A kind of preparation method of mesoporous-microporous 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 microporous crystal structure destruction, reduce zeolite catalytic activity, and low micropore surface area, and achieve high mesopore specific surface area and BET surface area improvement effect

Active Publication Date: 2014-10-15
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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  • A kind of preparation method of mesoporous-microporous zeolite molecular sieve material
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  • A kind of preparation method of mesoporous-microporous zeolite molecular sieve material

Examples

Experimental program
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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, fully stir and mix, and then place it in a microwave digestion apparatus for 30min, keep the temperature at 80°C; filter and wash. Place the washed mordenite in a beaker, add 1500 mL of 0.2mol / L hydrochloric acid solution, stir at room temperature for 20 minutes, transfer to a water bath at 70°C for 3 hours, filter, wash, and place in an oven to dry at 110°C for 12 hours , The sample number is CL1.

[0037] by figure 1 It can be seen that the CL1 sample has the characteristic spectrum of mordenite and still maintains a good zeolite structure. by image 3 It can be seen that after the modification treatment, there is an obvious concentration of mesopores in the microporous mordenite, the most likely pore size is 3.5nm, indicating that after the treatment, a large number of mesoporous structures are formed in the mordenite.

Embodiment 2

[0039] Take 30 g of microporous ZSM-5 zeolite, 1200 mL of 0.60 mol / L KOH solution, and 90 mL of ethanol to fully stir and mix, and then place it in a microwave digestion apparatus for 30 minutes, keeping the temperature at 90°C; then filter and wash. Place the washed ZSM-5 zeolite in a beaker, add 900 mL of 0.2mol / L nitric acid solution, stir at room temperature for 20 minutes, transfer to a water bath at 90°C for 2 hours, filter, wash, and place in an oven at 110°C After drying for 12 hours, the sample number is CL2.

Embodiment 3

[0041] Take 30 g of microporous β zeolite, 0.50 mol / L NaOH solution of 2100 mL, and 150 mL of propanol, stir and mix them thoroughly, and then place them in a microwave digestion apparatus for 30 minutes, keeping the temperature at 100°C; then filter and wash. Put the washed β zeolite in a beaker, add 1500mL of 0.8mol / L sulfuric acid solution, stir at room temperature for 30min, transfer to a water bath at 90℃ for 3h, filter, wash, and place in an oven at 110℃ to dry for 12h , The sample number is CL3.

[0042] by figure 2 It can be seen that the CL3 sample has the characteristic spectrum of β zeolite and still maintains a good β zeolite structure. by Figure 4 It can be seen that after the modification treatment, there is an obvious concentration of mesopore pore diameters in the microporous β zeolite, the most likely 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 method for preparing a mesoporous-microporous zeolite molecular sieve, belonging to the field of molecular sieve synthesis modification, specifically, a type of microporous zeolite is modified to prepare a mesoporous-microporous composite pore system Zeolite molecular sieve. Background technique [0002] Microporous zeolite is widely used in the petroleum industry due to its regular microporous structure, suitable acidity, good thermal stability and hydrothermal stability. However, microporous zeolites inevitably have some natural defects. Its narrow pores (less than 2nm) can easily cause excessive mass transfer and diffusion resistance of the reaction materials in reactions involving macromolecules, and it is extremely difficult for macromolecular reactants to enter the crystal pores. The internal reaction will not give full play to the catalytic performance of the zeolite; and it is also difficult for macromolecular products to...

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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