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A kind of preparation method of polyvinylidene fluoride hollow fiber porous membrane

A technology of polyvinylidene fluoride and polyvinylidene fluoride resin, which is applied in the field of preparation of polyvinylidene fluoride hollow fiber porous membranes, and can solve problems such as voids, uneconomical and environmental protection, and widened pore size distribution

Active Publication Date: 2022-02-15
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since a strong alkaline aqueous solution is required to extract hydrophobic silica, the polyvinylidene fluoride resin constituting the membrane is easily degraded, affecting the service life of the membrane in engineering applications, and a large amount of inorganic wastewater is generated during the membrane making process , needs to be treated by other means in the later stage, which is very uneconomical and environmentally friendly. At the same time, the added silica is prone to agglomeration, which makes it easy to form relatively large void defects in the membrane after extraction, widens the pore size distribution of the membrane, and reduces the impact on pollutants. interception effect

Method used

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  • A kind of preparation method of polyvinylidene fluoride hollow fiber porous membrane
  • A kind of preparation method of polyvinylidene fluoride hollow fiber porous membrane
  • A kind of preparation method of polyvinylidene fluoride hollow fiber porous membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Preparation of modified MOF materials:

[0062] a. Weigh 4g of ZIF-11 solid powder, put it into 100mL of toluene, stir evenly, add 5mmol of ethylenediamine, and reflux for 12 hours; cool and filter after the reaction to obtain ZIF-NH 2 Nanoparticles were washed repeatedly with absolute ethanol, dried in vacuum, and ground for later use;

[0063] b. Add 8g ZIF-NH 2 Nanoparticles and 500mL dichloromethane were ultrasonically dispersed for 1 h, cooled to room temperature, and 4 g of RAFT reagent 4-cyano-4-[(dodecylsulfanylthiocarbonyl)sulfanyl]pentanoic acid (CDP) was added, iced After bathing for 30 min, add 10 g of dicyclohexylcarbodiimide (DCC) and 2 g of 4-dimethylaminopyridine (DMAP), and react for 48 h at room temperature to immobilize CDP on the surface of ZIF nanoparticles to form ZIF-CDP, and centrifuge to separate the product , and freeze-dried after being fully washed with ethanol and pure water for use;

[0064] c. Add 50g of the N,N-dimethylacetamide (D...

Embodiment 2

[0070] (1) Preparation of modified MOF materials:

[0071] The modified MOF material is prepared by the method in Example 1, the difference is that the MOF material is selected from ZIF-8, and the amphiphilic copolymer is an ethylene-vinyl alcohol copolymer, and the addition of the copolymer in step (1).c The amount is 40% of the mass of ZIF-CDP nanoparticles. Calculated by weighing method, the graft ratio of the copolymer in ZIF-8 is 15%.

[0072] (2) Preparation of PVDF hollow fiber porous membrane:

[0073] The PVDF hollow fiber porous membrane is prepared by the method in Example 1, the difference is that the material and the corresponding mass ratio are: 10% of the above-mentioned modified ZIF-8 crystal, 22% trioctyl trimellitate, 5% diphenylmethylbenzene Ketone, 60% polyvinylidene fluoride, 3% antioxidant 1010. The mass ratio of organic pore formers (trioctyl trimellitate and benzophenone) to ethanol was 1:1.

Embodiment 3

[0075] (1) Preparation of modified MOF materials:

[0076] The modified MOF material is prepared by the method in Example 1. The difference is that the MOF material is selected from MIL-100 (Cr), and the amphiphilic copolymer is ethylene-vinyl alcohol polymer, and the copolymer is in step (1).c The amount added in is 80% of the ZIF-CDP nanoparticle mass. Calculated by weighing method, the graft ratio of the copolymer in ZIF-8 is 33%.

[0077] (2) Preparation of PVDF hollow fiber porous membrane:

[0078] Adopt the method in embodiment 1 to prepare PVDF hollow fiber porous membrane, the difference is that, material and corresponding mass ratio are: 40% above-mentioned modified MIL-100 (Cr) crystal, 34.5% acetyl tributyl citrate, 25% poly Vinylidene fluoride, 0.5% heat stabilizer. The mass ratio of organic pore former (acetyl tributyl citrate) to ethanol is 5:1.

[0079] Measuring the pore size and pore size distribution of the hollow fiber porous membrane prepared in this e...

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Abstract

The invention provides a preparation method of polyvinylidene fluoride hollow fiber porous membrane, comprising the following steps: 1) configuring the following components by weight ratio: polyvinylidene fluoride resin 25-65%, organic pore-forming agent 10-60% 10% to 50% of the modified MOF material, 0% to 5% of the additive; 2) Mix the modified MOF material with the ethanol solution of the organic pore-forming agent according to the above weight ratio, then add polyvinylidene fluoride resin, and mix the additive evenly; Drying to remove ethanol to obtain mixed powder for film casting; 3) Melting and extruding the mixed powder, cooling in coagulation bath, then stretching and heat setting; 4) Extracting and removing organic pore-forming agent to obtain polyvinylidene fluoride hollow fiber porous membrane. The method is simple and effective, and the three wastes are produced less in the membrane-making process, and the prepared PVDF hollow fiber porous membrane has excellent performance and uniform pore size distribution.

Description

technical field [0001] The invention relates to a preparation method, in particular to a preparation method of a polyvinylidene fluoride hollow fiber porous membrane, and belongs to the technical field of membranes. Background technique [0002] At this stage, with the advancement of technology, the industrial application of microfiltration membranes and ultrafiltration membranes has become one of the new chemical unit operations. Microfiltration membranes and ultrafiltration membranes can be used in the separation, concentration, purification of biological products, pharmaceutical products and food industries, and can also be used in terminal treatment devices in blood treatment, wastewater treatment and ultrapure water preparation. [0003] Among microfiltration and ultrafiltration membrane materials, polyvinylidene fluoride (PVDF) is a membrane material with excellent performance. Due to its hydrophobicity, heat resistance, chemical stability, radiation resistance and goo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D67/00B01D69/08B01D71/34
CPCB01D71/34B01D69/08B01D67/0002
Inventor 魏汉辉游彦伟赵伟国王世宇孙家宽
Owner WANHUA CHEM GRP CO LTD
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