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Eingeladener Vortrag
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For the industrial production of chemicals a safe process design is required to avoid harm to people and
environment. It becomes tremendous important if one or more of the following points are characteristic for
the synthesis: high heat release, explosive atmosphere, presence of toxic and/or of thermal unstable substances.
One substance group, known for being unstable, is the group of organic peroxides. They are potential
high energetic substances. Many syntheses of organic peroxides are carried out in semi-batch
mode to control the heat release in a good manner. With the aim to increase process control, the advantages
of continuous reaction mode, combined with micro reaction technology, are used for the synthesis
of one specific organic peroxide in this work.
This approach is not only characterised by shorter residence time, good heat transfer, but also by smaller
quantities of managed chemicals, and, therefore, by a lower hazard potential. Often yield and selectivity
can be improved additionally.
For the study a peroxyester, namely tert-Butyl peroxy-2-ethylhexanoate (TBPEH), with known thermal
hazard potential was chosen. The two phase liquid/liquid reaction was carried out in three types of reactors.
A small scale tubular reactor, stressed by ultrasound, and two different micro structured reactors were
used. One of them had a meandering and the other a split-and-recombine channel structure. Synthesis
temperature was also varied.
From preliminary studies it was known that the side reaction of the involved carboxylic acid chloride to the
corresponding acid can become more important in continuous mode compared to semi-batch mode. The
effect of reactor type and temperature on selectivity and therefore yield of TBPEH was analysed and compared.
In result the reaction could be carried out in a safe manner. The high heat-exchanging efficiency of the
used reactors and the short residence time allowed synthesis temperature near the onset temperature of
decomposition of TBPEH. In relation to the results of the capillary tube and of the reactor with meandering
channel structure (MR), the results for the split-and-recombine reactor (SAR) showed the best trend line.
Further studies have to underline the result. Compared to the traditional reaction path (the semi-batch
mode), a higher space time yield could be achieved. This promising information is accompanied by the fact
of low reaction volumes. In consequence the productivity is low without a numbering up of reaction channels
or a scaling up of it. The nowadays existing philosophy of producing a specific quantity of product by a
company, followed by the transport to the costumer may change. Just organic peroxides, used in small
quantities, e.g. as initiators for polymerisation processes or as resin hardeners, provide the opportunity for
an on-demand-production.
Die Technische Regel für Anlagensicherheit (TRAS) 410 mit
dem Titel Erkennen und Beherrschen exothermer Reaktionen
stellt im Rahmen der Betrachtung der thermischen
Prozesssicherheit eine Anleitung zur systematischen Erarbeitung
von Gefahren bei chemischen Stoffumwandlungen
im Industriemaßstab dar. Sie unterstützt bei der Bewertung
der Gefahren und bei der Erstellung von Maßnahmen, um
Störfälle zu verhindern. Am Beispiel der exotherm ablaufenden
Synthese von tert.-Butylperoxypivalat, einem organischen
Peroxid, wird die Vorgehensweise dargestellt. Organische
Peroxide sind als thermisch instabile Verbindungen bekannt
und besitzen dadurch ein zusätzliches Gefahrenpotential.
Die Technische Regel für Anlagensicherheit (TRAS) 410 mit
dem Titel "Erkennen und Beherrschen exothermer Reaktionen"
stellt im Rahmen der Betrachtung der thermischen
Prozesssicherheit eine Anleitung zur systematischen Erarbeitung
von Gefahren bei chemischen Stoffumwandlungen
im Industriemaßstab dar. Sie unterstützt bei der Bewertung
der Gefahren und bei der Erstellung von Maßnahmen, um
Störfälle zu verhindern. Am Beispiel der exotherm ablaufenden
Synthese von tert.-Butylperoxypivalat, einem organischen
Peroxid, wird die Vorgehensweise dargestellt. Organische
Peroxide sind als thermisch instabile Verbindungen bekannt
und besitzen dadurch ein zusätzliches Gefahrenpotential.
A closed pressure vessel test (CPVT) screen for explosive properties of energetic organic compounds
(2007)
Results of a round-robin test on a mini-autoclave are reported and previously proposed criteria reviewed. Criteria based upon the results for three standard materials are now put forward. These standards-based criteria, in contrast to numerical criteria, theoretically allow any laboratory to utilize the data accumulated to date, irrespective of the equipment used. The practical requirement is that adequate discrimination can be achieved. Data to assess this are given.