Preparation method of mesoporous-microporous zeolite molecular sieve

A microporous zeolite and molecular sieve technology, applied in the field of molecular sieve synthesis and modification, can solve the problems of reducing zeolite catalytic activity, microporous crystal structure damage, low mesopore specific surface area, etc., and achieve BET surface area improvement, high mesopore specific surface area, The effect of increasing the specific surface area

Active Publication Date: 2014-04-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet prior art also has two obvious shortcoming: the one, the produced mesopore specific surface area is still relatively low; The 2nd, when obtaining higher mesopore specific surface area, the microporous crystal structure of microporous zeolite is destroyed more seriously, Too low a pore surface area, which severely reduces the catalytic activity of the zeolite

Method used

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  • Preparation method of mesoporous-microporous zeolite molecular sieve
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  • Preparation method of mesoporous-microporous zeolite molecular sieve

Examples

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Effect test

Embodiment 1

[0037] Take 30g of microporous mordenite and 2400mL of 0.30 mol / L NaOH solution in a beaker, stir at room temperature for 30min, transfer to a closed reaction kettle, add 75mL of methanol, treat at 60°C for 4h, filter and wash . Put the washed mordenite in a beaker, add 1500mL of 0.2mol / L hydrochloric acid solution, stir at room temperature for 20min, transfer to a water bath at 70°C for 3h, filter, wash, and dry in an oven at 110°C for 12h. The obtained sample number is CL1.

[0038] Depend on figure 1 It can be seen that the CL1 sample has the characteristic spectrum of mordenite and still maintains a good zeolite structure. Depend on image 3 It can be seen that after the modification treatment, there is an obvious concentration of mesopores in the microporous mordenite, and the most probable pore diameter is 3.5nm, indicating that after the treatment, a large number of mesoporous structures are formed in the mordenite.

Embodiment 2

[0040] Take 1 g of microporous ZSM-5 zeolite and 40 mL of 0.60 mol / L KOH solution in a beaker, stir at room temperature for 30 min, transfer to a closed reaction kettle, add 3 mL of ethanol, and treat at 80 °C for 3 h. Filter and wash. Put the washed ZSM-5 zeolite in a beaker, add 30mL of 0.2mol / L nitric acid solution, stir at room temperature for 20min, transfer to a water bath at 90°C for 2h, filter, wash, and dry in an oven at 110°C 12h, the obtained sample number is CL2.

Embodiment 3

[0042] Take 30 g of microporous β, 2100 mL of 0.50 mol / L NaOH solution in a beaker, stir at room temperature for 30 min; then transfer to a closed reaction kettle, add 150 mL of propanol, and treat at 100 ° C for 4 h; filter , Washing; put the washed zeolite beta into a beaker, add 1500mL of 0.8mol / L sulfuric acid solution, stir at room temperature for 30min, transfer to a water bath at 90°C for 3h, filter, wash, and place in an oven for 110 ℃ drying for 12h, the obtained sample number is CL3.

[0043] Depend on figure 2 It can be seen that the CL3 sample has the characteristic spectrum of zeolite beta and still maintains a good structure of zeolite beta. Depend on Figure 4 It can be seen that after the modification treatment, there is an obvious concentration of mesoporous pore diameters in the microporous zeolite β, and the most probable pore diameter is 3.5 nm.

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Abstract

The invention discloses a preparation method of a mesoporous-microporous zeolite molecular sieve. The method comprises the steps of: firstly, treating microporous zeolite in a closed system containing an organic solvent with low molecular weight by utilizing alkali solution; secondly, treating the microporous zeolite by acid solution; and lastly, separating, washing and drying to obtain the mesoporous-microporous zeolite. According to a modification method of the zeolite provided by the invention, when the alkali is treated, the generation of a mesoporous structure is promoted by the added organic solvent, so that a microporous structure is more effectively converted to a mesopore while the microporous structure is stabilized and protected; and amorphous alumina in a zeolite crystal can be eluted by a sequential acid treatment process, so that a hole channel is dredged and a total specific surface area is increased, thus the method provided by the invention can be used for keeping more integrated micropores in the mesoporous-microporous zeolite, providing more mesopores and increasing the BET (Brunauer Emmett Teller) specific surface area.

Description

technical field [0001] The invention relates to a preparation method of mesoporous-microporous zeolite molecular sieve, which belongs to the field of synthesis and modification of molecular sieves. Specifically, a kind of mesoporous-micropore composite channel system is prepared by modifying a type of microporous zeolite. Zeolite molecular sieve. Background technique [0002] Microporous zeolites are widely used in the petroleum industry because of their regular micropore structure, suitable acidity, good thermal stability and hydrothermal stability. However, microporous zeolite inevitably has some natural defects. Its narrow pores (less than 2nm) can easily cause excessive mass transfer and diffusion resistance of reaction materials in reactions involving macromolecules, and it is extremely difficult for macromolecular reactants to enter the crystal pores. In this way, the catalytic performance of zeolite cannot be fully utilized; and it is also difficult for macromolecula...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
Inventor 范峰凌凤香王少军杨春雁杨卫亚
Owner CHINA PETROLEUM & CHEM CORP
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