Core-shell structure zeolite multilevel ordered mesopore and micropore composite material and preparation method thereof

A composite material and shell structure technology, applied in the direction of crystalline aluminosilicate zeolites, chemical instruments and methods, molecular sieve catalysts, etc., to achieve the effect of product structure stability

Inactive Publication Date: 2007-10-17
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above materials show good catalytic performance in certain reactions, such as vacuum oil cracking, the mesoporous and microporous molecular sieve materials that are close in structure to mechanical mixing cannot overcome their respective shortcomings and give full play to the advantages of mesoporous and microporous molecular sieves. Synergy

Method used

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  • Core-shell structure zeolite multilevel ordered mesopore and micropore composite material and preparation method thereof
  • Core-shell structure zeolite multilevel ordered mesopore and micropore composite material and preparation method thereof
  • Core-shell structure zeolite multilevel ordered mesopore and micropore composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Ni-Al alloy was gradually added to 90° C. sodium silicate aqueous solution and stirred for 2 hours to extract aluminum in the Ni-Al alloy. Then add ethylamine and concentrated sulfuric acid under vigorous stirring, and adjust the pH=9.6, the molar composition of the entire reaction solution is SiO 2 :Na 2 O:Ni:Al:C 2 h 5 NH 2 :H 2 SO 4 :H 2 O=1:1:0.22:0.48:1.26:0.63:19. After the reaction solution was evenly stirred, it was put into a reaction kettle, sealed, crystallized at 180°C for 8 days, suction filtered, washed with water until neutral, dried at room temperature, and then calcined at 550°C for 6 hours. The obtained product corresponds to the characterization results shown in Figures 1-4.

Embodiment 2

[0018] Example 2: Gradually add Ni-Al alloy into sodium silicate aqueous solution at 100° C. and vigorously stir for 1 hour to extract aluminum in Ni-Al alloy. Then add ethylamine and concentrated sulfuric acid under vigorous stirring, and adjust the pH=10, the molar composition of the entire reaction solution is SiO 2 :Na 2 O:Ni:Al:C 2 h 5 NH 2 :H 2 SO 4 :4H 2 O=1:1:0.22:0.48:1.34:0.63:24. After the reaction solution was evenly stirred, it was put into a reaction kettle, sealed, crystallized at 200°C for 72 hours, filtered with suction, washed with water until neutral, dried at room temperature, and then calcined at 600°C for 3 hours. The obtained product corresponds to the characterization results in Figure 1 and Figure 5a.

Embodiment 3

[0019] Example 3: Ni-Al alloy was gradually added to 95° C. sodium silicate aqueous solution and vigorously stirred for 1.5 h to extract aluminum in the Ni-Al alloy. Then add ethylamine and concentrated sulfuric acid under vigorous stirring, and adjust the pH=9.8, the molar composition of the entire reaction solution is SiO 2 :Na 2 O:Ni:Al:C 2 h 5 NH 2 :H 2 SO 4 :H 2 O=1:1:0.22:0.48:1.30:0.63:22. After the reaction solution was evenly stirred, it was put into a reaction kettle, sealed, crystallized at 150°C for 14 days, filtered with suction, washed with water until neutral, dried at room temperature, and then calcined at 550°C for 6 hours. The obtained product corresponds to the characterization results in Figure 1 and Figure 6b.

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Abstract

The invention belongs to the field of media-micro-hole composite materials techniques. In particular, the invention relates to a shell-core structured zeolite multi-layered media-micro-hole composite material and method for preparing same. The material is a regular polyhedron in appearance and has shell-core structure. The polyhedron shell is of single-crystal structure and the core is piled up by nano-crystals, and the material also has the inherent micro-holes of the zeolite molecular screen and the media-holes produced by piling up of the nano-crystal. Therefore, the material has the media-micro-hole two hole-channels compound holes structure. The invention uses NaSiO3 as the silica source, the metal Al extracted from Ni / Al alloy by the NaSiO3 as the aluminum source and athylamine and the residue Raney Ni of Ni / Al alloy extraction as the auxiliary. The material is obtained by crystallizing the zeolite synthesizing solution in the regular crystallization condition and the shell thickness of the single-crystal and the core nano-crystal appearance can be controlled by crystallization temperature and time.

Description

technical field [0001] The invention belongs to the technical field of mesoporous and microporous composite materials, and in particular relates to a core-shell structure analcite (ANA) multilevel ordered mesoporous composite material and a preparation method thereof. Background technique [0002] According to the definition of the International Society of Pure and Applied Chemistry, porous materials can be divided into three categories according to the pore size: microporous materials (pore size<2nm), mesoporous materials (2nm<pore size<50nm) and macroporous materials (pore size>50nm). Zeolite is a very representative class of microporous materials. It has a unique and regular crystal structure and pore structure, so it has a special "shape-selective catalysis" function and strong adsorption and separation performance, so it is widely used in catalysis, adsorption and field of separation. However, limited by the narrow pore structure, microporous zeolites are u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B01J29/70
Inventor 陈雪莹乔明华范康年贺鹤勇
Owner FUDAN UNIV
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