High silica/ aluminum ratio octagonal zeolite synthesizing method

A faujasite and synthesis method technology, applied in the direction of crystalline aluminosilicate zeolite, faujasite crystalline aluminosilicate zeolite, etc., can solve the problem of inability to combine crystallinity with amorphous silicon, low skeleton silicon-aluminum ratio, water/oxidation Low silicon ratio and other problems, to achieve the effect of improving synthesis efficiency, short synthesis time, and low sodium content

Active Publication Date: 2007-04-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ratio of water / silicon oxide synthesized in this patent is very low, requiring no more than 6, so the amorphous silicon in the raw material cannot be well combined into the molecular sieve framework and ensure good crystallinity
The amount of alkali used in this patented method is relatively large, such as M in the feeding + / SiO 2 =0.2-1.0 (molar ratio), M + It is an alkali metal, and the amount of alkali is converted to Na 2 O / SiO 2 The molar ratio of the zeolite is 0.4-2.0. Although the amount of alkali is too high, although it is beneficial to the formation of Y-type zeolite, it will lead to a sharp decline in the silicon-aluminum ratio of the product. The actual skeleton silicon-aluminum ratio of the zeolite product obtained by this method is generally not high.
[0008] US5549881 discloses a method for preparing faujasite. This patent also uses an organic template to synthesize a certain molecular sieve composite with the structural characteristics of faujasite, but it still uses the need to add some sodium aluminosilicate crystal seeds, and Crystallization time up to 8-14 days

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] Using silica sol as a silicon source, sodium aluminate as an aluminum source, and tetrapropylammonium hydroxide as a template, the zeolite of the invention is synthesized by hydrothermal crystallization. Reactant ingredients molar ratio: n(SiO 2 ): n(Na 2 O):n(template):n(Al 2 o 3 ):n(H 2 (0)=6:1.8:1.2:1:110. Synthesis method: according to the proportion of reactants, add sodium hydroxide and sodium aluminate into 25% tetrapropyl ammonium hydroxide solution, mix well and then add silica sol. After the above mixture was stirred at 50°C for 24 hours, it was transferred into an autoclave with polytetrafluoroethylene, sealed, and statically crystallized at 100°C for 120h. After the crystallization is completed, the product is filtered, washed with water, dried at 110°C, and then calcined at 550°C to remove the template agent to obtain the sample of the present invention.

example 2

[0026] Using silica sol as a silicon source, sodium aluminate as an aluminum source, and tetrabutylammonium hydroxide as a template, the zeolite of the invention is synthesized by hydrothermal crystallization. Reactant ingredients molar ratio: n(SiO 2 ): n(Na 2 O):n(template):n(Al 2 o 3 ):n(H 2(0) = 12:3.5:0.8:1:180. Synthesis method: according to the ratio of reactants, add sodium hydroxide and sodium aluminate into water, then add 25% tetrabutylammonium hydroxide solution, mix well, and then add silica sol. The above mixture was stirred at 60°C for 6 hours, then aged at room temperature for 24 hours, moved into an autoclave with polytetrafluoroethylene, sealed, and statically crystallized at 110°C for 180h. After the crystallization is completed, the product is filtered, washed with water, dried at 110°C, and then calcined at 550°C to remove the template agent to obtain the sample of the present invention.

example 3

[0028] Using water glass and silica sol as a mixed silicon source, sodium aluminate as an aluminum source, and tetraethylammonium hydroxide as a template, the zeolite of the invention is synthesized by hydrothermal crystallization. Reactant ingredients molar ratio: n(SiO 2 ): n(Na 2 O):n(template):n(Al 2 o 3 ):n(H 2 (0)=16:4.0:2.5:1:320. Synthesis method: according to the proportion of reactants, add sodium aluminate to 35% tetraethylammonium hydroxide solution, mix well, then add silica sol and water glass (the silicon source provided by both is 2:1). After the above mixture was stirred at 30°C for 3 hours, it was placed at room temperature for 48 hours, then moved into an autoclave with polytetrafluoroethylene, sealed, statically crystallized at 120°C for 18 hours, and dynamically (stirring speed 200 rpm) Crystallized for 54h. After the crystallization is completed, the product is filtered, washed with water, dried at 110°C, and then calcined at 550°C to remove the tem...

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PUM

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Abstract

The invention discloses a synthesizing method of high-silicon aluminium rate octahedra zeolite, which is characterized by the following: adopting moulding agent to synthesize the product through hydrothermal crystallizing method under fitful sodium condition directly.

Description

technical field [0001] The invention relates to a method for synthesizing faujasite, in particular to a method for synthesizing high-silicon-aluminum ratio faujasite under hydrothermal conditions. Background technique [0002] Zeolite molecular sieves are regular crystal structures with unique pore structures, mainly crystalline aluminosilicates. Zeolite molecular sieves come in many varieties, each with pores of a specific size and shape. Zeolite molecular sieves form a ring structure from silicon-oxygen tetrahedrons or aluminum-oxygen tetrahedrons through oxygen bridges, and then further link into various cage structures. Faujasite (FAU-type zeolite) is composed of β cages and hexagonal column cages, and it gets its name from the faujasite cages surrounded by them. Faujasite includes X-type and Y-type. The difference between the two lies in the aluminum content, that is, the silicon-aluminum ratio (SiO 2 / Al 2 o 3 ) is different, generally the X type is about 2-3, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/20
Inventor 陈松张晓萍刘利军谷明镝
Owner CHINA PETROLEUM & CHEM CORP
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