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Preparation method of W-SSZ-13 zeolite with high crystallinity and high hydrophobicity

A technology of W-SSZ-13 and high hydrophobicity, applied in the field of preparation of W-SSZ-13 zeolite, can solve problems such as difficulty in synthesizing heteroatom zeolite, and achieve the effects of reducing synthesis cost, shortening crystallization time, and lowering reaction temperature

Active Publication Date: 2020-04-03
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Generally, the incorporation of heteroatoms through the framework of zeolites will improve their performance, but it is difficult to synthesize heteroatom zeolites by one-step method

Method used

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  • Preparation method of W-SSZ-13 zeolite with high crystallinity and high hydrophobicity
  • Preparation method of W-SSZ-13 zeolite with high crystallinity and high hydrophobicity
  • Preparation method of W-SSZ-13 zeolite with high crystallinity and high hydrophobicity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Synthesis of fully crystalline SSZ-13

[0025] First, dissolve 0.22g of sodium metaaluminate in 19.7mL of water, stir for 15min to make the solution clear, weigh 0.12g of sodium hydroxide into the solution, stir for 5min, measure 4.8mL of N, N-trimethyl 1-adamantane aqueous solution of ammonium hydroxide (25%), stirring for 15 min. Finally, 3.5 mL of silica sol (30%) was measured and stirred for 4 hours. The aging solution was put into the reaction kettle and reacted hydrothermally at 160°C for 4 days. The sample was centrifuged and washed with water and dried at 110°C for 12 hours.

Embodiment 2

[0026] Example 2: Synthesis of incompletely crystalline SSZ-13 zeolite

[0027] First, dissolve 0.22g sodium metaaluminate in 19.7mL water, stir for 15min to make the solution clear, weigh 0.12g sodium hydroxide into the solution, stir for 5min, measure 4.8mL N, N-trimethyl-1- Adamantane ammonium hydroxide aqueous solution (25%). Stir for 15min. Finally, measure 3.5 mL of silica sol (30%) and stir for 4 hours. The aging solution was put into the reaction kettle and reacted hydrothermally at 160°C for 1 day. The sample was centrifuged and washed with water and dried at 110°C for 12 hours.

Embodiment 3

[0028] Example 3: Synthesis of incompletely crystalline SSZ-13 zeolite doped with tungsten

[0029] First, dissolve 0.22g of sodium metaaluminate in 19.7mL of water, stir for 15min to make the solution clear, weigh 0.12g of sodium hydroxide into the solution, stir for 5min, measure 4.8mL of N, N-trimethyl-1 -Amantadine ammonium hydroxide aqueous solution (25%), stir for 15 min. Weigh 0.037g of sodium tungstate into the solution and stir for 15 minutes. Finally, 3.5 mL of silica sol (30%) was measured and stirred for 4 hours. In the future, the aging solution will be put into the reaction kettle, and hydrothermally reacted at 160°C for 1 day. The sample was centrifuged and washed with water and dried at 110°C for 12 hours.

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Abstract

The invention belongs to the technical field of preparation of heteroatom-containing zeolite materials, and particularly relates to a preparation method of W-SSZ-13 zeolite with high crystallinity andhigh hydrophobicity. According to the method, tungsten ions are doped into an SSZ-13 zeolite synthesis system, so that the zeolite crystallization process is promoted, the crystallization temperatureis reduced, and the crystallization time is shortened. The preparation method comprises the following specific preparation steps: sequentially adding water, an alkali source, an organic template agent, a silicon source, a tungsten source and the like into a container; stirring the substances well; putting the container into a reaction kettle, and carrying out crystallization for 1-4 days at 100-200 DEG C; and centrifugally washing a product for multiple times, and drying the product at 80-110 DEG C. Under the same reaction conditions, the crystallinity of the W-SSZ-13 zeolite is higher than that of the SSZ-13 zeolite, which indicates that the addition of tungsten ions can promote the crystallization of the zeolite and tungsten atoms can enter the framework structure of the zeolite. The W-SSZ-13 zeolite shows excellent hydrophobic performance, is high in organic matter adsorption capacity and has a wide application prospect in the fields of catalysis and adsorption.

Description

Technical field [0001] The invention belongs to the technical field of preparation of heteroatom-containing zeolite materials, and specifically relates to a preparation method of W-SSZ-13 zeolite. Background technique [0002] SSZ-13 zeolite is a microporous molecular sieve with a chabazite (CHA) structure. It has a high silicon-to-aluminum ratio and an eight-membered ring-shaped crystal structure. The framework contains A1O 4 And SiO 4 Tetrahedrons are connected end to end through oxygen atoms, and Al-(OH)-Si bridged hydroxyl groups can be formed at the adjacent oxygen atoms, so that the skeleton has a certain acidity and cation exchange. [0003] Generally, zeolite incorporates heteroatoms through the framework to improve its performance, but it is difficult to synthesize heteroatom zeolites by one-step method. Ren et al. used Cu-tetraethylenepentamine complex (Cu-TEPA) as a structure directing agent to synthesize Cu-SSZ-13 by a one-step method, which has good NH 3 -SCR catalytic...

Claims

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Application Information

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IPC IPC(8): C01B39/48
CPCC01B39/48C01P2004/04
Inventor 程晓维邓勇辉
Owner FUDAN UNIV
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