Preparation method of mesopore-micropore zeolite molecular sieve

A technology of microporous zeolite and molecular sieve, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of reducing the catalytic activity of zeolite, low micropore surface area, damage to the micropore crystal structure, etc., and achieve the effect of improving the BET surface area.

Active Publication Date: 2014-07-23
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 mesopore-micropore zeolite molecular sieve
  • Preparation method of mesopore-micropore zeolite molecular sieve
  • Preparation method of mesopore-micropore zeolite molecular sieve

Examples

Experimental program
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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, place it in an ultrasonic cleaner (4.12W / 100mL alkali solution, 40KHz), add mechanical stirring, and ultrasonically treat for 30min; then transfer to a closed reaction In the still, 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 , and 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 ...

Embodiment 2

[0040] Take 30 g of microporous ZSM-5 zeolite and 1200 mL of 0.60 mol / L KOH solution in a beaker, place it in an ultrasonic cleaner (12.5W / 100mL alkali solution, 25KHz), add mechanical stirring, and ultrasonicate for 20 minutes; Stir at low temperature for 30min, transfer to a closed reaction kettle, add 90mL of ethanol, treat at 80°C for 3h, filter and wash. Put the washed ZSM-5 zeolite in a beaker, add 900mL 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 place in an oven at 110°C After drying for 12 hours, the obtained sample number is CL2.

Embodiment 3

[0042] Take 30 g of microporous β, 0.50 mol / L NaOH solution 2100mL in a beaker, put it in an ultrasonic cleaner (4.76W / 100mL alkali solution, 45KHz), add mechanical stirring, ultrasonic treatment for 40min; then transfer to a closed reaction Add 50mL of propanol to the kettle, and treat it at 100°C for 4h; filter and wash; 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 Treat in a water bath at 90°C for 3h, filter, wash, and then dry in an oven at 110°C 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 mesopore-micropore zeolite molecular sieve, comprising the following steps of: firstly mixing micropore zeolite and aqueous alkali and carrying out ultrasonic treatment; then carrying out heat treatment on the micropore zeolite in an enclosed system in the presence of an organic solvent; and finally processing the micropore zeolite by the use of an acid solution. According to the method, supersonic wave can generate a cavitation effect so as to activate the micropore zeolite's framework silicon atom; during the alkali treatment, the addition of the organic solvent can promote the generation of a meso-structure so as to more efficiently convert the micropore structure to mesopores and simultaneously stabilize and protect the micropore structure; and acid treatment can reach the purpose of dredging pore canal and increasing total specific surface area. By the adoption of the method, more complete mircopores of the mesopore-micropore zeolite molecular sieve can be retained, more mresopores can be provided, and simultaneously the total BET specific surface area can be increased.

Description

technical field [0001] The invention relates to a preparation method of a mesoporous-microporous zeolite molecular sieve, which belongs to the field of synthesis and modification of molecular sieves. Specifically, a kind of microporous zeolite is modified to prepare a mesoporous-micropore composite channel system. zeolite molecular sieves. 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 macromolecular produ...

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
Owner CHINA PETROLEUM & CHEM CORP
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