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Method for preparing ZSM-5 zeolite in small crystal grain

A ZSM-5, small grain technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high cost, large amount of template agent, long crystallization time, etc. , to reduce the dosage, speed up the crystallization speed, and achieve the effect of good technical effect

Active Publication Date: 2007-02-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that there are problems such as large amount of template agent, long crystallization time and high cost in the prior art, and a new method for preparing small crystal grain ZSM-5 zeolite is provided

Method used

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  • Method for preparing ZSM-5 zeolite in small crystal grain
  • Method for preparing ZSM-5 zeolite in small crystal grain
  • Method for preparing ZSM-5 zeolite in small crystal grain

Examples

Experimental program
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Effect test

Embodiment 1～3

[0019] Seed directing agent: Tetrapropylammonium hydroxide (TPAOH) solution and tetraethyl orthosilicate (TEOS) are used as raw materials, and the molar ratio is (TPA) 2 O: 5.5 TEOS: 90H 2 The mixture of O was stirred overnight at room temperature to mix uniformly, and then aged at 80 °C for 72 hours to prepare the seed directing agent.

[0020] Using silica sol and aluminum sulfate as raw materials, the molar ratio of the crystallization reaction mother liquor is 28 Na 2 O: 1.5 Al 2 o 3 : 100SiO2 2 : 4000H 2 O, add 10% of its weight seed crystal directing agent to the crystallization reaction mother liquor, the reaction system is reacted in 300 milliliter crystallization tank at 180 ℃ for 10 hours, 12 hours and 14 hours, the XRD pattern of the product shows that the product is high crystallinity ZSM-5 zeolite, SEM characterization results show that the zeolite particle size is about 100 nanometers, and its BET specific surface area is greater than 360 square meters per g...

Embodiment 4～6

[0022] Using silica sol and aluminum sulfate as raw materials, the molar ratio of the crystallization reaction mother liquor is 28 Na 2 O: 1.5Al 2 o 3 : 100SiO2 2 : 4000H 2 O, add its weight 2.7% seed crystal directing agent described in Example 1 to the crystallization reaction mother liquor, and the reaction system was reacted in a 300 milliliter crystallization kettle at 180° C. for 10 hours, 12 hours and 14 hours, and the XRD spectrum of the product showed The product is ZSM-5 zeolite with high crystallinity, and the SEM characterization result shows that the particle size of the zeolite is 100-200 nanometers.

Embodiment 7～9

[0024] Using silica sol and aluminum sulfate as raw materials, the molar ratio of the crystallization reaction mother liquor is 28 Na 2 O: 1.5 Al 2 o 3 : 100SiO2 2 : 4000H 2O, add its weight 1.0% seed crystal directing agent described in Example 1 to the crystallization reaction mother liquor, and the reaction system reacts in a 300 milliliter crystallization kettle at 180° C. for 10 hours, 12 hours and 14 hours, and the XRD spectrum of the product shows The product is ZSM-5 zeolite with high crystallinity, and the SEM characterization result shows that the particle size of the zeolite is 100-250 nanometers.

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Abstract

This invention relates to a method for preparing ZSM-5 zeolite with fine grains. The method comprises: (1) adopting water glass, silica sol or white carbon black as the Si source, and Al salt or aluminate as the Al source with Na2O : Al2O3 : SiO2 : H2O = (4-36) : (0-3) : 100 : (1400-6000); (2) adding a small amount of crystal seed directing-agent into the crystallization mother liquid; (3) crystallizing to obtain ZSM-5 zeolite with fine grains. The method solves the problems of large amounts of templating agent, long crystallization time, and serious environmental pollution, and can be used in industrial manufacture of ZSM-5 zeolite.

Description

technical field [0001] The present invention relates to a method for preparing small crystal grain ZSM-5 zeolite. Background technique [0002] Zeolite molecular sieve is the most important class of crystalline microporous materials. It has uniform and ordered micropores, large specific surface area, high hydrothermal stability, good ion exchange performance and rich and adjustable surface physical and chemical properties. It is widely used In the fields of catalysis, adsorption, ion exchange and functional materials. However, with the development of fine chemical industry, large-grain zeolite materials cannot achieve the expected catalytic effect in reactions involving macromolecules or liquid phases due to their narrow pores and high diffusion resistance. The zeolite molecular sieve with small crystal grains can provide more active sites due to its large external specific surface area and high intracrystalline diffusion rate, and the reactant m...

Claims

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Application Information

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IPC IPC(8): C01B39/38C01B39/40
Inventor 王德举刘仲能李道贵侯闽渤
Owner CHINA PETROLEUM & CHEM CORP
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