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Method for preparing high performance zsm-5 molecular sieve in solid phase system

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of no molecular sieve morphology control, and achieve high crystallinity, high efficiency, simple steps

Active Publication Date: 2020-01-07
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there has been no report on the regulation of the morphology of molecular sieves in solid-phase synthesis.

Method used

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  • Method for preparing high performance zsm-5 molecular sieve in solid phase system
  • Method for preparing high performance zsm-5 molecular sieve in solid phase system
  • Method for preparing high performance zsm-5 molecular sieve in solid phase system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take by weighing 13.15g sodium silicate nonahydrate, 3.47g fumed silica, 0.25g sodium metaaluminate, 2.4g tetrapropylammonium bromide, 4.2g ammonium chloride, 0.14g urea, 0.25gZSM-5 molecular sieve (crystal Seed, seed), put into the pulverizer and pulverize, so that the solid reactants are evenly mixed. Then the raw material was transferred to a 100ml polytetrafluoroethylene-lined stainless steel autoclave, and placed in an oven for crystallization at 180°C for 48h. After the crystallization is completed, the product is washed, filtered, and dried, and then calcined at 550° C. for 6 hours to obtain a high-performance ZSM-5 molecular sieve synthesized by solid phase.

[0041] figure 1 It is the XRD characterization result of the product, it can be seen that the product has a typical MFI structure and has a good relative crystallinity.

[0042] figure 2 It is the SEM scanning electron microscope photo of the product. It can be seen that the particle size of the product ...

Embodiment 2

[0047] Take by weighing 13.15g sodium silicate nonahydrate, 3.47g fumed silica, 0.25g sodium metaaluminate, 2.4g tetrapropylammonium bromide, 4.2g ammonium chloride, 0.4g urea, 0.25g ZSM-5 molecular sieve ( Seed, seed), put into pulverizer and pulverize, make the solid reactants mix evenly. Then the raw material was transferred to a 100ml polytetrafluoroethylene-lined stainless steel autoclave, and placed in an oven for crystallization at 180°C for 48h. After the crystallization is completed, the product is washed, filtered, and dried, and then calcined at 550° C. for 6 hours to obtain a high-performance ZSM-5 molecular sieve synthesized by solid phase.

[0048] Image 6 It is the XRD characterization result of the product, it can be seen that the product has a typical MFI structure and has a good relative crystallinity.

[0049] Figure 7 It is the SEM scanning electron microscope photo of the product. It can be seen that the particle size of the product is 0.7-5 μm, where...

Embodiment 3

[0051] Take by weighing 13.15g sodium silicate nonahydrate, 3.47g fumed silica, 0.25g sodium metaaluminate, 2.4g tetrapropylammonium bromide, 4.2g ammonium chloride, 0.8g urea, 0.25g ZSM-5 molecular sieve ( Seed, seed), put into pulverizer and pulverize, make the solid reactants mix evenly. Then the raw material was transferred to a 100ml polytetrafluoroethylene-lined stainless steel autoclave, and placed in an oven for crystallization at 180°C for 48h. After the crystallization is completed, the product is washed, filtered, and dried, and then calcined at 550° C. for 6 hours to obtain a high-performance ZSM-5 molecular sieve synthesized by solid phase.

[0052] Figure 8 It is the XRD characterization result of the product, it can be seen that the product has a typical MFI structure and has a good relative crystallinity.

[0053] Figure 9 It is the SEM scanning electron microscope photo of the product. It can be seen that the particle size of the product is 0.7-5 μm, wher...

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Abstract

The invention discloses a method for preparing a high-performance ZSM-5 molecular sieve in a solid phase system, and relates to the field of molecular sieve synthesis. The method comprises the following steps: crushing and mixing a solid phase silicon source, an aluminum source, a templating agent, ammonium or amine substance and seed crystal, ensuring that crystallization reaction is performed at 120 to 220 DEG C and the crystallization reaction time is 2 to 168 h, and performing filtering, washing and calcining on an obtained product, so as to obtain the high-performancne ZSM-5 molecular sieve, wherein the ammonium or amine substance adopts one or a mixture of ammonium chloride, urea, lauryl amine, cetylamine and 1, 6-hexamethylenediamine. An obtained product through the method has not only high methanol-to-gasoline activity and reaction life, but also the characteristics of high degree of crystallinity, low external surface area and high performance. The method is simple is step and high in efficiency, does not produce waste water pollution, realizes a green synthesis path, reduces the production cost, and has industrial application value and social benefit.

Description

technical field [0001] The invention relates to the field of synthesis of molecular sieves, in particular to a method for preparing high-performance ZSM-5 molecular sieves in a solid phase system. Background technique [0002] Molecular sieves are important inorganic functional materials that play key roles in catalytic processes due to their tunable acidity and shape selectivity. The ZSM-5 molecular sieve widely used in the petrochemical industry is a microporous silica-alumina molecular sieve, which has two intersecting ten-membered ring channel systems with a pore size of about 0.55nm. One of the straight channels is parallel to the b-axis direction, and the other Z The font channel is parallel to the c-axis direction. The pore size of ZSM-5 is suitable for industrial catalytic processes such as selective dewaxing of petroleum, xylene isomerization and methanol alkylation. [0003] However, due to the limitation of the ZSM-5 pore size, the product macromolecules cannot ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03
Inventor 刘子玉吴丹陈新庆任淑丘明煌金秋魏伟孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI