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Method for fast eliminating disulfide ester end groups of RAFT polymers

A polymer and dithioester technology, applied in the field of polymer dithioester end group removal, can solve the problems of difficult complete removal, long reaction time, unsatisfactory removal effect, etc., so that the biological activity will not be affected Effect

Inactive Publication Date: 2012-06-06
湖南宏泰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is only suitable for ultraviolet light, especially short-wave ultraviolet light; this method has a good effect on the removal of aromatic dithiocarboxylate end groups, but it is not effective for aliphatic dithiocarboxylate and trithiocarbonate , dithiocarbamate and xanthate end group removal effect is not ideal, the reaction time is long, it is difficult to completely remove

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  • Method for fast eliminating disulfide ester end groups of RAFT polymers
  • Method for fast eliminating disulfide ester end groups of RAFT polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The RAFT random copolymer 203.0g (M n =10.0Kg / mol, M w / M n =1.23, with trithiocarbonate end group -SC(S)SC 12 h 25 0.0203 mole) dissolved in 340g toluene, put into 1L ordinary glass reactor, and add photoinitiator (1-hydroxycyclohexyl) benzophenone 4.6g (0.0223 mole), stir at room temperature for 5 minutes, make photoinitiator dissolve completely , and then stirred and reacted for 1 hour under the irradiation of a 500-watt high-pressure mercury lamp, the yellow leg of the solution went away, and the detection of the ultraviolet-visible absorption spectrum showed that the trithiocarbonate end group-SC(S)SC 12 h 25 The characteristic absorption peak at 436nm disappears, and GPC detects that the molecular weight of the polymer after removing the end group is M n =9.5Kg / mol, molecular weight distribution index M w / M n = 1.26.

Embodiment 2

[0021] With the RAFT random copolymer 156.0g (M n =7.8Kg / mol, M w / M n =1.28, with trithiocarbonate end group -SC(S)SC 12 h 25 0.020 mol) was dissolved in 344g ethanol, added to a 1L ordinary glass reactor, and 3.6g (0.022 mol) of photoinitiator 1-phenyl-2-hydroxyl-2-methyl-1-acetone was added, and stirred at room temperature for 5 minutes , the photoinitiator was completely dissolved, then stirred and reacted for 1 hour under the irradiation of a 500-watt high-pressure mercury lamp, the yellow leg of the solution went away, and the detection of the ultraviolet-visible absorption spectrum showed that the end group of trithiocarbonate-SC(S)SC 12 h 25 The characteristic absorption peak at 436nm disappears, and GPC detects that the molecular weight of the polymer after removing the end group is M n =7.5Kg / mol, molecular weight distribution index M w / M n = 1.30.

Embodiment 3

[0023] The RAFT homopolymer 98.0g (M n =12.4Kg / mol, M w / M n =1.25, with dithiop-fluorobenzoate end group -SC(S)C 6 h 4 F 0.0072 mol) was dissolved in 147g toluene, added in a 1L ordinary glass reactor, and 1.2g (0.0072 mol) of photoinitiator 1-phenyl-2-hydroxyl-2-methyl-1-propanone was added, stirred at room temperature for 5 Minutes, the photoinitiator was completely dissolved, then stirred and reacted for 0.5 hour under the irradiation of a 500-watt high-pressure mercury lamp, the red color of the solution went, and the UV-Vis absorption spectrum detection showed that dithio-p-fluorobenzoic acid ester terminal group-SC( S)C 6 h 4 The characteristic absorption peak of F at 507nm disappears, and GPC detects that the molecular weight of the polymer after removing the end group is M n =12.1Kg / mol, molecular weight distribution index M w / M n = 1.26.

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Abstract

The invention discloses a method for fast eliminating disulfide ester end groups of RAFT polymers, which comprises the following steps: adding an RAFT polymer solution and light triggers into a reaction vessel according to the mol ratio of 1 / 1 to 2.5; and carrying out photochemical reaction under the ultraviolet-visible light irradiation for the eliminating disulfide ester end groups of the RAFT polymers, wherein the RAFT polymers are vinyl homopolymerors or vinyl copolymers containing the disulfide ester end groups. The invention can solve the problem of each damage of functional groups suchas epoxy functional groups, estolide functional groups and the like when nucleophilic reagents such as primary amine, secondary amine and the like are used for eliminating the disulfide ester end groups of the RAFT polymers with active functional groups such as epoxy functional groups, estolide functional groups and the like at the room temperature.

Description

technical field [0001] The invention belongs to the field of macromolecule modification, and specifically relates to a method for removing dithioester end groups of polymers prepared by a reversible addition-fragmentation chain transfer (RAFT) free radical controllable polymerization method. Background technique [0002] In 1998, the reversible addition-fragmentation chain transfer (RAFT) radical polymerization method (WO 98 / 01478, WO 99 / 31144) discovered by Moad and Rizzardo et al. in Australia is recognized as the most promising controllable / "Living" free radical polymerization method, which is widely used in the synthesis of block, star and other complex structure polymers. RAFT polymerization only needs to add dithioester (including dithiocarboxylate, trithiocarbonate, dithiocarbamate and xanthate) chain transfer agent in the traditional free radical polymerization system, also called The RAFT reagent can realize the controllable polymerization reaction. The prepared p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/32C08F220/18C08F8/00C08F220/28C08F220/06C08F120/32C08F222/08C08F212/08C08F220/22
Inventor 卢礼灿蔡远利罗樟华彭叶陈朝岚
Owner 湖南宏泰新材料有限公司