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Method for separating and recovering iridium salt catalysts for catalyzing light-controlled atom transfer radical polymerization (ATRP)

A technology of atom transfer and catalyst, applied in the field of active polymerization catalyzed by iridium salts, to achieve high reaction efficiency, increase reaction efficiency, simple separation and recycling

Active Publication Date: 2018-04-17
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Given the economics and efficiency of catalyst recovery strategies for iridium salt-catalyzed light-controlled LRP, it is highly attractive and challenging to develop catalyst separation and recycling methods for visible light-regulated ATRP systems.

Method used

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  • Method for separating and recovering iridium salt catalysts for catalyzing light-controlled atom transfer radical polymerization (ATRP)
  • Method for separating and recovering iridium salt catalysts for catalyzing light-controlled atom transfer radical polymerization (ATRP)
  • Method for separating and recovering iridium salt catalysts for catalyzing light-controlled atom transfer radical polymerization (ATRP)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] General steps of photocatalytic photocontrolled atom transfer radical polymerization and separation and recovery method of iridium salt catalyst

[0038] in [PEGMA] 0 / [EBPA] 0 / [ fac -[Ir(ppy) 3 ]] 0 = 100 / 1 / 0.1 The polymerization process at the molar ratio: PEGMA (1.0 mL, 2.18 mmol), EBPA (3.82 μL, 2.18×10 -2 mmol), fac -[Ir(ppy) 3 ] (1.43 mg, 2.18×10 -3 mmol), and 1,2-dichlorobenzene (1.0 mL) and ethanol (0.5 mL) and a magnetic stir bar were added to a 5 mL dry ampoule. Oxygen was vented from the reaction mixture and an argon (Ar) atmosphere was provided by at least three freeze-pump-thaw cycles. The ampoule was then flame-sealed and transferred to a model Flex Strip-VNC 3528 (4.8 W) blue LED (λmax = 464 nm, 0.15 mW cm -2 ) in a magnetic stirring device under the light strip irradiation. Carry out the polymerization reaction at room temperature (25 ℃), carry out the polymerization during the light time specified in the chart, and cool with an electric f...

Embodiment 2

[0040] Recovery and recycling method of iridium salt catalyst that catalyzes light-controlled atom transfer radical polymerization

[0041] The feature of the present invention is that it can keep the residual amount of metal in the polymer extremely low after polymerization, and the catalyst can be recycled. The chlorobenzene phase (catalyst dissolved) is placed in another clean ampoule of equal volume, and only a predetermined amount of monomer, initiator, and predetermined volume of ethanol are added (the amount of the remaining components added in this recovery experiment is the same as that before recovery equal), the next round of aggregation can be performed. The experiments under different recovery times are shown in Table 1.

[0042] Table 1. Visible light-regulated ATRP catalysts of PEGMA (1.0 mL) ( fac -[Ir(ppy) 3 ]) Loop experiment

[0043]

[0044] a Aggregation condition: 1st use: [PEGMA] 0 / [EBPA] 0 / [ fac -[Ir(ppy) 3 ]] 0 =100 / 1 / 0.1; V PEGMA ...

Embodiment 3

[0047] Preparation of Polymers by Photocontrolled Atom Transfer Radical Polymerization Catalyzed by Different Concentrations of Iridium Salt Catalysts

[0048] The photocatalyst concentration largely determines the reaction speed and controllability of the polymerization. Therefore, the influence of the photocatalyst concentration on the polymerization reaction was explored, and the results are shown in Table 2.

[0049] Table 2. Using fac -[Ir(ppy) 3 ] As a photoredox catalyst, the ATRP process of PEGMA (1.0 mL) with a target degree of polymerization of 50 regulated by visible light. a

[0050]

[0051] a Polymerization conditions: Feed ratio R = [PEGMA] 0 / [EBPA] 0 / [ fac -[Ir(ppy) 3 ]] 0 ; V PEGMA = 1.0 mL, V 邻二氯苯 = 1.0 mL, V 乙醇 = 0.5 mL, temperature = room temperature, polymerized under blue light; b conversion rate by 1 H NMR spectrum determination; c theoretical molecular weight ( M n,th = M EBPA + [PEGMA] 0 / [EBPA] 0 x M PEGMA × conv...

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Abstract

The invention provides a water-induced phase separation light-induced atom transfer radical polymerization (ATRP) system based on iridium salt catalysis under blue light irradiation, and an iridium salt catalyst recycling method. The method comprises the following steps: (1) taking polyethylene glycol monomethyl ether methacrylate as a model monomer, taking ethyl alpha-bromophenylacetate as an initiator, taking a surface tris[2-phenylpyridinato-C2,N]iridium as a catalyst, and taking 1,2-dichlorobenzene / ethanol as a mixed solvent; (2) adding purified water into a polymerization system to inducephase separation after polymerization, so that the iridium salt catalysts easily realize in-situ separation to be recycled; and (3) adding novel monomers and initiators into the recycled catalyst solution so as to perform the next-round polymerization. The sustainable light-controlled ATRP system has the characteristics of visible light radiation, high catalytic activity, good controllability ofmolecular weight and distribution, attractive 'activity' features, high-efficiency separation ability, low metal residue content, reutilization of the catalyst and the like.

Description

technical field [0001] The invention relates to the technical field of active polymerization catalyzed by iridium salts, in particular to a method for separating and recovering an iridium salt catalyst that catalyzes light-controlled atom transfer radical polymerization, and prepares polymerization by recycling and utilizing iridium salts to catalyze light-controlled atom transfer radical polymerization way of things. Background technique [0002] In recent years, photopolymerization has attracted considerable attention due to its advantages such as mild polymerization conditions, low activation energy, high efficiency, and good stability. During photopolymerization, various external stimulus light sources such as ultraviolet light, visible light, and near-infrared (NIR) can be provided by household light bulbs, xenon lamps, high-pressure mercury lamps, light-emitting diodes (LEDs), continuous wave (CW) lasers, and even sunlight . By selecting responsive photoredox catalys...

Claims

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Application Information

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IPC IPC(8): C08F6/06C08F299/02C08F2/46C08F4/80
CPCC08F2/46C08F4/80C08F6/06C08F299/02Y02P20/584
Inventor 程振平倪媛媛刘晓东张丽芬朱秀林
Owner SUZHOU UNIV
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