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CHEMICAL ENGINEERING TRANSACTIONS
VOL. 48, 2016
A publication of
The Italian Association
of Chemical Engineering
Online at www.aidic.it/cet
Guest Editors: Eddy de Rademaeker, Peter Schmelzer
Copyright © 2016, AIDIC Servizi S.r.l.,
ISBN 978-88-95608-39-6; ISSN 2283-9216
Self-Ignition Behaviour of Growing Dust Layers
Bernd Broeckmann, Martin Gosewinkel, René Dworschak
Inburex Consulting GmbH, Hamm, Germany
Martin.Gosewinkel@Inburex.com
Despite all precautions in the dust-processing industry there are often hazardous situations leading to damage
to property and persons. In drying processes self-ignition respectively smoldering fires of dust accumulations
are often considered as leading causes for such incidents.
Several well-established experimental test methods exist to analyse the self-ignition behaviour. These
procedures have specific advantages and disadvantages, such as testing time, energy consumption and
especially their different capability of scale-up from laboratory to industrial scale.
Within the scope of a safety assessment of drying procedures these test methods often lead to a temperature
level at which heat production exceeds the natural heat losses of the bulk and lead to spontaneous
combustion. For the assessment of deposits in dryers etc. the described methods can be directly applied in
the majority of cases, as well as to process conditions, e.g. a dust deposit with a defined thickness at different
operating temperatures concerning their thermal hazards ( ignition source: glowing particle).
But one point will be unidentified in this point of view: changes in the physical properties of dust accumulations
over time and mainly for non-uniform layer thickness. These changes, however, remain unknown and are
mostly ignored as possible source of spontaneous combustion.
These parameters often represent the decisive issue to trigger a run-away reaction, especially in case of spray
dryers with variable dust accumulations on the inner wall. To take this effect into account the conventional test
procedures were adapted to simulate experimentally the layer increase during the drying process depending
on the operating temperature and time.
Initial situation
In addition to spray drying units, also conveyers or milling plants, are often affected by fires or explosions
(BIA-Report, 1997). The following figure shows a possible setup of a spray drying unit.
There are several hazards that can develop
into hazardous situations (Broeckmann et al.,
1996).
Firstly, the hazard of developing an explosive
atmosphere exists e.g. in the cone of the spray
dryer, the subsequent fluidized bed or in the
vessels for dust collection (VDI 2263/7, 2010).
Secondly, the possible presence of potential
ignition sources has to be kept in mind as
hazard.
Typical ignition sources are mechanical sparks,
hot surfaces which are induced by friction on
the atomizer disc in the spray dryer
(Broeckmann et al., 1996) and self-ignition
inside the spray dryer.
Results of the self-ignition process are
smoldering dust deposits, open flames and
fires as well as the development of additional
smolder gas (main component carbon
Figure 1: Charting of a spray-dryer-unit (VDI 2263/7, 2010)
DOI: 10.3303/CET1648075
Please cite this article as: Gosewinkel M., Dworschak R., Broeckmann B., 2016, Self-ignition behavior of growing dust layers, Chemical
Engineering Transactions, 48, 445-450 DOI:10.3303/CET1648075
445
monoxide) (Bartknecht, 1993). Smoldering nests are often located at the dispersion components of the spray
dryer such as the atomizer disc (figure 2) and on the inside of the dryer as deposit (Gosewinkel & Meistes,
2010).
Several safety measures are in place to prevent these hazardous
situations and to reduce the risk to a minimal level. Among those
safeguards are temperature alarms and interlocks, gas analysis devices
(measuring the level of CO) (Zockoll, 1992), (Zockoll, 1996), (Gosewinkel
& Meistes, 2010) and constructive measures (VDI 2263/7, 2010), (Abott,
1990), (Broeckmann et al. 1996).
1. Ignition source “Self-ignition”
Self-ignition of dust in bulk is caused by the rate of heat generation from
oxidation and/ or decomposition reactions of the dust being greater than
the rate of heat loss (Bowes, 1984) (DIN EN 15188, 2007).
The self-ignition behavior of combustible dusts depends on their chemical
composition as well as on related substance properties (e.g. the size and
geometry of the body of material, ambient temperature).
In general self-ignition or spontaneous combustion is limited to solid
materials with high specific surfaces. Oxygen can react on the surfaces
throughout the bulk as long as the air exchange is sufficiently high, which has to be assumed for the beginning
of a self-ignition process. The oxidation process may start at room temperature depending on the substance.
At the beginning of the self-ignition (better: self-warming) the reaction power is marginal and hardly to detect.
If the heat production by oxidation exceeds the natural heat losses of the bulk the self-warming process turns
into a self-heating or self-ignition process.
A heat balance, as can be seen in the following picture, involving the heat produced inside the bulk (quantity
of reactive surface molecules, gross calorific value) and the heat loss to the surroundings (heat conductivity
and dimension of the bulk, heat transfer coefficient on the outside surface of the bulk and the size of the latter)
is decisive if
• A steady state temperature is reached at a slightly higher temperature level, that means that the heat
loss terms are greater than the heat production terms (see Figure 3, case 1) or
• Temperatures in the bulk will continue to rise up to self-ignition of the dust (see Figure 3, case 2), if
heat transport away from the system is insufficient, which results in greater heat production
compared to the heat loss.
For a better understanding it is useful to use the so-called Semenov-diagram, which is often used in terms of
thermal explosion. The following assumption forms the base for this type of application of the thermal theory
• The physical effects on large deposits and those on laboratory scale are equivalent.
• The chemical reaction is of zero order
• The initial temperature equals the ambient and surface temperature.
The exothermic reaction follows an
Arrhenius type rate law, i.e. exponentially
dependent, whereas the heat loss is
assumed to be governed by Newtonian
cooling, i.e. linearly dependent. The rate of
heat loss intersects the exponential heat
production curve at two points, where the
chemical heat production is balanced by
the heat removal capacity.
The low temperature point (Figure 3: point
1) represents a stable point. Here the rate
of heat loss is greater than the rate of heat
production and the temperature will return
to this point. The other point (Figure 3:
point 2) represents an unstable point
because any slight temperature increase
will cause an increase in the rate of heat
production which is not matched by the rate of heat loss and an accelerating runaway will occur.
Figure 2: Example of a
smoldering dust deposit at the
atomizer system
Figure 3: Semenov-diagram
446
The tangential point of heat loss and heat production describes the critical situation where the heat production
is just equal to the heat removal. The appropriate ambient temperature is equal to the self-ignition temperature
TSIT.
2. Experimental determination of the self-ignition
Several well-established experimental test methods exist to evaluate the spontaneous ignition behavior of
dusts accumulations, e.g. Grewer-test, Aearated-cell test, Air-over-layer test, test A.16 Guideline 440/2008,
hot-storage tests according to EN 15188).
These procedures have specific advantages and disadvantages, such as testing time, energy consumption
and especially in their different capability of scale-up from laboratory to industrial scale. The main point of
criticism regards to the prediction of safety criteria like safety temperature levels or storage time.
Mostly the investigation of the self-ignition
behavior of dusts will be provided by so-called hot
storage tests according to (DIN EN 15188, 2007).
The sample is kept in a wire basket of cylindrical
or cubic form of different volumes in an oven of
sufficient volume.
The oven can work with natural convection or air
circulation. They shall have an air inlet opening in
the lower section and an air outlet opening in the
upper section, as shown in the following
schematic drawing.
They should have a useful volume of about 120
litres and be controllable in a temperature range
from 25 °C to 300 °C. The samples have to be
loosely filled into mesh wire baskets of different
volumes. The baskets have to be open at the top
and closed at the bottom.
They consist of a narrow-meshed wire net, made
of stainless steel. Recommended shapes of the
mesh wire baskets are that of a cylinder with a
height to diameter ration of 1 or that of a cube.
3. Assessment of the self-ignition behaviour and their problems
According to (DIN EN 15188, 2007) the experimental basis for describing the self-ignition behavior of a given
dust is the determination of the self-ignition temperature (SIT) of differently-sized bulk volumes of the dust by
isothermal hot storage experiments in commercially available drying ovens. The results thus measured reflect
the dependence of self-ignition temperatures upon
dust volume. The following picture shows a typical
temperature-time-plot of such a hot-storage test.
This test result is classified as self-ignition
because the sample temperature exceeds the
oven temperature of more than 60 K (DIN EN
15188, 2007).
Plotting the logarithms of volume/surface ratios
(log V/A) of differently sized dust deposits vs. the
reciprocal values of the respective self-ignition
temperatures (1/T in K-1) ( Pseudo Arrhenius
Plot) produce straight lines, allowing interpolation,
to characterize the self-ignition behavior of dust
deposits of different scale.
Figure 4: Positioning of a sample and thermocouples in
the drying chamber for hot storage tests (DIN EN 15188,
2007)
Figure 5: Typical temperature-time-plot of a hot-
storage-test according to (DIN EN 15188,
2007);sample: cinnamon, basket volume: 400 ml
447
Within the scope of safety assessment
of drying procedures the mentioned
test methods often lead to a
temperature level at defined geometry
with defined dimensions ( cube,
cylinder, layer thickness….) at which
heat production exceeds the natural
heat losses of the bulk and lead to
spontaneous combustion.
For the assessment of deposits in
dryers etc. the results of these methods
on self-ignition behavior can be directly
applied in the majority of cases, as well
as to process conditions, e.g. a dust
deposit with a defined thickness at
different operating temperatures
concerning their thermal hazards (
ignition source: glowing particle).
But one point is not kept into
consideration: changes in the physical
properties of dust accumulations over time (glass transition temperature, density, viscosity, thermal
conductivity and heat capacity) and mainly for non-uniform layer thickness. These changes, however, remain
unknown and are mostly ignored as possible source of spontaneous combustion. But these parameters often
represent the decisive issue to trigger a run-away reaction, especially in case of spray dryers with variable
dust accumulations on the inner wall. To take this effect into account conventional test procedures were
adapted to simulate experimentally the layer increase during the drying process depending on the operating
temperature and time. The basic approach of this new method is displayed in Figure 7.
This test is based on the “Air-over-layer”-test according to Abbott (1996). The “Air-over-layer”-test procedure
simulates the full scale situation if the powder layer thickness reflects that likely to arise in the dryer, and
therefore the temperature from which an exothermic reaction can progress to a self-ignition can be used for
defining safe drying procedures. The adapted test procedure should give general information about the layer
thickness depending on the drying temperature.
Therefore, a layer with a defined layer thickness of
the sample is inserted in the wire basket with a
defined edge length and placed into the oven at
ambient temperature. The sample is heated up to a
specific temperature, normally equal to a typical
drying temperature, and held isothermally at this
temperature for e.g. 8 hours.
Then a new layer with the same height as the first
layer is filled into the wire basket, i.e. the old layer is
8 h old, and now a new layer is brought up to this
old layer and is stored at specific temperature for 8
hours. Subsequently, a new layer with the same
height as the other ones is brought up to the old
layers and should be stored for several hours.
The oven will be continuously purged with a defined
air flow rate. The CO-concentration is continuously
measured in the outlet air. Before the CO-
concentration is measured, the air will be
conditioned (cleaned and diluted). Furthermore, the
temperature profiles of the sample (centre of the
sample layers, sample surface, half width of the
sample) and the oven temperature will be
continuously recorded.
An additional thermocouple can be placed above the sample to determine potential inflammations.
Figure 6: Evaluation of the tests to determine self-ignition behavior
of the tested products: Pseudo-Arrhenius plot of self-ignition
temperatures (DIN EN 15188:2007)
Figure 7: Basic approach of the adapted test
procedures
448
4. Example of the application of the new test method
In the experiment, the process conditions of a spray dryer for the manufacturing of infant food should be
evaluated. The spray dryer is displayed in figure 8.
Basically it should be determined to
which extent a maximum dust layer of
15 cm is allowable at a maximum air
inlet temperature of 140 °C and a
continuous operating time of 45 h.
As a first step, conventional hot-
storage tests were carried out in a
wire mesh basket with a length of
15 cm.
The following figure shows the
temperature-time-dependence as well
as the sample after the testing.
It can be seen, that the conventional
hot storage test, displayed in figure 8,
shows only a slight self-heating of the
investigated sample. Also the sample
itself showed no typical self-ignition
behaviour. In the next diagram the
result of the new test method is
shown.
The introduction of new layers can be seen by a sharp decrease of the temperature profiles, which are
represented by the upper lines. The CO-detection is described by the line at the bottom of the diagram.
After reaching the oven temperature the first sample layer temperature (layer 0) showed stable behaviour and
no significant CO-emission. After bringing up the second layer (layer 1) the temperature of this layer also
showed a normal a stable behaviour.
Shortly after bringing up the second layer, that means after a complete testing time of about 30 hours, the
temperature profile of the middle layer (layer 1) does sharply decrease because of the cooling effect of the
new layer.
Figure 9: conventional hot storage test according to EN 15188, 15 cm wire basket
But now the middle layer and the new layer are heated up quickly and after a testing time of about 33 hours
the sample runs directly in the exothermic reaction.
In contrast to figure 9, figure 10 shows a direct self-ignition process of the sample.
Figure 8: Manufacturing process conditions of children’s food
449
The introduction of a new dust
layer (sharp decrease of the
temperature profiles) leads to heat
accumulation at the interface
between “old” (thermal aged) and
“new” layer due to a deteriorated
heat removal and changes of
material properties and so
promotes the entire sample in a
supercritical state ( self-ignition
process).
This behavior can be explained by
a change in the thermal properties
of the sample during deposition
(thermal conductivity, heat
capacity) and their direct impact on
the heat balance as displayed in
figure 3. The process conditions of
the future production were finally
determined as follows after finishing the testing procedures:
– Maximum air inlet temperature: 140 °C
– Maximum thickness of dust deposit in the spray dryer: 10 cm
– Production time: 45 h
5. Conclusions
For the assessment of deposits in dryers etc. the results of the conventional experimental test procedures e.g.
regarding CEN 2007, will be directly applied concerning their thermal hazards ( ignition source: glowing
particle). But these procedures don’t consider changes in the physical properties of dust accumulations over
time and for time-dependent layer growth. Therefore these points often remain unknown and disregarded as
possible source of spontaneous combustion, but often represent the decisive issue to trigger a run-away
reaction, especially in case of spray dryers with variable dust accumulations on the inner wall.
To take this effect into account a conventional test method was adapted to simulate experimentally the layer
increase during the drying process depending on the operating temperature and time.
Due to this modified method spontaneous combustion processes could be identified precisely as ignition
source in several incidents compared to the results of conventional test procedures (Broeckmann et al., 2014).
Reference
Abott, J.: Prevention of Fires and Explosions in Dryers, IChmE, 2nd edition, 1990
Bartknecht, W. Zahlen, G.: Explosionsschutz: Grundlagen und Anwendungen, 1993
BIA-Report 11/97: Dokumentation Staubexplosionen – Analyse und Einzelfalldarstellung, Deutsche
Gesetzliche Unfallversicherung e.V. (DGUV), 1997
Bowes, P. C.: Self-Heating: Evaluating and Controlling the Hazards. Elsevier, Amsterdam, 1984
Broeckmann, B.; Alfert, F.; Rogers, R.L.: Brand- und Explosionsschutz in Trocknungsanlagen, Gefahrstoffe -
Reinhaltung der Luft 56 (1996), S. 383-387
Broeckmann, B; Gosewinkel, M.; Dworschak, R.: Selbstentzündung von Stäuben beim Schichtwachstum,
Jahrestreffen Agglomerations- und Schüttguttechnik, Magdeburg, 2014
DIN EN 15188: Bestimmung des Selbstentzündungsverhaltens von Staubschüttungen; Deutsche Fassung EN
15188:2007
Gosewinkel, M.; Meistes, J.: Präventiver Brand- und Explosionsschutz; CO-Monitoring - vom Labormaßstab
zum Großprozess 10. Fachtagung Anlagen-, Arbeits- und Umweltsicherheit Köthen, 2010
VDI 2263/7, Brand- und Explosionsschutz an Sprühtrocknungsanlagen, Verein Deutscher Ingenieure e.V.,
Düsseldorf, 2010
Zockoll, C.: Brandfrüherkennung durch CO-Detektion am Beispiel von Sprühtrocknern der Milchindustrie, VDI
Berichte 975, 1992
Zockoll, C.: Früherkennung von Bränden durch CO-Detektion, VDI Berichte 272, 1996
Figure 10: adapted test procedure, 15 cm wire basket
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