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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

AI Technical Summary

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 stronger basic TPAOH (tetrapropylamine ammonium hydroxide) due to the rapid crystallization, the spherical structure collapses, and the connection between silicon oxides is easy to break, so it cannot be made into a hollow molecular sieve ball

Method used

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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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Effect test

Embodiment 1

[0021] put 10.5 g NaAlO 2 and 56 mL of TPAOH were dissolved in 100 mL of deionized water to obtain a solution with a pH value of about 9, and then weigh the raw material mesoporous silica solid ball 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, transferred to a Buchner funnel with filter paper, and added the previously prepared solution drop by drop to the raw material on the filter paper in the state of suction filtration under reduced pressure. After suction filtration and wetting, it was transferred to a crystallization kettle and crystallized at 170°C for 48 hours. Cool the crystallized slurry to room temperature, and filter the obtained powder under reduced pressure until the pH of the washing liquid is close to neutral; dry at 70°C for 10 hours; then bake at 540°C for 6 hours, the resulting molecular sieve is labeled HS-1, and its pr...

Embodiment 2

[0023] put 2.1 g NaAlO 2 and 28mL TPAOH were dissolved in 50 mL of deionized water to obtain a solution, the pH value of the solution was about 9, and then the raw material (mesoporous silica solid ball molecular sieve with a particle size of 400nm, a pore size of 2.9nm, and a specific surface area 1080m 2 / g, the pore volume is greater than 0.35cm 3 / g) 50 grams, transferred to a Buchner funnel with filter paper, and added the previously prepared solution drop by drop to the raw material on the filter paper in the state of suction filtration under reduced pressure. After suction filtration and wetting, it was transferred to a crystallization kettle and crystallized at 170°C for 48 hours. Cool the crystallized slurry to room temperature, and filter the obtained powder under reduced pressure until the pH of the washing liquid is close to neutral; dry at 70°C for 10 hours; then bake at 540°C for 6 hours, the resulting molecular sieve is labeled HS-2, and its properties are sh...

Embodiment 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 which was about 9, and then the raw material (mesoporous silica solid ball molecular sieve with a particle size of 400 nm and a pore size of 2.9 nm, the ratio Surface area is 1080m 2 / g, the pore volume is greater than 0.35cm 3 / g) 150 grams, transferred to a Buchner funnel with filter paper, and added the previously prepared solution drop by drop to the raw material on the filter paper in the state of suction filtration under reduced pressure. After suction filtration and wetting, it was transferred to a crystallization kettle and crystallized at 170°C for 48 hours. Cool the crystallized slurry to room temperature, and filter the obtained powder under reduced pressure until the pH of the washing liquid is close to neutral; dry at 70°C for 10 hours; then bake at 540°C for 6 hours, the resulting molecular sieve is labeled HS-3, and its properties are shown ...

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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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