A kind of method and application of synthesizing diamine-terminated polystyrene based on ATRP active polymerization method

A polystyrene and bis-amine-based sealing technology is applied in the synthesis of bis-amine-terminated polystyrene based on an ATRP active polymerization method and the application field, and can solve the problems of high use cost, complex synthesis conditions, unfavorable large-scale application, and the like, Achieve the effect of low production cost, mature technical route and easy industrial production

Active Publication Date: 2021-07-20
SOUTHWEST PETROLEUM UNIV
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  • Abstract
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AI Technical Summary

Problems solved by technology

However, its synthesis conditions are relatively complicated, and its use cost is relatively expensive, which is not conducive to large-scale application.

Method used

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Effect test

preparation example Construction

[0031] The invention describes a method for synthesizing diamine-terminated polystyrene based on ATPR active polymerization for reducing oil / water interfacial tension. The steps are as follows:

[0032] Using N-bromomethylphthalimide as the ATRP initiator, using CuBr / 2,2'-bipyridine as the catalyst, and styrene as the monomer for atom transfer radical polymerization, by adjusting the ATRP initiator and The ratio between styrene, polymerized at 110°C for 0.5-3h, to obtain modified polystyrene with different molecular weights; then react the synthesized modified polystyrene with potassium phthalimide in anhydrous DMF 12h, obtain the polystyrene that two phthalimide group protects; Finally, reduce under the action of hydrazine hydrate, obtain the polystyrene that end-blocks with diamine group; Finally, dissolve the polystyrene with diamine group in toluene as In the oil phase, the functionalized nanoparticles are dissolved in water, and the pH value of the aqueous phase solution ...

Embodiment 1

[0046] Embodiment 1: the preparation of diamine-based polystyrene (1)

[0047] Mix 0.1mol potassium phthalate and 1mol dibromomethane in a certain proportion, add 40mL of anhydrous DMF as a solvent, and react at 60°C for 6h. After the reaction, pour the reaction solution into ice water to obtain a crude product; dissolve in Recrystallize three times in hot ethanol, put into vacuum oven and dry for 24h to obtain pure initiator N-bromomethylphthalimide; place the initiator and styrene monomer in a molar ratio of 1:15 In the reaction system, after three times of vacuuming and argon circulation, after closing the reaction system, under the action of a catalyst, react at 110°C for 0.5h, open the reaction system to allow oxygen to enter the quenching reaction, and add the mixed solution after the reaction to a certain amount Dilute it with chloroform, pass it through a neutral alumina chromatography column, collect the liquid and pour it into methanol to precipitate the polymer, aft...

Embodiment 2

[0049] Embodiment 2: the preparation of diamine-based polystyrene (2)

[0050] Mix 0.1mol potassium phthalate and 1mol dibromomethane in a certain proportion, add 40mL of anhydrous DMF as a solvent, and react at 60°C for 6h. After the reaction, pour the reaction solution into ice water to obtain a crude product; dissolve in Recrystallize three times in hot ethanol, put into vacuum oven and dry for 24h to obtain pure initiator N-bromomethylphthalimide; place the initiator and styrene monomer in a molar ratio of 1:15 In the reaction system, after three cycles of vacuuming and argon circulation, after closing the reaction system, under the action of a catalyst, react at 110°C for 1 hour, open the reaction system to allow oxygen to enter the quenching reaction, and add a certain amount of the reaction mixture Diluted with chloroform, passed through a neutral alumina chromatography column, collected the liquid and poured it into methanol to precipitate the polymer, after several ti...

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Abstract

The invention provides a method and application for synthesizing diamine-terminated polystyrene based on ATRP living polymerization method, the steps are as follows: react potassium phthalimide and methylene bromide in anhydrous DMF, and purify Finally, the initiator N-bromomethylphthalimide is obtained; then the initiator and styrene monomer are subjected to atom transfer radical polymerization under the action of a catalyst, and react at 110°C for 0.5-3h to generate different molecular weights Modified polystyrene; then modified polystyrene and potassium phthalimide react in anhydrous DMF to obtain polystyrene protected by two phthalimide groups; finally pass Hydrazine hydrate reduces bis-phthalimide-protected polystyrene to obtain bis-amine-terminated polystyrene. Then compound the synthesized diamine-terminated polystyrene with functional nanoparticles, which can greatly reduce the oil / water interfacial tension by more than 85%, and can be used in fields such as emulsion breaking.

Description

technical field [0001] The invention belongs to the technical field of reducing oil / water interfacial tension by compounding polymer-functionalized nanoparticles, and specifically relates to the synthesis of functionalized polystyrene, especially the preparation of diamine-terminated polystyrene based on ATRP active polymerization method The method and application are a method of synthesizing low-molecular-weight diamine-terminated polystyrene by using ATRP and compounding it with functional nanoparticles to reduce the oil / water interfacial tension. Background technique [0002] Adding functionalized polymers into the oil / water mixed system can play a certain role in surface activity. Although the functionalized nanoparticles themselves have no interfacial activity, they can enhance the interfacial activity of the polymer after they are compounded with the polymer. This method can realize rapid reduction of oil / water interfacial tension at low concentration, and has simple o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/32C08F8/30C08F112/08
CPCC08F8/30C08F8/32C08F2438/01C08F112/08
Inventor 林凌时辰亮邓茂青李雪玲
Owner SOUTHWEST PETROLEUM UNIV
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