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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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 rea

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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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Example Embodiment

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

[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 prepare a 3-50wt% solution, bubbling with nitrogen for 10-60 minutes, heating to 90-210℃, and distilling out the total solvent 10-40wt% aromatic hydrocarbons;

[0069] Continue to lower the temperature to 0°C under nitrogen flow and add organic amines or pyridine compounds as acid binding agents, or introduce the hydrogen halide acidic tail gas generated by the reaction into the lye absorption device;

[0070] Then, add the halogenated acid halide to the above solution. After the halogenated acid halide is added dropwise, keep stirring to make the reaction complete, stand still, filter to remove solid insolubles, and distill and recover...

Example Embodiment

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

Example Embodiment

[0102] Example 2: The first 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 and evaporated After 50ml of toluene was discharged, the temperature was reduced to 0°C under nitrogen flow and 45mmol of triethylamine was added as an acid binding agent; then 45mmol of 2-bromopropionyl bromide was added dropwise. After the addition of 2-bromopropionyl bromide was completed, Keep stirring to make the reaction complete, stand still, filter to remove solid insolubles, and distill and recover the solvent in the filtrate to obtain a crude product of low molecular weight carbon dioxide copolymer containing halogen atom bromine at the end. The crude product was dissolved in 350ml of dichloromethane solvent, and then washed with 50ml of saturated ammonium chloride solution, saturated sodium bicarbonate solution an...

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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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