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Preparation method of composite zeolite with core/shell structure

A technology of composite zeolite and core-shell structure, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc. It has the advantages of good thermal and hydrothermal stability, simplified synthesis steps, and easy industrialization.

Inactive Publication Date: 2014-12-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This is because the grain size of Y-type zeolite is about 1 μm, and the grain size of ZSM-5 zeolite is much larger than this. Large ZSM-5 zeolite is very difficult. Due to the effect of steric hindrance, the growing ZSM-5 zeolite grains are far apart in the end, and it is difficult to wrap the Y-type zeolite crystals for growth, and it is impossible to obtain Y-type zeolite crystals. Zeolite as core, core / shell structure composite zeolite with ZSM-5 zeolite as shell

Method used

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  • Preparation method of composite zeolite with core/shell structure
  • Preparation method of composite zeolite with core/shell structure
  • Preparation method of composite zeolite with core/shell structure

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Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0012] At room temperature, add 10g of high-silicon Y-type zeolite with a silicon-aluminum atomic ratio of 5, 0.8g of sodium hydroxide, 9g of tetraethylammonium bromide and 3g of ammonia water into 90g of deionized water, stir well, and then Slowly add 24g of silica sol with a mass percentage of 40% and mix evenly, then move it into a stainless steel reaction kettle, crystallize at 180°C for 72h, then cool it to room temperature with tap water, wash the product with distilled water until it is neutral, and filter it at 100°C ℃ drying in an oven for 12 hours, and then calcining in a muffle furnace at 550 ℃ for 6 hours under the condition of ventilation. Combined with XRD and SEM analysis, it shows that the obtained sample is a high-silicon Y-type zeolite as the nucleus, nano-polycrystalline ZSM -5 zeolite is the core / shell compound zeolite shell, and the EDS analysis shows that the silicon-aluminum atomic ratio of ZSM-5 is 15.

Embodiment approach 2

[0014] At room temperature, add 5 g of high-silicon Y-type zeolite with a silicon-aluminum atomic ratio of 2.5, 0.4 g of sodium hydroxide, and 2 g of tetrapropylammonium bromide into 80 g of deionized water. After stirring evenly, slowly drop Add 30g of silica sol with a mass percentage of 20% and mix evenly, move it into a stainless steel reaction kettle, crystallize at 170°C for 28h, then cool it to room temperature with tap water, wash the product with distilled water until it is neutral, filter it, and put it in a 100°C Dry it in an oven for 12 hours, then bake it in a muffle furnace at 550°C for 6 hours under the condition of air ventilation. Combined with XRD and SEM analysis, it shows that the obtained sample is a nano-polycrystalline ZSM-5 with high silicon Y-type zeolite as the nucleus. The zeolite is a core / shell type composite zeolite, and the EDS analysis shows that the silicon-aluminum atomic ratio of ZSM-5 is 20.

Embodiment approach 3

[0016] At room temperature, add 20g of high-silicon Y-type zeolite with a silicon-aluminum atomic ratio of 10, 1g of sodium hydroxide, and 3.7g of ethylenediamine into 100g of deionized water. After stirring evenly, slowly add 20g of After mixing evenly with 40% silica sol, move it into a stainless steel reaction kettle, crystallize at 160°C for 24h, then cool it to room temperature with tap water, wash the product with distilled water until neutral, filter, and dry in an oven at 100°C for 12h , in a muffle furnace at 550 ° C, roasted under the condition of air for 6 hours, combined with XRD and SEM analysis shows that the obtained sample is a high-silicon Y-type zeolite as the core, with nano-polycrystalline ZSM-5 zeolite as the shell Core / shell type composite zeolite, EDS analysis shows that the atomic ratio of silicon to aluminum of ZSM-5 is 25.

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Abstract

The invention discloses a preparation method of composite zeolite with a core / shell structure, belonging to the fields of fine chemical engineering and inorganic materials. The preparation method is characterized by being a preparation method of composite zeolite taking high-silicon Y type zoelite as a core and taking nano-polycrystalline ZSM-5 zeolite as a shell. The method takes the high-silicon Y type zoelite as a raw material and obtains the product by one-step crystallization by using a conventional template. According to the preparation method, the difficulty that the conventional methods cannot synthesize the core / shell type composite zoelite which takes Y type zoelite as a core and takes ZSM-5 zeolite as a shell is solved. The shell layer is a nano-polycrystalline ZSM-5 zeolite layer, and from the shell to the core, the spreading course is unique, the spreading route is greatly shortened and a hierarchical pore structure among nanocrystals exists on the surface, so that the composite zeolite with the core / shell structure has potential application value in the aspects of catalytic cracking, hydrogen cracking and the like in the fine chemical engineering and the petrochemical engineering.

Description

technical field [0001] A method for preparing a composite zeolite with a core-shell structure belongs to the fields of fine chemicals and inorganic materials. Specifically, the industrial high-silicon Y-type is used as a raw material to obtain high-silicon Y-type zeolite as the core, and nano-polycrystalline ZSM-5 zeolite A method for preparing a composite zeolite having a core / shell structure as a shell. technical background [0002] Y-type zeolite is the main active component of catalytic cracking catalyst, and the preparation and modification of Y-type zeolite are closely related to the performance of catalytic cracking catalyst. In the past ten years, researchers have spent considerable energy on modifying Y-type zeolite, among which preparing composite zeolite materials of Y-type zeolite and other zeolites is an effective way. Composite zeolite or combined channel zeolite is a new type of zeolite material newly developed in recent years. Such materials mainly use spec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40C01B39/04
Inventor 郑家军李瑞丰潘梦刘宇键田辉平马静红
Owner TAIYUAN UNIV OF TECH
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