Method for preparing MCM-22 molecular sieve in high silicon

A technology of MCM-22 and molecular sieves, applied in molecular sieves and base exchange compounds, chemical instruments and methods, inorganic chemistry, etc.

Inactive Publication Date: 2006-07-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

And the method for preparing the MCM-22 molecular sieve with high silicon-aluminum ratio and high purity by ammonium fluorosilicate post-treatment is then not reported

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  • Method for preparing MCM-22 molecular sieve in high silicon

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Embodiment 1

[0013] 1) The silicon-aluminum ratio is Si / Al 2 The former powder of MCM-22 molecular sieve of =27 is roasted at 500°C to remove the template agent, and it is converted into an intermediate ammonium form by ammonium ion exchange method; ammonium ion source NH 4 NO 3 , Ammonium ion exchange conditions: ammonium ion concentration 0.2mol / L, volume liquid-solid ratio 5, temperature 20°C.

[0014] 2) Treat the molecular sieve obtained in step 1 with 0.01mol / L ammonium fluorosilicate solution under reflux at room temperature for 0.5h, wash with deionized water three times, dry at 100-120°C, and dry at 550°C. ℃, the resulting MCM-22 molecular sieve has a silicon-aluminum ratio of 50, a relative crystallinity of >99%, and no other crystal phases, see attached figure 1 .

Embodiment 2

[0016] The preparation method of ammonium type molecular sieve is the same as embodiment 1, ammonium ion source NH 4 Cl, ammonium ion exchange conditions: ammonium ion concentration 1mol / L, volume liquid-solid ratio 10, temperature 80°C. The obtained ammonium molecular sieve was treated with 0.03mol / L ammonium fluorosilicate solution under reflux at 70°C for 10 hours, washed repeatedly with deionized water three times, dried at 100-120°C, and calcined at 600°C to obtain MCM-22 Molecular sieve has a silicon-aluminum ratio of 99, a relative crystallinity of >99%, and no other crystalline phases, see attached figure 1 .

Embodiment 3

[0018] The preparation method of ammonium type molecular sieve is the same as embodiment 1, ammonium ion source (NH 4 ) SO 4 , Ammonium ion exchange conditions: ammonium ion concentration 1.2mol / L, volume liquid-solid ratio 5, temperature 100°C. The obtained ammonium molecular sieve was treated with 0.8mol / L ammonium fluorosilicate solution at 100°C for 48 hours under reflux, washed three times with deionized water, dried at 100-120°C, and calcined at 400°C to obtain MCM-22 Molecular sieve has a silicon-aluminum ratio of 180, a relative crystallinity > 80%, and no other crystal phases, see attached figure 1 .

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Abstract

This is the preparation of MCM-22 zeolite with high silicon. By using this method, at room temperature to100 deg.C, MCM-22 zeolite with low silicon aluminium ratio (Si/Al2ú“30) and 0.01-0.8mol/L fluorin ammonium silicate was reacted for 0.5h-48h, and MCM-22 zeolite with high silicon was obtained. In addition, the silicon aluminium ratio can be changed in the range of 50í½180, these products with high crystal degree, meanwhile, there is no other crystal phase formed in the treatment process.

Description

technical field [0001] The invention relates to a preparation method of high silicon MCM-22 molecular sieve. Specifically, it relates to a method for preparing high-silicon MCM-22 molecular sieves by dealuminating low-silicon-aluminum ratio MCM-22 molecular sieves by way of post-treatment. Background technique [0002] MCM-22 molecular sieve is a new type of molecular sieve developed by Mobil Corporation of the United States in 1990. Its structure is MWW type, and it has two kinds of pore systems that are not connected to each other. One set is a two-dimensional sinusoidal channel with an effective aperture of a ten-membered ring, and the other set is composed of a supercage containing a twelve-membered ring, and its opening is also a ten-membered ring. Due to its unique pore structure, high specific surface area, good thermal and hydrothermal stability, and adjustable acidity, it can be used in reactions such as alkylation, aromatization, toluene disproportionation, and xy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/46
Inventor 徐龙伢朱向学宋月芹谢素娟刘盛林
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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