Thermal degradation of poly(alkyl methacrylate) synthesized via ATRP using 2,2,2-tribromoethanol as initiator

Author(s)

Rodrigues Camilo, Ana Paula ^[1] ; de Almeida, Paula ^[1] ; Petzhold, Cesar Liberato ^[2] ; Felisberti, Maria Isabel ^[1]

Affiliation

^[1] Univ Estadual Campinas, Inst Chem, POB 6154, BR-13083970 Campinas, SP - Brazil

^[2] Univ Fed Rio Grande do Sul, Inst Chem, PO 15003, BR-91501970 Porto Alegre, RS - Brazil

• Document type: Journal article
• Source: Polymer Degradation and Stability; v. 158, p. 1-13, DEC 2018.
• Web of Science Citations: 2

Abstract

Poly(alkyl methacrylate)s (alkyl = methyl, ethyl, n-butyl and n-hexyl) synthesized by Atom Transfer Radical Polymerization (ATRP) using 2,2,2 tribromoethanol as initiator present a first mass loss below 200 degrees C in thermogravimetric experiments. In order to investigate the possible mechanism of this degradation step, the polymers were subjected to thermal treatment at 150 degrees C under argon atmosphere. The volatiles were analyzed by gas chromatography coupled to mass spectrometry, while the thermally treated polymers were analyzed by thermogravimetry, H-1 and C-13 nuclear magnetic resonance and size exclusion chromatography. The main mechanism of the first step of degradation is HBr elimination from initiator fragments attached to the chain ends, resulting in vinylidene, lactone and aldehyde terminal groups of the polymer chains. Moreover, volatiles produced by the chain-end elimination were mainly alkyl bromides, alkyl alcohols, alkyl methacrylates and products successive to HBr elimination and polymer chain scission. The amount of monomer release at 150 degrees C varied with the alkyl group in the range of 3-17 wt %; however, polymer chain configuration, molar mass and dispersity did not significantly change. Polymer chains free of the ATRP initiator were thermally stable at least up to 250 degrees C. (C) 2018 Elsevier Ltd. All rights reserved. (AU)

• FAPESP's process: 10/17804-7 - Polymeric composites
• Grantee: Maria Isabel Felisberti
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 16/03394-8 - Synthesis of amphiphilic and block copolymers via RAFT and ATRP
• Grantee: Maria Isabel Felisberti
• Support Opportunities: Research Grants - Visiting Researcher Grant - Brazil
• FAPESP's process: 15/25406-5 - Organizing matter: colloids formed by association of surfactants, polymers and nanoparticles
• Grantee: Watson Loh
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 13/09277-5 - Synthesis of amphiphilic block copolymers based on poly(sucrose methacrylate)
• Grantee: Paula de Almeida
• Support Opportunities: Scholarships in Brazil - Master