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Modification treatment method of ZSM-5 zeolite

A ZSM-5, processing method technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of reducing the catalytic activity of zeolite, the destruction of microporous crystal structure, and the specific surface area of ​​mesopores. Low problems, to achieve the effect of BET surface area improvement

Active Publication Date: 2014-08-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still two obvious shortcomings in the prior art: one is that the mesopore specific surface area is still relatively low, the highest is CN1530322A, which is close to 250 m 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 treatment method of ZSM-5 zeolite
  • Modification treatment method of ZSM-5 zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Take 30g of ZSM-5 zeolite, 75mL of methanol, and 2400mL of 0.30 mol / L NaOH solution into a beaker, place in an ultrasonic cleaner (4.17W / 100mL alkali solution, 40KHz), add mechanical stirring, and ultrasonically treat for 30min; Put it into a closed reaction kettle, and treat it at 60°C for 3 hours; then filter and wash the obtained sample until the pH value is neutral, and then dry it in an oven at 110°C for 12 hours. 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 10g of ZSM-5 zeolite, 30mL of ethanol, and 400mL of 0.60 mol / L KOH solution into a beaker, place it in an ultrasonic cleaner (25W / 100mL alkali solution, 45KHz), add mechanical stirring, and ultrasonicate for 25min; then transfer to In a closed reaction kettle, treat at 80°C for 2 hours; then filter and wash the obtained sample until the pH value is neutral, and then dry it in an oven at 110°C for 12 hours. The obtained sample number is CL2.

Embodiment 3

[0037] Take 10g of ZSM-5 zeolite, 15mL of propanol, and 700mL of 0.50 mol / L NaOH solution into a beaker, place in an ultrasonic cleaner (14.3W / 100mL alkali solution, 25kHz), add mechanical stirring, and ultrasonically treat for 35min; Transfer to a closed reaction kettle and treat at 100°C for 3 hours; then filter and wash the obtained sample until the pH value is neutral, and then dry it in an oven at 110°C for 12 hours. The obtained sample number is CL3.

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Abstract

The invention discloses a modification treatment method of ZSM-5 zeolite. The method comprises the following steps of: adding a certain proportion of aqueous alkali and a low molecular weight organic solvent into ZSM-5 zeolite, performing ultrasonic treatment on the system, transferring to an enclosed system for alkali treatment, and finally separating and drying to obtain the modified ZSM-5 zeolite. The supersonic wave can generate a super strong cavitation effect so as to activate the ZSM-5 zeolite's framework silicon atom and help the next alkali treatment. During the alkali treatment process, aqueous alkali selectively removes part of silicon element in the ZSM-5 crystals such that structural rearrangement is generated in micropores so as to form mesopores. The addition of the low molecular weight organic solvent can promote the generation of the meso-structure so as to make the micropore structure more efficiently to be converted to mesopores and simultaneously stabilize and protect the micropore structure. By the adoption of the method, more complete micropores can be retained, more mesopores can be provided, and total BET specific surface area also can be increased.

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] With the development of chemical synthesis methods, people began to introduce ultrasonic waves into the synthesis of materials in order to find more effective means. The high efficiency of ultrasonic waves plays a role in material chemistry that cannot be achieved by light, electricity, and thermal methods. Ultrasound has long been widely used in many fields such as metal exploration, geological prospecting, marine exploration and biodegradation; ultrasonic has also shown great advantages in organic synthesis, polymerization, crystallization process, extraction and separation, and ultrafine powder preparation. ,have a broad vision of application. [0003] Ultrasound has been widely reported in the synthesis of special mo...

Claims

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Application Information

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