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Preparation method of nano ZSM-5 molecular sieve

A technology of ZSM-5 and molecular sieve, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of product separation and collection difficulties, low synthesis efficiency, environmental pollution, etc., and achieve high synthesis efficiency , easy operation, large specific surface area effect

Inactive Publication Date: 2018-11-13
SHENYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a simple, efficient, environment-friendly and easy-to-industrial production method for overcoming the defects of difficult product separation and collection, low synthesis efficiency and environmental pollution in the existing nano ZSM-5 molecular sieve synthesis technology

Method used

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  • Preparation method of nano ZSM-5 molecular sieve
  • Preparation method of nano ZSM-5 molecular sieve
  • Preparation method of nano ZSM-5 molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The feature of the nano ZSM-5 molecular sieve prepared by the present invention is characterized by the following methods:

[0035] The phase structure and crystallinity of molecular sieves were characterized by powder X-ray diffraction (XRD).

[0036] The crystal morphology and size of molecular sieves can be observed intuitively by scanning electron microscope (SEM) and transmission electron microscope (TEM).

[0037] The nitrogen adsorption experiment was used to measure the surface area, isotherm adsorption curve and pore size distribution of the molecular sieve, and judge its pore structure.

[0038]A kind of preparation method of nanometer ZSM-5 molecular sieve, the high molecular polymer polyvinylpyrrolidone of 3.2g is dissolved in the deionized water of 40.0g, room temperature is stirred to fully dissolving, forms mixed solution A; Adds the aluminum source of 0.2g and 10.4g of silicon source, continue to stir at constant temperature until it is uniformly mixed ...

Embodiment 2

[0041] A preparation method of nanometer ZSM-5 molecular sieves, comprising: dissolving 1.6g of high molecular polymer polyvinylpyrrolidone in 40.0g of deionized water, stirring at room temperature until completely dissolved to form mixed solution A; adding 0.2g of aluminum source in turn and 10.4g of silicon source, continue to stir at constant temperature until they are uniformly mixed to form solution B; then add 3.0g of structure directing agent dropwise to solution B to form a mixed solution, and stir and age the above mixed solution in a constant temperature water bath at 60°C for 24 hours to form a sol-gel Glue; Dry the above-mentioned sol-gel to obtain dry glue, transfer the ground dry glue to a crystallization kettle, use steam-assisted crystallization to realize the molecular sieve crystallization process, crystallize at 180°C for 36h, and the obtained product is filtered, Dry to obtain the molecular sieve powder. Put the original molecular sieve powder in a muffle f...

Embodiment 3

[0043] A kind of preparation method of nanometer ZSM-5 molecular sieve: the polymer polyvinylpyrrolidone of 6.4g is dissolved in the deionized water of 40.0g, stirs at room temperature until completely dissolving, forms mixed solution A; Adds the aluminum source of 0.2g and 10.4g of silicon source, continue to stir at constant temperature until it is uniformly mixed to form solution B; then add 3.0g of structure directing agent dropwise to solution B to form a mixed solution, and stir and age the above mixed solution in a constant temperature water bath at 60°C for 24 hours to form a sol-gel Dry the above-mentioned sol-gel to obtain dry glue, transfer the ground dry glue to a crystallization kettle, use steam-assisted crystallization method to realize the molecular sieve crystallization process, crystallize at 180°C for 36h, and the obtained product is filtered and dried Dry to obtain molecular sieve powder. Put the original molecular sieve powder in a muffle furnace and roast...

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Abstract

The invention belongs to the technical field of synthesis of zeolite molecular sieves, aims at providing a preparation method of a green and simple nano ZSM-5 molecular sieve, and in particular relates to a method for preparing the nano ZSM-5 molecular sieve through adding a high molecular polymer, a silicon source, an aluminum source, an organic structure directing agent and de-ionized water intoa synthesis process and uniformly mixing to form sol-gel of a molecular sieve synthetic precursor, and then preparing the sol-gel into dry glue, and utilizing a water steam assisted crystallization method. According to the method provided by the invention, the prepared nano ZSM-5 molecular sieve has the characteristics of relatively high crystallization degree, the crystal size capable of being regulated to be between 10 and 100nm, a mesoporous-micropore composite multi-grade structure, relatively great specific surface area and the like. According to the preparation method of the nano ZSM-5molecular sieve, provided by the invention, the technical defects that the nano molecular sieve is difficult to separate and collect from a mother solution, a lot of synthetic waste liquid is discharged and the like are avoided, and the synthesis efficiency also can be improved; the preparation method is a simple and efficient, and environment-friendly synthetic route and has a certain industrialized application prospect.

Description

technical field [0001] The invention relates to the technical field of synthesis of zeolite molecular sieves, in particular to provide a green and simple preparation method of nanometer ZSM-5 molecular sieves. Background technique [0002] ZSM-5 molecular sieve is a new type of crystalline aluminosilicate material successfully developed in 1972 by Mobile Oil Company of the United States. Due to its excellent channel shape selectivity, suitable acidity and good hydrothermal stability, it has gradually become one of the most important catalytic materials in the petroleum refining and chemical industry. However, because it only contains micropores, the mass transfer and diffusion capacity is limited, which not only cannot effectively catalyze the conversion of macromolecular raw materials, but also easily causes catalyst carbon deposition and deactivation. Compared with conventional micron ZSM-5 molecular sieves, the grain size of nano ZSM-5 molecular sieves is generally less ...

Claims

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Application Information

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IPC IPC(8): C01B39/40B82Y30/00
CPCB82Y30/00C01B39/40C01P2002/72C01P2004/03C01P2004/04C01P2004/64
Inventor 赵震肖霞范晓强孔莲于学华
Owner SHENYANG NORMAL UNIV
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