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Modification method of ZSM-5 zeolite

A ZSM-5 modification technology, applied in chemical instruments and methods, crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of reducing the catalytic activity of zeolite and destroying the microporous crystal structure , low micropore surface area, etc., to achieve the effect of increasing the total specific surface area, increasing the BET surface area, and dredging the channels

Active Publication Date: 2012-05-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the prior art still has two obvious disadvantages: one is that the mesopore specific surface area is still relatively low, the highest being CN1530322A, which is close to 250m 2 / g; Second, when higher mesopores are obtained, the microporous crystal structure of ZSM-5 zeolite is severely damaged, and the micropore surface area is too low, which will seriously reduce the catalytic activity of zeolite

Method used

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  • Modification method of ZSM-5 zeolite
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  • Modification method of ZSM-5 zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take 30g of ZSM-5 zeolite and 2400mL of 0.30mol / 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 ZSM-5 zeolite 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 12h, the obtained sample number is CL1.

[0033] Depend on figure 1 It can be seen that the CL1 sample has the XRD characteristic spectrum of ZSM-5 zeolite, and still maintains a good ZSM-5 zeolite structure. Depend on figure 2 It can be seen that after the modification treatment, there is obvious concentration of mesopores in the ZSM-5 zeolite, and the most probable pore diameter is 3.5nm.

Embodiment 2

[0035] Take 1g of ZSM-5 zeolite and 40mL of 0.60mol / L KOH solution in a beaker, stir at room temperature for 30min, transfer to a closed reaction kettle, add 3mL of ethanol, treat at 80°C for 3h, 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

[0037] Take 1g of ZSM-5 zeolite and 70mL of 0.50mol / L NaOH solution in a beaker, stir at room temperature for 30min; then transfer to a closed reaction kettle, add 5mL of propanol, and treat at 100°C for 4h; filter , Washing; put the washed ZSM-5 zeolite in a beaker, add 50mL 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 then place in an oven Dry at 110°C for 12 hours, and the obtained sample number is CL3.

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Abstract

The invention discloses a modification method of a ZSM-5 zeolite. The method comprises: in a closed system containing a low molecular weight organic solvent, first treating a ZSM-5 zeolite with an alkali solution; then treating a ZSM-5 zeolite with an acid solution, and finally conducting separation, washing and drying so as to obtain a modified ZSM-5 zeolite. In the zeolite modification method provided in the invention, the organic solvent added during alkali treatment can promote the generation of a mesoporous structure so as to make a micropore structure convert to a meso-pore efficiently,and can stablize and protect the micropore structure. The subsequent acid treatment can elute amorphous aluminum in a zeolite crystal so as to reach the purposes of dredging pore channels and increasing the total specific surface area. Therefore, the method of the invention can reserve more complete micropores in the ZSM-5 zeolite and provide more mesopores, and simultaneously can increase the total BET (Brunauer-Emmett-Teller) specific surface area.

Description

technical field [0001] The invention relates to a method for modifying zeolite, which belongs to the field of molecular sieve synthesis and modification, in particular to a post-treatment modification method for ZSM-5 zeolite. Background technique [0002] ZSM-5 zeolite is widely used in the petroleum industry because of its regular microporous structure, suitable acidity, good thermal stability and hydrothermal stability. ZSM-5 zeolite has two intersecting pore systems with pore diameters of 5.1×5.5nm and 5.3×5.6nm respectively, which is a typical microporous structure. Microporous ZSM-5 zeolite in the reaction involving macromolecules, its narrow channel (less than 2nm) can easily cause the mass transfer and diffusion resistance of the reaction material to be too large, and it is extremely difficult for the macromolecular reactant to enter the inside of the crystal channel for reaction, so that The catalytic performance of zeolite cannot be fully utilized; and it is also ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J29/40
Inventor 范峰凌凤香王少军杨春雁杨卫亚
Owner CHINA PETROLEUM & CHEM CORP
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