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Optimizing the process efficiency of reactive extrusion in the synthesis of vinyltrimethoxysilane-grafted ethylene-octene-copolymer (EOC-g-VTMS) by response surface methodology

  • Thermoplastic polymers like ethylene-octene copolymer (EOC) may be grafted with silanes via reactive extrusion to enable subsequent crosslinking for advanced biomaterials manufacture. However, this reactive extrusion process is difficult to control and it is still challenging to reproducibly arrive at well-defined products. Moreover, high grafting degrees require a considerable excess of grafting reagent. A large proportion of the silane passes through the process without reacting and needs to be removed at great expense by subsequent purification. This results in unnecessarily high consumption of chemicals and a rather resource-inefficient process. It is thus desired to be able to define desired grafting degrees with optimum grafting efficiency by means of suitable process control. In this study, the continuous grafting of vinyltrimethoxysilane (VTMS) on ethylene-octene copolymer (EOC) via reactive extrusion was investigated. Successful grafting was verified and quantified by 1H-NMR spectroscopy. The effects of five process parameters and their synergistic interactions on grafting degree and grafting efficiency were determined using a face-centered experimental design (FCD). Response surface methodology (RSM) was applied to derive a causal process model and define process windows yielding arbitrary grafting degrees between <2 and >5% at a minimum waste of grafting agent. It was found that the reactive extrusion process was strongly influenced by several second-order interaction effects making this process difficult to control. Grafting efficiencies between 75 and 80% can be realized as long as grafting degrees <2% are admitted.

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Metadaten
Author of HS ReutlingenUlitzsch, Steffen; Bäuerle, Tim; Lorenz, Günter; Kandelbauer, Andreas
URN:urn:nbn:de:bsz:rt2-opus4-29058
DOI:https://doi.org/10.3390/polym12122798
ISSN:2073-4360
Erschienen in:Polymers / Molecular Diversity Preservation International
Publisher:MDPI
Place of publication:Basel
Document Type:Article
Language:English
Year of Publication:2020
Tag:design of experiments; ethylene-octene copolymer; grafting degree; grafting efficiency; process optimization; reactive extrusion; silane modification
Volume:12
Issue:12
Page Number:18
First Page:1
Last Page:18
Article Number:2798
DDC classes:540 Chemie
Open Access?:Ja
Licence (German):License Logo  Creative Commons - CC BY - Namensnennung 4.0 International