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Preparation method of hydrophilic polyvinylidene fluoride (PVDF) hybrid membrane

A polyvinylidene fluoride, hydrophilic technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of unstable hydrophilic performance of separation membranes, and achieve the effect of protein reduction

Active Publication Date: 2017-09-05
QUJING NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to disclose a method for preparing a hydrophilized polyvinylidene fluoride hybrid membrane, which solves the problem that the nanoparticles are prone to agglomeration in the process of modifying the PVDF membrane with inorganic nanoparticles, which causes the hydrophilic property of the separation membrane to be unstable. defects, using polydimethylaminoethyl methacrylate (PDMAEMA) on ZrO 2 Nanoparticles are functionalized and modified so that they can be evenly distributed in the PVDF membrane, and a hybrid PVDF flat separation membrane with stable hydrophilic properties is obtained

Method used

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  • Preparation method of hydrophilic polyvinylidene fluoride (PVDF) hybrid membrane
  • Preparation method of hydrophilic polyvinylidene fluoride (PVDF) hybrid membrane

Examples

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Effect test

Embodiment 1

[0036] (1) KH-230 to ZrO 2 Nanoparticle treatment: weigh 5g dry ZrO 2 Nanoparticles were placed in 100 ml of toluene, ultrasonically dispersed for 30 min, then 30 ml of γ-chloromethyltriethoxysilane (KH-230) was added, and refluxed at 80 °C for 24 h. After the reaction, the reaction solution was centrifuged, the product was repeatedly washed with absolute ethanol and pure water three times, and dried in an oven at 60°C for 24 hours to obtain ZrO 2 -Cl nanoparticles.

[0037] (2) ZrO 2 - Synthesis of g-PDMAEMA: Weigh 2 g of dry ZrO 2 -Cl is immersed in 100 ml N-methylpyrrolidone (NMP) solvent, and the protective agent N 2 After ultrasonication for 30 min, 0.025 mol of DMAEMA monomer, 300 μl of PMDETA, and 0.12 g of CuCl were added, and vacuumed with a vacuum pump. React in an oil bath at 70°C for 24 hours under airtight conditions. After the reaction, the reaction solution was centrifuged, the product was repeatedly washed with absolute ethanol and pure water three times,...

Embodiment 2

[0041] (1) KH-230 to ZrO 2 Nano particle processing: same as embodiment 1.

[0042] (2) ZrO 2 -Synthesis of g-PDMAEMA: the main synthesis process is the same as in Example 1. The main difference is that the amount of DMAEMA monomer added is 0.05mol.

[0043] (3) PVDF / ZrO 2 - Preparation of g-PDMAEMA hybrid separation membrane (M2): The preparation process is the same as in Example 1, the main difference is that the added ZrO 2 -g-PDMAEMA is the nanoparticle synthesized when the addition amount of DMAEMA monomer is 0.05mol.

[0044] In this example, the obtained PVDF / ZrO 2 - The initial water contact angle of g-PDMAEMA hybrid membrane M2 is 75º, and the adsorption capacity of BSA is 87μg / cm 2 .

Embodiment 3

[0046] (1) KH-230 to ZrO 2 Nano particle processing: same as embodiment 1.

[0047] (2) ZrO 2 -Synthesis of g-PDMAEMA: the main synthesis process is the same as in Example 1. The main difference is that the amount of DMAEMA monomer added is 0.075mol.

[0048] (3) PVDF / ZrO 2 - Preparation of g-PDMAEMA hybrid separation membrane (M3): The preparation process is the same as in Example 1, the main difference is that the added ZrO 2 -g-PDMAEMA is the nanoparticle synthesized when the addition amount of DMAEMA monomer is 0.075mol.

[0049] In this example, the obtained PVDF / ZrO 2 - The initial water contact angle of g-PDMAEMA hybrid membrane M3 is 68º, and the adsorption capacity of BSA is 64μg / cm 2 .

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Abstract

The invention relates to a preparation method of a hydrophilic polyvinylidene fluoride (PVDF) hybrid membrane. The method comprises the following steps: treating zirconium dioxide (ZrO2) nano particles by using a silane coupling agent, i.e., gamma-chloropropyl triethoxysilane (KH-230) so as to obtain ZrO2-Cl nano particles having chlorine group-containing surfaces; grafting poly(N, N-dimethylaminoethyl methacryIate) (PDMAEMA) onto the ZrO2-Cl nano particles by using an atom transfer radical polymerization (ATRP) method so as to obtain ZrO2-g-PDMAEMA nano particles of PDMAEMA-modified ZrO2; preparing the hydrophilic PVDF / ZrO2-g-PDMAEMA hybrid separating separation membrane by taking PVDF as a membrane material and taking ZrO2-g-PDMAEMA and polyethylene glycol (PEG) as additives. The hydrophilia of the hydrophilic PVDF hybrid membrane is superior to that of a pure PVDF membrane, and protein adsorbed on the surface of the hydrophilic PVDF hybrid membrane is obviously reduced, so that the hydrophilic PVDF hybrid membrane can be used as a sewage treatment separation membrane.

Description

technical field [0001] The invention belongs to a preparation method of a hydrophilized polyvinylidene fluoride hybrid membrane, and in particular relates to a preparation technology of a hydrophilized organic-inorganic hybrid polyvinylidene fluoride separation membrane. Background technique [0002] In recent years, with the continuous deepening of membrane separation technology research and the expansion of the application market, membrane separation technology has gradually become an important force in the application of sewage treatment, petrochemical, food industry and other industries. The core of membrane separation technology is the separation membrane material. At present, the commonly used separation membranes are mainly organic polymer materials, among which polyvinylidene fluoride (PVDF) has good mechanical properties, chemical stability and film-forming properties, and can be used to prepare ultrafiltration and microfiltration membranes. PVDF membrane has stron...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/34B01D69/02B01D69/06B01D67/00C02F1/44
Inventor 申向汪帆
Owner QUJING NORMAL UNIV
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