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Nanometer hollow H type ZSM-5 molecular sieve, and preparation method thereof

A technology of ZSM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of catalytic performance degradation, catalytic activity deactivation, deactivation, etc., and achieve a solution Easy to deposit carbon, improve adsorption characteristics, and reduce contact effects

Inactive Publication Date: 2019-01-11
QINGDAO UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the catalytic reaction, the catalytic performance of ZSM-5 molecular sieve is closely related to its grain size, specific surface area, pore structure, acidity and other physical and chemical parameters; especially in the catalytic cracking of long-chain alkanes, C4 alkylation, low-temperature catalytic oxidation of volatile organic compounds In reactions such as ZSM-5, the service life of ZSM-5 molecular sieves is easily affected by factors such as its surface structure, thermal stability, acidic carbon and other reaction intermediate species, which will lead to a decrease in its catalytic performance or even inactivation.
Although high-temperature calcination of deactivated molecular sieve catalytic materials is an important means to achieve local regeneration of their active sites, high-temperature calcination will also cause changes in molecular sieve structure and surface properties, especially for noble metal or metal oxide-supported ZSM-5 catalysts. The process will cause the agglomeration and sintering of metal particles, resulting in irreversible complete deactivation of catalytic activity.

Method used

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  • Nanometer hollow H type ZSM-5 molecular sieve, and preparation method thereof
  • Nanometer hollow H type ZSM-5 molecular sieve, and preparation method thereof
  • Nanometer hollow H type ZSM-5 molecular sieve, and preparation method thereof

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preparation example Construction

[0021] The preparation method of nanometer hollow H type ZSM-5 molecular sieve, carries out according to the following steps:

[0022] 1. Taking tetraethyl orthosilicate as silicon source, sodium metaaluminate as aluminum source, and tetrapropyl ammonium hydroxide as organic template; wherein the molar ratio of silicon source, aluminum source, organic template and water is 1: (0.01~0.04):(0.1~0.4):(5~15).

[0023] 2. Dissolve tetraethyl orthosilicate and sodium metaaluminate in deionized water to form a clear solution, slowly add tetrapropylammonium hydroxide to the solution, and stir at 30-50°C for 4-6h.

[0024] 3. Transfer the above solution to a reaction kettle lined with polytetrafluoroethylene, first crystallize at 100-140°C for 2-4 hours, then crystallize at 170-200°C for 18-24 hours, then cool to room temperature, and centrifuge Wash until neutral, dry in an oven at 100°C, place in a muffle furnace, heat up to 400-600°C and bake for 5-10 hours to obtain Na-type ZSM-5 ...

Embodiment 1

[0029] The preparation method of nanometer hollow H type ZSM-5 molecular sieve, carries out according to the following steps:

[0030] 1. Weigh 15.6 g of tetraethyl orthosilicate, 0.123 g of sodium metaaluminate, 12.18 g of tetrapropyl ammonium hydroxide solution with a mass fraction of 25%, and 7 g of deionized water.

[0031] 2. Dissolve tetraethyl orthosilicate and sodium metaaluminate in deionized water according to the amount weighed above to form a clear solution, slowly add tetrapropylammonium hydroxide to the solution, and stir at 30°C for 6h.

[0032] 3. Transfer the solution obtained in step 2) to a reaction kettle lined with polytetrafluoroethylene, first crystallize at 120°C for 2h, then crystallize at 170°C for 24h, then cool to room temperature, and use a 6000r / min centrifuge Centrifuge and wash with deionized water until neutral, oven-dried at 100°C, place in a muffle furnace, heat up to 550°C and roast for 6 hours to obtain Na-type ZSM-5 powder;

[0033] 4. Pu...

Embodiment 2

[0041] Example 2: The only difference between this embodiment and Example 1 is that the mixing and stirring time of the silicon source, the aluminum source, and the template agent in step 2 is 6 hours.

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Abstract

The invention belongs to the field of catalytic material preparation, and more specifically relates to a nanometer hollow H type ZSM-5 molecular sieve, and a preparation method thereof. The preparation method comprises following steps: a Na type molecular sieve is added into an inorganic aqueous alkali for treatment, ice-water cooling, centrifugation washing, and drying are carried out, ammonium exchange is adopted, sintering is carried out so as to obtain the H type ZSM-5 molecular sieve (HZSM-5) with a nanometer hollow structure. The preparation method is short in synthesis period, and simple in technology process. The H type ZSM-5 molecular sieve prepared using the preparation method possesses a nanometer scale meso pore-micropore multistage pore composite structure; the specific surface area and the exterior surface area are larger; and the H type ZSM-5 molecular sieve can be used in a plurality of catalytic reactions as a catalyst or an active component carrier material.

Description

technical field [0001] The invention belongs to the field of preparation of catalytic materials, in particular to a nano hollow H-type ZSM-5 molecular sieve and a preparation method thereof. Background technique [0002] ZSM-5 molecular sieve catalyst has high specific surface area, regular pore structure and adjustable surface acidity, and is widely used in petroleum refining, fine chemical industry, gas separation and purification and other fields. It can be directly used as an adsorption or catalytic material, and can also be used as a support material for a variety of supported catalysts for a variety of catalytic reactions such as C4 alkylation, NO x Selective catalytic reduction, VOCs catalytic oxidation, etc. [0003] In the catalytic reaction, the catalytic performance of ZSM-5 molecular sieve is closely related to its grain size, specific surface area, pore structure, acidity and other physical and chemical parameters; especially in the catalytic cracking of long-c...

Claims

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Application Information

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IPC IPC(8): C01B39/40
CPCC01B39/40
Inventor 张传辉曾凯王超邓志勇
Owner QINGDAO UNIV
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