Metal element modified ZSM-5 molecular sieve composite membrane as well as preparation method and application thereof

A technology of ZSM-5 and metal elements, which is applied in the field of ZSM-5 molecular sieve composite membranes modified by metal elements, to achieve the effect of enhanced selective permeability, good continuity and excellent separation performance

Active Publication Date: 2012-02-15
BEIJING CLP JIAMEI ENVIRONMENTAL PROTECTION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-prepared heteroatom molecular sieve membranes have relatively large deficiencies in molecular sieve crystal grains, film thickness, film continuity and large-area preparation of films.

Method used

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  • Metal element modified ZSM-5 molecular sieve composite membrane as well as preparation method and application thereof
  • Metal element modified ZSM-5 molecular sieve composite membrane as well as preparation method and application thereof
  • Metal element modified ZSM-5 molecular sieve composite membrane as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A certain amount of TPABr, TEOS, sodium hydroxide (NaOH), tin tetrachloride (SnCl 4 ) and deionized water in a certain molar ratio, namely n(NaOH):n(TEOS):n(TPABr):n(SnCl 4 ):n(H 2 (0)=0.3:1:0.3:0.03:60 configure the molecular sieve synthesis liquid. Stir at room temperature for 12 hours, pour into a stainless steel crystallization kettle lined with polytetrafluoroethylene, seal it and place it in an oven at 175°C for crystallization for 36 hours. The reactor was taken out, cooled, rinsed with deionized water, dried, and programmed to heat up to 500°C for 7 hours to obtain the Sn-ZSM-5 molecular sieve, whose XRD spectrum was as follows: figure 1 (a) shown.

[0037] According to the mass ratio of Sn-ZSM-5 molecular sieve: PDMS: solvent = 1: 0.1: 2, prepare the casting solution, and obtain the casting solution after ultrasonic dispersion for 15 minutes; the casting solution is loaded on the PVC microfiltration membrane by pulling method, Dry at 50°C, and repeat the co...

Embodiment 2

[0039] With water glass (sodium silicate) as silicon source, iron sulfate (FeSO 4 ) is the metal source, EDA is the templating agent, Al 2 SO 3 18H 2 O is the aluminum source, NaOH is the alkali source, and the molar ratio n(NaOH):n(TEOS):n(EDA):n(FeSO 4 ):n(H 2 (0)=0.2:1:0.1:0.05:500 Prepare molecular sieve synthesis solution, age at room temperature for 24 hours, and crystallize in a stainless steel crystallization kettle at 180° C. for 72 hours. Take out the reaction kettle, cool, rinse with deionized water, dry, and heat up to 700 ° C for 7 hours to obtain Fe-ZSM-5 molecular sieve, such as figure 1 (b) shown.

[0040] According to the mass ratio of Fe-ZSM-5 molecular sieve: PDMS: solvent = 1: 0.2: 3, prepare the casting solution, and obtain the casting solution after ultrasonic dispersion for 15 minutes; the casting solution is loaded on the PTFE microfiltration membrane by pulling method, Drying at 60°C and repeat coating three times to obtain a complete Fe-ZSM-5 mo...

Embodiment 3

[0042] Using water glass as silicon source, magnesium nitrate (Mg(NO 3 ) 2 ) is the metal source, EDA is the templating agent, Al 2 SO 3 18H 2 O is the aluminum source, NaOH is the alkali source, and the molar ratio n(NaOH):n(TEOS):n(EDA):n(Mg(NO 3 ) 2 ):n(H 2 (0)=0.2:1:0.1:0.1:600 ​​Prepare molecular sieve synthesis solution, age at room temperature for 24 hours, and crystallize in a stainless steel crystallization kettle at 180° C. for 80 hours. The reactor was taken out, cooled, rinsed with deionized water, dried, programmed to heat up to 600° C. and calcined for 7 hours to obtain Mg-ZSM-5 molecular sieve.

[0043] According to the mass ratio of Mg-ZSM-5 molecular sieve: PDMS: solvent = 1: 0.2: 3, prepare the casting solution, and obtain the casting solution after ultrasonic dispersion for 15 minutes; the casting solution is loaded on the PTFE microfiltration membrane by pulling method, Dry at 60°C and repeat coating three times to obtain a complete Mg-ZSM-5 molecula...

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PUM

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Abstract

The invention provides a ZSM-5 molecular sieve composite membrane, comprising a separation layer and a support layer, wherein the separation layer is a metal element modified ZSM-5 molecular sieve; and metal elements are selected from Fe, Al, Sn, Ca, Ni, Cu, Mg, Ge, Zn or Zr and is respectively from metal compounds containing the metal elements. The metal element modified ZSM-5 molecular sieve composite membrane selectively causes organic matters to penetrate, has the advantages of simple preparation method, high membrane forming speed, easily-controlled membrane thickness and good membrane continuity, is easy to prepare on a large area and is practically applied industrially.

Description

technical field [0001] The present invention relates to a molecular sieve membrane, in particular to an organosolvent-friendly molecular sieve composite membrane, more specifically to a metal element modified ZSM-5 molecular sieve composite membrane applied in pervaporation, and a preparation method thereof. Background technique [0002] Pervaporation is a new membrane separation technology for separating liquid mixtures, which has the advantages of high efficiency, simple equipment, and no secondary pollution. Since the establishment of small industrial plants in the early 1980s, pervaporation technology has been greatly developed, but in general, pervaporation technology is still a developing technology. In the whole process of pervaporation development, membrane selection and large-area preparation and application have always been urgent problems to be solved in the whole process development and application. At present, there are many organic polymer membranes on the mar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D69/12B01D67/00B01D61/00
Inventor 张环茹王建强樊少斌戴云帆
Owner BEIJING CLP JIAMEI ENVIRONMENTAL PROTECTION TECH
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