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...
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| Format: | Article |
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MDPI AG
2020-11-01
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| Series: | Polymers |
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| Online Access: | https://www.mdpi.com/2073-4360/12/12/2798 |
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| author | Steffen Ulitzsch Tim Bäuerle Thomas Chassé Günter Lorenz Andreas Kandelbauer |
| author_facet | Steffen Ulitzsch Tim Bäuerle Thomas Chassé Günter Lorenz Andreas Kandelbauer |
| author_sort | Steffen Ulitzsch |
| collection | DOAJ |
| description | 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 <sup>1</sup>H-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. |
| first_indexed | 2024-03-10T14:32:43Z |
| format | Article |
| id | doaj.art-169183b3e29c4fbf9e82eef362ee1e48 |
| institution | Directory Open Access Journal |
| issn | 2073-4360 |
| language | English |
| last_indexed | 2024-03-10T14:32:43Z |
| publishDate | 2020-11-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Polymers |
| spelling | doaj.art-169183b3e29c4fbf9e82eef362ee1e482023-11-20T22:26:00ZengMDPI AGPolymers2073-43602020-11-011212279810.3390/polym12122798Optimizing the Process Efficiency of Reactive Extrusion in the Synthesis of Vinyltrimethoxysilane-Grafted Ethylene-Octene-Copolymer (EOC-g-VTMS) by Response Surface MethodologySteffen Ulitzsch0Tim Bäuerle1Thomas Chassé2Günter Lorenz3Andreas Kandelbauer4Center for Process Analysis & Technology (PA&T), School of Applied Chemistry, Reutlingen University, Alteburgstrasse 150, 72762 Reutlingen, GermanyCenter for Process Analysis & Technology (PA&T), School of Applied Chemistry, Reutlingen University, Alteburgstrasse 150, 72762 Reutlingen, GermanyInstitute of Physical and Theoretical Chemistry, University of Tübingen, Auf der Morgenstelle 18, 72076 Tübingen, GermanyCenter for Process Analysis & Technology (PA&T), School of Applied Chemistry, Reutlingen University, Alteburgstrasse 150, 72762 Reutlingen, GermanyCenter for Process Analysis & Technology (PA&T), School of Applied Chemistry, Reutlingen University, Alteburgstrasse 150, 72762 Reutlingen, GermanyThermoplastic 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 <sup>1</sup>H-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.https://www.mdpi.com/2073-4360/12/12/2798reactive extrusionsilane modificationdesign of experimentsethylene-octene copolymergrafting degreegrafting efficiency |
| spellingShingle | Steffen Ulitzsch Tim Bäuerle Thomas Chassé Günter Lorenz Andreas Kandelbauer Optimizing the Process Efficiency of Reactive Extrusion in the Synthesis of Vinyltrimethoxysilane-Grafted Ethylene-Octene-Copolymer (EOC-g-VTMS) by Response Surface Methodology Polymers reactive extrusion silane modification design of experiments ethylene-octene copolymer grafting degree grafting efficiency |
| title | Optimizing the Process Efficiency of Reactive Extrusion in the Synthesis of Vinyltrimethoxysilane-Grafted Ethylene-Octene-Copolymer (EOC-g-VTMS) by Response Surface Methodology |
| title_full | Optimizing the Process Efficiency of Reactive Extrusion in the Synthesis of Vinyltrimethoxysilane-Grafted Ethylene-Octene-Copolymer (EOC-g-VTMS) by Response Surface Methodology |
| title_fullStr | Optimizing the Process Efficiency of Reactive Extrusion in the Synthesis of Vinyltrimethoxysilane-Grafted Ethylene-Octene-Copolymer (EOC-g-VTMS) by Response Surface Methodology |
| title_full_unstemmed | Optimizing the Process Efficiency of Reactive Extrusion in the Synthesis of Vinyltrimethoxysilane-Grafted Ethylene-Octene-Copolymer (EOC-g-VTMS) by Response Surface Methodology |
| title_short | Optimizing the Process Efficiency of Reactive Extrusion in the Synthesis of Vinyltrimethoxysilane-Grafted Ethylene-Octene-Copolymer (EOC-g-VTMS) by Response Surface Methodology |
| title_sort | optimizing the process efficiency of reactive extrusion in the synthesis of vinyltrimethoxysilane grafted ethylene octene copolymer eoc g vtms by response surface methodology |
| topic | reactive extrusion silane modification design of experiments ethylene-octene copolymer grafting degree grafting efficiency |
| url | https://www.mdpi.com/2073-4360/12/12/2798 |
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