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Zinc modified hierarchical porous zsm-5 nano zeolite and preparation method thereof

A ZSM-5, nano-zeolite technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of narrow pore structure, low product selectivity, easy deactivation, etc. To achieve the effect of prolonging the life of the catalyst

Active Publication Date: 2022-06-17
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 porous zsm-5 nano zeolite and preparation method thereof
  • Zinc modified hierarchical porous zsm-5 nano zeolite and preparation method thereof
  • Zinc modified hierarchical porous 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 Nano Zeolite for 120:

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

[0037] ② Mix 1.354g of aluminum chloride hexahydrate with 45g of water to define solution B;

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

[0039] ④ Add solution B dropwise to solution A, 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 72h, centrifuge, and dry at 80°C. 540 ℃ roasting.

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

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

[0042] ② Mix 0.37 g of zinc nitrate hexahydrate with an appropriate amo...

Embodiment 2

[0050] Preparation of SiO 2 / Al 2 O 3 ZSM-5 Nano Zeolite for 160:

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

[0052] ② Mix 1.016g of aluminum chloride hexahydrate with 45g of water to define solution B;

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

[0054] ④ Add solution B dropwise to solution A, 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 72h, centrifuge, and dry at 80°C. 540 ℃ roasting.

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

[0056] Figure 7 It is the 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 the samples with different Si / Al ratios will form cavitie...

Embodiment 3

[0058] Preparation of SiO 2 / Al 2 O 3 ZSM-5 Nano Zeolite for 135:

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

[0060] ② Mix 0.813g of aluminum chloride hexahydrate with 45g of water to define solution B;

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

[0062] ④ Add solution B dropwise to solution A, 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 72h, centrifuge, and dry at 80°C. 540 ℃ roasting.

[0063] The zinc-modified ZSM-5 nano-zeolite Zn-3 was prepared as in Example 1.

[0064] Figure 8 It is the 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 the samples with different Si / Al ratios will form cavities i...

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Abstract

The invention provides a zinc-modified hierarchical porous ZSM-5 nano zeolite. The ZSM-5 nano zeolite has a hierarchical pore structure inside, and zinc particles are coated inside the ZSM-5 nano zeolite. The present invention also provides a preparation method of the catalyst, mixing nanometer ZSM‑5 zeolite with aqueous sodium hydroxide solution to obtain hierarchically porous ZSM‑5 nanometer zeolite, performing ammonium exchange on the hierarchically porous ZSM‑5 nanometer zeolite, impregnating zinc, Then, the silica sol is used to extrude and convert through dry gel to obtain the zinc-modified hierarchical porous ZSM‑5 nanometer zeolite. The zinc-modified hierarchically porous ZSM-5 nano zeolite of the present invention has a hierarchical porous structure, and zinc particles are coated inside the ZSM-5 nano-zeolite, which not only solves the problem of the traditional zinc-modified ZSM-5 zeolite in the methanol-to-aromatics reaction The problem of narrow channels and easy deactivation also solves the problem of low selectivity for zinc-modified mesoporous ZSM-5 zeolite aromatics.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(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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