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Preparation method of hydrophilic polyvinylidene fluoride flat sheet membrane and hollow fiber membrane

A polyvinylidene fluoride and hydrophilic technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve problems such as unfavorable large-scale production, difficult modification, technical complexity, etc. Poor capacity, guaranteed water flux, uniform cross-linking effects

Active Publication Date: 2014-06-18
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the good chemical stability of PVDF, the C-F bond energy on its molecular chain is large, and chemical reactions are not easy to occur, so surface modification has disadvantages such as difficult modification and complicated technology, which is not conducive to large-scale production

Method used

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  • Preparation method of hydrophilic polyvinylidene fluoride flat sheet membrane and hollow fiber membrane
  • Preparation method of hydrophilic polyvinylidene fluoride flat sheet membrane and hollow fiber membrane
  • Preparation method of hydrophilic polyvinylidene fluoride flat sheet membrane and hollow fiber membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) In a 150ml three-necked flask, add 6g of hydroxypropyl silicone oil (500g / mol), 3g of triethylamine and 20ml of tetrahydrofuran, then place it in an ice-water bath, slowly add 7g of 2-bromoiso The mixture of butyryl bromide and 20ml tetrahydrofuran was removed from the ice-water bath after the dropwise addition, and the reaction was continued for 16 hours at room temperature. After the reaction is complete, remove the insoluble ammonium salt by suction filtration with a Buchner funnel, concentrate the filtered solution, then separate the liquid through a separatory funnel to obtain a macromolecular initiator, add anhydrous magnesium sulfate to dry for 24 hours, and filter to remove anhydrous sulfuric acid. Magnesium derived ATRP macroinitiator bromodimethylsiloxane.

[0058] (2) Add 0.01mol of macromolecular initiator bromodimethylsiloxane, complexing agent pentamethyldiethylenetriamine 0.02mol, monomer methyl methacrylate 1mol and 20 ml of solvent toluene and 0.02...

Embodiment 2

[0061] (1) In a 150mL three-necked flask, add 6g of hydroxymethyl silicone oil (1000g / ml), 1.5g of triethylamine and 20ml of tetrahydrofuran, and slowly add 3.5g of 2-bromoisobutyl through a constant pressure dropping funnel under nitrogen protection The mixture of acid chloride and 10ml tetrahydrofuran, after the dropwise addition, the ice-water bath was removed, and the reaction was continued at room temperature for 24h. After the reaction is completed, remove the insoluble ammonium salt by suction filtration with a Buchner funnel, concentrate the filtered solution and separate the liquid through a separatory funnel to obtain a modified chlorine-terminated polydimethylsiloxane, and then add anhydrous magnesium sulfate After drying for 24 hours and removing anhydrous magnesium sulfate by filtration, macromolecular ATRP initiator-terminated chlorodimethylsiloxane was obtained.

[0062] (2) In a 100ml flask under an argon atmosphere, add macromolecular initiator terminal chloro...

Embodiment 3

[0065](1) In a 250ml three-necked flask, add 30g of hydroxybutyl silicone oil (2000g / ml), 3.5g of triethylamine and 40ml of dichloromethane, and slowly add 7.5g of 2-bromo The mixture of isobutyryl bromide and 20ml of dichloromethane was removed after the dropwise addition, and the ice-water bath was removed, and the reaction was continued at room temperature for 24h. After the reaction is completed, remove the insoluble ammonium salt by suction filtration with a Buchner funnel, concentrate the filtered solution and separate the liquid through a separatory funnel to obtain a modified bromopolydimethylsiloxane, and then add anhydrous magnesium sulfate to dry After 24 hours, anhydrous magnesium sulfate was removed by filtration to obtain macromolecular ATRP initiator-terminated bromodimethylsiloxane.

[0066] (2) In a 100ml flask under an argon atmosphere, add 0.01mol of macromolecular initiator bromodimethylsiloxane, 0.02mol of complexing agent pentamethyldiethyltriamine, and m...

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Abstract

The invention provides a preparation method of a hydrophilic polyvinylidene fluoride flat sheet membrane and a hollow fiber membrane. The preparation method of the hydrophilic polyvinylidene fluoride flat sheet membrane and the hollow fiber membrane is characterized by comprising the following particular steps: adding macroinitiator halogen-terminated dimethyl siloxane, a complexing agent, a monomer and a solvent as well as a catalyst cuprous halide to a reaction container under the protection of inert gases, heating to 40-120 DEG C under the condition of magnetic stirring, reacting for 1-24 hours, and purifying so as to obtain a triblock copolymer; adding the triblock copolymer, the complexing agent, the monomer, the solvent and the catalyst cuprous halide, which are obtained in the first step to another reaction container under the protection of inert gases, heating to 50-120 DEG C under the stirring condition, reacting for 6-24 hours, and purifying so as to obtain an amphiphilic five-block copolymer; and casting membranes so as to obtain the hydrophilic polyvinylidene fluoride membrane. The preparation method provided by the invention is simple, achieves the aim of hydrophilic modification by blending amphiphilic polymers, and finally improves the pollution resistance of the membranes.

Description

technical field [0001] The invention belongs to the field of preparation of ultrafiltration / microfiltration membranes, in particular to a preparation method of a hydrophilic polyvinylidene fluoride flat membrane and a hollow fiber membrane. Background technique [0002] Polyvinylidene fluoride (PVDF) is one of the mainstream membrane material raw materials in the water treatment membrane market. Because of its good chemical stability, corrosion resistance, radiation resistance and weather resistance, and excellent mechanical properties, it has been widely used in various Water purification treatment, such as oily wastewater treatment, printing and dyeing wastewater treatment, heavy metal wastewater treatment, urban sewage treatment, etc. In addition, PVDF membranes have been widely used in microfiltration, ultrafiltration, gas separation, seawater desalination, etc. [0003] Due to the extremely low surface energy of polyvinylidene fluoride, it is a typical hydrophobic mate...

Claims

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Application Information

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IPC IPC(8): B01D71/34B01D69/06B01D69/08B01D69/02B01D67/00
Inventor 何春菊李丹
Owner DONGHUA UNIV