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ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof

A technology of ZSM-11 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem that nano-molecular sieve cannot realize industrial application value, the grain size of nano-molecular sieve is reduced, Solve problems such as poor thermal and hydrothermal stability, achieve good thermal and hydrothermal stability, reduce benzene content, and low cost

Inactive Publication Date: 2013-08-21
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when used as a catalytic material, nano-molecular sieves are easy to coalesce, have poor thermal and hydrothermal stability, difficult regeneration, and filtration and recovery are difficult to achieve industrialization, which are important reasons why nano-molecular sieves cannot realize their industrial application value.
In addition, due to the greatly reduced grain size of nano-molecular sieves, its selectivity to certain products is reduced, which also affects its application value.

Method used

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  • ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof
  • ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof
  • ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Under stirring conditions, prepare the following two working solutions respectively:

[0045] Mixture I: 15g of silica sol (40% SiO 2 , 60%H 2 O, hereinafter the same), 0.97g tetrabutylammonium bromide (99%), 11.3g deionized add in the beaker and mix homogeneously;

[0046] Mixture II: a homogeneous solution prepared from 1.33g of aluminum sulfate, 1.50g of sodium hydroxide and 15g of deionized water;

[0047] Under constant stirring, slowly add mixture II to mixture I, continue to stir until uniform, and the mass ratio of the obtained reaction mixture is Na 2 O:Al 2 o 3 : SiO 2 :(TBA) 2 O:H 2 O=9.0:1.0:50:0.75:1000, transfer the obtained initial gel to a reaction kettle with a polytetrafluoroethylene lining, seal it and place it in a hydrothermal synthesis oven, and keep the temperature at 90°C for 24h, Then the temperature was raised to 150°C and the temperature was maintained for 24h. After the reaction kettle was cooled, the solid was separated from the mot...

Embodiment 2

[0050] Under stirring conditions, prepare the following two working solutions respectively:

[0051] Solution I: Add 15g silica sol, 3.23g tetrabutylammonium bromide, and 40.2g deionized into a beaker and mix well.

[0052] Solution II: a homogeneous solution prepared by 1.33g aluminum sulfate, 2.00g sodium hydroxide and 40g deionized water

[0053] Under continuous stirring, slowly add solution II to solution I, and continue stirring until uniform. The molar ratio of the initial gel is Na 2 O:Al 2 o 3 : SiO 2 :(TBA) 2 O:H 2 O=12.0:1.0:50:2.5:2500. The crystallization conditions are the same as in Example 1. The final product powder is analyzed by X-ray diffraction, and the result is the same as figure 1 (a) are basically consistent, and its morphology measured by scanning electron microscopy is consistent with that of figure 2 (a) match.

Embodiment 3

[0055] The raw materials, composition and process flow of this example are the same as in Example 1, the difference is: after the raw materials are mixed evenly, they are transferred to a reaction kettle with a polytetrafluoroethylene lining, and after sealing, the temperature is kept at 90°C for 384h, and then the temperature is raised Continue constant temperature to 180°C for 8h. The product is ZSM-11 molecular sieve with a crystallinity of 98.39% and a particle size of 1.5 μm. The final product powder is analyzed by X-ray diffraction, and the result is the same as figure 1 (a) are basically consistent, and its morphology measured by scanning electron microscopy is consistent with that of figure 2 (a) match.

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Abstract

A ZSM-11 molecular sieve with a hierarchical porous structure is characterized in that X-X-ray diffraction spectrum of the molecular sieve is as shown in Figure 1(a) / table 1; the molecular sieve has an even spherical appearance, each ball is formed through self assembly of rod-shaped crystallites (Figure 2), the molecular sieve is formed by evenly mixing raw materials of substance containing IVA elements, substance containing IIIA element, alkali metal hydroxide, template and water, and then through two stages of crystallization processes, the molecular sieve product has pure crystalling phase, is relatively high in degree of crystallinity, and has an excellent heat and water heat stability, namely, the method is relatively low in cost, the performance of the ZSM-11 molecular sieve is excellent, and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a ZSM-11 molecular sieve, in particular to a ZSM-11 molecular sieve with a hierarchical pore structure and a preparation method thereof. Background technique [0002] ZSM-11 (MEL) was first synthesized by Mobil in the 1970s. It is a member of the high-silicon ZSM series molecular sieves. It has a tetragonal crystal system and belongs to the Pentasil type zeolite (five-membered ring type zeolite) together with ZSM-5. ZSM-11 and ZSM-5 (MFI) have similar structures and chemical compositions, both of which are cross channel structures composed of ten-membered rings. The difference is that ZSM-11 is a two-dimensional straight channel with a channel size of 0.53*0.54nm ; while the ZSM-5 channel is composed of a straight cylinder and a sinusoidal cross, with a pore size of 0.51*0.56nm. The basic structural units of the two skeletons are connected by silicon (aluminum) oxygen tetrahedra [5 8 ] unit, by sharing edges and forming and b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/36
Inventor 李春义于庆君陈静
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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