A kind of amphiphilic copolymer endowing membrane material with pH responsiveness and preparation method thereof
An amphiphilic copolymer and membrane material technology, applied in the field of amphiphilic copolymers, can solve the problems of poor compatibility between hydrophobic segments and membrane matrix, introduction of pH-responsive functional segments, and few types of compatible hydrophobic segments. , to achieve precise control of molecular weight and molecular weight distribution, easy large-scale production, and simple operation.
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[0049] In the preparation method of the present invention, the reaction temperature and time described in the step (1), step (2) and step (3) are based on the specific type of the reaction compound, the predetermined structural unit repeating numbers n and m, the predetermined two The number average molecular weight of the pro-copolymer is adjusted.
[0050] In the preparation method of the present invention, the number average molecular weight of the hydroxypropyl silicone oil described in step (1) is 3000-5000 g / mol, such as 3000, 4000 or 5000 g / mol.
[0051] For convenience of description, the material used in the examples is abbreviated as follows:
[0052] name
abbreviation
name
abbreviation
Hydroxypropyl silicone oil
HO-PDMS-OH
AAA
PDMS
MAA
2-Bromoisobutyryl bromide
BIBB
tert-butyl acrylate
tBA
PDMS macroinitiator
Br-PDMS-Br
tert-but...
Embodiment 1
[0064] (1) Macroinitiator Br-PDMS 54 -Br (wherein the subscript 54 is the number of dimethylsiloxane structural units in PDMS, and the subscript Arabic numerals below all indicate the number of structural units; when the subscript is not used, the number of structural units is limited in the present invention Within the range of n and m.) Synthesis. Add 30g HO-PDMS-OH (number average molecular weight 4000g / mol), 2.204mL triethylamine and 100mL THF into a 250mL three-neck flask, add 1.882mLBIBB and 20mL THF into a constant pressure funnel, and blow argon into the flask for 10min to remove Air, the liquid in the constant pressure funnel was slowly added dropwise to the three-neck flask in the ice-water bath, and the ice-water bath was removed after 1 hour, and reacted at room temperature for 16 hours. Remove ammonium salt by filtration, remove THF by rotary evaporation, then add 100mL n-hexane to dissolve, wash 3 times with 70mL deionized water in a separatory funnel, remove th...
Embodiment 2
[0068] (1) Macroinitiator Br-PDMS 54 - Preparation of Br. Method is the same as embodiment 1 step (1).
[0069] (2) Triblock copolymer PtBMA 25 -PDMS 54 -PtBMA 25 preparation. Add the macromolecular initiator Br-PDMS into the 100mL oblique two-necked flask 54 - Br 1.0g (0.25mmol), CuBr 0.072g (0.5mmol), sealed - frozen, evacuated - filled with argon 3 times. Add 13.17mL of butanone, 3.977mL (25mmol) of tert-butyl methacrylate (tBMA) and 100μL (0.5mmol) of pentamethyldiethylenetriamine (PMDETA) into a small beaker. In an open flask, stir at room temperature to completely dissolve the copper salt, then transfer to an oil bath at 60°C for 24 hours. After the reaction, use 10mL butanone to dilute the reaction solution, pass through a neutral alumina column, use butanone as the eluent to remove copper salt, and remove most of the solvent by rotary evaporation, then add the remaining solution dropwise to 200mL methanol and water (v / v 50:50), remove the solvent by filtration,...
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