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Core-shell structured Beta/MCM-56 composite molecular sieve and preparation method thereof

A technology of MCM-56 and composite molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problem that the composite degree of composite molecular sieve is difficult to control and so on.

Active Publication Date: 2016-05-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The degree of compounding of the composite molecular sieve obtained by this method is not easy to control, and a large amount of Beta and Y type molecular sieves do not form a core-shell structure
[0006] The preparation of the above-mentioned composite molecular sieves is basically the improvement of the two-step crystallization method for synthesizing composite molecular sieves with a core-shell structure by means of chemical treatment, and there are still various deficiencies.

Method used

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  • Core-shell structured Beta/MCM-56 composite molecular sieve and preparation method thereof
  • Core-shell structured Beta/MCM-56 composite molecular sieve and preparation method thereof
  • Core-shell structured Beta/MCM-56 composite molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A certain mass of Beta molecular sieve (grain size 1.7 μm) powder with a silicon-aluminum ratio of 23 was activated at 300°C for 3 hours, cooled naturally and placed in a vacuum plasma generator, and the system plasma excitation program was set (vacuum degree 70mTorr, gas flow rate 45sccm , Ar / H 2 0.8, power 50W), with Ar-H 2 Beta molecular sieves were treated in a plasma atmosphere for 5 min. Immerse the treated Beta molecular sieve into a certain concentration of HMI solution, and stir evenly to fully absorb the organic template agent. Then add sodium hydroxide, sodium metaaluminate, and silica sol to the above-mentioned Beta molecular sieve suspension in sequence and form a gel at room temperature. The final gel material ratio (Beta is not included) satisfies: SiO 2 / Al 2 o 3 30,OH - / SiO 2 0.12, H 2 O / SiO 2 35, HMI / SiO 2 is 0.35. The content of Beta is SiO 220% of the mass. The gel was crystallized under dynamic hydrothermal conditions at 150°C for 12 ho...

Embodiment 2

[0033] A certain mass of Beta molecular sieve (grain size 1.7 μm) powder with a silicon-aluminum ratio of 23 is activated at 350°C for 1 hour, cooled naturally and placed in a vacuum plasma generator, and the system plasma excitation program is set (vacuum degree 20mTorr, gas flow rate 60sccm , Ar / H 2 1.3, power 100W), with Ar-H 2 Beta molecular sieves were treated with plasma atmosphere for 10 min. Immerse the treated Beta molecular sieve into a certain concentration of HMI solution, and stir evenly to fully absorb the organic template agent. Then add sodium hydroxide, sodium metaaluminate, and silica sol to the above-mentioned Beta molecular sieve suspension in sequence and form a gel at room temperature. The final gel material ratio (Beta is not included) satisfies: SiO 2 / Al 2 o 3 35,OH - / SiO 2 0.16, H 2 O / SiO 2 40, HMI / SiO 2 is 0.25. The content of Beta is SiO 2 40% of the mass. The gel was crystallized under dynamic hydrothermal conditions at 140°C for 36h. ...

Embodiment 3

[0035] A certain mass of Beta molecular sieve (grain size 0.7 μm) powder with a silicon-aluminum ratio of 34 was activated at 200°C for 5 hours, and after natural cooling, it was placed in a vacuum plasma generator, and the system plasma excitation program was set (vacuum degree 50mTorr, gas flow rate 30sccm , Ar / H 2 3.0 power 200W) to Ar-H 2 Beta molecular sieves were treated with plasma atmosphere for 15 min. Immerse the treated Beta molecular sieve into a certain concentration of HMI solution, and stir evenly to fully absorb the organic template agent. Then add sodium hydroxide, sodium metaaluminate, and silica sol to the above-mentioned Beta molecular sieve suspension in sequence and form a gel at room temperature. The final gel material ratio (Beta is not included) satisfies: SiO 2 / Al 2 o 3 20,OH - / SiO 2 0.18, H 2 O / SiO 2 40, HMI / SiO 2 is 0.50. The content of Beta is SiO 2 50% of the quality.

[0036] The gel was crystallized under dynamic hydrothermal condi...

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Abstract

The invention discloses a core-shell structured Beta / MCM-56 composite molecular sieve and a preparation method thereof. The core-shell structured Beta / MCM-56 composite molecular sieve comprises a Beta molecular sieve as a core phase, an MCM-56 molecular sieve as a shell layer, the dimension of the core phase is 0.3-3.0[mu]m and preferably 0.7-2.0[mu]m, the thickness of the shell layer is 0.1-6.0[mu]m and preferably 0.3-5.0[mu]m, and the composite molecular sieve comprises 35-90wt% and preferably 50-80wt% of the shell layer. A preparation method of the composite molecular sieve comprises the following steps: carrying out surface plasma modification on the Beta molecular sieve, and preparing the Beta / MCM-56 composite molecular sieve with the modified Beta molecular sieve as a nucleus. The composite molecular sieve has a good core-shell cladding form, and has good application prospect in the alkylation reaction of olefin and benzene.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic materials, and in particular relates to a Beta / MCM-56 composite molecular sieve with a core-shell structure and a preparation method thereof. Background technique [0002] The topological type of MCM-56 molecular sieve is MWW, which belongs to the same type of molecular sieve material as MCM-22 and MCM-49. They have good application prospects in the alkylation reaction of olefins and benzene. Beta molecular sieves are also widely used in the production of cumene by alkylation of propylene and benzene. If MCM-56 and Beta molecular sieves with unique properties are organically compounded, and the compound crystal is endowed with reasonable acid distribution and good shape selectivity, and learn from each other, it can make full use of the shape selectivity and stability of MCM-56 molecular sieve And the advantages of high activity of Beta molecular sieve may have a special synergistic cataly...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 杨卫亚凌凤香王少军沈智奇季洪海王丽华郭长友
Owner CHINA PETROLEUM & CHEM CORP
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