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Synthesis method of MCM-22 family molecular sieve

A technology of MCM-22 and synthesis method, which is applied in the field of synthesis of MCM-22 family molecular sieves, and can solve problems affecting the synthesis formula and product quality stability, poor dispersion of hexamethyleneimine, uneven crystal phase of products, etc. problems, to achieve the effect of increased dispersion, high crystallinity, and uniform crystal phase

Active Publication Date: 2012-11-21
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its high toxicity, strong corrosiveness and high volatility, it is easy to cause great harm to the human body and affect the stability of synthetic formula and product quality
In addition, due to the poor dispersion of hexamethyleneimine in the initial gel, the crystal phase of the synthesized product is not uniform
Although some scholars try to synthesize MCM-22 molecular sieves by using binary templates, they cannot completely replace hexamethyleneimine templates.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Add 1 mol / L hydrochloric acid to the sealed container containing the hexamethyleneimine template while stirring, and cool with circulating water at the same time, stop adding acid when the pH value of the solution is neutral, and obtain the acidified Templating agent (R). According to the reports in the published documents and patents, the following raw material ratio was selected, and the acidified template was used to synthesize the MCM-22 molecular sieve. NaAlO 2 , NaOH, water, silica sol and acidified templating agent (R) in molar ratio of SiO 2 / Al 2 o 3 =30.0, OH - / SiO 2 =0.25,H 2 O / SiO 2 =30.0, Na + / SiO 2 =0.25, R / SiO 2 = 0.20 to prepare a homogeneous gel. In order to neutralize the amount of acid introduced in the acidification step of the template agent, an appropriate amount of ammonia water is added to the mixture to prepare a reaction mixture, wherein the amount of water added should be deducted from the amount of water introduced during the aci...

Embodiment 2

[0070] Repeat implementation 1, but the obtained MCM-22 molecular sieve slurry and tetrapropylammonium hydroxide (TPAOH), cetyltrimethylammonium bromide (CTAB) and water are: CTAB / MCM-22 = 1, TPAOH / MCM-22 = 1.1, H 2 O / MCM-22=16 is prepared into a slurry, and then the slurry is transferred to a three-neck bottle and expanded at 80°C for 16 hours. After cooling, the layer is peeled off by ultrasonic waves for 1 hour, and then the alkalinity of the mixed slurry is quickly adjusted with concentrated hydrochloric acid. The solid was collected by centrifugation until the pH value was less than 2. Finally, the above solid was washed, dried, and calcined at 540°C for 6h. XRD crystal phase analysis of the samples showed that the prepared samples were pure phase ITQ-2 molecular sieves.

Embodiment 3

[0072] Repeat implementation 1, but the obtained MCM-22 molecular sieve slurry is subjected to pillaring treatment according to the method described in the open literature, Chemical Journal of Universities, 2007, 28 (3): 530-534, and the obtained product is subjected to XRD crystal phase analysis, and the result It shows that the prepared sample is a pure phase MCM-36 molecular sieve.

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PUM

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Abstract

The invention discloses a synthesis method of an MCM-22 family molecular sieve. The method is characterized by comprising the steps of: adding a dilute acid water solution into a hexamethyleneimine template agent; adding a silicon source, an aluminium source, an alkali source, water and an acidified template agent (R) in proportion so as to prepare gel; conducting hydrothermal crystallization, opening a valve under constant temperature, carrying out pressure reduced evaporation to the molecular sieve slurry, recovering the liquid mixture and the template agent; adding a cold dilute acid watersolution into the residual slurry, and opening the kettle when the temperature of the residual slurry drops below 50DEG C, performing filtration so as to obtain a solid product, thus obtaining a MCM-22 family molecular sieve finally. With the method provided in the invention, the template agent no longer volatizes, and damage to the human body can be avoided. Meanwhile, stability of the synthesisformula and quality of the molecular sieve is guaranteed. When the template agent is acidified into a salt, the dispersibility is greatly increased, and the obtained MCM-22 family molecular sieve hasa uniform crystal phase as well as a high degree of crystallization. After crystallization, the synthesis slurry is subjected pressure reduced evaporation and the template agent is recovered. After acidification, the recovered template agent can be used for MCM-22 family molecular sieve synthesis again.

Description

technical field [0001] The invention belongs to the field of zeolite molecular sieve catalysts, and relates to a synthesis method of MCM-22 family molecular sieves. Background technique [0002] MCM-22 molecular sieve is a layered molecular sieve with MWW topology, which was first synthesized by Mobil in 1990 under the hexamethyleneimine template system. It has two independent pore systems: interlayer ten-membered ring (0.40 ×0.59nm) connected channel system, ten-membered ring two-dimensional sinusoidal channel system in the layer and twelve-membered ring holes (0.71×0.71×1.82nm) on the outer surface of the crystal. Later, molecular sieves such as MCM-49, MCM-56, MCM-36, ITQ-1 and ITQ-2 were synthesized under the hexamethyleneimine template system, and they were also found to be layers with MWW structure. shape molecular sieve. Therefore, these molecular sieves are collectively referred to as MCM-22 molecular sieves. MCM-22 molecular sieves have broad application prospect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 郭洪臣聂彬剑钱吉刘春燕郑步梅
Owner DALIAN UNIV OF TECH
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