (Mesoporous silica solid spherical molecular sieve, particle size of 400nm, pore size of 2.9nm, specific surface area 1080m 2 / g, the pore volume is greater than 0.35cm 3 / g) 50 grams, transfer to a Buchner funnel with filter paper, and add the previously prepared solution dropwise to the raw material on the filter paper under vacuum filtration. After suction filtration and wetting, it was transferred to a crystallization kettle and crystallized at 170°C for 48 hours. The crystallization slurry was cooled to room temperature, and the powder obtained was filtered under reduced pressure until the pH value of the washing solution was close to neutral; drying was performed at 70°C for 10 hours; and then calcined at 540°C6 Hours, the obtained molecular sieve is labeled HS-2, and the properties are shown...

Example Embodiment

[0024] Example 3

[0025] Put 2.1 g NaAlO 2 And 84 mL of TPAOH were dissolved in 150 mL of deionized water to obtain a solution. The pH of the solution was about 9, and then weigh the raw materials (mesoporous silica solid sphere molecular sieve, with a particle size of 400 nm and a pore size of 2.9 nm. Surface area is 1080m 2 / g, the pore volume is greater than 0.35cm 3 / g) 150 grams, transfer to a Buchner funnel with filter paper, and add the previously prepared solution dropwise to the raw material on the filter paper under vacuum filtration. After suction filtration and wetting, it was transferred to a crystallization kettle and crystallized at 170°C for 48 hours. The crystallization slurry was cooled to room temperature, and the powder obtained was filtered under reduced pressure until the pH value of the washing solution was close to neutral; drying was performed at 70°C for 10 hours; and then calcined at 540°C6 Hours, the obtained molecular sieve is labeled HS-3, and the ...

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Abstract

The invention discloses a preparation method of a hollow ball ZSM-5 molecular sieve. The preparation method comprises the following steps: mixing TPAOH, NaAlO2, and water according to a specific ratio so as to prepare a solution, controlling the pH value of the solution in a range of 8 to 10, in a condition of reduced pressure suction filtration, dropwise adding the solution into mesoporous silicon dioxide solid ball molecular sieve dry glue, carrying out a suction filtration treatment and a wetting treatment, carrying out crystallization reactions for 1 to 2 days at a temperature of 160 to 180 DEG C, filtering and washing the crystallized slurry, and finally drying and burning so as to obtain the hollow ball ZSM-5 molecular sieve. The preparation method has the advantages of simple synthesis steps, easily-controllable operation process, cheap raw material, and little preparation time. The prepared molecular sieve can be applied to an FCC gasoline selective hydro-desulfurization process, has a very good olefin protection characteristic, and can maximally reduce the loss of gasoline octane value.

Description

technical field [0001] The invention relates to a preparation method of a microporous hollow sphere molecular sieve, in particular to a preparation method of a microporous hollow sphere molecular sieve with a ZSM-5 structure. The molecular sieve is especially suitable for FCC gasoline selective hydrodesulfurization catalyst. Background technique [0002] In recent years, people are more and more interested in the preparation of hollow spherical molecular sieves. Because there is a relatively large cavity inside the hollow spherical molecular sieve, although the shell isolates the internal cavity from the external environment, the micropores or mesopores on the surface of the shell can still provide channels for molecules to enter and exit the cavity. Because of this unique structure, hollow spherical molecular sieves are placed with special hopes in the fields of catalysis, adsorption, acoustics, optics, electromagnetics, and heat. [0003] Usually, hollow sphere molecular...

Claims

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Application Information

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IPC IPC(8): C01B39/40B01J29/40C10G45/08
Inventor 张金昌杨成敏丁莉尹泽群王继锋
Owner CHINA PETROLEUM & CHEM CORP
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