Preparation of Polymers by Atom Transfer Radical Polymerization Catalyzed by Cyclic Iron Salts at Room Temperature

一种聚合物、铁盐的技术，应用在原子转移自由基聚合中催化剂的回收领域，能够解决不能用、温度高、无法回收纯的催化剂等问题，达到金属残留低、缩短聚合时间、单体转化率高的效果

Active Publication Date: 2021-06-18
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Preparation of Polymers by Atom Transfer Radical Polymerization Catalyzed by Cyclic Iron Salts at Room Temperature
  • Preparation of Polymers by Atom Transfer Radical Polymerization Catalyzed by Cyclic Iron Salts at Room Temperature
  • Preparation of Polymers by Atom Transfer Radical Polymerization Catalyzed by Cyclic Iron Salts at Room Temperature

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Experimental program
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Embodiment 1

[0038] Embodiment 1: Catalyst recovery method in the atom transfer radical polymerization catalyzed by iron salt at room temperature

[0039] 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

[0054] Embodiment 2: the recycling experiment of catalyst

[0055] 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.

[0056] Table 2 Comparison of single-point polymerization experiments under different recycling times

[0057] usage count Conversion rate(%) Theoretical molecular weight (g / mol) GPC molecular weight (g / mol) PDI Metal residue in polymer (ppm) ...

Embodiment 3

[0060] Embodiment 3: Catalyst recovery method in the atom transfer radical polymerization catalyzed by iron salt at room temperature

[0061] 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 method for preparing a polymer by catalyzing atom transfer radical polymerization at room temperature by means of circulating iron salts. 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

[0001] The present invention belongs to the divisional application of the patent application titled Catalyst Recovery Method in Atom Transfer Radical Polymerization Catalyzed by Iron Salt at Room Temperature, with the filing date of January 19, 2017 and the application number of 201710038548.9. technical field [0002] 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 [0003] 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 inorgan...

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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