Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman Spectroscopy
We present the modification of ethylene-propylene rubber (EPM) with vinyltetra-methydisiloxane (VTMDS) via reactive extrusion to create a new silicone-based material with the potential for high-performance applications in the automotive, industrial and biomedical sectors. The radical-initiated modif...
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| Format: | Article |
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MDPI AG
2021-04-01
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| Series: | Polymers |
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| Online Access: | https://www.mdpi.com/2073-4360/13/8/1246 |
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| author | Steffen Ulitzsch Tim Bäuerle Mona Stefanakis Marc Brecht Thomas Chassé Günter Lorenz Andreas Kandelbauer |
| author_facet | Steffen Ulitzsch Tim Bäuerle Mona Stefanakis Marc Brecht Thomas Chassé Günter Lorenz Andreas Kandelbauer |
| author_sort | Steffen Ulitzsch |
| collection | DOAJ |
| description | We present the modification of ethylene-propylene rubber (EPM) with vinyltetra-methydisiloxane (VTMDS) via reactive extrusion to create a new silicone-based material with the potential for high-performance applications in the automotive, industrial and biomedical sectors. The radical-initiated modification is achieved with a peroxide catalyst starting the grafting reaction. The preparation process of the VTMDS-grafted EPM was systematically investigated using process analytical technology (in-line Raman spectroscopy) and the statistical design of experiments (DoE). By applying an orthogonal factorial array based on a face-centered central composite experimental design, the identification, quantification and mathematical modeling of the effects of the process factors on the grafting result were undertaken. Based on response surface models, process windows were defined that yield high grafting degrees and good grafting efficiency in terms of grafting agent utilization. To control the grafting process in terms of grafting degree and grafting efficiency, the chemical changes taking place during the modification procedure in the extruder were observed in real-time using a spectroscopic in-line Raman probe which was directly inserted into the extruder. Successful grafting of the EPM was validated in the final product by <sup>1</sup>H-NMR and FTIR spectroscopy. |
| first_indexed | 2024-03-10T12:24:35Z |
| format | Article |
| id | doaj.art-e7029c3c86c8448d933c47389f0d1d7f |
| institution | Directory Open Access Journal |
| issn | 2073-4360 |
| language | English |
| last_indexed | 2024-03-10T12:24:35Z |
| publishDate | 2021-04-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Polymers |
| spelling | doaj.art-e7029c3c86c8448d933c47389f0d1d7f2023-11-21T15:10:34ZengMDPI AGPolymers2073-43602021-04-01138124610.3390/polym13081246Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman SpectroscopySteffen Ulitzsch0Tim Bäuerle1Mona Stefanakis2Marc Brecht3Thomas Chassé4Günter Lorenz5Andreas Kandelbauer6Center 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, 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, 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, GermanyWe present the modification of ethylene-propylene rubber (EPM) with vinyltetra-methydisiloxane (VTMDS) via reactive extrusion to create a new silicone-based material with the potential for high-performance applications in the automotive, industrial and biomedical sectors. The radical-initiated modification is achieved with a peroxide catalyst starting the grafting reaction. The preparation process of the VTMDS-grafted EPM was systematically investigated using process analytical technology (in-line Raman spectroscopy) and the statistical design of experiments (DoE). By applying an orthogonal factorial array based on a face-centered central composite experimental design, the identification, quantification and mathematical modeling of the effects of the process factors on the grafting result were undertaken. Based on response surface models, process windows were defined that yield high grafting degrees and good grafting efficiency in terms of grafting agent utilization. To control the grafting process in terms of grafting degree and grafting efficiency, the chemical changes taking place during the modification procedure in the extruder were observed in real-time using a spectroscopic in-line Raman probe which was directly inserted into the extruder. Successful grafting of the EPM was validated in the final product by <sup>1</sup>H-NMR and FTIR spectroscopy.https://www.mdpi.com/2073-4360/13/8/1246reactive extrusionsilane modificationhydride modificationvinyltetramethyldi-siloxane (VTMDS)response surface analysisethylene-propylene copolymer (EPM) |
| spellingShingle | Steffen Ulitzsch Tim Bäuerle Mona Stefanakis Marc Brecht Thomas Chassé Günter Lorenz Andreas Kandelbauer Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman Spectroscopy Polymers reactive extrusion silane modification hydride modification vinyltetramethyldi-siloxane (VTMDS) response surface analysis ethylene-propylene copolymer (EPM) |
| title | Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman Spectroscopy |
| title_full | Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman Spectroscopy |
| title_fullStr | Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman Spectroscopy |
| title_full_unstemmed | Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman Spectroscopy |
| title_short | Synthesis of an Addition-Crosslinkable, Silicon-Modified Polyolefin via Reactive Extrusion Monitored by In-Line Raman Spectroscopy |
| title_sort | synthesis of an addition crosslinkable silicon modified polyolefin via reactive extrusion monitored by in line raman spectroscopy |
| topic | reactive extrusion silane modification hydride modification vinyltetramethyldi-siloxane (VTMDS) response surface analysis ethylene-propylene copolymer (EPM) |
| url | https://www.mdpi.com/2073-4360/13/8/1246 |
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