Hollow molecular sieve fiber and preparation method thereof

A molecular sieve and solid fiber technology, applied in the direction of octahedral crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc. Control the effective hollow structure morphology, the harsh requirements of molecular sieve components, etc., to achieve the effect of good reaction and separation performance, fast speed and simple method

Active Publication Date: 2015-06-17
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is simple, only single-crystal hollow ZSM-5 molecular sieves can be obtained, and the requirements for the composition of the molecular sieves are relatively strict, and the morphology of the effective hollow structure cannot be controlled.
The mass loss of molecular sieve is large, and the preparation cost is high
At the same time, none of these methods can obtain a hollow molecular sieve structure with a large macroscopic size.

Method used

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  • Hollow molecular sieve fiber and preparation method thereof
  • Hollow molecular sieve fiber and preparation method thereof
  • Hollow molecular sieve fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] After mixing tetrapropylammonium hydroxide solution with a mass fraction of 25% and tetraethylorthosilicate at a mass ratio of 1:0.9 for 3 hours, pre-crystallized at 100°C for 48 hours to obtain ZSM-5 molecular sieve seed crystals. The total mass fraction of silicon and oxygen in the solid fiber containing silicon and oxygen elements is 100%, the outer diameter is 8 μm, and the aspect ratio is 20:1 (hereinafter referred to as the solid fiber). The ZSM-5 molecular sieve crystal seed, the solid fiber Mix with sodium metaaluminate at a molar ratio of 100:10:10 for 3 hours to make the ZSM-5 molecular sieve seeds evenly adhere to the surface of the solid fiber, then remove it and dry at 120°C for 0.2 hours to obtain a dry powder .

[0044] Place a support with a height of 3 times the diameter of the hydrothermal kettle in a hydrothermal kettle with a polytetrafluoroethylene liner, and pour water into it to control the amount of water added to just submerge the bracket, place...

Embodiment 2

[0048] After mixing tetrapropylammonium hydroxide solution with a mass fraction of 50% and tetraethylorthosilicate at a mass ratio of 3:1 for 1 hour, pre-crystallized at 120°C for 72 hours to obtain ZSM-5 molecular sieve seed crystals. The total mass fraction of silicon and oxygen in the solid fiber containing silicon and oxygen elements is 80% (other components are sodium and calcium elements), the outer diameter is 0.5 μm, and the aspect ratio is 1000:1 (hereinafter referred to as solid fiber). Mix the ZSM-5 molecular sieve crystal seed, solid fiber and sodium metaaluminate at a molar ratio of 20:5:0.5 for 0.3 hours, so that the ZSM-5 seed crystal evenly adheres to the surface of the solid fiber, then pull it out, and Dry at 100°C for 3 hours to obtain dry powder.

[0049] Place a support with a height of 0.3 times the diameter of the hydrothermal kettle in a hydrothermal kettle with a polytetrafluoroethylene liner, and pour in water, control the amount of water added to jus...

Embodiment 3

[0052] After mixing tetrapropylammonium hydroxide solution with a mass fraction of 40% and tetraethylorthosilicate at a mass ratio of 1:1 for 3 hours, pre-crystallized at 105°C for 72 hours to obtain ZSM-5 molecular sieve seed crystals. The total mass fraction of silicon and oxygen in the solid fiber containing silicon and oxygen is 90% (others are potassium, aluminum, iron), the outer diameter is 2 μm, and the aspect ratio is 200:1 (hereinafter referred to as solid fiber). Mix the ZSM-5 molecular sieve crystal seed, solid fiber and sodium metaaluminate at a molar ratio of 10:5:0.1 for 1 hour, so that the ZSM-5 molecular sieve seed crystal evenly adheres to the surface of the solid fiber, and then remove it , and dried at 110° C. for 1 hour to obtain dry powder.

[0053] Place a support with a height of 1 times the diameter of the hydrothermal kettle in a hydrothermal kettle with a polytetrafluoroethylene liner, and pour water, control the amount of water added to just submerg...

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Abstract

The invention relates to a hollow molecular sieve fiber and a preparation method thereof. The external diameter of the hollow molecular sieve fiber is 1-30 mu m, the internal diameter is 0.5-20 mu m, the length-diameter ratio is 20:1-1000:1, and the specific area is 350-700 m<2> / g. The preparation method comprises the following steps: attaching a small amount of molecular sieve crystal seed to a solid silicon-oxygen-containing fiber used as a silicon source; and by using a steam reforming process, generating a molecular sieve film layer on the solid fiber surface, growing the molecular sieve microcrystal in the normal direction of the molecular sieve film surface, and finally, gradually emigrating the silicon source from inside to form the hollow fiber. The method is suitable for preparing ZSM-5-type, beta-type, Y-type, titanium-silicon-type and other molecular sieves. The preparation method is simple; and the product has the advantages of high purity, complete structure and high mechanical strength, and is suitable to be used as a film separation material or a catalyst for catalytic reaction.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves and their preparation, and in particular relates to a hollow molecular sieve fiber and a preparation method thereof. Background technique [0002] Molecular sieves are a class of porous substances with regular channels and sizes, and are widely used in catalytic reaction processes and adsorption separation processes. According to the different skeleton structures, it can be divided into ZSM-5, β, Y, X, SAPO and other types. Such substances are generally generated by self-assembly under the action of a template agent under a hydrothermal environment using a Si source and an Al source. [0003] However, the molecular sieves prepared by most methods are nano- or micro-sized crystals, and generally the absolute size is not greater than 100 μm. In actual use, molecular sieves need to be molded together with other ingredients to make macroscopic particles. The presence of other components in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38C01B39/24C01B39/08
Inventor 骞伟中沈葵魏飞
Owner TSINGHUA UNIV
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