Preparation method of hierarchical porous molecular sieve membrane

A technology of molecular sieves and channels, which is applied in the field of preparation of molecular sieve membrane materials, can solve problems such as cracks and affecting the compactness of molecular sieve membranes, and achieve the effects of high success rate, excellent hydrophobicity, and good permeation flux

CN106006662AInactive Publication Date: 2016-10-12QINGDAO UNIV OF SCI & TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2016-10-12
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention provides a preparation method of a hierarchical porous molecular sieve membrane. According to the method, a micropore-mesopore / macropore hierarchical porous structure is acquired through alkali treatment on the molecular sieve membrane; the alkali treatment means that the molecular sieve membrane is subjected to dissolution for a certain period of time at a certain temperature with a mixed system containing a molecular sieve, inorganic base or organic ammonium base and water, namely, a molecular sieve-alkaline suspension; a crystal form of the molecular sieve in the molecular sieve-alkaline suspension is matched with that of the molecular sieve membrane. Compared with a traditional microporous molecular sieve membrane, the hierarchical porous molecular sieve membrane prepared with the method has higher gas permeation flux. Besides, elemental composition of the molecular sieve membrane can be regulated through the alkali treatment. The method has a simple and efficient process, good repeatability and high success rate, and the prepared hierarchical porous molecular sieve membrane is applicable to chemical processes such as catalysis, separation and the like.
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Description

technical field

[0001] The invention relates to the field of preparation of molecular sieve membrane materials, in particular to a preparation method of multi-stage channel type molecular sieve membranes. Background technique

[0002] Molecular sieve membrane is a new type of inorganic membrane developed in recent years. In addition to the characteristics of general inorganic membranes, molecular sieve membranes also have small and uniform pore size, cations in molecular sieve crystals can be exchanged by other ions (such as Ti, Fe, etc.), Si / Al ratio can be adjusted, and Si or Al atoms can be exchanged by other ions. Heteroatom substitution and other characteristics. Among them, the important prerequisite for the application of molecular sieve membrane is that it has good compactness to ensure its excellent performance. On the basis of obtaining a dense molecular sieve membrane, improving the permeation flux of the molecular sieve membrane is a further improvement of the ...

Examples

Embodiment 1

[0024] Embodiment 1: the preparation of MFI type titanium silicon molecular sieve (TS-1) type molecular sieve membrane

[0025] (1) Prepare an alkaline suspension containing molecular sieves:

[0026] Disperse 0.15g of TS-1 molecular sieve in a mixture of 0.75g of TPAOH (tetrapropylammonium hydroxide, 25wt.%) and 11.25g of ultrapure water, and ultrasonicate for 30min to obtain a molecular sieve-alkaline suspension;

[0027] (2) Erosion molecular sieve membrane:

[0028] The prepared TS-1 molecular sieve membrane is horizontally placed on the support, submerged with the molecular sieve-alkaline suspension obtained in step (1), with the membrane facing down, placed in a polytetrafluoroethylene-lined stainless steel crystallization kettle, and the The stainless steel crystallization kettle was placed in a constant temperature box, the temperature was raised to 160°C, and the constant temperature was dissolved for 48 hours; after the dissolution, the TS-1 molecular sieve membrane...

Embodiment 2

[0036] The specific steps are the same as in Example 1, except that the molecular sieve membrane used is a ZSM-5 molecular sieve membrane. In this example, the method of alkali treatment and erosion is used to obtain the multi-stage channel type ZSM-5 molecular sieve membrane.

[0037] (1) Prepare an alkaline suspension containing molecular sieves:

[0038] Disperse 0.15g of ZSM-5 molecular sieve in a mixture of 0.75g of TPAOH (tetrapropylammonium hydroxide, 25wt.%) and 10g of ultrapure water, and ultrasonicate for 30min to obtain a molecular sieve-alkaline suspension;

[0039] (2) Erosion molecular sieve membrane:

[0040] The prepared ZSM-5 molecular sieve membrane is horizontally placed on the support, submerged with the molecular sieve-alkaline suspension obtained in step (1), with the membrane facing down, placed in a stainless steel crystallization kettle lined with polytetrafluoroethylene, and the The stainless steel crystallization kettle was placed in a constant tem...

Embodiment 3

[0043] The specific steps are the same as in Example 2, except that the alkali in the molecular sieve-alkaline suspension is sodium hydroxide. Step (1), preparation of an alkaline suspension containing molecular sieves: disperse 0.50 g of ZSM-5 molecular sieves in a mixture of 1.00 g of NaOH and 15.00 g of ultrapure water, and sonicate for 30 minutes to prepare a molecular sieve-alkaline suspension. In step (2), the dissolution temperature is 120° C., and the treatment time is 24 hours.