Microporous molecular separation membrane with high hydrothermal stability

A microporous, organic technology, applied in the field of microporous organic-inorganic hybrid membranes, which can solve the problems of inability to provide thermal stability and selectivity

Active Publication Date: 2009-04-29
NEDERLANDSE ORG VOOR TOEGEPAST-NATUURWETENSCHAPPELIJK ONDERZOEK (TNO)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These prior art methods and products do not provide microporous (<2nm) separation membranes with sufficient thermal stability and selectivity for continuous and efficient gas or liquid separation

Method used

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  • Microporous molecular separation membrane with high hydrothermal stability
  • Microporous molecular separation membrane with high hydrothermal stability
  • Microporous molecular separation membrane with high hydrothermal stability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0100] Example 1: Preparation of hybrid organic / inorganic silica sol

[0101] The precursor BTESE (1,2-bis(triethoxysilyl)ethane, 96% pure, Aldrich) was distilled to remove impurities and water before use. MTES (methyl-triethoxysilyl-ethane, 99% pure, Aldrich) was used directly. Dry the ethanol before using it, and use sodium aluminum silicate molecular sieve balls with a pore size of 1.0 nm. The precursors were dissolved separately in ethanol. Add MTES / ethanol (molar ratio 1:20) to BTESE / ethanol (molar ratio 1:20).

[0102] In an ice bath, the reaction mixture was stirred using a magnetic stirrer. Water and acid solution (HNO 3 , 65wt%, Aldrich) mixed. Half of the acid / water mixture was added to the precursor mixture and the sol was refluxed at 60°C for 1.5 hours. Next, the remaining half of the acid / water mixture was added and refluxed for an additional 1.5 hours. The reaction was quenched by cooling the reaction mixture while stirring in an ice bath.

[0103] The mo...

Embodiment 2

[0104] Example 2: Preparation of a hydrophobic silica membrane supported by alumina

[0105] The gamma-alumina film was dip-coated with the sol prepared according to Example 1. The [BTESE] / [MTES] ratio of the sol is 1, [H 2 O] / ([BTESE]+[MTES]) ratio was 2 (sol A, from membrane A) or 4 (sol B, from membrane B). At 300°C, N 2 In atmosphere, the film was calcined for 3 hours with a heating and cooling rate of 0.5°C / min.

[0106] As described by Campaniello et al. (Chem. 2 In atmosphere, the film was calcined for 3 hours with a heating and cooling rate of 0.5°C / min.

[0107] A microporous layer is thus formed on the tubular membrane with an average pore size of 0.24-0.28 nm as determined by the adsorption technique described above, with substantially no pores larger than 0.30 nm.

[0108] The Kelvin pore size distribution determined by permporometry of this membrane is very similar to that of the methylated silica membrane prepared according to De Vos.

[0109] Pervaporation...

Embodiment 3

[0112] Example 3: Preparation of BTESE-based hybrid organic / inorganic silica sol.

[0113] The precursor BTESE (1,2-bis(triethoxysilyl)ethane, 96% pure, Aldrich) was distilled to remove impurities and water before use. Ethanol (p.a., Aldrich) was used directly. Dissolve the precursor in ethanol. In an ice bath, the reaction mixture was stirred using a magnetic stirrer. Dilute water with acid solution (HNO 3 , 65wt%, Aldrich) mixed. The acid / water / ethanol mixture was added dropwise to the precursor mixture, and the resulting sol was refluxed at 60°C for 2-3 hours. The reaction was quenched by cooling the reaction mixture while stirring in an ice bath.

[0114] The molar ratio of the reactants is [H 2 O] / [BTESE]=(3-6), [H + ] / [BTESE]=(0.02-0.4). The amount of water included with the acid catalyst (HNO 3 ) and water introduced together with the solvent (ethanol).

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Abstract

A hydrothermally stable, microporous organic-inorganic hybrid membrane based on silica, having an mean pore diameter of between 0.2 and 1.5 nm, is characterised in that between 5 and 40 mole% of the Si-O-Si bonds have been replaced by mo ieties having the one of the formulas: Si-{[CmH(n-1)X]-Si-}q, Si-[CmH(n-2)X2]-Si or Si-CmHn-Si{(CmHn)-Si-}y in which m = 1-8, n = 2m, 2m-2, 2m-4, 2m-6 or 2m-8; provided that n = 2, X = H or (CH2)pSi, p = 0 or 1, and q = 1, 2, 3 or 4. The membrane can be produced by acid-catalysed hydrolysis of suitable bis- silane precursors such as bis(trialkoxysily)alkanes, preferably in the presence of monoorganyl-silane precursors such as trialkoxy-alkylsilanes.

Description

[0001] The present invention relates to a microporous organic-inorganic hybrid membrane for the separation of gases and liquids and a method for preparing the membrane. Background technique [0002] Existing microporous pure silica membranes show good separation performance in both gas and liquid separations, but water adsorption occurs at room temperature due to the hydrophilic nature of the silica surface. DeVos et al. (J.Membr.Sci.158, 1999, 277-288; J.Membr.Sci.143, 1998, 37; EP-A1 089806) developed hydrophobic silica membranes for the separation of gases and liquids (also known as methylated silica membranes), and proposed a method to reduce the interaction of water molecules by introducing precursors containing hydrophobic groups. Campaniello et al. (Chem. Commun., 2004, 834-835) conducted further studies on methylated silica films, which were dehydrated by pervaporation of organic solvents. They found that the reduction in water flux could be restored by increasing the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/70C08G77/50C08G77/52C08L83/14
CPCB01D71/027B01D71/70B01D69/148B01D67/0048B01D67/0079B01D2323/12B01D61/362C08G77/58Y10T428/12542Y10T428/31663Y02E60/32
Inventor A·沙赫H·L·卡斯特里卡姆J·F·文特D·H·A·布兰克J·E·坦恩埃尔斯霍夫
Owner NEDERLANDSE ORG VOOR TOEGEPAST-NATUURWETENSCHAPPELIJK ONDERZOEK (TNO)
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