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Separating and recycling method for atom transfer radical polymerization catalyst

A polymerization catalyst and atom transfer technology, applied in the direction of chemical recovery, etc., can solve the problems of inapplicability and limited use range, etc., achieve the effect of fast separation time, broaden the use range, and avoid the post-processing process

Active Publication Date: 2014-06-25
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above method is not suitable for systems where the reaction substrate is sensitive to water, which greatly limits the range of application of this technology. At the same time, this technology also requires a complex synthesis process to obtain a temperature-controlling ligand.

Method used

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  • Separating and recycling method for atom transfer radical polymerization catalyst
  • Separating and recycling method for atom transfer radical polymerization catalyst
  • Separating and recycling method for atom transfer radical polymerization catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment one: a kind of atom transfer radical polymerization catalyst separation and recycling method, used chemical reagent is:

[0027] Methyl methacrylate (MMA), 99%, China Pharmaceutical (Group) Shanghai Chemical Reagent Company; Azobisisobutyronitrile, 99%, ethyl α-bromophenylacetate (ie ethyl 2-bromophenylacetate) , 98%, China National Pharmaceutical (Group) Shanghai Chemical Reagent Company; polyethylene glycol (molecular weight: 200), vitamin C (ascorbic acid, VC), analytically pure, sodium ascorbate (VCNa), analytically pure, tris[(2-pyridine Base) methyl] amine, 99%, China National Pharmaceutical (Group) Shanghai Chemical Reagent Company; solvents such as tetrahydrofuran (THF), toluene, p-xylene, o-xylene and methanol, analytically pure, China National Pharmaceutical (Group) Shanghai Chemical Reagent company.

[0028] Test equipment and conditions:

[0029] Gel Permeation Chromatography: Model 1515 GPC from Waters, USA.

[0030] Determination conditions: ...

Embodiment 2

[0035] Embodiment two: Catalyst is separated and recycled from generating polymer:

[0036] According to the molar ratio n(MMA):n(initiator):n(CuBr 2 ) : n (ligand): n (AIBN) = 200:1:0.8:2.4:0.8, add CuBr in turn 2 , ligand, MMA (1 mL), initiator, AIBN, polyethylene glycol 200, p-xylene in a 5 mL ampoule, and seal the tube under an inert gas Ar atmosphere. Place the sealed ampoule in an oil bath at a constant temperature (70°C) for a predetermined time to react. The reaction proceeds in homogeneous phase. End the reaction respectively according to the set reaction time. After the end, take out the sealed tube, cool it to room temperature with cold water, open the sealed tube, separate the two phases, dissolve the organic phase with 2~5 mL of tetrahydrofuran, pour it into 250 mL of methanol and let it stand overnight, then suction filter, wash with water, and dry in vacuum Polymethyl methacrylates of different molecular weights can be obtained by drying. The polyethylene g...

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Abstract

The invention discloses a separating and recycling method for an atom transfer radical polymerization catalyst. The separating and recycling method is characterized by comprising the following steps of adding a radical polymerization monomer, an initiator, a catalyst, a ligand, a reducing agent, a first solvent and a second solvent into a reaction vessel, wherein the monomer is an MMA (methyl methacrylate) oil-soluble monomer, the initiator is selected from 2-bromoisobutyryl ethyl ester and ethyl 2-bromopheny lacetate, the reducing agent is azobisisobutyronitrile, the first solvent is polyethylene glycol 200, and the second solvent is selected from methylbenzene or dimethylbenzene; heating the reaction system to reaction temperature to enable the first solvent and the second solvent to mutually dissolve; carrying out atom transfer radical polymerization reaction under a homogeneous phase; after the reaction is ended, cooling to room temperature to enable the first solvent and the second solvent to be layered; separating two phases to enable the catalyst and the ligand to exist in the first solvent and a polymer to exist in the second solvent so as to realize the separation and recycling of the catalyst.

Description

technical field [0001] The invention relates to an atom transfer radical polymerization catalytic reaction, in particular to a method for separating and recycling an atom transfer radical polymerization catalyst. Background technique [0002] In 1995, the two research groups of Matyjaszewski and Sawamoto proposed Atom Transfer Radical Polymerization (ATRP) almost simultaneously. . It has the advantages of wide range of monomers unique to free radical polymerization, diverse synthesis processes, simple operation, low industrialization cost, etc., and has a strong molecular design function. After more than ten years of development, Activators Generated by Electron Transfer for ATRP (AGET ATRP) and Initiators for Continuous Activator Regeneration ATRP (Initiators for Continuous Activator Regeneration ATRP) have appeared successively. ICAR ATRP) and other new methods based on ATRP to improve the activity of the catalytic system. Since these methods allow high-valence metal ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F6/06C08F6/12
CPCY02P20/584
Inventor 程振平潘金龙朱秀林张丽芬姜孝武
Owner SUZHOU UNIV
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