ZSM-5 molecular sieve and preparation method thereof

A ZSM-5, molecular sieve technology, applied in nanotechnology, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problems of low product yield, high raw material cost, long synthesis cycle, etc. High, low cost of raw materials, short synthesis cycle

Active Publication Date: 2019-11-19
WISON ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing synthetic methods generally have disadvantages such

Method used

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  • ZSM-5 molecular sieve and preparation method thereof
  • ZSM-5 molecular sieve and preparation method thereof
  • ZSM-5 molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Raw material ratio is SiO 2 :Al 2 o 3 :n-Butylamine:Na 2 O:H 2 O=1:0.02:0.13:0.06:10. According to the ratio of raw materials, add 23.60g of sodium metaaluminate, 15.18g of sodium hydroxide and 166.57g of deionized water into the stainless steel crystallization kettle and stir evenly, then add 45.56g of n-butylamine and stir evenly, and finally add 300g of silica gel particles and seal the crystallization After stirring and crystallizing at 110°C for 35 hours, the remaining 666.27g of deionized water was added to the crystallization kettle through a metering pump, and then the crystallization temperature was raised to 170°C to continue crystallization for 20 hours. The product was washed, dried, and Roasting, ion exchange obtain final product, and this product has the characteristic diffraction peak of ZSM-5 through XRD characterization (see image 3 ), the SEM picture shows that the crystal grains of the ZSM-5 molecular sieve are around 150nm (see Figure 4 ).

Embodiment 2

[0047] Raw material ratio is SiO 2 :Al 2 o 3 :n-Butylamine:Na 2 O:H 2 O=1:0.01:0.25:0.10:12. According to the ratio of raw materials, add 10.22g of sodium metaaluminate, 29.60g of sodium hydroxide and 261.82g of deionized water into the stainless steel crystallization kettle and stir evenly, then add 75.93g of n-butylamine and stir evenly, and finally add 260g of silica gel particles and seal the crystal After stirring and crystallizing at 110°C for 40 hours, the remaining 610.91 g of deionized water was added to the crystallization kettle through a metering pump, and then the crystallization temperature was raised to 160°C to continue crystallization for 25 hours. The product was washed, dried, and Roasting, ion exchange obtain final product, and this product has the characteristic diffraction peak of ZSM-5 through XRD characterization (see Figure 5 ), the SEM picture shows that the grains of the ZSM-5 molecular sieve are between 100 and 300nm (see Image 6 ).

Embodiment 3

[0049] Raw material ratio is SiO 2 :Al 2 o 3 :n-Butylamine:Na 2 O:H 2 O=1:0.006:0.360:0.120:15. Add 6.60g of sodium metaaluminate, 40.38g of sodium hydroxide and 472.25g of deionized water into the stainless steel crystallization kettle according to the ratio of raw materials and stir evenly, then add 117.77g of n-butylamine and stir evenly, and finally add 280.05g of silica gel particles and seal Crystallization kettle, after stirring and crystallizing at 110°C for 50h, add the remaining 708.37g of deionized water into the crystallization kettle through a metering pump, and then raise the crystallization temperature to 170°C to continue crystallization for 15h, and the product is washed and dried , roasting, and ion exchange to obtain the final product, which has the characteristic diffraction peak of ZSM-5 through XRD (see Figure 7 ), the SEM picture shows that the grains of the ZSM-5 molecular sieve are between 100 and 200nm (see Figure 8 )

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Abstract

The invention provides a ZSM-5 molecular sieve and a preparation method thereof. The preparation method includes the following steps: a) mixing an aluminum source, an alkali source and part of total water consumption, and then adding a template for mixing; b) adding a silicon source, and stirring the materials at 100 DEG C-120 DEG C for crystallization; and c) adding the remaining water for continuous crystallization at 150 DEG C-180 DEG C to obtain the ZSM-5 molecular sieve. The ZSM-5 molecular sieve with good crystal form, high crystallinity and high yield is prepared by using granular silica gel, the cheap template and a small amount of water and adjusting the template concentration in the crystallization process and changing the crystallization temperature by adding water in stages. The method has the advantages of low cost, short synthesis cycle, simple process and easy industrialization.

Description

technical field [0001] The invention relates to the field of molecular sieve synthesis, in particular to a preparation method of a ZSM-5 molecular sieve. Background technique [0002] ZSM-5 molecular sieve was first successfully synthesized by Mobil Corporation in the 1970s. Since then, because of its special shape-selective catalytic function and high catalytic activity, it has attracted many researchers to conduct in-depth and extensive research on it. The grain size of ZSM-5 molecular sieve has micron and nanometer scales. Generally, the molecular sieve whose average grain size is less than 300nm is defined as nano ZSM-5 molecular sieve. The pore structure of nano ZSM-5 molecular sieve is almost the same as that of traditional micron ZSM-5 molecular sieve, but nano ZSM-5 molecular sieve has smaller grain size, larger specific surface area, shorter channel and higher intracrystalline Advantages such as diffusion rate, its main features are as follows: [0003] (1) Due to...

Claims

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Application Information

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IPC IPC(8): C01B39/40B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B39/40C01P2002/72C01P2004/03C01P2004/62C01P2004/64
Inventor 吴勇军胡治军杨文书
Owner WISON ENG
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