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A kind of preparation method of hierarchical porous ZSM-11 molecular sieve

A ZSM-11, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of complex process route and difficult realization.

Active Publication Date: 2022-03-18
天津博创工程科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zhao Zhen (CN 108658093A) etc. also disclosed a preparation method and application of a multi-stage porous ZSM-5 molecular sieve, adopted hexadecyltrimethylammonium bromide as a soft templating agent, and made much more Level hole ZSM-5, the above process route is complicated and difficult to realize

Method used

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  • A kind of preparation method of hierarchical porous ZSM-11 molecular sieve
  • A kind of preparation method of hierarchical porous ZSM-11 molecular sieve
  • A kind of preparation method of hierarchical porous ZSM-11 molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0027] According to the molar ratio of reaction materials, SiO 2 :0.005Al 2 o 3 :0.2NaOH:0.3Template:25H 2 O, prepare the reaction mixture. Wherein, the silicon source is ethyl orthosilicate, the aluminum source is sodium metaaluminate, and the template agent is N-butyl-N-methylpiperidine bromide. After mixing the raw materials in order and vigorously stirring them evenly, statically crystallize at 150°C for 48 hours. After crystallization, the mother liquor undergoes solid-liquid separation, washing, drying, and roasting to obtain ZSM-11 molecular sieve. X-ray diffractometer (attached figure 1 ) and SEM images (attached figure 2 ) The obtained crystal is ZSM-11 molecular sieve, and the molecular sieve pore size distribution diagram (attached image 3 ) shows that the prepared ZSM-11 molecular sieve is a hierarchical porous molecular sieve with micropores and mesoporous pores (the same below).

Embodiment 2

[0029] According to the molar ratio of reaction materials, SiO 2 :0.01Al 2 o 3 :2NaOH:0.1Template:50H 2 O, prepare the reaction mixture. Wherein, the silicon source is silica sol, the aluminum source is aluminum sulfate, and the template agent is N-butyl-N-methylpiperidine bromide. After mixing the raw materials in order and vigorously stirring them evenly, statically crystallize at 300°C for 1 hour. After crystallization, the mother liquor is subjected to solid-liquid separation, washing, drying, and roasting to obtain a multi-stage porous ZSM-11 molecular sieve.

Embodiment 3

[0031] According to the molar ratio of reaction materials, SiO 2 :0.05Al 2 o 3 :0.1NaOH:1Template:10H 2 O, prepare the reaction mixture. Wherein, the silicon source is water glass, the aluminum source is pseudoboehmite, and the template agent is N-butyl-N-methylpiperidine bromide. After mixing the raw materials in order and vigorously stirring them evenly, statically crystallize at 100°C for 100 hours. After crystallization, the mother liquor is subjected to solid-liquid separation, washing, drying, and roasting to obtain a multi-stage porous ZSM-11 molecular sieve.

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Abstract

A kind of preparation method of multistage hole ZSM-11 molecular sieve, silicon source, aluminum source, alkali source, templating agent, water are pressed SiO 2 :0.005~0.05Al 2 o 3 :0.1~2NaOH:0.1~1 template agent:10~50H 2 The molar ratio of O is mixed, and after being fully stirred, it is transferred into a crystallization tank for crystallization. After crystallization, the mother liquor is subjected to solid-liquid separation, washing, drying, and roasting to obtain ZSM-11 molecular sieve. The present invention adopts one-step hydrothermal method to synthesize multi-level porous ZSM-11 molecular sieve in situ, and the template agent used is N-butyl-N-methylpiperidinium bromide ionic liquid, which has extremely low vapor pressure and can reduce the synthesis process The problem of environmental pollution caused by volatilization; the ZSM-11 molecular sieve synthesized by this template has a multi-level pore structure with micropores and mesopores, which is more conducive to the mass transfer process in the channels. The preparation process is simple to operate, is practical, and is conducive to transforming into industrialized production.

Description

technical field [0001] The invention belongs to the field of synthesis of molecular sieve materials, in particular to a method for preparing a multi-stage porous ZSM-11 molecular sieve. [0002] technical background [0003] ZSM-11 molecular sieve is a MEL type high silicon molecular sieve, which was first synthesized by Mobil Company of the United States in the early 1970s, and its structure was reported by Kokotailo et al. in 1978. Both ZSM-11 and ZSM-5 are Pentasil zeolites with a two-dimensional channel system. The channel structures of the two are different. ×0.54nm); ZSM-11 is composed of two-dimensional straight channels (0.51nm×0.55nm) intersected by oval ten-membered rings. Both have similar pore sizes and have excellent catalytic properties, and are widely used in very important industrial chemical processes such as alkylation, cracking, aromatization, and disproportionation. Compared with ZSM-5, ZSM-11 has excellent catalytic performance in some reactions, such a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/36
CPCC01B39/36C01P2006/17C01P2004/03C01P2002/72
Inventor 仝新利程欢张舜光
Owner 天津博创工程科技有限公司