Hierarchical pore zeolite molecular sieve preparation method

A technology of zeolite molecular sieve and multi-level pores, applied in the direction of crystalline aluminosilicate zeolite, etc., to achieve the effect of improved diffusion path and low cost

Inactive Publication Date: 2013-05-01
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the preparation method of a kind of multi-stage pore zeolite molecular sieve of the present invention is, in order to solve the synthesis of the multi-stage pore zeolite molecular sieve material that exists in the above-mentioned prior art either through aftertreatment or utilize expensive hard templating agent to realize the manufacture of mesopores problem, thereby disclosing a method for synthesizing multi-stage pore zeolite molecular sieves by utilizing the traditional template tetraethylammonium bromide TEABr or tetraethylammonium hydroxide TEAOH synthesized by zeolite as a template

Method used

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  • Hierarchical pore zeolite molecular sieve preparation method

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Experimental program
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Embodiment approach 1

[0015] Step 1: At room temperature, mix 1.28g sodium metaaluminate, 1.89g sodium hydroxide, 18ml silica sol and 54ml distilled water to form a uniform white jelly, put it into a stainless steel reaction kettle, and conduct hydrothermal treatment at 170°C for 24 hours , then vacuum filtration, and retain the filtrate for subsequent use;

[0016] Step 2: Take 55ml of the above-mentioned filtrate, add 12.5g template agent tetraethylammonium bromide TEABr, 6ml ammonia water and 3ml silica sol to the filtrate, stir evenly, crystallize at 140 degrees Celsius for 7 days, then cool with tap water To room temperature, the product was washed with distilled water until neutral, filtered, dried in an oven at 100°C for 12 hours, and calcined in a muffle furnace at 550°C for 6 hours under the condition of ventilation to obtain the final sample. Analysis by XRD and SEM shows that the obtained sample is a ZSM-12 polycrystalline aggregate of about 10 microns in size composed of nano-sized grai...

Embodiment approach 2

[0019] Step 1: At room temperature, mix 1.28g sodium metaaluminate, 1.89g sodium hydroxide, 18ml silica sol and 54ml distilled water to form a uniform white jelly, put it into a stainless steel reaction kettle, and conduct hydrothermal treatment at 170°C for 24 hours , then vacuum filtration, and retain the filtrate for subsequent use;

[0020] The second step: take 50ml of the above-mentioned filtrate, add 10g template agent tetraethylammonium bromide TEABr, 5ml ammonia water and 15ml silica sol to the filtrate, stir evenly, crystallize at 170 degrees Celsius for 4 days, then cool with tap water to At room temperature, the product was washed with distilled water until neutral, filtered, dried in an oven at 100°C for 12 hours, and calcined in a muffle furnace at 550°C for 4 hours under air ventilation to obtain the final sample. Analysis by XRD and SEM shows that the obtained sample is a ZSM-12 polycrystalline aggregate of about 50 microns overall composed of nano-sized grains...

Embodiment approach 3

[0023] Step 1: At room temperature, mix 1.28g sodium metaaluminate, 1.89g sodium hydroxide, 18ml silica sol and 54ml distilled water to form a uniform white jelly, put it into a stainless steel reaction kettle, and conduct hydrothermal treatment at 170°C for 24 hours , then vacuum filtration, and retain the filtrate for subsequent use;

[0024] Step 2: Take 72ml of the above-mentioned filtrate, add 19.3g template agent tetraethylammonium bromide TEABr, 5ml ammonia water and 5ml silica sol to the filtrate, stir evenly, crystallize at 180 degrees Celsius for 5 days, then cool with tap water To room temperature, the product was washed with distilled water until neutral, filtered, dried in an oven at 100°C for 12 hours, and calcined in a muffle furnace at 550°C for 5 hours under the condition of ventilation to obtain the final sample. The XRD characterization results show that the characteristic diffraction peaks of ZSM-12 are obviously broadened, See figure 1 , It is precisel...

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Abstract

The invention relates to a hierarchical pore zeolite molecular sieve and a preparation method, which belongs to the fine chemical and inorganic material field. The invention relates to a ZSM-12 zeolite molecular sieve having intergranular mesoporous and macroporous and a preparation method, the invention is characterized in that a traditional template tetraethyl ammonium bromide TEABr or a tetraethyl ammonium hydroxide TEAOH synthesized by zeolite are taken as a template to synthesize the hierarchical pore zeolite molecular sieve, the problem that the synthesis of the hierarchical pore zeolite molecular sieve employs post-treatment or expensive hard template to prepare the mesoporous can be solved, according to the material, the diffusion path is substantially shortened and the acid site accessibility is enhanced, and the material has important utility value on fine chemical, catalysis of petroleum chemical, adsorption and separating.

Description

technical field [0001] The invention discloses a method for preparing a multi-level pore zeolite molecular sieve, which belongs to the field of fine chemicals and inorganic materials, and specifically relates to a method for preparing a ZSM-12 zeolite molecular sieve with intercrystalline mesopores or macropores. Background technique [0002] As a microporous material, zeolites are widely used in the fields of catalysis, adsorption and separation. This material has demonstrated unique acid-catalytic and shape-selective properties in the fields of oil refining, basic chemistry, and fine chemistry. In addition to providing shape-selective performance, the intricate pore system in the molecular size range (0.3-1.5nm) in zeolite not only restricts the diffusion of reactive molecules passing through its channels, but also, when the spatial size of the reactive molecules passing through the channels is in line with the Close pore sizes in zeolites also induce high back pressures ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 李瑞丰郑家军白亚东马静红潘梦张球
Owner TAIYUAN UNIV OF TECH
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