Method for synthesizing oriented MFI type molecular sieve membrane by means of microwave heating

A technology of microwave heating and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of high preparation cost and complicated operation steps, and achieve the effects of uniform grain size, continuous film layer and shortened synthesis time

Inactive Publication Date: 2010-02-10
ZHEJIANG UNIV
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

The oriented molecular sieve membrane synthesized by the secondary growth method can better control the oriented growth of the molecular sieve crystal due to the existence of the seed crystal, but the secondary growth method needs to obtain a uniformly coated seed crystal layer, the operation steps are relatively complicated, and the preparation cost is high
So far, there is no report on microwave synthesis of b-axis oriented MFI molecular sieve membranes

Method used

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  • Method for synthesizing oriented MFI type molecular sieve membrane by means of microwave heating
  • Method for synthesizing oriented MFI type molecular sieve membrane by means of microwave heating
  • Method for synthesizing oriented MFI type molecular sieve membrane by means of microwave heating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 Synthesis of Oriented MFI Molecular Sieve Membrane by Traditional Heating Method

[0027] The molar ratio is ethyl orthosilicate: tetrapropyl ammonium hydroxide: water = 1: 0.32: 165 40 milliliters of synthesis solution was stirred at room temperature for 4 hours to obtain a clear and transparent solution, and then this synthesis solution was supported by a stainless steel sheet Put the body together in a 100 ml synthesis kettle with a polytetrafluoroethylene liner, then put the sealed synthesis kettle into a blast oven at 165°C for crystallization for 2 hours, and finally take out the crystallized synthesis kettle After quenching to room temperature, the support body was taken out, washed with deionized water and dried. The scanning electron microscope pictures of the dried molecular sieve membranes are as follows: figure 1 As shown, the obtained molecular sieve membrane is a continuous b-axis oriented MFI type molecular sieve membrane.

Embodiment 2

[0028] Example 2 Synthesis of Oriented MFI Molecular Sieve Membrane by Aging at Room Temperature and Microwave Heating

[0029] Stir 20 milliliters of synthetic solution with a molar ratio of tetrapropylammonium hydroxide: water = 1:0.32:165 at room temperature for 4 hours to obtain a clear and transparent solution, and then stir and age at room temperature for 20 hours , and then put the synthetic solution together with the stainless steel sheet support into a 70 ml synthesis kettle with a polytetrafluoroethylene liner, and then put the sealed synthesis kettle into a microwave oven and raise the temperature to 165 ° C for 35 minutes to crystallize. Finally, the crystallized synthesis kettle was naturally cooled to room temperature, and then the support was taken out, washed with deionized water, and then dried. The scanning electron microscope pictures of the dried molecular sieve membranes are as follows: figure 2 As shown, the obtained molecular sieve membrane is a contin...

Embodiment 3

[0030] Example 3 Synthesis of Oriented MFI Molecular Sieve Membrane by Aging at Room Temperature and Microwave Heating

[0031] Same as Example 2, aging with stirring at room temperature for 50 hours. From the scanning electron microscope picture of the dried molecular sieve membrane, it can be seen that the obtained molecular sieve membrane is a continuous b-axis oriented MFI type molecular sieve membrane.

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Abstract

The invention discloses a method for synthesizing an oriented MFI type molecular sieve membrane by means of microwave heating. The method comprises the following steps of: 1) preparation of molecularsieve synthetic fluid, wherein the synthetic fluid consists of tetraethoxysilane, tetrapropylammonium hydroxide and water, which follow a mol ratio of 1:0.2-0.6:100-250; 2) stirring the synthetic fluid at the room temperature for 1-4 h, adding support body, carrying out aging for a time ranging from 10 min to 50 h in the condition of the room temperature or heating, or carrying out aging first fora time ranging from 10 min to 50 h in the condition of the room temperature or heating and then adding the support body, and synthesizing a molecular sieve membrane by means of microwave heating, wherein the synthesis temperature is 100-200 DEG C and the synthesis time is 10-30 min; and 3) washing and drying and finally obtaining the oriented MFI type molecular sieve membrane from the support body. The MFI type molecular sieve membrane synthesized with the method is b-axis oriented and has good synthetic repetition. The microwave heating greatly accelerates the nucleation and crystallizationspeed of the molecular sieve, remarkably reduces the molecular sieve membrane synthesis time and the energy consumption and is helpful for cost reduction.

Description

technical field [0001] The invention relates to the synthesis of MFI molecular sieve membranes, in particular to a method for synthesizing oriented MFI molecular sieve membranes by microwave heating. Background technique [0002] Molecular sieve membrane has a regular pore structure, unique mechanical and electronic properties, and excellent thermal stability, chemical stability and biological stability, so it is widely used in material separation, membrane reactors, chemical sensors, electrodes, low dielectric Constant materials and anti-corrosion coatings and many other fields. At present, the molecular sieve membranes reported in the literature mainly include LTA type, T type, MFI type, FAU type, MOR type, etc., among which the MFI type molecular sieve membrane has attracted much attention. This is because: (1) the pore size of the MFI molecular sieve is equivalent to the molecular size of many important industrial chemicals; (2) the MFI molecular sieve has a complex thr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 王正宝李显明
Owner ZHEJIANG UNIV
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