Method for preparing oriented molecular sieve membrane by using diauxic growth method

A secondary growth, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of poor orientation and a large number of seed layers.

Inactive Publication Date: 2012-03-07
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

T.Ban et al. used ultrasonic method to load ZSM-5 seeds on α-Al 2 o 3 On the carrier, a b-axis oriented seed layer is formed, and then the b-axis oriented ZSM-5 molecular sieve membrane is prepared by secondary growth. This method is easy to operate and the equipment is simple, but the prepared seed layer has poor orientation and non-b-axis Oriented seeds still exist in large numbers

Method used

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  • Method for preparing oriented molecular sieve membrane by using diauxic growth method
  • Method for preparing oriented molecular sieve membrane by using diauxic growth method
  • Method for preparing oriented molecular sieve membrane by using diauxic growth method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0022] (1) Disperse 0.25 g of TS-1 seed crystals in 49.75 g of tetrapropylammonium hydroxide TPAOH aqueous solution to prepare seed crystal liquid, the pH of which is 3.5. Put a petri dish with built-in filter paper in the ultrasonic cleaner, put the carrier on the filter paper in the petri dish, soak the carrier and filter paper with tetrapropylammonium hydroxide TPAOH aqueous solution with pH=3.5, and set the temperature at 200W, 40KHz, 40 Under the ultrasonic condition of ℃, 0.5ml of the aforementioned seed liquid was added dropwise on the carrier, ultrasonicated until the surface of the carrier was dry, and then taken out to obtain a b-axis orientation TS-1 molecular sieve seed layer.

[0023] (2) Disperse 0.05 g of TS-1 seed crystals in 49.95 g of tetrapropylammonium hydroxide TPAOH aqueous solution according to the method of (1) to prepare a seed crystal solution, the pH of which is 6. Under ultrasonic conditions of 100W, 40KHz, and 65°C, 1ml of the aforementioned seed l...

Embodiment approach 2

[0026]The seed layer was prepared according to the method of (1) in Example 1. In the aqueous solution of 10.83ml tetrapropyl ammonium hydroxide (20%) TPAOH, add the water of 96.77ml, stir for 15 minutes, then dropwise add the silica sol (40%) of 16 grams wherein, the tetrabutyl titanate of 0.145 grams Dissolve the ester in 3.5ml of isopropanol, add it dropwise to the aforementioned sol at 0°C under the protection of nitrogen, stir for 20 minutes, heat up to 80°C, stir at this temperature, evaporate and remove the alcohol in the sol, and add water to The original liquid level is cooled to room temperature, stirred for 1 hour, and the secondary growth liquid is obtained, and its composition is: 1SiO 2 :0.004TBOT:0.1TPAOH:60H 2 O.

[0027] Put the carrier loaded with the seed crystal and the secondary growth solution together in the crystallization reaction kettle, place the carrier horizontally, and the carrier seed layer loaded with the seed crystal is in contact with the se...

Embodiment approach 3

[0029] Prepare the seed crystal layer according to the method of (2) in Example 1, on the basis of Example 2, according to the method of Example 2, add 56.68 to the aqueous solution of tetrapropyl ammonium hydroxide (20%) TPAOH of 7.04ml ml of water, stirred for 15 minutes, then added dropwise 11.09 g of tetrabutyl titanate to it, dissolved 0.145 g of tetrabutyl titanate in 3.5 ml of isopropanol, and dropped at 0°C under the protection of nitrogen Add to the aforementioned sol, stir for 20 minutes, raise the temperature to 82°C, stir at this temperature, evaporate and remove the alcohol in the sol, add water to the original liquid level, cool to room temperature, and stir for 1 hour to obtain the secondary growth solution. Its composition is: 1TEOS:0.008TBOT:0.13TPAOH:65H 2 O, secondary growth at 175°C for 36 hours to prepare a b-axis oriented TS-1 molecular sieve membrane.

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Abstract

The invention relates to a method for preparing an oriented molecular sieve membrane by using a diauxic growth method, which comprises that molecular sieve seed crystals are carried on a carrier by using an electrostatic absorption-ultrasound method to form a seed crystal layer; the pH value of seed crystal liquid is adjusted to form a surface electrostatic layer, and the seed crystals are made to contact with the carrier with the maximum a-c surface through the assistance of ultrasound to form an even and successive b-axis oriented molecular sieve seed crystal layer; the molecular sieve seedcrystal layer is prepared into a dense and successive b-axis oriented molecular sieve seed crystal membrane through diauxic growth. The method has the advantages of easy control of the thickness and orientation of molecular sieve membranes, repeatability and suitability for scale 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 TS-1 molecular sieve membrane on a porous ceramic carrier and a silicon chip by using a secondary growth method. Background technique [0002] In 1983, Taramasso et al. introduced the transition metal titanium into the framework of pure silicalite (Silicalite-1) to synthesize titanium-silicon molecular sieve TS-1 (Titanium silicalite-1), which belongs to the ZSM-5 series of zeolite molecular sieves with MFI Topology. Titanium-silicon molecular sieve (TS-1) membrane not only has the excellent catalytic oxidation performance of titanium-silicon molecular sieve, but also has the characteristics of zeolite membrane material, which can realize the effective integration of reaction process and separation process, improve the reaction conversion rate and strengthen the reaction process, which has caused extensive attention of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38
Inventor 王晓东黄伟延静
Owner TAIYUAN UNIV OF TECH
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