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: 2010-07-14
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 pre

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

Example Embodiment

[0021] Embodiment 1

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

[0023] (2) According to the method of (1), 0.05 g TS-1 seed crystals were dispersed in 49.95 g of tetrapropyl ammonium hydroxide TPAOH aqueous solution to prepare seed crystal liquid, the pH=6. Under ultrasonic conditions of 100W, 40KHz, and 65°C, 1 ml of the aforementioned seed solution was dropped on the carr...

Example Embodiment

[0025] Embodiment 2

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

[0027] Place the above-mentioned carrier with seed crystals and the secondary growth solution together in the crystallization reaction kettle. The carrier is placed horizontally, and the seed layer of the carrier with the seed crystals ...

Example Embodiment

[0028] Embodiment 3

[0029] The seed layer was prepared according to the method of (2) in Example 1. On the basis of Example 2, according to the method of Example 2, 56.68 was added to 7.04ml of tetrapropylammonium hydroxide (20%) TPAOH aqueous solution. ml of water, stir for 15 minutes, and then add 11.09 g of ethyl orthosilicate dropwise to it, dissolve 0.145 g of tetrabutyl titanate in 3.5 ml of isopropanol, and then drop at 0°C under nitrogen protection. Add to the aforementioned sol, stir for 20 minutes, warm to 82°C, stir at this temperature to 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 a secondary growth liquid. 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 seed crystal 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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IPC IPC(8): C01B39/38
Inventor 黄伟王晓东延静
Owner TAIYUAN UNIV OF TECH
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