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Preparation method of amphiphilic triblock copolymer modified ultrafiltration membrane with pH-responsive property

A copolymer modification, amphiphilic technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the irreversible pollution of organic substances such as proteins, insufficient control of membrane pore functionalization, and strong hydrophobicity of separation membranes. and other problems, to achieve the effect of controllable product structure, wide range of applicable monomers, and narrow molecular weight range

Inactive Publication Date: 2018-12-07
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the shortcomings of the prior art described above, the purpose of the present invention is to prepare a simple and easy method for a high-flux antifouling membrane with pH responsiveness, so as to solve the problem of strong hydrophobicity and low water flux of traditional separation membranes. Disadvantages, as well as insufficient control over the functionalization of membrane pores and susceptibility to irreversible contamination by organics such as proteins during the separation process

Method used

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  • Preparation method of amphiphilic triblock copolymer modified ultrafiltration membrane with pH-responsive property
  • Preparation method of amphiphilic triblock copolymer modified ultrafiltration membrane with pH-responsive property
  • Preparation method of amphiphilic triblock copolymer modified ultrafiltration membrane with pH-responsive property

Examples

Experimental program
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Effect test

Embodiment 1

[0025] PVDF / PAA 13 -b-PMMA 80 -b-PAA 13 Membrane preparation

[0026] It uses PAMA as a blending modifier, and prepares a pH-responsive amphiphilic block copolymer modified polyvinylidene fluoride membrane by immersion precipitation phase inversion method, which includes the following steps:

[0027]

[0028] 1. Dissolve refined methyl methacrylate, RAFT reagent and azobisisobutyronitrile in toluene. Use a water pump to evacuate for 30 minutes to remove the air in the reaction solution. Use a double-row tube to repeatedly freeze and thaw three times to remove oxygen, stir and react at 70°C for 24 hours under the protection of argon, remove part of the solvent by rotary evaporation, add the polymer solution to ice n-hexane for precipitation, collect the precipitate, and vacuum-dry to constant weight , to obtain PMMA-RAFT. A certain amount of PMMA-RAFT, acrylic acid and azobisisobutyronitrile were dissolved in 60mL of N,N-dimethylformamide, stirred and reacted at 70°C fo...

Embodiment 2

[0031] PVDF / PAA 83 -b-PMMA 80 -b-PAA 83 Membrane preparation

[0032] Prepare PAA according to Example 1 83 -b-PMMA 80 -b-PAA 83 , specifically control the degree of polymerization of PMMA and PAA according to the molar ratio of methyl methacrylate and acrylic acid input.

[0033] Weigh 15g PVDF, 7.25g PEG, 1.125g PAA 83 -b-PMMA 80 -b-PAA 83and N,N-dimethylformamide were put into a three-necked flask, fully stirred at 60°C for 12 hours, and dissolved to obtain a homogeneous casting solution, vacuum defoaming, and evenly poured the casting solution into a dry, clean On the glass plate, a 200 μm film was manually scraped out with a scraper, and the glass plate was placed in a coagulation bath in parallel. The coagulation bath was ethanol / water (V / V) 1 / 3, and the temperature was 25°C. The prepared flat membrane was soaked in deionized water for a period of time to remove the solvent, and then freeze-dried to prepare a pH-responsive amphiphilic block copolymer modified po...

Embodiment 3

[0035] PVDF / PAA 83 -b-PMMA 80 -b-PAA 83 Preparation of modified membrane

[0036] Weigh 15g PVDF, 7.25g PEG, 1.125g PAA 83 -b-PMMA 80 -b-PAA 83 and N,N-dimethylformamide were put into a three-necked flask, fully stirred at 60°C for 12 hours, and dissolved to obtain a homogeneous casting solution, vacuum defoaming, and evenly poured the casting solution into a dry, clean On the glass plate, a 200 μm film was manually scraped out with a scraper, and the glass plate was placed in a coagulation water bath in parallel at a temperature of 25°C. After the membrane fell off the glass plate, the modified membrane was taken out from the coagulation bath and immersed in deionized water, and the water was changed twice a day until the solvent was basically replaced, and then freeze-dried to obtain a pH-responsive amphiphilic block copolymer Modified polyvinylidene fluoride film M-4.

[0037] In order to characterize the pH responsiveness of the modified membrane, the modified membr...

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Abstract

The invention discloses a preparation method of an amphiphilic triblock copolymer modified ultrafiltration membrane with pH-responsive property. The method comprises the following steps: taking methylmethacrylate (MMA) and acrylic acid (AA) as raw materials, and preparing PAA-b-PMMA-b-PAA (PAMA) with a controllable structure by adopting reversible addition-fragmentation chain transfer (RAFT) polymerization. The amphiphilic triblock copolymer modified ultrafiltration membrane is directly prepared by adopting immersion precipitation phase inversion. According to a segregation behavior of the modifier on the membrane surface, the ultrafiltration membrane has a certain hydrophilic property and pollution resistance. The PMMA chain segments in the modifier PAMA adopted in the invention and polyvinylidene fluoride have excellent compatibility, and the membrane is kept stable in the application process. The PAA serving as a hydrophilic segment is enriched on the membrane surface and membranepores, the hydrophilic property of the membrane is improved, and adhesion of pollutants on the membrane surface and membrane pores is avoided. In addition, the ultrafiltration membrane has high anti-pollution capacity and retention rate of proteins and exists effective aperture conversion at the pH value of 3-8, and effective pore size regulation under external environmental stimulation is realized.

Description

technical field [0001] The invention belongs to the field of polymer material science, and relates to an amphiphilic triblock copolymer modified ultrafiltration membrane, in particular to a modified amphiphilic block polymer with a pH-responsive segment as a hydrophilic segment Preparation method of polyvinylidene fluoride film. Background technique [0002] Water is the source of life. Nowadays, the ecological environment has been severely damaged, water bodies are seriously polluted, and the global shortage of fresh water resources is gradually emerging. In addition to actively developing fresh water resources, the secondary utilization of water resources has become the focus of attention. With the continuous development of water treatment technology, the full-membrane water treatment process is becoming more and more mature, which can achieve no need for acid-base regeneration, continuous water production, and stable water quality. It is widely used in water treatment pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D71/34B01D71/80B01D69/02
CPCB01D67/0002B01D69/02B01D71/34B01D71/80
Inventor 赵军强韩洪蕊杨景李冬阳王齐齐赵义平陈莉
Owner TIANJIN POLYTECHNIC UNIV
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