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Synthetic method of thin rod-shaped zsm-22 molecular sieve

A synthesis method and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of poor thermodynamic stability of the product, lack of specificity of TON topology orientation, etc., and achieve shortened crystallization time, high crystallinity, and high specific surface area Effect

Active Publication Date: 2019-11-12
SHANDONG QILU HUAXIN HIGH TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the synthesis of ZSM-22 molecular sieve system, the TON topological orientation of the template lacks specificity, and ZSM-22 molecular sieve is a metastable zeolite, and the thermodynamic stability of the product is poor

Method used

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Experimental program
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Effect test

Embodiment 1

[0029] The synthetic method of described thin rod shape ZSM-22 molecular sieve, comprises the steps:

[0030] Add potassium carbonate, C-type silica gel, aluminum sulfate octadecahydrate, seed crystals, and structural aid dodecyltrimethylammonium bromide to the deionized water in sequence, stir quickly and fully, then transfer to a high-pressure reactor, and cool down to - 5°C, aging for 12h. After aging, the temperature was slowly raised to 120° C. for 16 hours of crystallization, and the heating rate was 1° C. / min. A directing agent solution (GA-1) was obtained. Its molar ratio is: SiO 2 :Al 2 o 3 :K + :H 2 O=1:0.02:0.2:15, the amount of seed crystal added is 6% of the mass of silicon oxide, and the amount of structural aid added is 8% of the sum of the mass of silicon oxide and aluminum oxide.

[0031] Mix water, C-type silica gel, sodium hydroxide, aluminum sulfate octadecahydrate, and 1.6-hexamethylenediamine to obtain a homogeneous gel a. Its molar ratio is: SiO ...

Embodiment 2

[0033] The synthetic method of described thin rod shape ZSM-22 molecular sieve, comprises the steps:

[0034] Potassium chloride, silica sol, pseudoboehmite, seed crystals and citric acid were sequentially added into the deionized water, stirred thoroughly, then transferred to a high-pressure reactor, cooled to -10°C, and aged for 8 hours. After aging, the temperature was slowly raised to 110° C., crystallized for 20 hours, and the heating rate was 1° C. / min. The directing agent (GA-2) was obtained. Its molar ratio is: SiO 2 :Al 2 o 3 :K + :H 2 O=1:0.015:0.25:15, the amount of seed crystal added is 7% of the mass of silicon oxide, and the amount of structural aid added is 9% of the sum of the mass of silicon oxide and aluminum oxide.

[0035] Mix water, silica sol, potassium hydroxide, pseudoboehmite, and 1.6-hexamethylenediamine uniformly to obtain a homogeneous gel b, and its molar ratio is: SiO 2 :K 2 O: Al 2 o 3 :H 2 O: Templating agent = 1:0.08:0.01:20:0.03. A...

Embodiment 3

[0037] The synthetic method of described thin rod shape ZSM-22 molecular sieve, comprises the steps:

[0038] Add the directing agent solution GA-1 into the gel b, stir and mix thoroughly, then transfer to the reaction kettle, rapidly raise the temperature to 160°C, crystallize for 30h, and the heating rate is 40°C / min. The amount of GA-1 added is 6% of the mass of silicon oxide. After the crystallization, filter the product with suction, wash with water, and dry the raw ZSM-22 molecular sieve powder. Put the raw powder in a muffle furnace and roast at 600°C for 6 hours to obtain a thin rod-shaped ZSM-22 molecular sieve (Z-3) .

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Abstract

The invention relates to a synthesis method of a fine bar-shaped ZSM-22 molecular sieve, belonging to the field of synthesis of molecular sieves. The method comprises the steps of firstly, adding a potassium source and structure additives to prepare gel, aging and nucleating to obtain a guiding agent solution; then, adding the guiding agent solution into gel synthesized by using a template agent and alkali, and crystallizing to obtain product slurry; carrying out suction filtration, washing, drying and calcining to obtain the fine bar-shaped ZSM-22 molecular sieve. The method provided by the invention reduces the use of the organic amine template agent by using a guiding agent; furthermore, compared with the prior art, the method can reduce the crystallization temperature and shorten crystallization time. After the method is adopted, the production cost is greatly lowered, and the production efficiency is increased.

Description

technical field [0001] The invention relates to a method for synthesizing thin rod-shaped ZSM-22 molecular sieves, belonging to the field of molecular sieve synthesis. Background technique [0002] ZSM-22 molecular sieve is a microporous, high-silica molecular sieve developed by Mobil Corporation of the United States, which belongs to the TON topology. It has only one-dimensional channels of ten-membered rings, and the size of the pores is 0.44nm×0.55nm. Due to its more suitable pore structure and acidity, ZSM-22 molecular sieve has good catalytic performance in alkane isomerization reaction, especially Pt / ZSM-22 molecular sieve has important application in hydroisomerization reaction. At the same time, it also exhibits good catalytic performance in the toluene-methanol alkylation reaction. [0003] In the synthesis of ZSM-22 molecular sieve system, the TON topological orientation of the template agent lacks specificity, and ZSM-22 molecular sieve is a metastable zeolite, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/03
Inventor 王龙张梓钧明曰信刘环昌陈文勇彭立
Owner SHANDONG QILU HUAXIN HIGH TECH
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