Zinc-modified hierarchical pore ZSM-5 nano-zeolite and preparation method thereof

A technology of ZSM-5 and nano-zeolite, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of narrow channel structure, low product selectivity, easy deactivation, etc. To achieve the effect of increasing selectivity

Active Publication Date: 2019-04-12
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of zinc-modified multi-level porous ZSM-5 nano zeolite, solve the problem that traditional zinc-modified ZSM-5 zeolite channel structure is narrow, easily inactivated; The problem of low product selectivity

Method used

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  • Zinc-modified hierarchical pore ZSM-5 nano-zeolite and preparation method thereof
  • Zinc-modified hierarchical pore ZSM-5 nano-zeolite and preparation method thereof
  • Zinc-modified hierarchical pore ZSM-5 nano-zeolite and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of SiO 2 / Al 2 o 3 ZSM-5 nanometer zeolite of 120:

[0036] ① Mix 66.67g of silica sol solution (30% by mass fraction), 17.78g of tetrapropylammonium bromide (TPABr) and 2.08g of seed crystal solution, stir at 35°C for 30 minutes, and define it as solution A;

[0037] ②Mix 1.354g of aluminum chloride hexahydrate with 45g of water, and define it as solution B;

[0038] ③ 30g ethylamine aqueous solution is defined as C solution;

[0039] ④ Add solution B to solution A dropwise, stir at 35°C for 90 minutes, then add solution C dropwise to the mixed solution, continue stirring at 35°C for 30 minutes, crystallize at 170°C for 72 hours, centrifuge, and dry at 80°C. Baking at 540°C.

[0040] Preparation of Zinc Modified ZSM-5 Nano Zeolite

[0041] ① Mix 5 g of the prepared ZSM-5 nano-zeolite with 150 ml of 0.2 mol / L sodium hydroxide aqueous solution, stir for 30 minutes at 80°C, centrifuge, and dry at 80°C.

[0042] ② Mix 0.37g of zinc nitrate hexahydrate wi...

Embodiment 2

[0050] Preparation of SiO 2 / Al 2 o 3 ZSM-5 nano zeolite of 160:

[0051] ① Mix 66.67g of silica sol solution (30% by mass fraction), 17.78g of tetrapropylammonium bromide (TPABr) and 2.08g of seed crystal solution, stir at 35°C for 30 minutes, and define it as solution A;

[0052] ② Mix 1.016g of aluminum chloride hexahydrate with 45g of water, and define it as solution B;

[0053] ③ 30g ethylamine aqueous solution is defined as C solution;

[0054] ④ Add solution B to solution A dropwise, stir at 35°C for 90 minutes, then add solution C dropwise to the mixed solution, continue stirring at 35°C for 30 minutes, crystallize at 170°C for 72 hours, centrifuge, and dry at 80°C. Baking at 540°C.

[0055] 5. Preparation of zinc-modified ZSM-5 nanometer zeolite Zn-2, same as in Example 1.

[0056] Figure 7 It is a TEM image of the zinc-modified ZSM-5 nano zeolite of Example 2 of the present invention. It can be seen from the figure that samples with different silicon-aluminu...

Embodiment 3

[0058] Preparation of SiO 2 / Al 2 o 3 ZSM-5 nano zeolite of 135:

[0059] ① Mix 66.67g of silica sol solution (30% by mass fraction), 17.78g of tetrapropylammonium bromide (TPABr) and 2.08g of seed crystal solution, stir at 35°C for 30 minutes, and define it as solution A;

[0060] ②Mix 0.813g of aluminum chloride hexahydrate with 45g of water, and define it as B solution;

[0061] ③ 30g ethylamine aqueous solution is defined as C solution;

[0062] ④ Add solution B to solution A dropwise, stir at 35°C for 90 minutes, then add solution C dropwise to the mixed solution, continue stirring at 35°C for 30 minutes, crystallize at 170°C for 72 hours, centrifuge, and dry at 80°C. Baking at 540°C.

[0063] The preparation of zinc-modified ZSM-5 nano zeolite Zn-3 is the same as in Example 1.

[0064] Figure 8 It is a TEM image of the zinc-modified ZSM-5 nano zeolite of Example 3 of the present invention. It can be seen from the figure that samples with different silicon-alumin...

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Abstract

The invention provides a zinc-modified hierarchical pore ZSM-5 nano-zeolite. ZSM-5 nano-zeolite has a hierarchical pore structure internally, and zinc particles are coated inside the ZSM-5 nano-zeolite. The invention also provides a preparation method of the catalyst. The method includes: mixing nano-ZSM-5 zeolite with a sodium hydroxide aqueous solution to obtain hierarchical pore ZSM-5 nano-zeolite, subjecting the hierarchical pore ZSM-5 nano-zeolite to ammonium exchange, conducting zinc impregnation, then utilizing silica sol for strip extrusion, and then conducting dry gel conversion, thusobtaining the zinc-modified hierarchical pore ZSM-5 nano-zeolite. The zinc-modified hierarchical pore ZSM-5 nano-zeolite provided by the invention has a hierarchical pore structure, and the zinc particles are coated inside the ZSM-5 nano-zeolite, thus solving the problems of narrow pore channel and easy inactivation of traditional zinc-modified ZSM-5 zeolite in methanol-to-aromatics reaction, andalso solving the problem of low aromatic hydrocarbon selectivity of zinc-modified mesoporous ZSM-5 zeolite.

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis, in particular to a preparation method of zinc-modified ZSM-5 nanometer zeolite. Background technique [0002] Zeolite molecular sieves have been widely used in the fields of adsorption, separation and catalysis because of their large specific surface area, excellent shape-selective properties, and good hydrothermal stability. In many reactions, using only ZSM-5 zeolite as catalyst, the selectivity of the target product is low. To solve this problem, people use zinc-modified ZSM-5 zeolite. This method can effectively improve the selectivity of aromatics in the methanol-to-aromatics reaction, so it has attracted the attention of researchers. However, due to the narrow pore structure of ZSM-5 zeolite, the catalyst is easily deactivated. Although the introduction of mesopores on the modified ZSM-5 zeolite can effectively solve this problem, it will reduce the selectivity of aromatics. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
CPCC01B39/38C01P2004/03C01P2004/04C01P2002/72C01P2004/62
Inventor 刘民郭新闻崔滕
Owner DALIAN UNIV OF TECH
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