Preparation method of novel MOFs-PVDF (Metal-Organic Frameworks-Polyvinylidene Fluoride) composite film

A composite membrane, a new type of technology, applied in the direction of chemical instruments and methods, membranes, membrane technology, etc., can solve the problems of reduced water flux, low mechanical strength, and poor hydrophilicity of the modified membrane, and increase the porosity , good hydrophilicity and high production efficiency

Inactive Publication Date: 2017-08-08
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the poor hydrophilicity of the membrane in the existing membrane modification method, the agglomeration behavior of nanoparticles makes its dispersion in the casting membrane solution poor, easy to block the membrane pores so that the water flux of the modified membrane decreases, mechanical The strength is not high, and it has the characteristics of simple and easy operation, low energy consumption, short time consumption, and is suitable for industrial applications.

Method used

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  • Preparation method of novel MOFs-PVDF (Metal-Organic Frameworks-Polyvinylidene Fluoride) composite film
  • Preparation method of novel MOFs-PVDF (Metal-Organic Frameworks-Polyvinylidene Fluoride) composite film

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Experimental program
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Effect test

Embodiment 1

[0031] Step 1 Measure the mixed solution of DBP / DMF with a mass ratio of 4 / 6 as a mixed diluent, add PVDF polymer, 10% polyethylene glycol-400 in turn under heating and stirring, and configure a PVDF concentration of 18%. Casting solution.

[0032] Step 2. Gradually raise the temperature of the prepared casting solution to 140°C under constant stirring, and heat and stir for 6 hours.

[0033] Step 3 After the casting solution is mixed evenly, stop stirring and keep warm for 10 hours for defoaming.

[0034] Step 4 After defoaming, prepare and form at 140°C, and enter a deionized water coagulation bath at 20°C for phase inversion to form a film after passing through an air bath;

[0035] Step 5 Soak the spun membrane in absolute ethanol for 24 hours, then soak it in deionized water for 24 hours, take it out and wash it.

[0036] Step 6 Immerse the washed membrane in the mixture of glycerin and deionized water to moisturize and shape it.

Embodiment 2

[0038] Step 1 First, dissolve 1.984g Cu(NO3)2·3H2O and 0.946g trimesic acid in 20mL DMF and 40mL ethanol / deionized water (volume ratio 1:1) mixed solution respectively, The solutions were mixed, hydrothermally reacted at 85 °C for 8 h, filtered, and washed with ethanol three times to obtain a blue solid powder.

[0039] Step 2 Measure 71wt% DBP / DMF mixture with a mass ratio of 4 / 6 as the mixed diluent, weigh 1% blue Cu3(BTC)2 powder in step 1, and ultrasonically disperse in the mixed diluent for 4 hours.

[0040] Step 3 Add 18% PVDF polymer and 10% polyethylene glycol-400 in turn to the solution after ultrasonic dispersion in step 2 under heating and stirring, and configure it as a casting solution in which MOFs are dispersed.

[0041] Step 4 The casting solution in Step 3 was gradually heated up to 140° C. under continuous stirring, and heated and stirred for 6 hours.

[0042] Step 5 After the casting solution is mixed evenly, stop stirring and keep warm for 10 hours for def...

Embodiment 3

[0047]Step 1 Measure the mixed solution of DBP / DMF with a mass ratio of 4 / 6 as a mixed diluent, add PVDF polymer, 10% polyethylene glycol-400, and 1% Cu( NO3) 2.3H2O and trimesic acid, and finally configure a casting solution with a PVDF concentration of 18%.

[0048] Step 2. Gradually raise the temperature of the prepared casting solution to 140°C under constant stirring, and heat and stir for 6 hours.

[0049] Step 3 After the casting solution is mixed evenly, stop stirring and keep warm for 10 hours for defoaming.

[0050] Step 4 After the degassing is completed, the molding is prepared at 140°C, and the nascent film passes through an air bath and enters a deionized water coagulation bath at 20°C to undergo phase inversion to form a film;

[0051] Step 5 Soak the spun membrane in absolute ethanol for 24 hours, then soak it in deionized water for 24 hours, take it out and wash it.

[0052] Step 6 Immerse the washed membrane in the mixture of glycerin and deionized water to...

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Abstract

The invention discloses a preparation method of a novel MOFs-PVDF (Metal-Organic Frameworks-Polyvinylidene Fluoride) composite film. The preparation method is mainly characterized in that a synthesizing environment of MOFs is controlled to be consistent with a casting solution preparation condition, an organic ligand and metal ions are added into a casting solution by a simple one-step synthetic method, intermolecular acting force between the organic ligand and PVDF is regulated and controlled, the PVDF is chemically combined with the MOFs through a hydrogen bond of an 'F' atom, chemical bonding of a PVDF polymer and the MOFs is realized, and an MOFs-PVDF polymer is synthesized in the casting solution, so that the formation of a chemical bonding hole and the formation of an MOFs-PVDF novel film are performed simultaneously in a spinning process. The method is easy and efficient; moreover, the prepared film combines the advantages of an MOFs and PVDF composite film; the prepared novel MOFs-PVDF composite film has the advantages of high chemical stability, high mechanical strength, controllable aperture, large surface specific area and high porosity.

Description

[0001] Technical field [0002] The patent of the present invention relates to the technical field of membrane separation materials, and specifically refers to a preparation method of a novel high-performance MOFs-PVDF composite membrane. Background technique [0003] With the increasingly prominent environmental problems, membrane separation technology has been applied more and more in life and production, and has received extensive international attention. As a new and efficient fluid separation technology, this technology has developed rapidly in recent years and has achieved remarkable research results. It plays an important role in the application of water supply engineering, industrial wastewater, pharmaceutical industry, food industry, energy industry and other fields. Especially in the role of water resources utilization and environmental protection is even more important. Although membrane separation technology has developed rapidly, there are still many problems to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/12B01D69/08B01D67/00B01D71/34
CPCB01D67/0011B01D69/08B01D69/12B01D71/34B01D2325/02B01D2325/24
Inventor 王薇邵冉冉
Owner TIANJIN POLYTECHNIC UNIV
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