Novel method for preparing ferrocenyl polymer from controllable type polyacrylonitrile resin

A polyacrylonitrile resin and ferrocene-based technology, applied in the field of functional polymer materials, can solve problems such as side reactions, increase reaction costs, limit the use of alkyne compounds, etc., and achieve the effect of convenient design

Inactive Publication Date: 2016-11-16
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of preparing polymer brushes by click chemistry, if more active alkynyl groups are connected to polymer monomer units, it is easy to cause side reacti

Method used

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  • Novel method for preparing ferrocenyl polymer from controllable type polyacrylonitrile resin
  • Novel method for preparing ferrocenyl polymer from controllable type polyacrylonitrile resin
  • Novel method for preparing ferrocenyl polymer from controllable type polyacrylonitrile resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1: Controllable polyacrylonitrile resin synthesized by Cu(0) regulated CRP method

[0057] According to the ratio [AN] 0 : [EBiB] 0 : [Cu(0)] 0 : [PMDETA] 0 = 500:1:1:1, sequentially add Cu(0), AN (2.0mL), PMDETA, DMSO (2.0 mL) and EBiB to a 5 mL ampoule, add a stirring bar, and go through 6 standard freezing- After the pump-thaw-fill cycle, seal the tube in an oxygen-free atmosphere. Place the sealed ampoule at a constant temperature (25 o C) Under the magnetic water bath, the reaction is carried out according to the predetermined time. After the reaction, take out the ampoule, open the sealed tube, dissolve it with 2-5 mL of DMF, pour it into 250 mL of methanol, leave it overnight, filter it with suction, and dry it to obtain polyacrylonitrile.

[0058] figure 1 It is the kinetic diagram of the controllable radical polymerization of acrylonitrile (AN) monomer regulated by Cu(0) in Example 1.

[0059] Polymerization conditions: AN = 2.0 mL; [AN] 0 / [E...

Embodiment 2

[0065] Example 2: Preparation of polyvinyl tetrazole (PVT) by click chemical reaction of nitrile group.

[0066] According to the mass ratio, polyacrylonitrile: sodium azide: ammonium chloride = 100:120:50, in the ampoule bottle of 5 mL, add the PAN ( M n,GPC = 16.1 × 10 3 g / mol, M w / M n = 1.29) 0.4188 g, sodium azide 0.5025 g, ammonium chloride 0.2094 g, add N , N - Dimethylformamide (DMF) 3 mL, after fully dissolved, add a stirring bar, place the ampoule at 120 o Carry out click chemical reaction of nitrile groups in a heat-collecting constant temperature heating magnetic stirrer of C. After 5 hours of reaction, take out the ampoule bottle, add an appropriate amount of deionized water to dissolve, and add 1.0 mol / L hydrochloric acid solution to acidify, and stir to obtain a flocculent Solid precipitated, washed 3-5 times with deionized water, placed in 40 oC Vacuum constant temperature drying oven, after the sample is completely dried, the intermediate product...

Embodiment 3

[0070]Example 3: Preparation of ferrocenyl polymer (PVT-FeC) by Mitsunobu reaction.

[0071] By mass ratio, PVT: ferrocenemethanol: triphenylphosphine: diethyl azodicarboxylate=1:2:2:2, in a 50 mL round bottom flask, add the intermediate product PVT 0.3075 obtained in Example 2 g, ferrocenemethanol 0.6150g, triphenylphosphine 0.6150g, diethyl azodicarboxylate 0.6150g, add 10 mL dichloromethane (CH 2 Cl 2 ), at a constant temperature (15 o C) The reaction time in the magnetic water bath is 22 hours. After the reaction, the reaction solution was poured into 200 mL deionized water, and after being fully dispersed, the solid precipitate was separated by a high-speed centrifuge, and placed in a freeze-vacuum drying oven for freeze-drying for 24 h to obtain the final product, ferrocene-based polymerization material (PVT-FeC).

[0072] image 3 (C) is the ferrocene-based polymer (PVT-FeC) obtained in Example 3 1 H NMR chart.

[0073] Measuring conditions: INOVA 400 MHz nuclear...

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Abstract

The invention discloses a novel method for preparing a ferrocenyl polymer from controllable type polyacrylonitrile resin. The reaction of the novel method comprises the following steps of (1) preparing the polyacrylonitrile resin into a reaction system of polyvinyl tetrazolium (PVT) through a nitrile based click chemistry reaction, and enabling polyacrylonitrile, sodium azide, a catalyst and a solvent to be subjected to a reaction at certain temperature for a certain time so as to obtain an intermediate product PVT; and (2) preparing a reaction system of the ferrocenyl polymer (PVT-FeC) through a Mitsunobu reaction, and enabling the intermediate product PVT prepared in the step (1), ferrocenemethanol, triphenylphosphonium and diethyl azodicarboxylate to be subjected to a reaction at appropriate temperature for a certain time so as to obtain the ferrocenyl polymer. The molecular weight of the obtained polymer can be conveniently designed, besides, the end group of the polymer can still have activity, and the polymer can be used for synthesizing some other functional copolymers with a topological structure.

Description

technical field [0001] The invention relates to a new method for preparing ferrocene-based polymers from controllable polyacrylonitrile resins, including a polymerization system for preparing polyacrylonitrile resins through controlled free radical polymerization regulated by zero-valent copper and a nitrile click method The invention relates to a method for preparing a ferrocene-based polymer by reacting with Mitsunobu, which belongs to the field of functional polymer materials. Background technique [0002] Polyacrylonitrile (PAN) resin is usually used as the precursor of many polymer materials due to its excellent properties such as high hardness, good chemical stability, compatibility with polar substances, and low gas permeability. Most of the commonly used polyacrylonitrile is prepared from acrylonitrile monomer through traditional free radical polymerization. Since the molecular weight is usually low and the molecular weight distribution is often wide, it is difficult...

Claims

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Application Information

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IPC IPC(8): C08F120/44C08F4/50C08F8/30C08F8/42
CPCC08F4/50C08F8/42C08F120/44C08F8/30
Inventor 柏良久王文香陈厚
Owner LUDONG UNIVERSITY
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