Method for preparing orientation molecular sieve membrane

A technology of molecular sieve membrane and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve problems such as fast hydrolysis speed of germanium source, mismatching degree of hydrolysis, and influence of molecular sieve membrane formation , to achieve the effect of easy control of synthesis conditions and reduction of adverse effects

Inactive Publication Date: 2010-02-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The problem to be solved in the present invention is that in the process of preparing the molecular sieve membrane precursor glue, one is that the hydrolysis rate of the silicon source is slow, and the hydrolysis rate of the germanium source is fast, and the degree of hydrolysis of the two does not match, which affects the entry of germanium atoms into the skeleton; There is a large amount of alcohol in the precursor glue, and the presence of alcohol will affect the formation of molecular sieve membrane

Method used

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  • Method for preparing orientation molecular sieve membrane
  • Method for preparing orientation molecular sieve membrane

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Experimental program
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Embodiment approach 1

[0022] Add 14.46ml of water to the aqueous solution of 1ml of tetrapropyl ammonium hydroxide (50%), stir for 10 minutes, then add 7.21 grams of silica sol dropwise therein, and dissolve 0.125 grams of tetraethyl germanate in 11.10 grams of Add isopropanol dropwise to the aforementioned liquid, stir for 10 minutes, raise the temperature to 80°C, keep the temperature constant for 20 minutes, add water to the original liquid level, cool to room temperature, and stir for 5 hours to obtain the molecular sieve membrane precursor glue, which Composed of: 1SiO 2 : 0.01GeO 2 :0.05TPAOH:23H 2 O,

[0023] The above precursor glue and α-Al 2 o 3 The carrier is placed in the crystallization reactor together, and the α-Al 2 o 3The lower surface of the carrier is in contact with the synthesis solution, heated and crystallized at 180°C for 24 hours, then taken out and cooled to room temperature, washed with deionized water until neutral, dried, and calcined at 550°C for 8 hours to remov...

Embodiment approach 2

[0025] On the basis of Example 1, according to the method of Example 1, the hydrolysis temperature of the silicon source and the germanium source was raised to 80°C, the crystallization time of the molecular sieve membrane was shortened to 12 hours, and the crystallization preparation of the molecular sieve membrane was carried out again. and cooled to room temperature, then washed with deionized water until neutral, dried at 550°C, and fired for 8 hours to remove the template agent to prepare a molecular sieve film grown along the b-axis orientation, such as Figure 5 with 6 .

Embodiment approach 3

[0027] According to the method of embodiment 1, in the aqueous solution of the tetrapropyl ammonium hydroxide (50%) of 0.89ml, add the water of 14.39ml, stir for 10 minutes, then dropwise add the silica sol of 8.23 ​​grams wherein, the germanium of 0.125 grams After dissolving 11.10 g of isopropanol, add tetraethyl ester dropwise to the aforementioned liquid, stir for 10 minutes, increase the hydrolysis temperature to 90°C, extend the constant temperature time to 30 minutes, add water to the original liquid level, and cool to room temperature , stirred for 5 hours to obtain the composition of the molecular sieve membrane precursor glue solution: 1SiO 2 : 0.009GeO 2 :0.04TPAOH:20H 2 O,

[0028] The crystallization temperature of the molecular sieve membrane was lowered to 175° C., and the crystallization time was extended to 40 hours for crystallization and film formation, and a molecular sieve membrane grown along the b-axis orientation was prepared.

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Abstract

The invention provides a method for preparing an orientation molecular sieve membrane, comprising the following steps: removing alcohol in pro-glue solution in an evaporation way by improving the hydrolysis temperature of silicon source and germanium source and promoting the hydrolysis thereof; directly contact heating up the pro-glue solution and a carrier; crystallizing under self-generated pressure; and preparing b-axial orientation Ge-ZSM-5 molecular sieve membrane. The orientation molecular sieve membrane is even and compact, and has no defect of large holes, wherein molecular sieve membrane crystalloid is oriented along the b axis, thereby being good for the process of mass transferring. The method can obviously improve the capability of the synthetic Ge-ZSM-5 molecular sieve membrane, has high repetitiveness and high raw materials utilization factor, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing a molecular sieve membrane, in particular to a method for preparing a b-axis oriented Ge-ZSM-5 molecular sieve membrane on a porous ceramic carrier by an in-situ hydrothermal crystallization method. Background technique [0002] Molecular sieve (molecular sieve) is a kind of porous medium with special pore or cage structure. It has regular and orderly open pore structure and large pore volume and specific surface area. It is widely used in catalysis and fine chemical industry and other fields. Gabelica and Guth et al. replaced silicon atoms in pure silicalite (Silicalite-1) with germanium atoms to prepare Ge-ZSM-5 molecular sieves. Since germanium atoms are four-coordinated like silicon atoms, the introduction of germanium atoms generally does not generate acidic sites, but it will change the pore structure of molecular sieves and increase the concentration of lattice defects. These changes in physical p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40C04B41/85
Inventor 王晓东黄伟赵潞潞延静石芳
Owner TAIYUAN UNIV OF TECH
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