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Preparation method of LTA type molecular sieve film and prepared LTA type molecular sieve film

A technology of molecular sieve and sieve membrane, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems affecting the performance of molecular sieve membrane and the difficulty of synthesizing high-performance molecular sieve membrane.

Active Publication Date: 2013-04-24
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In-situ hydrothermal synthesis is currently the most commonly used synthesis method, but because in-situ hydrothermal synthesis is very sensitive to the synthesis conditions and the chemical and physical properties of the substrate, a slight change in a certain synthesis condition will affect the performance of the molecular sieve membrane, so usually Difficult to synthesize high performance molecular sieve membranes

Method used

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  • Preparation method of LTA type molecular sieve film and prepared LTA type molecular sieve film
  • Preparation method of LTA type molecular sieve film and prepared LTA type molecular sieve film
  • Preparation method of LTA type molecular sieve film and prepared LTA type molecular sieve film

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[0039] Preparation method of LTA type molecular sieve membrane

[0040] The preparation method of LTA type molecular sieve membrane of the present invention comprises the following steps:

[0041] (a) Through the covalent bonding reaction between the substrate with hydroxyl groups on the surface and organosilanes with haloalkyl groups and active groups that can be covalently bonded to hydroxyl groups, a silane linker with haloalkyl groups is introduced on the surface of the substrate to obtain a surface functionalized substrates; and

[0042] (b) Contact the above-mentioned surface functionalized modified substrate with the preparation solution containing the silicon-aluminum precursor for the synthesis of LTA molecular sieve membrane, so that the halogenated alkyl group of the silane linker located on the surface of the substrate is hydrothermally synthesized with The silicon-aluminum precursor undergoes a covalent bonding reaction, thereby preparing an LTA-type molecular si...

Embodiment 1

[0080] (1) Prepare the substrate with functionalized modification on the surface:

[0081] Put the porous alumina ceramic matrix into a toluene solution (solution concentration: 0.2 mol / L) dissolved in CPTMS, and react at 383K for 1 hour, thereby introducing silane connectors with chloropropyl groups on the surface of the porous alumina ceramic matrix.

[0082] (II) Preparation of LTA type molecular sieve membrane synthesis solution:

[0083] Weigh 22.22g of NaOH and dissolve in 47.5g of distilled water, add 0.30g of aluminum foil after clarification, and stir to form an aluminum solution; weigh 4.17g of silica sol and add it to 50g of preheated distilled water, and stir thoroughly; slowly dissolve the preheated aluminum solution Added into the silica sol, stirred well, then the solution continued to stir at room temperature for 24h. The final preparation contains Na 2 O, Al 2 o 3 , SiO 2 and H 2 O (equivalent to containing NaAlO 2 and Na 2 SiO 3 The silicon-aluminum ...

Embodiment 2-12

[0094] Embodiments 2 to 12 adopt substantially the same steps as in Example 1 to prepare LTA molecular sieve membranes, but the type of substrate used in step (I), the type of organosilane, the composition of the preparation solution in step (II), and the composition of step (III) The heating method, temperature and time are all different, and the parameters of each embodiment are listed in Table 1 on the next page.

[0095] Because the surface and section SEM identification results and X-ray diffraction spectrum of the LTA type molecular sieve membrane that embodiment 2 to 12 make are very similar to embodiment 1, for saving space, this paper does not show the SEM and XRD result of embodiment 2 to 12 .

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Abstract

The invention relates to a preparation method of an LTA type molecular sieve film and the prepared LTA type molecular sieve film. According to the method, through a covalent bonding reaction of a substrate having a hydroxyl on the surface and organosilane having halogenated alkyl and active groups capable of covalently bonding with the hydroxyl, the surface of the substrate is introduced with a silane coupling body having the halogenated alkyl, thereby obtaining the substrate with a functionally modified surface. The method further comprises contacting the substrate having the functionally modified surface with a preparation liquid containing silica-alumina precursors used for synthesizing the LTA type molecular sieve film, so that the halogenated alkyl of the silane coupling body on the surface of the substrate is subjected to a covalent bonding reaction with the silica-alumina precursors in a hydrothermal synthesis, thereby preparing the LTA type molecular sieve film on the surface of the substrate. The method and the prepared LTA type molecular sieve film are suitable for separation of mixed gases containing more than two kinds of gases selected from H2, N2, CO2 and low-carbon alkane gas.

Description

technical field [0001] The invention belongs to the field of molecular sieve membranes used in gas separation and liquid separation, and in particular relates to a method for preparing an LTA molecular sieve membrane and the LTA molecular sieve membrane prepared by the method. Background technique [0002] Molecular sieve refers to a series of inorganic microporous crystal materials with regular pore structure, which use silica and alumina tetrahedron as the basic structural unit. Molecular sieves have been widely used in industry as adsorbents, ion exchangers and catalysts. In addition, the excellent properties of molecular sieves have made them excellent inorganic membrane separation materials recently. Molecular sieves have many advantages as inorganic membrane materials. Molecular sieves have well-regulated pores with a single pore size distribution, and the pore size of molecular sieves is similar to that of many important industrial raw materials. Gas / liquid molecule...

Claims

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Application Information

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IPC IPC(8): C01B39/02
Inventor 黄爱生刘倩黄冰心
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI