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Catalyst Recovery Method in Iron Salt Catalyzed Atom Transfer Radical Polymerization at Room Temperature

A recovery method and catalyst technology, which is applied in the field of catalyst recovery in atom transfer radical polymerization, can solve the problems of high temperature, inability to use, and inability to recover pure catalysts, and achieve good catalytic efficiency, low metal residues, and high separation efficiency Effect

Active Publication Date: 2019-01-01
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its unique mild polymerization conditions and high reaction efficiency, photochemistry has developed rapidly in recent years, but the existing catalyst recovery system is subject to various limitations, such as high temperature and cannot be used in photochemical polymerization systems; the special defect is that it cannot When recovering pure catalysts, most methods recover complexes formed between catalysts and ligands, which cannot truly recover catalysts

Method used

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  • Catalyst Recovery Method in Iron Salt Catalyzed Atom Transfer Radical Polymerization at Room Temperature
  • Catalyst Recovery Method in Iron Salt Catalyzed Atom Transfer Radical Polymerization at Room Temperature
  • Catalyst Recovery Method in Iron Salt Catalyzed Atom Transfer Radical Polymerization at Room Temperature

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: Catalyst recovery method in the atom transfer radical polymerization catalyzed by iron salt at room temperature

[0038] Water-soluble monomer mPEGMA 500 (1.0 mL, 2.1 mmol), initiator EBPA (4.6 μL, 2.6×10 -2 mmol), catalyst iron tetraphenylporphyrin Fe(III)-TPP (7.5 mg, 1.1×10 -2 mmol), ligand n-butylammonium bromide TBA-Br (20.5 mg, 6.3×10 -2 mmol), UV photoinitiator TPO were added to 5 mL ampoule, then p-xylene (1.0 mL) and absolute ethanol (1.0 mL) were added to it, the tube was melted and sealed, and the temperature of the ampoule was transferred to room temperature The polymerization was carried out under the condition of magnetic stirring under the ultraviolet lamp. After the scheduled polymerization time (4 h) was reached, the tube was broken, and pure water (1.0 mL) was added to induce the separation of the catalyst-dissolved p-xylene phase and the polymer-dissolved ethanol phase, and the upper p-xylene layer was removed For recycling, the re...

Embodiment 2

[0053] Embodiment 2: the recycling experiment of catalyst

[0054] The present invention is characterized in that it can keep the metal residues in the polymer extremely low after polymerization, and can recycle the catalyst. After the polymerization, the upper p-xylene phase (dissolved with the catalyst) is taken out and placed in another equal-volume In a clean ampoule, just add a predetermined amount of monomer, initiator, ligand, UV photoinitiator and predetermined volume of ethanol (the amount of the remaining components added in this recovery experiment is equal to that before recovery), and then the next round of aggregation. The single-point experiments under different recovery times are shown in Table 2.

[0055] Table 2 Comparison of single-point polymerization experiments under different recycling times

[0056] usage count

Conversion rate(%)

Theoretical molecular weight (g / mol)

GPC molecular weight (g / mol)

PDI

Metal residue in polymer...

Embodiment 3

[0059] Embodiment 3: Catalyst recovery method in the atom transfer radical polymerization catalyzed by iron salt at room temperature

[0060] According to the ratio of Example two, the water-soluble monomer N,N-dimethylaminoethyl methacrylate, initiator EBPA, catalyst tetraphenylporphyrin iron Fe(III)-TPP, ligand n-butyl bromide Ammonium chloride TBA-Br and UV photoinitiator TPO were added to a 5 mL ampoule, then p-xylene (1.0 mL) and absolute ethanol (1.0 mL) were added to it, the tube was melted and sealed, and the ampoule was transferred to Polymerization was carried out under a UV lamp (50 W) at room temperature with magnetic stirring. Break the tube after the scheduled polymerization time (4 h), and add pure water (1.0 mL) to induce the separation of the catalyst-dissolved p-xylene phase and the polymer-dissolved ethanol phase, and pipette the upper p-xylene layer For recycling, the remaining ethanol layer is dialyzed to obtain the desired polymer, which is passed throug...

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Abstract

The invention discloses a catalyst recovery method in atom transfer radical polymerization catalyzed by iron salt at room temperature. Specifically, the method includes the following steps: 1) ATRP polymerization is carried out in a mixed solvent of p-xylene / ethanol; 2) after the polymerization is completed, a certain amount of water is added to induce the layering of the solution, and the solution containing the catalyst is obtained after treatment and the polymerization 3) Add new monomer, initiator ligand and UV photoinitiator to the recovered catalyst solution to carry out the next round of polymerization. The ATRP reaction of the present invention realizes the use of iron salt as a catalyst at room temperature, and polymerizes under ultraviolet light irradiation to obtain a polymer with good controllability, and can recycle and reuse the catalyst, and keep the residual amount of the catalyst in the polymer extremely low. Low.

Description

technical field [0001] The invention belongs to the technical field of active polymerization catalyzed by iron salts, in particular to a catalyst recovery method in atom transfer radical polymerization catalyzed by iron salts at room temperature. Background technique [0002] Atom transfer radical polymerization (ATRP) is a widely used living polymerization method, and the catalyst plays a key role in ATRP, but a large amount of metal residues seriously affects the application of polymer materials in electronic materials and biological materials. So far, there are mainly three methods to solve the catalyst residue problem. One is to develop metal-free catalyzed ATRP, but the inorganic catalysts used for catalysis are complex in structure and difficult to synthesize, and there are many controversies about their toxicity; the other is to develop AGET-ATRP or ICAR-ATRP, using various reducing agents and The high-valence state transition metal reacts in situ to generate a low-v...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F6/12C08F6/06C08F2/48C08F4/80C08F120/28C08F120/54C08F120/34
CPCC08F2/48C08F4/80C08F6/06C08F6/12C08F120/28C08F120/34C08F120/54C08L33/14C08L33/24Y02P20/584
Inventor 程振平吴健章冰洁张丽芬朱秀林
Owner SUZHOU UNIV
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