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Multi-stage structure molecular sieve hollow microsphere, preparation methods and application

A technology of hollow microspheres and molecular sieves, which is applied in the field of molecular sieves, can solve the problems of not being able to meet the requirements of high acidity strength for catalytic reactions, weak mechanical strength of multi-level structures, and restricted channel shape selection, etc., to achieve wide application range and strong acidity , no quality loss effect

Active Publication Date: 2016-01-27
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high external specific surface area of ​​hierarchical molecular sieves, severe external surface reactions will occur during application, which limits their channel shape selection.
In addition, the limitation of preparation technology makes the current multi-level structure silicon aluminum ratio unable to meet the requirement of high acid strength for catalytic reaction
Moreover, compared with micron-sized molecular sieves, the hierarchical structure has weaker mechanical strength, which severely limits its practical application.
So far, the preparation of hierarchically structured molecular sieves with rational structures and high acidic strengths remains a challenge.

Method used

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  • Multi-stage structure molecular sieve hollow microsphere, preparation methods and application
  • Multi-stage structure molecular sieve hollow microsphere, preparation methods and application
  • Multi-stage structure molecular sieve hollow microsphere, preparation methods and application

Examples

Experimental program
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Effect test

Embodiment 1

[0036] The tetrapropylammonium hydroxide solution with a mass fraction of 10% was mixed with tetraethyl orthosilicate at a mass ratio of 1:0.3 for 3 hours, and then precrystallized at 100° C. for 48 hours to obtain ZSM-5 molecular sieve seed crystals. Mix ZSM-5 molecular sieve seed crystals, amorphous silica microspheres (0.5 μm outer diameter) and sodium metaaluminate at a mass ratio of 0.1:1:1.7 for 3 hours to make the ZSM-5 molecular sieve crystal seeds evenly adhere on the surface of silica microspheres. Then, the silica microspheres adhered with ZSM-5 molecular sieve seeds were dried at 120° C. for 0.2 hour to obtain dry powder.

[0037] Place a bracket whose height is 3 times the diameter of the hydrothermal kettle in a hydrothermal kettle with a polytetrafluoroethylene liner, and pour a certain amount of water to control the amount of water added to only submerge the bracket. A small container is placed above the support, and the resulting dry powder is put into the sm...

Embodiment 2

[0041] After mixing tetrapropylammonium hydroxide solution with a mass fraction of 50% and tetraethyl orthosilicate at a mass ratio of 1:5 for 1 hour, precrystallization was performed at 100°C for 144 hours to obtain ZSM-5 molecular sieve seed crystals. Mix ZSM-5 molecular sieve seed crystals, amorphous silica microspheres (outer diameter 0.5 μm) and sodium metaaluminate at a mass ratio of 1:10:0.04 for 0.3 hours to make ZSM-5 molecular sieve seed crystals evenly adhere Silica microsphere surface. Then, the silica microspheres adhered with ZSM-5 molecular sieve seeds were dried at 100° C. for 3 hours to obtain dry powder.

[0042] Place a bracket with a height of 0.3 times the diameter of the hydrothermal kettle in a hydrothermal kettle with a polytetrafluoroethylene liner, and pour a certain amount of water to control the amount of water added to only submerge the bracket. Place a small container above the stand, put the dry powder into the small container so that the water ...

Embodiment 3

[0046] After mixing tetrapropylammonium hydroxide solution with a mass fraction of 40% and tetraethylorthosilicate at a mass ratio of 1:1 for 3 hours, precrystallization was performed at 100°C for 72 hours to obtain ZSM-5 molecular sieve seed crystals. Mix ZSM-5 molecular sieve seeds, amorphous silica microspheres (outer diameter 10 μm) and sodium metaaluminate at a mass ratio of 0.5:5:0.8 for 1 hour, so that the ZSM-5 molecular sieve seeds evenly adhere to the Amorphous silica microsphere surface. Then, the silica microspheres adhered with ZSM-5 molecular sieve seeds were dried at 110° C. for 4 hours to obtain dry powder.

[0047] Place a bracket with a height of 1 times the diameter of the hydrothermal kettle in a hydrothermal kettle with a polytetrafluoroethylene liner, and pour a certain amount of water to control the amount of water added to only submerge the bracket. Place a small container above the stand, put the dry powder into the small container so that the water d...

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Abstract

The present invention discloses a multi-stage structure molecular sieve hollow microsphere, preparation methods and application thereof, the molecular sieve hollow microsphere outer diameter is 1-50mum, the inner diameter is 0.5-45mum; inner and outer surfaces are grown with molecular sieve nanometer single crystals directionally growing along the c-axis, the molecular sieve nanometer single crystal diameter is 20-300nm, the molecular sieve nanometer single crystal length is 200-5000nm, the molecular sieve nanometer single crystal and molecular sieve hollow microsphere surface angle is 60-120 degrees; the molecular sieve hollow microsphere includes any one or a plurality of multi-stage structure ZSM-5 molecular sieve hollow microsphere, multi-stage structure beta-type molecular sieve hollow microsphere and multi-stage structure Y-type molecular sieve hollow microsphere; the present invention also discloses preparation methods of the three molecular sieve hollow microspheres, the preparation methods have wide use range, ZSM-5 molecular sieve, beta-type molecular sieve and Y-type molecular sieve can be obtained by the preparation methods, and the cost of the preparation methods is 60-80% lower than that of the method in prior art for preparing corresponding molecular sieves an aqueous solution.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and in particular relates to a molecular sieve hollow microsphere with a multi-level structure, a preparation method and an application thereof. Background technique [0002] Molecular sieves are crystalline silicates or aluminosilicates, which are formed by connecting silicon-oxygen tetrahedrons or aluminum-oxygen tetrahedrons through oxygen bridges. According to the different skeleton structures, it can be divided into ZSM-5, β, Y, X, SAPO and other types. Molecular sieves are widely used in catalysis, petrochemical, adsorption separation, sensors and other fields due to their large specific surface area, unique pore shape selection and good thermal stability. [0003] Molecular sieves are generally produced by self-assembly under the action of template agents under hydrothermal conditions with Si sources and Al sources. In the actual application process, molecular sieves usually nee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 骞伟中王宁魏飞
Owner TSINGHUA UNIV
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