Preparation method for molecular sieve/organic composite permeable vaporization membrane

A technology of pervaporation membrane and molecular sieve, which is applied in the field of membrane separation, can solve the problems of easy formation of defects in the phase interface, poor permeation separation performance, complicated preparation process, etc., and achieves good membrane surface continuity, increased filling area, and simple preparation process. Effect

Inactive Publication Date: 2012-06-20
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zhou et al. (H.L. Zhou, Y. Su, X.R. Chen, S.L Yi, Y.H Wan. Modification of silicalite-1 by vinyltrimethoxysilane (VTMS) and preparation of silicalite-1 filled polydimethylsiloxane (PDMS) hybrid pervaporation membranes. Separation and Purification Technology, 2010, 75(3), 286-294) Adding vinyltrimethoxysilane-modified silicalite-1 into polydimethylsiloxane (PDMS) to prepare a hybrid membrane, and using it in acetone, butanol and For the separation of ethanol aqueous solution, pure organic membranes have poor osmotic separation performance, and there are insurmountable defects in thermal stability, mechanical stability and chemical stability. Although pure molecular sieve membranes have a high separation factor, this The membrane preparation process is complicated and expensive, so it is limited in practical applications. Organic-inorganic hybrid membranes are a type of pervaporation membrane prepared by blending organic polymers and inorganic materials. At present, most researchers use microporous molecular sieves. It is prepared by directly blending with silicone rubber. The molecular sieve and silicone rubber in the membrane obtained by this method are in a microscopically completely separated two-phase state, and defects are easily formed at the phase interface, which affects the stability of the membrane.

Method used

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  • Preparation method for molecular sieve/organic composite permeable vaporization membrane
  • Preparation method for molecular sieve/organic composite permeable vaporization membrane
  • Preparation method for molecular sieve/organic composite permeable vaporization membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Preparation of nano-scale Silicatile-1 molecular sieve: Sodium hydroxide, tetraethylorthosilicate (TEOS), tetrapropylammonium hydroxide (TPAOH) and water were mixed in molar ratio n (NaOH) : n (TEOS) : n (TPAOH) : n (H 2 O) = 1: 50 : 18 : 1000 to prepare molecular sieve synthesis liquid, stir magnetically at room temperature, age for 40 h, crystallize in a reaction kettle at 100 ° C for 60 h, take it out and cool it, centrifuge, wash with deionized water until neutral and dried, and calcined at 550 °C for 6 h to obtain nano-scale Silicatile-1 molecular sieves.

[0028] Using ethanol as a solvent, Silicatile-1 molecular sieve was prepared into a suspension with a mass fraction of 10% by ultrasonic oscillation. The ultrasonic power was 100W, and the oscillation was 20 minutes. The film was coated on the PTFE membrane by spraying method. The PTFE membrane had a pore size of 0.05 μm and dried at room temperature. , to obtain a Silicatile-1 / PTFE molecular sieve base fil...

Embodiment 2

[0033] Carry out the synthesis of Ge-ZSM-5 / PTFE composite membrane according to the step of Example 1, the difference is that the metal salt doped in the molecular sieve synthesis liquid is germanium ethylate, the PTFE membrane aperture is 0.05 μ m, and the Silicatile-1 molecular sieve suspension mass concentration is 5 %, Ge-ZSM-5 molecular sieve was prepared into a suspension with a mass fraction of 5%, the thickness of the bottom membrane of the molecular sieve was 10 μm, and the thickness of the separation layer was 10 μm. The obtained Ge-ZSM-5 / PTFE spiral-wound composite membrane was used in acetone / water pervaporation separation, the results are shown in Table 1.

Embodiment 3

[0035] Carry out the synthesis of Sn-ZSM-5 / PP composite membrane according to the step of example 1, difference is that molecular sieve base film adopts TS-1 molecular sieve, and the mass concentration of TS-1 molecular sieve suspension is 15%, and Sn-ZSM-5 molecular sieve is formulated into The suspension with a mass fraction of 15%, the pore size of the PP membrane is 0.5 μm, the thickness of the molecular sieve bottom membrane is 5 μm, and the thickness of the separation layer is 25 μm. The X-ray diffraction and scanning electron microscopy of the prepared Sn-ZSM-5 / PP composite membrane are respectively See image 3 and Figure 4 , Sn-ZSM-5 / PP spiral-wound composite membrane was used for the pervaporation separation of methanol / water. The results are shown in Table 1.

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Abstract

The invention belongs to the field of membrane separation and particularly relates to a preparation method for inorganic / organic high polymer composite permeable vaporization membrane taking molecular sieve materials as a separation layer and an organic high polymer microfiltration membrane as a support body. The composite membrane can use permeable vaporization to enable organic matters in organic systems such as alcohols, ketones, amines and the like to pass through preferentially, so as to achieve the separation of organic matters and water.

Description

technical field [0001] The invention belongs to the field of membrane separation, and specifically relates to a method for preparing an inorganic / organic polymer composite pervaporation membrane with molecular sieve material as a separation layer and an organic polymer microfiltration membrane as a support body. The composite membrane can utilize pervaporation to make alcohol Organic substances in organic systems such as ketones, ketones and amines are preferentially permeated, and the separation of organic substances and water is realized. Background technique [0002] Pervaporation is a membrane process that uses the difference in the dissolution (or adsorption) and diffusion properties of the components in the liquid mixture to achieve component separation. It has the advantages of high efficiency, low energy consumption, simple equipment, and small process amplification effect. , can effectively replace traditional separation methods such as distillation and extraction, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/12B01D71/36B01D71/26B01D71/34B01D67/00
Inventor 韶晖钟璟黄维秋陈若愚张琪张环茹周轶
Owner CHANGZHOU UNIV
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