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Preparation method of ferrocene-based azo-phenyl amphiphilic segmented copolymer material for preparing regular honeycomb membrane

A ferrocene-based azophenyl group and amphiphilic block technology, which is applied in the field of amphiphilic block copolymer material preparation, can solve the problems of irregular pore arrangement and limited pore shape, and achieve good thermal stability , the ratio is flexible and adjustable, and the stimulus response phenomenon is obvious.

Inactive Publication Date: 2018-09-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Common amphiphilic block copolymers have disadvantages such as irregular pore arrangement and limited pore shape (usually regular hexagonal or circular) in the process of preparing honeycomb porous membrane by water droplet template method.

Method used

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  • Preparation method of ferrocene-based azo-phenyl amphiphilic segmented copolymer material for preparing regular honeycomb membrane
  • Preparation method of ferrocene-based azo-phenyl amphiphilic segmented copolymer material for preparing regular honeycomb membrane
  • Preparation method of ferrocene-based azo-phenyl amphiphilic segmented copolymer material for preparing regular honeycomb membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] ① Under anhydrous and oxygen-free conditions, dissolve 9.4195g (40.9mmol) of ferrocenecarboxylic acid in reflux-dried 100mL of dichloromethane solvent, add 3.2mL of pyridine as catalyst, and 5.0mL of oxalyl chloride (58.6mmol) as Acyl chloride reagent, reflux reaction for 5 hours, remove the solvent and excess oxalyl chloride in a vacuum, add 100mL of petroleum ether (60-90°C), reflux for 2 hours, filter under reduced pressure, and remove the petroleum ether in a vacuum to obtain ferrocenecarbonyl chloride;

[0044]②Add reflux-dried 80mL tetrahydrofuran to 8.7020g (35.0mmol) ferrocenecarbonyl chloride as a solvent, 4.0mL triethylamine as a catalyst, slowly add 4.0mL (35.4mmol) hydroxyethyl methacrylate dropwise, and reflux for 5h , filtered under reduced pressure, the filtrate was rotary evaporated, and the solvent was removed to obtain the crude product of ferroceneformyloxyethyl methacrylate, which was successively washed with 250mL saturated Na 2 CO 3 The solution a...

Embodiment 2

[0053] Front four steps are as embodiment 1, and back two steps are as follows:

[0054] ⑤ Weigh 2.0590 g (2 mmol) of polyethylene glycol monomethyl ether with a molecular weight of 1000, and vacuumize to remove water and dry for 0.5 h. Under the protection of argon, add 40mL of reflux-dried THF to dissolve, add 0.6mL (4mmol) triethylamine, slowly add 0.5mL (4mmol) 2-bromoisobutyryl bromide dropwise under ice-water bath, and react at 25°C 10h. After the reaction was completed, filter under reduced pressure, concentrate the filtrate by rotary evaporation, add dropwise to 250 mL of n-hexane for precipitation, and extract the precipitate by suction filtration. The precipitate was dissolved in 2 mL of THF, then precipitated with 250 mL of n-hexane and filtered, and the operation was repeated three times. The obtained precipitate was dried in a vacuum oven at 20°C for 24 hours to obtain the product.

[0055] ⑥Add 114.0mg of PEO-Br, 1.7275g of FcEMA, and 1.8345g of MAAZOOHEE in tu...

Embodiment 3

[0059] Front four steps are as embodiment 1, and back two steps are as follows:

[0060] ⑤ Weigh 4.0183 g (2 mmol) of polyethylene glycol monomethyl ether with a molecular weight of 2000, and vacuumize to remove water and dry for 0.5 h. Under the protection of argon, add 40mL of reflux-dried THF to dissolve, add 0.6mL (4mmol) triethylamine, slowly add 0.5mL (4mmol) 2-bromoisobutyryl bromide dropwise under ice-water bath, and react at 25°C 10h. After the reaction was completed, filter under reduced pressure, concentrate the filtrate by rotary evaporation, add dropwise to 250 mL of n-hexane for precipitation, and extract the precipitate by suction filtration. The precipitate was dissolved in 2 mL of THF, then precipitated with 250 mL of n-hexane and filtered, and the operation was repeated three times. The obtained precipitate was dried in a vacuum oven at 20°C for 24 hours to obtain the product.

[0061] ⑥Add 214.6mg of PEO-Br, 1.7066g of FcEMA, and 1.8250g of MAAZOOHEE in tu...

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Abstract

The invention discloses a preparation method of a ferrocene-based azo-phenyl amphiphilic segmented copolymer material for preparing a regular honeycomb membrane. The preparation method comprises the following steps: preparing chlorocarbonyl ferrocene from ferrocenecarboxylic acid, and then preparing ferrocenyl methoxyethyl methacrylate monomers from chlorocarbonyl ferrocene and hydroxyethyl methacrylate; preparing azo-phenyl-6-hydroxyl from 4-hydroxyl azobenzene, and then preparing azobenzene monomers from azo-phenyl-6-hydroxyl; preparing a macromolecular initiator from polyethylene glycol monomethyl ether; mixing the ferrocenyl methoxyethyl methacrylate monomers, the azobenzene monomers and the macromolecular initiator, and adding CuBr and PMDETA, thus obtaining the regular honeycomb membrane errocene-based azo-phenyl amphiphilic segmented copolymer material (PEO-b-P(FcEMA-co-MAAZOOHEE)s. The polymer hydrophilic-hydrophobic chain segment ratio is flexible to adjust, the material heatstability is good, the stimulation response phenomenon is apparent, and convenience in photoelectric response detection can be realized.

Description

technical field [0001] The invention relates to the field of preparation of amphiphilic block copolymer materials, in particular to a preparation method of a ferrocenyl azophenyl amphiphilic block copolymer material used for preparing regular honeycomb membranes. Background technique [0002] Honeycomb porous membranes are widely used in separation, superhydrophobic materials, tissue engineering, photolithography and other fields. The water droplet template method is a commonly used method to prepare honeycomb membranes. The film-forming material is an important factor for the preparation of honeycomb porous membrane by the water drop template method. Amphiphilic block copolymer is the most commonly used material, and the ratio of its hydrophilic and hydrophobic segments affects the regularity of the honeycomb porous membrane. Key factor. [0003] Common amphiphilic block copolymers have disadvantages such as irregular pore arrangement and limited pore shape (usually regula...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F230/04C08F220/36C08J5/18C08L53/00
CPCC08F220/36C08F230/04C08F293/00C08J5/18C08J2353/00
Inventor 俞豪杰夏霞王立
Owner ZHEJIANG UNIV
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