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A kind of beta/mcm‑22 composite molecular sieve with core-shell structure and preparation method thereof

A technology of composite molecular sieve and core-shell structure is applied in the field of inorganic material preparation, which can solve the problems such as difficulty in controlling the composite degree of composite molecular sieve.

Active Publication Date: 2017-09-29
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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  • A kind of beta/mcm‑22 composite molecular sieve with core-shell structure and preparation method thereof
  • A kind of beta/mcm‑22 composite molecular sieve with core-shell structure and preparation method thereof
  • A kind of beta/mcm‑22 composite molecular sieve with core-shell structure 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 0.10, H 2 O / SiO 2 40, 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 170°C for 24h. ...

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 45,OH - / SiO 2 is 0.08, H 2 O / SiO 2 40, HMI / SiO 2 is 0.20. The content of Beta is SiO 2 40% of the mass. The gel was crystallized under dynamic hydrothermal conditions at 150°C for 72...

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 45,OH - / SiO 2 0.10, H 2 O / SiO 2 40, HMI / SiO 2 is 0.20. 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 Beta / MCM-22 composite molecular sieve with a core-shell structure. The Beta molecular sieve is used as the core phase, the MCM-22 molecular sieve is used as the shell layer, the size of the core phase is 0.3-3.0 μm, preferably 0.7-2.0 μm, and the shell layer The thickness is 0.1-6.0 μm, preferably 0.3-5.0 μm, based on the weight of the composite molecular sieve, and the shell content is 35%-90%, preferably 50%-80%. The preparation method is as follows: firstly, the surface plasma of Beta molecular sieve is modified, and then Beta / MCM‑22 core-shell composite molecular sieve is prepared by using it as the crystal nucleus. It has a good application prospect in the alkylation reaction.

Description

technical field [0001] The invention relates to a Beta / MCM-22 composite molecular sieve with a core-shell structure and a preparation method thereof, belonging to the field of inorganic material preparation. Background technique [0002] MCM-22 and Beta are two kinds of molecular sieve catalytic materials that are widely used in the production of cumene by alkylation of propylene and benzene. MCM-22 and Beta have relatively good catalytic performance in the alkylation reaction of propylene and benzene. , but each has a unique response advantage. Since MCM-22 and Beta molecular sieves have different catalytic properties, if the two molecular sieves are organically compounded, and the composite crystal is endowed with reasonable acid distribution and good shape selectivity, it can make full use of the selectivity of MCM-22 molecular sieve. Due to the advantages of shape, stability and high activity of Beta molecular sieve, it may have a special synergistic catalytic effect on...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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