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Pahl Et Al-2005-Chemical Engineering & Technology
Pahl Et Al-2005-Chemical Engineering & Technology
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References
1 Introduction
______________________
Explosions Limits of H2S/CO2/air and
H2S/N2/air
By Robert Pahl and Kai Holtappels*
For the evaluation of the dangers of explosions, which can
take place while handling H2S, only literature values exist,
which had not been determined according to actual standard
methods. Therefore the explosion limits of the two ternary
gas systems H2S/CO2/air and H2S/N2/air were determined at
20 C and 1 bar(a) according to the bomb method of the new
European standard EN 1839. A comparison of these mea
[*]
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sured values with the literature values results in a clear expansion of the explosion range for both gas systems. Thus
the explosion limits for H2S/air were found at 3.9 mol-%
(LEL) and 49.8 mol-% (UEL) in relation to literature values
of 4.3 mol-% and 45.5 mol-%. Adding CO2 or N2 to the gas
systems in particular the UEL was found at higher amounts
of H2S than reported in the literature. Hence the LOC values are smaller. For the system H2S/CO2/air a LOC value of
10.5 mol-% (literature value: 12.1 mol-%), for H2S/N2/air
9.1 mol-% (literature value: 10.8 mol-%) was determined.
Dipl.-Ing. R. Pahl, Dr. K. Holtappels (kai.holtappels@bam.de), Bundesanstalt fr Materialforschung BAM, II.1 Gase, Gasanlagen, Unter den
Eichen 87, D-12205 Berlin, Germany.
2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
2 Experimental Section
The explosion limits of both ternary gas systems H2S/CO2/
air and H2S/N2/air were determined according to the bomb
method of the new European Norm EN 1839. In Fig. 1 the
experimental setup is shown schematically.
The mixture production was executed according to the
partial pressure method. The mixtures were produced directly in the ignition vessel (spherical high-grade steel
autoclave, V = 14 dm3). Therefore the ignition vessel was
evacuated and then the individual components were dosed
DOI: 10.1002/ceat.200500066
Communications
TIR
201
ERY
301
I,U
PIR
101
pressurized air
CO2
H2S
EL.
H 2O
TIC
202
http://www.cet-journal.de
747
Communications
H2S
0
100
90
80
Coward/Jones [4]
BAM
10
20
30
70
40
60
50
H2S
50
in mol-%
40
N2
in
mol-%
60
70
30
80
20
10
0
Luft
90
100
100 90
80
70
60
50 40 30
air in mol-%
20
10
0 N2
Literature
[1]
[2]
[3]
[4]
[5]
[6]
http://www.cet-journal.de
Communications
[7]
M. Molnarne, T. Schendler, V. Schrder, Sicherheitstechnische Kenngren, Band 2, Explosionsbereiche von Gasgemischen, Wirtschaftsverlag NW, Bremerhaven 2003.
This paper was also published in German in Chem. Ing. Tech. 2004, 76 (10), 1558.
______________________
A Modular Microreactor for Mixed Acid
Nitration
By Lder Henke and Hansjrgen Winterbauer*
A corrosion resistant microreactor made of PTFE and
Tantalum has been developed for the simulation of different
nitration reactions. The new microreactor can be easily
adapted to the conditions in an industrial plant due to the
modular type of construction, and in most cases the results
can be directly scaled up and pilot scale plants are not required. The new microreactor can be used for isothermal as
well as for adiabatic nitrations, and thermally unstable and
sensitive compounds can be produced as the whole reactor
can be operated at very low temperatures.
1 Introduction
A well known method to add nitro groups to organic compounds is the mixed acid nitration. This technology for the
production of intermediates and final products has been
applied for decades. For process optimization, extensive laboratory tests followed by tests in large scale plants were necessary in the past. Generally, the lab equipment cannot be
adapted sufficiently to large scale plant conditions. The common procedure is disadvantageous because obtained results
only give tendencies and direct scale up is difficult. Therefore, a corrosion resistant microreactor made of PTFE and
Tantalum was developed. Combining the advantages of micro reaction technology and modular type construction enables the simulation of different nitration reactions. A
screening of parameters is now possible in less time and with
fewer costs. The new microreactor can be easily adapted to
the conditions in an industrial plant due to the modular type
of construction. Additionally, it is easy to simulate the influence of changes in the equipment. In most cases the results
can be directly scaled up and pilot scale plants are not required. The number of tests at industrial scale production
plants is minimized. The new microreactor can be used for
isothermal as well as for adiabatic nitrations.
[*]
DOI: 10.1002/ceat.200500096
3 Microreactor Development
The targeted microreactor has to be resistant against
mixed nitration acid and organic compounds. Additionally,
the variation of mixing devices, reaction chambers, heat exchanges, etc. should be easy. This is achieved using PTFEcomponents which are connected via PTFE-tubes. The
PTFE-components have a thread with related nuts. The
tubes are put in and are fixed by tightening the nuts. No gaskets are required because the covering part of the PTFE 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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