Method for preparing mesopore-micropore zeolite molecular sieve material

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

Active Publication Date: 2013-01-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • 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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Examples

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Effect test

Embodiment 1

[0036] Take 30g of microporous mordenite, 2400mL of 0.30 mol / L NaOH solution, and 75mL of methanol and mix them thoroughly, then place them in a microwave digestion apparatus for 30min, keep the temperature at 80°C; then 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.

[0037] 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

[0039] Take 30g of microporous ZSM-5 zeolite, 1200mL of 0.60 mol / L KOH solution, and 90mL of ethanol and mix them thoroughly, then place them in a microwave digestion apparatus for 30min, keep the temperature at 90°C; then 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

[0041] Take 30 g of microporous zeolite beta, 2100 mL of 0.50 mol / L NaOH solution, and 150 mL of propanol and mix them thoroughly, then place them in a microwave digestion apparatus for 30 minutes, and keep the temperature at 100 °C; then 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 a water bath at 90°C for 3h, filter, wash, and dry in an oven at 110°C for 12h , and the obtained sample number is CL3.

[0042] 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 method for preparing a mesopore-micropore zeolite molecular sieve material. The method comprises the following steps of: mixing an alkaline solution, an organic solvent and micropore zeolite, and performing microwave treatment; performing acid solution treatment, separating, washing and drying to obtain the mesopore-micropore zeolite. By the method, the micropore zeolite is subjected to microwave treatment in the existence of the organic solvent and the alkaline solution, so that formation of mesopores can be promoted, and micropores are efficiently converted into the mesopores and can be stabilized and protected; amorphous aluminum in a pore channel of a zeolite crystal can be eluted in the subsequent acid treatment process, so that aims of dredging the pore channel and increasing the total specific surface area are fulfilled; and the relatively complete micropores can be reserved in the mesopore-micropore zeolite, a plurality of mesopores are provided, and simultaneously, the total Brunauer, Emmett and Teller (BET) specific surface area can be increased.

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 Applications(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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