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H-type MCM-22 molecular sieve, preparation method and application thereof

A molecular sieve, mole fraction technology, applied in molecular sieve catalysts, chemical instruments and methods, hydrocarbons, etc., can solve the problems of cumbersome production steps, high external surface area, thick lamellae, etc., and achieve excellent catalytic performance and a large number of acid centers. , the effect of high external surface area

Active Publication Date: 2021-03-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the technical problems to be solved by the present invention is to solve the problem of low external area and thick sheet of H-type MCM-22 molecular sieve, and provide an H-type MCM-22 molecular sieve, which has the advantages of high external area and sheet thickness not exceeding 20nm
[0007] The second technical problem to be solved by the present invention is to solve the problem in the prior art that the production steps are cumbersome, multiple times of ammonium ion exchange is required, and there is a large amount of ammonium nitrogen wastewater discharge, and a new H-type MCM-22 molecular sieve preparation is provided. method

Method used

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  • H-type MCM-22 molecular sieve, preparation method and application thereof
  • H-type MCM-22 molecular sieve, preparation method and application thereof
  • H-type MCM-22 molecular sieve, preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0044] Molar ratio SiO 2 : Dimethyldiethoxysilane: B 2 o 3 :piperidine:H 2 O is 1: 0.035: 0.6: 1.5: 20 Mix the corresponding amount of water, piperidine, boric acid, 60 grams of fumed silica and dimethyldiethoxysilane evenly to form a gel. Thermal crystallization for 5.5 days, centrifugation, washing, drying at 80°C for 16 hours, and calcination at 550°C in an air atmosphere for 10 hours to obtain B-MWW molecular sieves. Next, mix B-MWW molecular sieves with 2mol / L hydrochloric acid solution at a mass ratio of 1:50, treat at 120°C for 24 hours, centrifuge, wash, and dry at 80°C for 16 hours to obtain deboronated B-MWW molecular sieves. Then, the deboronated B-MWW molecular sieve was mixed with aluminum nitrate and deionized water at a mass ratio of 1:0.5:50, treated at 120°C for 24 hours, centrifuged, washed, and dried at 80°C for 16 hours, and air atmosphere at 550°C Calcined for 10 hours to obtain the H-type MCM-22 molecular sieve product. The X-ray diffraction figure a...

Embodiment 2

[0046] Molar ratio SiO 2 : Dimethyldiethoxysilane: B 2 o 3 : Hexamethyleneimine: H 2 O is 1: 0.035: 0.6: 1.5: 20 Mix the corresponding amount of water, hexamethyleneimine, boric acid, 60 grams of fumed silica and dimethyldiethoxysilane to form a gel, at 50rpm, Dynamic hydrothermal crystallization at 170°C for 5.5 days, centrifugation, washing, drying at 80°C for 16 hours, and calcination at 550°C in an air atmosphere for 10 hours to obtain B-MWW molecular sieves. Next, mix B-MWW molecular sieves with 2mol / L hydrochloric acid solution at a mass ratio of 1:50, treat at 120°C for 24 hours, centrifuge, wash, and dry at 80°C for 16 hours to obtain deboronated B-MWW molecular sieves. Then, the deboronated B-MWW molecular sieve was mixed with aluminum nitrate and deionized water at a mass ratio of 1:0.5:50, treated at 120°C for 24 hours, centrifuged, washed, and dried at 80°C for 16 hours. Calcined for 10 hours to obtain the H-type MCM-22 molecular sieve product. The X-ray diffr...

Embodiment 3

[0048] Molar ratio SiO 2 : Dimethyldiethoxysilane: B 2 o 3 : Hexamethyleneimine: H 2 O is 1: 0.035: 0.6: 1.5: 20. Mix the corresponding amount of water, hexamethyleneimine, boric acid, 60 grams of fumed silica and dimethyldiethoxysilane to form a gel. Dynamic hydrothermal crystallization at 170°C for 6.5 days, centrifugation, washing, drying at 80°C for 16 hours, and calcination at 550°C in an air atmosphere for 10 hours to obtain B-MWW molecular sieves. Next, mix B-MWW molecular sieves with 2mol / L hydrochloric acid solution at a mass ratio of 1:50, treat at 120°C for 24 hours, centrifuge, wash, and dry at 80°C for 16 hours to obtain deboronated B-MWW molecular sieves. Then, the deboronated B-MWW molecular sieve was mixed with aluminum nitrate and deionized water at a mass ratio of 1:0.5:50, treated at 120°C for 24 hours, centrifuged, washed, and dried at 80°C for 16 hours. Calcined for 10 hours to obtain the H-type MCM-22 molecular sieve product. The X-ray diffraction pa...

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Abstract

The invention discloses an H-type MCM-22 molecular sieve, a preparation method and application thereof. According to the H-type MCM-22 molecular sieve, diffraction peaks appear when 2 theta is 7.2+ / -0.09 degrees, 8.0+ / -0.10 degrees, 9.6+ / -0.07 degrees, 12.7+ / -0.10 degrees, 14.4+ / -0.07 degrees, 15.8+ / -0.08 degrees, 20.0+ / -0.11 degrees, 22.7+ / -0.15 degrees, 25.1+ / -0.15 degrees, 26.1+ / -0.12 degrees and 26.9+ / -0.13 degrees; the outer surface area is 270-500m<2> / g; and the lamella thickness is 2.5-20nm. The H-type MCM-22 molecular sieve provided by the invention has the advantages that the outer surface area is large, and the lamellar thickness does not exceed 20nm.

Description

technical field [0001] The invention relates to an H-type MCM-22 molecular sieve and its preparation method and application, belonging to the field of molecular sieve inorganic materials. Background technique [0002] MCM-22 molecular sieve is a silicon-alumina molecular sieve material with a topological structure of MWW synthesized by researchers from Mobil Corporation in the 1980s. It has two independent channel systems: one is a two-dimensional sinusoidal ten-membered ring channel in the layer. , with an effective aperture of 0.41nm x 0.51nm; the other set is an interlayer twelve-membered ring supercage with a size of 0.71nm x 0.71nm x 1.81nm, which communicates with the outside world through a ten-membered ring window with an aperture size of 0.40nm x 0.55nm connected. In addition, the molecular sieve also has a bowl-shaped twelve-membered ring semi-supercage located on the outer surface of the molecular sieve crystal. Due to good thermal stability, hydrothermal stabil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B01J29/70B01J35/10C07C2/66C07C15/073
CPCC01B39/02B01J29/7038C07C2/66C01P2002/72C01P2004/04B01J35/61C07C15/073Y02P20/52
Inventor 金少青孙洪敏沈震浩王达锐
Owner CHINA PETROLEUM & CHEM CORP
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