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Reverse atom transfer radical polymerization of aqueous solution of acrylamide

A technology of acrylamide and atom transfer, applied in the field of preparing high molecular weight polymers, can solve the problems of difficult preservation, high catalyst concentration, toxic initiator halide, etc., and achieve the effects of low external requirements and simple operation.

Inactive Publication Date: 2019-01-22
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ATRP has two disadvantages: (1) the initiator halide used is poisonous; (2) the metal catalyst in the reduced state is sensitive to oxygen or moisture, is not easy to store, and needs to be removed after polymerization.
But in this method, CuX 2 / FeX 3 The higher concentration of catalysts will cause unnecessary troubles for subsequent catalyst removal (X-T Wang, L Zhao, Q-Q Liu, J Song, W-Y Huang, G-Q Zhai European Polymer Journal 2018, 100, 37-47)

Method used

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  • Reverse atom transfer radical polymerization of aqueous solution of acrylamide
  • Reverse atom transfer radical polymerization of aqueous solution of acrylamide
  • Reverse atom transfer radical polymerization of aqueous solution of acrylamide

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Prepare an aqueous solution with a total volume of 50mL, wherein the initial concentration of AAm (denoted as [AAm] 0 ) is 3.75mol L -1 , the initial concentration of DMAE (denoted as [DMAE] 0 ) is 0.05mol L -1 , the initial concentration of NaCl (denoted as [NaCl] 0 ) is 2.50×10 -3 mol L -1 , Fe(NO 3 ) 3 The initial concentration (denoted as [Fe(NO 3 ) 3 ] 0 ) is 5.00×10 -4 mol L -1 , the initial concentration of disodium ethylenediaminetetraacetic acid (denoted as [EDTA] 0 ) is 1.00×10 -3 mol L -1 . Deoxygenation for 20 minutes, and then react at 70°C for 40 minutes. The reaction product was taken and tested to obtain a monomer conversion rate of 79.0%. The obtained PAAm was precipitated and separated, and the obtained PAAm was determined to be 3.73×10 6 .

Embodiment 2

[0025] Prepare an aqueous solution with a total volume of 50mL, where [AAm] 0 3.75mol L -1 、[DMAE] 0 0.05mol L -1 , [NaCl] 0 2.50×10 -3 mol L -1 , [Fe(NO 3 ) 3 ] 0 5.00×10 -4 mol L -1 、[EDTA] 0 1.00×10 -3 moL -1. Deoxygenation for 20 minutes, and then react at 70°C for 60 minutes. The reaction product was taken and tested to obtain a monomer conversion rate of 94.5%. The obtained PAAm was precipitated and separated, and the obtained PAAm was determined to be 3.93×10 6 .

Embodiment 3

[0027] Prepare an aqueous solution with a total volume of 50mL, where [AAm] 0 3.75mol L -1 、[DMAE] 0 0.05mol L -1 , [NaCl] 0 2.50×10 -3 mol L -1 , [Fe(NO 3 ) 3 ] 0 5.00×10 -4 mol L -1 、[EDTA] 0 1.00×10 -3 moL -1 . Deoxygenation was performed for 20 minutes, and then reacted at 70°C for 120 minutes. The reaction product was taken and tested to obtain a monomer conversion rate of 98.9%. The obtained PAAm was precipitated and separated, and the obtained PAAm was determined to be 4.86×10 by viscosity method. 6 .

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Abstract

The invention belongs to the field of a high molecular weight polymer, and relates to radical polymerization of an aqueous solution of acrylamide (AAm), a redox initiation system is formed by Fe<III>complex ions and aliphatic tertiary amine, the radical polymerization of AAm is initiated in an aqueous solution containing free X<->(X:Cl, Br or -SC(=S)N(C2H5)2), and the molecular weight of the polymer is gradually increased as the monomer conversion rate increases. A method comprises the following steps: adding a pre-prepared catalyst mother liquor, water-soluble aliphatic tertiary amine, halide salt solution mother liquor, AAm and water to a reactor in order, after stirring, uniformly mixing the components, and then introducing argon gas for deoxygenation for 20 minutes, and after sealing,heating and stirring the materials in a water bath at a certain temperature and then performing a reaction; according to the process conditions, precipitating the polymer after the reaction is carried out for a certain time, and after drying, measuring the viscosity average molecular weight of the polymer by a viscosity method. The invention utilizes the commercially available inexpensive raw materials which are stable to air moisture, the halide salt is used as a halide source, and reverse ATRP of AAm in the aqueous solution is realized.

Description

technical field [0001] The invention belongs to the field of preparing high-molecular-weight polymers, and is related to the free radical polymerization of acrylamide (AAm) in aqueous solution, in particular to redox of iron salt complexes with aliphatic tertiary amines in aqueous solutions containing halogen ions or pseudohalogen anions The reaction triggers the free radical polymerization of AAm, so that the molecular weight of the polymer increases gradually with the increase of the monomer conversion rate. Background technique [0002] Atom Transfer Radical (ATRP) is a living radical polymerization method that appeared in the 1990s. It is a catalytic process that can use some transition metal complexes with redox properties as catalysts. Among them, Cu I / L and X-Cu II / L is the most commonly used transition metal, and other researched metals include Ru, Fe, Mo, Os, etc. 2921-2990; A Allushi, S Jockusch, G Yilmaz*, Y Macromolecules 2016, 49, 7785-7792). The core of ...

Claims

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Application Information

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IPC IPC(8): C08F120/56C08F4/40
CPCC08F4/40C08F120/56C08F2438/01
Inventor 翟光群陈琪
Owner CHANGZHOU UNIV
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