RAFT (Reversible Addition-Fragmentation chain Transfer) reaction reagent based on low molecular weight carbon dioxide copolymer and preparation method of RAFT reaction reagent

A carbon dioxide, low molecular weight technology, applied in the field of RAFT reaction reagent and its preparation, can solve problems such as preparation methods that have not been reported

Active Publication Date: 2013-09-18
HUAQIAO UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] On the other hand, the RAFT reaction, that is, the reversible addition-fragmentation chain transfer radical polymerization reaction, is widely used in the molecular design and controllable construction of multi-component block polymers, and is suitable for the reversible addition-fragmentation chains of different polymerization reaction monomers. Reagents for transfer radical polymerization have been intensively studied and are becoming increasingly mature, but the development and preparation methods of reversible addition-fragmentation chain transfer radical polymerization reagents based on low molecular weight carbon dioxide copolymers have not been reported yet.

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  • RAFT (Reversible Addition-Fragmentation chain Transfer) reaction reagent based on low molecular weight carbon dioxide copolymer and preparation method of RAFT reaction reagent
  • RAFT (Reversible Addition-Fragmentation chain Transfer) reaction reagent based on low molecular weight carbon dioxide copolymer and preparation method of RAFT reaction reagent
  • RAFT (Reversible Addition-Fragmentation chain Transfer) reaction reagent based on low molecular weight carbon dioxide copolymer and preparation method of RAFT reaction reagent

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preparation example Construction

[0067] The present invention also relates to a preparation method of RAFT reaction reagent based on low molecular weight carbon dioxide copolymer, comprising the steps of:

[0068] The first step reaction: the low molecular weight carbon dioxide copolymer HO-(CO 2 -based polymer)-OH is dissolved in anhydrous aromatic hydrocarbon solvent under stirring to form a 3-50wt% solution, and after bubbling with nitrogen gas for 10-60 minutes, heat up to 90-210°C and evaporate the total solvent 10-40wt% aromatic hydrocarbons;

[0069] Continue to lower the temperature to 0°C under the condition of blowing nitrogen and add organic amine or pyridine compound as an acid-binding agent, or introduce the acidic tail gas of hydrogen halide generated by the reaction into the lye absorption device;

[0070] Then, add haloacyl halides to the above solution, keep stirring after the addition of haloacyl halides to complete the reaction, let stand, filter to remove solid insolubles, and distill and...

Embodiment 1

[0100] Embodiment 1: the first step reaction: 10mmol low molecular weight carbon dioxide copolymer (Mn=3000) is dissolved in 300ml anhydrous toluene / xylene (V 甲苯 / V 二甲苯 =50 / 50) in the mixed solvent, after nitrogen gas bubbling for 20 minutes, the temperature was raised to 130-140° C., after 50 ml of solvent was evaporated, the temperature was lowered to 0° C. and 26 mmol of pyridine was added as an acid-binding agent; Then add 26mmol of 2-chloro-2-methylpropionyl bromide dropwise, keep stirring after the addition of 2-chloro-2-methylpropionyl bromide to complete the reaction, let stand, filter to remove solid insolubles, and The solvent in the filtrate is recovered by distillation to obtain a low molecular weight carbon dioxide copolymer crude product containing halogen atom chlorine at the end. The crude product was dissolved in 200ml of dichloromethane solvent, then washed twice with 60ml of saturated ammonium chloride solution, 60ml of saturated sodium bicarbonate solution...

Embodiment 2

[0102] Example 2: The first step reaction: 19.2mmol of low molecular weight carbon dioxide copolymer (Mn=2500) was dissolved in 440ml of anhydrous toluene solvent under stirring, after bubbling with nitrogen for 30 minutes, the temperature was raised to 130-140°C, evaporated After removing 50ml of toluene, lower the temperature to 0°C under the condition of blowing nitrogen and add 45mmol of triethylamine as an acid-binding agent; then add 45mmol of 2-bromopropionyl bromide dropwise, and after the addition of 2-bromopropionyl bromide is completed, Keep stirring to make the reaction complete, let stand, filter to remove solid insolubles, and recover the solvent in the filtrate by distillation to obtain a low molecular weight carbon dioxide copolymer crude product containing halogen atom bromine at the end. The crude product was dissolved in 350ml of dichloromethane solvent, then washed twice with 50ml of saturated ammonium chloride solution, saturated sodium bicarbonate solution...

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Abstract

The invention provides an RAFT (Reversible Addition-Fragmentation chain Transfer) reaction reagent based on a low molecular weight carbon dioxide copolymer and a preparation method of the RAFT reaction reagent, wherein the RAFT reaction reagent is a dithioester end capped low molecular weight carbon dioxide copolymer. The preparation method comprises the following steps of: subjecting a low molecular weight carbon dioxide polymerization product with terminal hydroxyl and halogen acyl halide to reaction at low temperature through a molecular design by utilizing a low molecular weight product generated through polymerization reaction between carbon dioxide and an epoxy compound, and separating and purifying a product to obtain halogen atom end capped low molecular weight carbon dioxide copolymer resin; and dissolving a halogen atom end capped low molecular weight carbon dioxide copolymer into a dichloromethane solution, adding alkyl xanthate at the room temperature, and reacting to finally obtain the RAFT reaction reagent based on the low molecular weight carbon dioxide copolymer. By using the RAFT reaction reagent, the low molecular weight carbon dioxide copolymer can be effectively utilized, and the emission of carbon dioxide as greenhouse gas can be reduced; and the preparation method and process are simple and easy to control.

Description

【Technical field】 [0001] The invention relates to a RAFT reaction reagent based on a low molecular weight carbon dioxide copolymer and a preparation method thereof. 【Background technique】 [0002] Carbon dioxide copolymer represented by the copolymerization of carbon dioxide and epoxy compounds is a cheap synthetic biodegradable material, which has the value of large-scale production and is expected to be applied in biomedical materials and food packaging materials. Among them, the application of low-molecular-weight carbon dioxide copolymer resin has attracted attention: the Chinese patent application number 02134631 discloses a method for synthesizing aliphatic polycarbonate polyurethane foam materials with carbon dioxide as the starting material; the Chinese patent application number 201010224108.0 The patent discloses a polycarboxylic acid-based water reducer containing a low-molecular-weight carbon dioxide copolymer and its synthesis method; the Chinese patent with appl...

Claims

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Application Information

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IPC IPC(8): C08G64/42C08F2/38C08F293/00
Inventor 全志龙林志勇林松柏李钟慎
Owner HUAQIAO UNIVERSITY
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