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Preparation method of small grain ZSM-35 molecular sieve

A technology of ZSM-35 and molecular sieve, which is applied in the direction of molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc. It can solve the problems of not being able to obtain molecular sieve products in a simple way, environmental impact, and increased production costs. , to achieve good catalytic stability, uniform particle size and small particle size

Active Publication Date: 2015-04-08
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of method increases production costs and will have varying degrees of impact on the environment
The existing ZSM-35 molecular sieve preparation method cannot obtain a molecular sieve product with a particle size of less than 1 μm in a relatively cheap and simple way

Method used

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  • Preparation method of small grain ZSM-35 molecular sieve
  • Preparation method of small grain ZSM-35 molecular sieve
  • Preparation method of small grain ZSM-35 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 0.27g of sodium hydroxide (produced by Shenyang Xinxing Reagent Factory, analytically pure solid sodium hydroxide) and add it to 30.44g of deionized water, stir until completely dissolved, then add 1.65g of sodium aluminate (Zibo Zhoucun Tongjie Chemical Industry Co., Ltd. Ltd. Production, Al 2 o 3 Mass content is 40%), make it dissolve completely under stirring state, stand-by as solution A; Then, 9.15g templating agent ethylenediamine (produced by Quanrui Reagent Factory, analytically pure) is added to 27.06g silica sol (Qingdao ocean Produced by Chemical Co., Ltd., SiO 2 Mass content is 25%), mix uniformly, as solution B; under stirring state, solution B is slowly added dropwise in solution A, continue to stir for 30 minutes, obtain colloidal solution; The molar ratio of each component in this colloidal solution is: SiO 2 / Al 2 o 3 =18.5, R / SiO 2 =0.81, OH － / SiO 2 =0.06,H 2 O / SiO 2 =10; Add 0.1g of ZSM-35 molecular sieve powder with a particle size o...

Embodiment 2

[0034] Weigh 0.27g of sodium hydroxide (produced by Shenyang Xinxing Reagent Factory, analytically pure solid sodium hydroxide) and add it to 53.9g of deionized water, stir until completely dissolved, then add 1.65g of sodium aluminate (Zibo Zhoucun Tongjie Chemical Co., Ltd. Produced by the company, Al 2 o 3 Mass content is 40%), make it dissolve completely under stirring state, stand-by as solution A; Then, 9.15g ethylenediamine (produced by Quanrui Reagent Factory, analytically pure) is added to 27.06g silica sol (Qingdao Ocean Chemical Co., Ltd. Produced by the company, SiO 2 Mass content is 25%), mix uniformly, as solution B; Under stirring state, solution B is slowly added dropwise in solution A, continue to stir for 0.5 hour, obtain colloidal solution; The molar ratio of each component in this colloidal solution is: SiO 2 / Al 2 o 3 =18.5, R / SiO 2 =0.81, OH － / SiO 2 =0.06,H 2 O / SiO 2 =26. The colloidal solution was crystallized in a high-pressure crystallizati...

Embodiment 3

[0036] In Example 2, only the heating process of crystallization was changed, from room temperature to 80°C at a rate of 1°C / min, kept for 10 hours, then heated to 180°C at a rate of 4°C / min, and crystallized for 20 hours, other The condition remains unchanged, and the ZSM-35 molecular sieve is obtained, the grain size of which is about 1-3 μm.

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Abstract

The invention provides a preparation method of a small grain ZSM-35 molecular sieve. The method comprises the following steps: uniformly mixing a silicon source, an aluminum source, an alkaline source, a template and water to obtain a colloid liquid, the molar ratios of which are as follows: SiO2 / Al2O3=18.5-28.6, template / SiO2=0.81-1.25, OH<-> / SiO2=0.03-0.18 and H2O / SiO2=10-26; firstly crystallizing the colloid liquid for 5-30 hours at 15-80 DEG C and then continuously crystallizing for 10-30 hours at 150-200 DEG C; and filtering, washing and drying to obtain the small grain ZSM-35 molecular sieve. According to the preparation method, by using cheap ethidene diamine as the template, the crystallizing process is controlled to synthesize the small grain ZSM-35 molecular sieve by adding seed crystals and crystallizing in two stages, so that the grain size reaches about 0.5 micron at minimum.

Description

technical field [0001] The invention relates to a method for preparing a silica-alumina zeolite molecular sieve, in particular to a method for preparing a small-grain ZSM-35 molecular sieve, and belongs to the technical field of zeolite molecular sieves in the field of inorganic materials and catalysts. Background technique [0002] ZSM-35 molecular sieve is a medium-porous zeolite developed by Mobil Corporation, with a FER-type framework structure. Naturally occurring FER zeolite is a silicon-rich crystalline zeolite whose crystal structure belongs to the orthorhombic system. It has a two-dimensional channel system perpendicular to each other, that is, a ten-membered ring channel (0.42×0.54nm) parallel to the [001] plane and an eight-membered ring channel (0.35×0.48nm) parallel to the [010] plane. The ring channel and the six-membered ring channel intersect in the C direction to form a spherical cage (FER cage). [0003] The adsorption, stability and acidity of molecular ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/44
CPCC01B39/445C01P2002/72C01P2004/03C01P2004/61C01P2004/62
Inventor 胡云峰刘丽杰
Owner PETROCHINA CO LTD
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