prikaz prve stranice dokumenta Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy
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master's thesis
Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy
Zagreb: University of Zagreb, Faculty of Science, 2019. urn:nbn:hr:217:284848
Glotz, Gabriel
University of Zagreb
Faculty of Science
Department of Chemistry

Institutional repository: Repository of the Faculty of Science

Cite this document

Glotz, G. (2019). Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy (Master's thesis). Zagreb: University of Zagreb, Faculty of Science. Retrieved from https://urn.nsk.hr/urn:nbn:hr:217:284848

Glotz, Gabriel. "Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy." Master's thesis, University of Zagreb, Faculty of Science, 2019. https://urn.nsk.hr/urn:nbn:hr:217:284848

Glotz, Gabriel. "Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy." Master's thesis, University of Zagreb, Faculty of Science, 2019. https://urn.nsk.hr/urn:nbn:hr:217:284848

Glotz, G. (2019). 'Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy', Master's thesis, University of Zagreb, Faculty of Science, accessed 21 December 2024, https://urn.nsk.hr/urn:nbn:hr:217:284848

Glotz G. Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy [Master's thesis]. Zagreb: University of Zagreb, Faculty of Science; 2019 [cited 2024 December 21] Available at: https://urn.nsk.hr/urn:nbn:hr:217:284848

G. Glotz, "Continuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy", Master's thesis, University of Zagreb, Faculty of Science, Zagreb, 2019. Available at: https://urn.nsk.hr/urn:nbn:hr:217:284848

Metadata
TitleContinuous flow synthesis of a blocked polyisocyanate: process optimization and reaction monitoring by in-line FT-IR spectroscopy
Title (croatian)Sinteza zaštićenog poliizocijanata u kontinuiranom protoku: optimizacija procesa i praćenje reakcije FT-IR spektroskopijom in-line
AuthorGabriel Glotz
MentorChristian Oliver Kappe (mentor)
Committee memberSnežana Miljanić (predsjednik povjerenstva)
Committee memberVesna Petrović Peroković (član povjerenstva)
Committee memberŽeljka Soldin (član povjerenstva)
Committee memberInes Primožič (član povjerenstva)
GranterUniversity of Zagreb
Faculty of Science
(Department of Chemistry)
Zagreb
Defense date and country2019-04-08, Croatia
Scientific / art field,
discipline and subdiscipline		NATURAL SCIENCES
Chemistry
Abstract
Given that the traditional batch production of blocked isocyanates has significant drawbacks associated with the exothermic character of the reaction and the high viscosity of the materials involved, a continuous flow strategy was developed. The neat oxime and the viscous polyisocyanate were mixed using a Kenics® static mixer and the homogeneous mixture obtained was fully converted to the target blocked isocyanate in a residence time unit downstream of the mixer. Real-time reaction monitoring via in-line FT-IR spectroscopy at the reactor outlet has been implemented, enabling fast optimization of the reaction conditions and providing a sensitive and reliable control of the product quality. The process has been intensified by an increase in the flow rate of the reactants, a decrease in the residence unit volume and a stepwise increase in the temperature of the flow reactor. Full conversion to the blocked polyisocianate has been achieved at 155 °C after only 15 s of the overall residence time, providing productivity of ca. 1 kg per hour for a reactor of only 4.5 mL volume.
Abstract (croatian)
S obzirom da tradicionalna serijska proizvodnja zaštićenih izocijanata ima značajne nedostatke vezane uz egzotermni karakter reakcije i visoku viskoznost tvari koje sudjeluju u reakciji, razvijena je strategija sinteze u kontinuiranom protoku. Čisti oksim i viskozni poliizocijanat miješaju se pomoću statičke miješalice Kenics® te se dobivena homogena smjesa potpuno prevodi u ciljani zaštićeni izocijanat u protočnom reaktoru. Praćenje reakcije u realnom vremenu provedeno je FT-IR spektroskopijom in-line reakcijske smjese na izlasku iz reaktora, što je omogućilo brzu optimizaciju reakcijskih uvjeta te osiguralo osjetljivu i pouzdanu kontrolu kvalitete produkta. Proces je optimiziran povećanjem brzine protoka reaktanata, smjanjenjem volumena cijevnog reaktora te postupnim povećanjem temperature protočnog reaktora. Potpuna pretvorba u zaštićeni izocijanat postignuta je pri 155 °C nakon samo 15 s ukupnog vremena zadržavanja u reaktoru, čime je postignuta produktivnost od približno 1 kg na sat u reaktoru volumena od samo 4,5 mL.
Keywords
Keywords (english)
Languageenglish
URN:NBNurn:nbn:hr:217:284848
Study programmeTitle: Graduate university studies in chemistry; specializations in: Research programme
Course: Research programme
Study programme type: university
Study level: graduate
Academic / professional title: magistar/magistra kemije (magistar/magistra kemije)
Type of resourceText
File originBorn digital
Access conditionsOpen access
Embargo expiration date: 2021-04-08
Terms of useLicence In copyright icon
Created on2019-04-24 13:04:22