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Preparation method of ZSM-35 molecular sieve

A technology of ZSM-35 and molecular sieve, applied in the field of preparation of ZSM-35 molecular sieve, can solve the problems of agglomeration and easy agglomeration, etc.

Active Publication Date: 2019-03-22
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Small grains have excellent diffusion properties, but they are prone to agglomeration, resulting in macroscopic agglomeration

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Aluminum sulfate (Al 2 o 3 7.08%) and ethylenediaminetetraacetic acid (CA) were mixed and stirred uniformly to obtain solution a. Solution a was aged at 60°C for 8h. The molar ratio of each component in solution a is H 2 O: Al 2 o 3 :CA=200:1.0:0.1.

[0026] Silica sol (SiO 2 25%), aluminum sulfate (Al 2 o 3 7.08%), liquid caustic soda (Na 2 (36.72%), cyclohexylamine, water and ZSM-35 molecular sieve seed crystals were mixed uniformly to obtain gel b. The molar ratio of each component in gel b is as follows: H 2 O:SiO 2 :Al 2 o 3 :Na 2 O: templating agent=10:1:0.01:0.1:0.3. The gel b was transferred to a crystallization kettle and crystallized at 120°C for 12h. After the crystallization is completed, add the solution a into the crystallization kettle. Crystallized at 170°C for 48h. After the crystallization is completed, a molecular sieve slurry is obtained. The ZSM-35 molecular sieve is obtained after separating the mother liquor, washing with wat...

Embodiment 2

[0028] Aluminum sulfate (Al 2 o 3 7.08%), disodium edetate (CA) were mixed and stirred uniformly to obtain solution a. Solution a was aged at 90°C for 18h. The molar ratio of each component in solution a is H 2 O: Al 2 o 3 :CA=100:1.0:0.001.

[0029] Silica sol (SiO 2 30%), aluminum sulfate (Al 2 o 3 7.08%), liquid caustic soda (Na 2 (36.72%), cyclohexylamine, water and ZSM-35 molecular sieve seed crystals were mixed uniformly to obtain gel b. The molar ratio of each component in gel b is as follows: H 2 O:SiO 2 :Al 2 o 3 :Na 2 O: templating agent=12:1:0.1:0.5:0.05. The gel b was transferred to a crystallization kettle and crystallized at 100°C for 36h. After the crystallization is completed, add the solution a into the crystallization kettle. Crystallized at 155°C for 72h. After the crystallization is completed, a molecular sieve slurry is obtained. The ZSM-35 molecular sieve is obtained after separating the mother liquor, washing with water, exchanging,...

Embodiment 3

[0031] Aluminum sulfate (Al 2 o 3 7.08%), citric acid (CA) and stir evenly to obtain solution a. Solution a was aged at 80°C for 24h. The molar ratio of each component in solution a is H 2 O: Al 2 o 3 :CA=1000:1.0:0.1.

[0032] Silica sol (SiO 2 30%), aluminum sulfate (Al 2 o 3 7.08%), liquid caustic soda (Na 2 (36.72%), cyclohexylamine, water and ZSM-35 molecular sieve seed crystals were mixed uniformly to obtain gel b. The molar ratio of each component in gel b is as follows: H 2 O:SiO 2 :Al 2 o 3 :Na 2 O: templating agent=40:1:0.025:0.05:1. The gel b was transferred to a crystallization kettle and crystallized at 140°C for 10h. After the crystallization is completed, add the solution a into the crystallization kettle. Crystallized at 165°C for 48h. After the crystallization is completed, a molecular sieve slurry is obtained. The ZSM-35 molecular sieve is obtained after separating the mother liquor, washing with water, exchanging, drying and roasting. ...

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Abstract

The invention relates to a preparation method of a ZSM-35 molecular sieve, and belongs to the field of preparation of molecular sieves. The preparation method comprises the following steps: (a) preparing an aluminum source, a complexing agent and water into a solution a and aging the solution a at 10 to 100 DEG C for 1 to 48 hours to obtain aging liquid, wherein the aging condition in the preferred scheme that aging is performed for 6 to 24 hours at 30 to 70 DEG C; (b) uniformly mixing a silicon source, the aluminum source, an alkali source, a template agent, water and a ZSM-35 molecular sievecrystal seed to obtain gel b; (c) transferring the gel b into a crystallization kettle and crystallizing at 50 to 150 DEG C for 12 to 72 hours; (d) replenishing the aging liquid obtained in the step(a) into the crystallization kettle in the step (c), and crystallizing at 150 to 180 DEG C for 12 to 72 hours; (e) after the reaction ends, separating mother liquid, washing, exchanging, drying and calcining to obtain the ZSM-35 molecular sieve. The preparation method for preparing the ZSM-35 molecular sieve which has controllable silicon aluminum distribution, a mesoporous structure, small grainand high specific surface area is of great significance.

Description

technical field [0001] The invention relates to a preparation method of ZSM-35 molecular sieve, which belongs to the field of molecular sieve preparation. Background technique [0002] ZSM-35 molecular sieve is a medium-porous zeolite developed by Mobil Company of the United States in 1977. Its skeleton structure is formed by intersecting ten-membered ring channels and eight-membered ring channels perpendicular to each other. The eight-membered ring channels are on the c axis. The metarings interleave to form a FER cage. Natural FER zeolite belongs to silicon-rich crystalline zeolite, and its crystal structure belongs to the orthorhombic system. [0003] Since ZSM-35 molecular sieve has a vertically interspersed two-dimensional pore structure, it is widely used in catalytic reactions such as isomerization, aromatization and cracking of linear olefins. For example, ZSM-35 molecular sieve has outstanding performance in the isomerization reaction of 1-butene. However, it is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/44
CPCC01B39/445C01P2004/03C01P2002/72C01P2004/62C01P2006/14C01P2006/12Y02P20/52
Inventor 王龙陈文勇刘环昌彭立周泳冰徐辰
Owner SHANDONG QILU HUAXIN HIGH TECH
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