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Method for preparing ZSM-22 molecular sieve by using seed crystal synthesis method

A technology of molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of ZSM-22 that have not been reported, and achieve the effects of shortening the crystallization time, good catalytic activity, and low price

Active Publication Date: 2013-05-15
ZHEJIANG JIRUITONG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is an organic template in the synthesis of ZSM-22 zeolite at home and abroad, and there is no report on the route of synthesizing ZSM-22 without a template

Method used

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  • Method for preparing ZSM-22 molecular sieve by using seed crystal synthesis method
  • Method for preparing ZSM-22 molecular sieve by using seed crystal synthesis method
  • Method for preparing ZSM-22 molecular sieve by using seed crystal synthesis method

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: synthetic ZSM-22 seed crystal

[0020] First, 10.4g H 2 O mixed with 0.07g aluminum sulfate, then added 0.22g KOH to it, stirred and clarified, added 0.43g 1,6-hexanediamine (DAH), then added 3g tetraethyl orthosilicate (TEOS) under stirring, continued After stirring until the solution became uniform, the reaction raw materials were added to a polytetrafluoroethylene stainless steel dynamic tank, the dynamic kettle speed was 30 rpm, crystallization was complete at 160°C for 34 hours, the product was suction filtered, and dried to obtain the product.

[0021] Its structure is ZSM-22 zeolite molecular sieve through X-ray diffraction analysis, and it can be seen from scanning electron microscope photos that the product obtained by the seed crystal method has high purity.

[0022] attached figure 1 It is the scanning electron microscope photo (SEM) of the synthesized seed crystal. From the photo, we can see some rod-shaped or needle-shaped products, which sh...

Embodiment 2

[0023] Embodiment 2: The impact of crystallization time on ZSM-22 prepared by seed crystal method

[0024] First, 17g H 2 O and 0.192g of aluminum sulfate were mixed evenly, and then 0.209g of KOH was added to it, and after stirring and clarification, 3g of tetraethyl orthosilicate (TEOS) was added, and the stirring was continued until the solution became uniform, and 5% ZSM-22 molecular sieve was added as a seed crystal ( The amount of seed crystals is represented by input SiO 2 mass percent calculation). Then the reaction raw materials were added into a polytetrafluoroethylene stainless steel reaction kettle, the dynamic kettle rotation speed was 30rpm, crystallized at 140°C for 0.5-5 days respectively, the product was suction filtered, and the product was obtained after drying.

[0025] It can be found that ZSM-22 containing a lot of amorphous is obtained when crystallization is 0.5 days and 1 day; substantially pure ZSM-22 is obtained when crystallization is 1.5 days; ZS...

Embodiment 4

[0030] Example 4: Substituting NaOH for KOH as alkali source

[0031] First, 11.5g H 2 O and 0.096g of aluminum sulfate are mixed evenly, then 0.18g of NaOH is added to it, after stirring and clarification, 3g of tetraethyl orthosilicate (TEOS) is added, and the stirring is continued until the solution becomes uniform, then 5% ZSM-22 molecular sieve is added as a seed crystal (crystal The amount of seed is represented by input SiO 2 mass percent calculation). Then the reaction raw materials were added into a polytetrafluoroethylene stainless steel reaction kettle, the dynamic kettle speed was 30rpm, the crystallization was completed at 140°C for 2 days, and the product was suction filtered and dried to obtain ZSM-22.

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Abstract

The invention relates to a preparation method of a molecular sieve, and provides a method for preparing ZSM-22 molecular sieve by using a seed crystal synthesis method. The method comprises the following steps of: uniformly mixing deionized water with aluminum sulfate; adding alkali sources into a mixture; adding tetraethoxysilane under stirring; continuously stirring until the solution is uniform to form silicon-aluminum gel; adding ZSM-22 molecular sieve crystal seed to stir; putting the mixture into a reaction kettle for crystallization reaction; and filtering and drying a product to obtain ZSM-22 molecular sieve raw powder. By using the preparation method, the application of organic template agent is eliminated, the crystallization time is shortened, the crystallization temperature is reduced, and the industrial application is facilitated; the product keeps good crystallization degree and purity and high catalytic reaction activity; the unnecessary loss during production is reduced; the product has a potential application value on some important catalytic reaction; and inorganic raw materials used in production is environmentally-friendly and low in cost.

Description

technical field [0001] The invention belongs to a molecular sieve preparation method, in particular to a method for preparing a ZSM-22 molecular sieve by a seed crystal synthesis method. Background technique [0002] Zeolite molecular sieve is a kind of microporous crystal material with skeleton structure. Due to its structural and performance characteristics, it has been widely used in various fields such as catalysis, adsorption and ion exchange. In addition to its great role in the traditional chemical industry, zeolite is now slowly showing its development potential in other related material fields. [0003] In the 1980s, Mobil Corporation of the United States developed ZSM-22 zeolite, whose skeleton includes five-membered rings, six-membered rings, and ten-membered ring structures. It is a high-silicon molecular sieve material with a TON topology. Because ZSM-22 has good reaction selectivity and reactivity, it will continue to play a good catalytic role in catalytic d...

Claims

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Application Information

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IPC IPC(8): C01B39/02
Inventor 孟祥举王叶青王雄吴勤明肖丰收
Owner ZHEJIANG JIRUITONG NEW MATERIAL CO LTD
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