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Synthetic method of small-crystal-grain nano zeolite molecular sieve

A nano-zeolite and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminum silicate zeolite, etc.

Active Publication Date: 2016-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the methods described in the above patents, the fine temperature control method used in the present invention is rarely used to prepare uniform nano-sized ZSM-5 zeolite, and it is basically static crystallization without stirring during the crystallization process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Synthesis method: add 10g water, 0.1g aluminum sulfate octadecahydrate, 2g sodium hydroxide solution with a mass fraction of 30%, 4g sodium fluoride, and 13g tetrapropylammonium bromide into the reaction kettle, stir evenly, and then add 6g mass fraction For 40% silica sol, stir for 30 minutes, and age the gel for 8 hours at room temperature. Afterwards, under stirring at 150rpm, the room temperature was programmed to rise to 60°C at 0.83°C / min. After crystallization for 1 day, the temperature was programmed to rise to 100°C at 0.83°C / min. After 2 days of crystallization, the temperature was programmed to rise to 180°C at 0.83°C / min. 3 days. After cooling to room temperature, wash and centrifuge three times with deionized water, and dry at 80°C for 12 hours to obtain the final product.

[0022] The obtained product has the characteristic diffraction peak of ZSM-5, and has higher crystallinity. The SEM photographs of the obtained product with different magnifications c...

Embodiment 2

[0024] Synthesis method: Add 2g of 30% sodium hydroxide solution, 10g of water, 0.1g of aluminum sulfate octadecahydrate, 4g of sodium fluoride, and 5g of tetrapropylammonium bromide into the reaction kettle, stir well, and then add 6g of The silica sol with a fraction of 40% was stirred for 30 minutes, and the gel was aged for 8 hours at room temperature. Afterwards, under stirring at 150rpm, the room temperature was programmed to rise to 60°C at 1°C / min. After crystallization for 1 day, the temperature was programmed to rise to 100°C at 1°C / min. After 2 days of crystallization, the temperature was programmed to rise to 180°C at 1°C / min. 3 days. After cooling to room temperature, wash and centrifuge three times with deionized water, and dry at 80°C for 12 hours to obtain the final product.

[0025] According to the XRD characterization results of the sample, it can be seen that the product has the characteristic diffraction peak of ZSM-5, and the SEM photo shows that the sam...

Embodiment 3

[0027] Synthesis method: Add 2g of 30% sodium hydroxide solution, 0.1g of aluminum sulfate octadecahydrate, 0.54g of sodium fluoride, and 8g of tetrapropylammonium bromide into 10g of water, stir well, then add 6g of % silica sol, stirred for 30min, and aged for 8h at room temperature. Afterwards, under 150rpm stirring, the room temperature was programmed to rise to 80°C at 0.75°C / min. After crystallization for 1 day, the temperature was programmed to rise to 120°C at 0.75°C / min. After 2 days of crystallization, the temperature was programmed to rise to 180°C at 0.75°C / min. 3 days to get the final product. XRD shows that the sample has the characteristic diffraction peak of ZSM-5, and the SEM photo shows that the sample is a small particle nano-molecular sieve with a size of about 100nm.

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Abstract

The invention belongs to the technical field of synthesizing zeolite molecular sieves, and particularly provides a preparation method for synthesizing a small-crystal-grain nano zeolite molecular sieve with temperature controlled. In the field of synthesizing molecular sieves, particle size control on zeolite crystals is an important factor. In the method, the nano ZSM-5 zeolite is prepared with an accurate-control temperature programming reaction process. The method is simple in process and is low in operation cost. Sample XRD shows that the product is ZSM-5 zeolite and has excellent crystalline degree. SEM shows the zeolite is less in nano particle size.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve synthesis, in particular to a method for synthesizing small-grain nano-zeolite molecular sieves. Background technique [0002] Zeolite is an aluminosilicate with a tetrahedral framework structure. Because of its molecular sieving effect, it is usually called zeolite molecular sieve and is one of the most widely used substances in inorganic materials. Among them, ZSM-5, as a very important synthetic zeolite, was synthesized by Mobil Petroleum Company Argauer and Landelt in 1972 using tetrapropylamine as a template, becoming the first important member of the "Pentasil" family. [0003] Nanoparticles belong to mesoscopic substances, between atomic clusters and macroscopic objects, and their grain size is generally smaller than several hundred nanometers. The ratio of the number of atoms on the surface of nanoparticles to the total number of atoms in the bulk increases with the decrea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
Inventor 史静滕加伟谢在库
Owner CHINA PETROLEUM & CHEM CORP