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Application and preparation method of ZSM-5 molecular sieve with mesopores and micropores

A technology of ZSM-5 and molecular sieve, which is applied in the field of catalyst preparation, can solve the problems of economy, high environmental protection cost, complex synthesis procedure, molecular sieve loss, etc., and achieve the effect of low cost, simple synthesis method and simple steps

Active Publication Date: 2016-07-06
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In comparison, the direct synthesis method often needs to use a large amount of microporous templates and mesoporous templates at the same time, so the synthesis procedure is complicated, and the economic and environmental protection costs are high.
Although the alkaline solution post-treatment method does not need to use mesoporous template agent, the method is simple and easy, but it will cause the loss of molecular sieve and introduce mesoporous disorder

Method used

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  • Application and preparation method of ZSM-5 molecular sieve with mesopores and micropores
  • Application and preparation method of ZSM-5 molecular sieve with mesopores and micropores
  • Application and preparation method of ZSM-5 molecular sieve with mesopores and micropores

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Stir and mix Tetraethyl Silicate (TEOS), Tetrapropylamine Hydroxide (TPAOH), Aluminum Isopropoxide, and Deionized Water in a molar ratio of 1:0.28:0.03:15, and then add 30wt% of silicon oxide Polyethylene glycol-1000 was used to make a homogeneous sol, and aged at 100°C for 12 hours to obtain a precursor.

[0043] 150g silica sol (industrial grade, SiO 2 ≥30wt%) was dispersed in 60g of desalinated water, then 80g of NaOH solution with a mass fraction of 15% was added, and fully stirred at room temperature for 0.5 hour to prepare A solution; Mix with aluminum sulfate octadecahydrate, stir and fully dissolve at room temperature for 0.5 hours to prepare solution B; slowly add solution B to solution A, stir thoroughly at room temperature for 1 hour to form a uniform gel, and then transfer the gel to a synthesis kettle , aged with stirring at 100°C for 12h, then heated to 170°C for 20h with stirring and crystallized, cooled to room temperature, filtered and washed. The fil...

Embodiment 2

[0045] Repeat Example 1, but change tetrapropylammonium hydroxide to tetrapropylammonium bromide and polyethylene glycol-1000 to polyethylene glycol-4000 when preparing the precursor. The ZSM-5 sample was obtained after adding the precursor to the silica-alumina gel, which was marked as ZM-2. The relative crystallinity was 98%, and the crystal phase was similar to Example 1. The scanning electron microscope showed that the sample particle size was about 1 μm, spherical The morphology and surface are relatively rough, and the specific surface area of ​​the nitrogen physical adsorption test sample is 540m 2 / g, the total pore volume is 0.37cm 3 / g.

Embodiment 3

[0047] Repeat Example 1, but change polyethylene glycol-1000 to starch when preparing the precursor. The ZSM-5 sample was obtained after adding the precursor to the silica-alumina gel, which was marked as ZM-3. The relative crystallinity was 96%, and the crystal phase was similar to Example 1. The scanning electron microscope showed that the particle size of the sample was about 1-2 μm. , spherical shape, and the surface is relatively rough. The specific surface area of ​​the nitrogen physical adsorption test sample is 552m 2 / g, the total pore volume is 0.35cm 3 / g.

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Abstract

The invention provides an application and a preparation method of a ZSM-5 molecular sieve with mesopores and micropores. The preparation method includes steps of precursor preparation, silica-alumina gel preparation and preparation of the ZSM-5 molecular sieve with the mesopores and micropores.In a preparation process of a hierarchical porous catalyst, consumption of a microporous templating agent and a mesoporous templating agent can be substantially reduced, synthesis steps of the hierarchical porous catalyst are simple, and the synthesized molecular sieve is large in specific surface area, uniform in particle size and controllable in mesopore quantity and size, and intrinsic lipophilicity of the molecular sieve is enhanced due to abundant surface terminal hydroxide radicals. By adoption of the molecular sieve as the catalyst, a method for preparing cyclohexanol by direct hydration of cyclohexene is established, and the catalyst is high in cyclohexene conversion rate and cyclohexanol selectivity.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation methods, and in particular relates to a preparation method and application of a mesoporous ZSM-5 molecular sieve, more specifically, a molecular sieve mainly used for catalyzing the hydration of cyclohexene to prepare cyclohexanol Preparation. Background technique [0002] The direct hydration of cyclohexene is an important method to prepare cyclohexanol, an important chemical raw material. This method overcomes the cyclohexane that exists in the cyclohexane oxidation process for preparing cyclohexanol, which is easy to form an explosive mixture after mixing with air, the production process has poor safety, high energy consumption, high price of process raw material phenol, and large hydrogen consumption. And many other shortcomings, it has the advantages of safe production route, energy saving, good carbon atom economy, environmental friendliness and no waste, etc., and shows advant...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J35/10C07C29/04C07C35/08
CPCC07C29/04B01J29/40B01J2229/37B01J2229/38B01J35/617C07C35/08
Inventor 赵文平耿玉侠马国栋王元平孙承宇杜小宝吕睿张立兴宋辉
Owner CHINA TIANCHEN ENG
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