Preparation method of PIM-1@MOFs/polymer composite pervaporation membrane

A PIM-1, pervaporation membrane technology, applied in the field of preparation of PIM-1@MOFs/polymer composite pervaporation membranes, can solve the problems of not agglomerating MOFs, restricting applications, etc., achieving a simple preparation method, increasing separation performance, The effect of low production cost

Active Publication Date: 2019-07-19
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the easy agglomeration of MOF nanoparticles also limits its application.
So far, there have been many methods to improve the dispersion of MOF in polymer matrices, including pre-polymerization of polymer solution, ultrasonic probe ultrasound, etc., but due to the strong interaction between nanoparticles during the drying process of MOF However, none of these methods are effective enough to prevent MOF agglomeration

Method used

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  • Preparation method of PIM-1@MOFs/polymer composite pervaporation membrane
  • Preparation method of PIM-1@MOFs/polymer composite pervaporation membrane
  • Preparation method of PIM-1@MOFs/polymer composite pervaporation membrane

Examples

Experimental program
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Effect test

example 1

[0033](1) Weigh 0.75g of zinc nitrate hexahydrate and 1.65g of 2-methylimidazole and dissolve them in 35mL of methanol respectively, and ultrasonicate for 30min; quickly pour the resulting solution into a 100mL polytetrafluoroethylene reactor, and react at 150°C for 5h, Then cool to room temperature, centrifuge, wash off the white solid surface obtained by the reaction with methanol, which is the ligand of the reaction, wash it three times, centrifuge, and then stir it in methanol at 80°C for 12h, and replace it every 4 hours Methanol was separated by centrifugation, and the resulting solid was vacuum-dried at 80°C for 24 hours.

[0034] (2) Weigh 0.15g of PIM-1 and dissolve it in 5mL of chloroform, and ultrasonicate for 1 hour; weigh 0.0382g of the solid obtained in step 1 and soak in the above solution for 10min, centrifuge to separate ZIF-8, and dry it at room temperature. Wash the soaked ZIF-8 with chloroform for 3 times, then wash with methanol for 3 times, and dry it for...

example 2

[0038] (1) Weigh 0.75g of zinc nitrate hexahydrate and 1.65g of 2-methylimidazole and dissolve them in 35mL of methanol respectively, and ultrasonicate for 30min; quickly pour the resulting solution into a 100mL polytetrafluoroethylene reactor, and react at 150°C for 5h, Then cool to room temperature, centrifuge, wash off the white solid surface obtained by the reaction with methanol, which is the ligand of the reaction, wash it three times, centrifuge, and then stir it in methanol at 80°C for 12h, and replace it every 4 hours Methanol was separated by centrifugation, and the resulting solid was vacuum-dried at 80°C for 24 hours.

[0039] (2) Weigh 0.15g of PIM-1 and dissolve it in 5mL of chloroform, and ultrasonicate for 1 hour; weigh 0.0764g of the solid obtained in step 1 and soak in the above solution for 10min, centrifuge to separate ZIF-8, and dry it at room temperature. Wash the soaked ZIF-8 with chloroform for 3 times, then wash with methanol for 3 times, and dry it fo...

example 3

[0043] (1) Weigh 0.75g of zinc nitrate hexahydrate and 1.65g of 2-methylimidazole and dissolve them in 35mL of methanol respectively, and ultrasonicate for 30min; quickly pour the resulting solution into a 100mL polytetrafluoroethylene reactor, and react at 150°C for 5h, Then cool to room temperature, centrifuge, wash off the white solid surface obtained by the reaction with methanol, which is the ligand of the reaction, wash it three times, centrifuge, and then stir it in methanol at 80°C for 12h, and replace it every 4 hours Methanol was separated by centrifugation, and the resulting solid was vacuum-dried at 80°C for 24 hours.

[0044] (2) Weigh 0.15g of PIM-1 and dissolve it in 5mL of chloroform, and ultrasonicate for 1 hour; weigh 0.0115g of the solid obtained in step 1 and soak in the above solution for 10min, centrifuge to separate ZIF-8, and dry it at room temperature. Wash the soaked ZIF-8 with chloroform for 3 times, then wash with methanol for 3 times, and dry it fo...

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Abstract

The invention discloses a preparation method of a PIM-1@MOFs / polymer defect-free composite pervaporation membrane, which comprises the following steps: respectively dissolving zinc nitrate hexahydrateand 2-methylimidazole serving as raw materials into methanol, mixing the obtained solutions, and reacting at 120-150 DEG C for 3-8 hours to obtain MOF powder; immersing the MOF powder into a polymersolution with micropores, and carrying out centrifugal separation to obtain treated MOF powder; dissolving a high molecular weight polymer in an organic solvent B, and adding a cross-linking agent, acatalyst and the treated MOF powder to obtain a PIM-1@MOF / polymer mixed solution; taking an ultrafiltration porous membrane of a high-molecular polymer as a bottom membrane, and uniformly dipping andcoating the bottom membrane with the obtained PIM-1@MOF / polymer mixed solution to obtain the PIM-1@MOF / polymer composite membrane. According to the prepared membrane, the hydrophobicity of an originalmembrane can be improved, and the interface defects between MOFs and polymers can be reduced, so that the permeation flux and the separation effect of the membrane are improved. The preparation method disclosed by the invention is simple and feasible, low in price and wide in application prospect.

Description

[0001] (1) Technical field [0002] The invention relates to the preparation of ultra-thin hybrid membranes and its technical field in the separation of alcohol and water, in particular to a preparation method of a PIM-1@MOFs / polymer composite pervaporation membrane. [0003] (2) Background technology [0004] Pervaporation is a membrane separation technology that combines membrane permeation and evaporation for the selective separation of liquid molecular mixtures. The general process of pervaporation consists of the following steps: (1) A liquid mixture flows through the upstream side of a membrane. (2) Components in the feed pass through the membrane driven by a chemical potential difference, which can be obtained downstream of the membrane by vacuuming, gas sweeping, or thermal differential. (3) Steam seeps out from the downstream of the membrane. The mass transfer process in pervaporation membranes is generally described by solution diffusion mechanism and facilitated tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/70B01D61/36B01D69/12B01D67/00
CPCB01D61/362B01D67/0002B01D69/12B01D71/34B01D71/70B01D2323/30B01D2325/38
Inventor 张国亮程浩峰张旭苏鹏程孟琴
Owner ZHEJIANG UNIV OF TECH
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