(PDF) Drying Stages During The Heating of High-Alumina, Ultra-Low-Cement Refractory Castables

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66 Citations 12 References 4 Figures
Heating of High-Alumina, Ultra-Low-Cement Refractory Castables
n Journal of the American Ceramic Society 86(7):1146 - 1148 · December 2004 with 2,226 Reads
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2003.tb03438.x
Innocentini
Fábio A. Cardoso Mario M. Akyioshi
niversidade de Ribeirão Preto
ndolfelli
niversidade Federal de São Carlos Greenland is melting at an
Greenland was losing ice four time
new research has found. If it all m
level by seven meters. The study's
global warming is to blame. If the
relative to sea level at the turn of t
ork was to investigate the drying kinetics of high-alumina, ultra-low-cement refractory castables under continuous
hree main drying stages were identified during the castable heat-up and were related to the phase change of free water
tion of hydrated products present in the body. A clear correlation was found between the actual heating profile inside
dewatering stages under various heating schedules. Thermal analysis was used to assess the drying temperature that
t risk of steam pressure buildup and, thus, of explosive spalling.
tering
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unction of the furnace Drying stages related to the actual sample Drying profiles for CAC-containing and
us heating schedules. temperature for various furnace heating… cement-free samples at a furnace heating…
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J. Am. Ceram. Soc., 86 [7] 114

al
Drying Stages during the Heating of High-Alumina, Ultra-Low-Ce
Refractory Cast
Murilo D. M. Innocentini, Fábio A. Cardoso, Mario M. Akyioshi, and Victor C. Pand

Department of Materials Engineering, Federal University of São Carlos, São Carlos, São Paulo 13565-90
se of this work was to investigate the drying kinetics (calcined aluminas A1000 SG and A3000 FL, 22 wt%, d
mina, ultra-low-cement refractory castables under ␮m, where dp is the particle diameter) and the aggregat
heating conditions. Three main drying stages were (white fused aluminas, grades 4/10, 8/20, 10/36, 20/40, an
during the castable heat-up and were related to the 76 wt%, dp ⬍ 4.5 mm). The particle size distribution
nge of free water and to the decomposition of composition was adjusted to a theoretical curve based on A
roducts present in the body. A clear correlation was en’s packing model to obtain a potentially self-flow casta
ween the actual heating profile inside the castable a coefficient of distribution (q) of 0.21.
ewatering stages under various heating schedules. Samples were cast as 4 cm diameter ⫻ 4 cm thick c
nalysis was used to assess the drying temperature cured in the mold at 50°C (relative humidity of ⬃100%)
ents the highest risk of steam pressure buildup and, and heat-treated for 6 h at 800°C (heating rate of 1°C/min)
plosive spalling. casting, two thin K-type thermocouples (diameter of 0.2 m
inserted into some of these samples at a height of 20 mm,
at a depth of 1 mm (lateral surface) and the second at
I. Introduction (center of the body). To focus the analysis on the rem
physically absorbed water, the samples were saturated w
ORY castables are hydrated materials that require
tilled water under a vacuum for 2 h before each test.
l attention during their first heat-up. Depending on Dewatering tests were conducted in an electric furn
schedule applied, the steam that is generated may trolled by a proportional-integral-derivative (PID) syst
essurized within the ceramic structure, occasionally maximum temperature of 700°C and according to various
acking or even explosive disintegration of the prod-
schedules. The test sample was suspended in the cente
r this reason, the dry-out schedules of preshaped furnace to enable heat to reach every face of the body
are often divided into steps, aiming for safe removal neously. No forced air convection was provided in the
ree casting water at around 100°C and cement during the heat-up.
tion products at higher temperatures. However, the In the first set of experiments, the temperatures at the
uitable heating rates and dwell times is based mostly and center of the saturated specimen were monitored dur
al knowledge that takes into account the ceramic heating program. New tests were then conducted with
n, and the geometry and size of the product. In fact, samples without thermocouples to monitor the sample
able data on the duration and intensity of transfor- loss under the same heating conditions. Data on m
hat take place inside the heated structure make
temperature were computer-recorded at 5 s intervals thr
schedules preferable. This minimizes the risks of the experiments.
palling but makes the dry-out of green castables an Mass loss during drying was assessed through the no
and time-consuming operation. parameter W, which measures the cumulative fraction
ontext, this study focused on the optimization of the expelled during the heat-up per total amount of water
process of high-alumina, ultra-low-cement refractory present in the body. W varies from 0%–100% and is def
mpositions. The drying kinetics of physically absorbed
assessed during the castable heat-up at various heating
water loss pattern was directly related to the temperature
easured in the sample, allowing for the identification of
W共%兲 ⫽ 100 ⫻ 冉 Mo ⫺ M
冊
Mo ⫺ Mf
rying stages and providing guidelines to optimize where M is the instantaneous mass recorded at time ti du
astable heating schedules. heating stage, Mo the initial mass, and Mf the final mas
tested sample.
The experimental drying rate during heat-up was
II. Experimental Procedure through the derivative dW/dt by
able composition chosen for this study consisted of a dW Wi⫹1 ⫺ Wi⫺1
⫽
98 t% l i 2 t% l i l i t t
冉冊
98 wt%allalumina, 2See
wt%all ›calcium aluminate › cement
14, See
oa 66
Alcoa,› Pittsburgh,
(Brazil and U.S.)
Citations
PA), See all
and 4.52 wt%
supplied the matrix
12 References
water (dry
powders
4 Figures
冉冊
dt i ti⫹1 ⫺ ti⫺1
III. Results and Discussion

(1) Drying Stages
—contributing editor
The dewatering of a moistened porous medium under
conditions occurs in stages that are driven by different
mechanisms.6 – 8 Initially, water evaporates adiabatically
No. 186688. Received September 17, 2002; approved December 30, surface of the body in a stage known as the constant rat
(CRP).6 In this stage, the evaporation rate is greatly influe
by the Brazilian research funding institution FAPESP, by Alcoa S.A.,
sita S.A. external conditions, such as temperature and partial vap
American Ceramic Society. sure. In an isothermal environment, the evaporation rate
1146
Drying Stages of High-Alumina, Ultra-Low-Cement Refractory Castables
ng as the transport forces maintain the flux of water

es toward the body’s surface. However, as drying
evaporation front eventually recedes into the inter-
when the water transport, initially occurring by fluid
s driven by vapor diffusion through increasingly
engths. This process is characterized by gradual
e decreases with time, in a sequence of two stages
falling rate periods (FRP). 6
complete removal of moisture and hydrate decom-
dry-out of refractory castables must be conducted at
above the normal boiling point of water. Therefore,
f ambient temperature to 100°C, the drying process
rs at a constant heating rate rather than under
nditions, and the drying stages, as previously de-
go remarkable changes.
ce of continuous heating on the drying kinetics of a Fig. 2. Drying stages related to the actual sample temperature for v
table is shown in Fig. 1. Instead of the typical CRP furnace heating schedules.
blished for an isothermal environment, dewatering
e stages, identified by the peaks in the drying rate
the furnace heat-up. For the composition tested here, the pretreatment temperat
eaks appear to shift to higher temperatures as the 800°C is insufficient to start the sintering process. Henc
ncreases, the two first drying stages shown in Fig. 1 calcined phases of the calcium aluminate cement and th
ve the elimination of physically absorbed water. The alumina particles in the castable matrix can still be pa
misleading result is that the temperature of reference reactive, rehydrating when in contact with liquid water or w
’ location is set in the furnace rather than in the pressurized steam generated in the previous drying stages.
The aforementioned hypothesis that compares the dewa
uch more consistent pattern is observed when the profiles of three different samples heated at 10°C/min to 70
s involve the actual castable temperature, as illus- corroborated in Fig. 3. Sample A refers to a green, 2 wt%
2. The temperature range for each drying stage castable cured in the mold at 50°C and tested with its or
, and the main influence of the heating schedule is on moisture content; sample B, with a composition similar to t
and no longer on the location of the peaks. sample A, was prefired at 800°C and then moistened with di
tage, which takes place from ambient temperature to water for 2 h under vacuum; sample C refers to a cemen
main drying mechanism is evaporation of free water, composition also prefired and moistened before the test.
curs under adiabatic conditions. However, both CRP As depicted in Fig. 3, the lack of a third drying stage
affected by the temperature increase. Thus, although cement-free composition confirms that dehydration is in fa
on rate is enhanced by the greater water vapor cause of the minor water loss between 200°– 400°C for
simultaneously reduced by the progressive retreat of green and fired CAC-containing samples. According t
nt into the porous network. The temporary equilib- literature, this temperature range is typical for the decom
these two opposite effects is represented by the first tion of gibbsite (Al(OH 3)) and hexahydrated tricalcium a
ying rate curve at 50°– 60°C. nate (3CaO. Al 2O3 .6H2 O).10
able continues to be heated, the temperature at the Figure 3 also shows some changes in the drying rates in th
nterface eventually reaches the boiling point, and the first stages according to the type of sample tested. The fac
tant drying stage begins with the ebullition of free evaporation and ebullition occur in consecutive stages duri
s stage, the generation of steam is substantially drying process implies that as less water is evaporated, mor
ncrease in the castable temperature, when the steam remains during ebullition and vice versa. For this reaso
mes the main driving force for the flux of mass intensities of peaks in both stages usually display opposite
dy. The peak in the range of 100°-170°C results from when a variation occurs in the heating rate (as seen Fig. 2)
etween the increase of the rate at which steam is some property of the material. In the case of curves in Fig.
d the progressive shrinkage of the drying front differences in the permeability level among the samples
nter of the body. explain the different drying rates observed in each stage
tage in the drying profiles of Fig. 2 occurs in the instance, the green sample, displaying a lower permeability
ange of 200°– 400°C and is apparently not related to than the prefired one, had a higher resistance to dewatering
ut instead to hydrated products formed during the initial stage (lower evaporation peak), consequently leav
the sample or even during the dewatering process. larger amount of water to be boiled (higher ebullition
g profiles as a function of the furnace temperature for Fig. 3. Drying profiles for CAC-containing and cement-free samp
schedules. furnace heating rate of 10°C/min.
Journal of the American Ceramic Society—Innocentini et al. Vol. 86,
the similarities among the drying profiles of the and center of the body. In this case, the abrupt increase
d samples confirmed that removal of unbound water heating rate at the center signals the end of the boiling proce
t, be the main concern during the heat-up process of of the second dewatering stage, reestablishing similar h
w-cement compositions, requiring further attention to profiles for the center and surface for the remainder of the
ve pore pressurization and explosive spalling. Therefore, although heated to over 100°C, the body r
water in liquid form during most of the second drying stage
Changes during Dewatering may occur if the structure’s permeability is sufficiently l
is associated with important thermal transforma- increase the vapor pressure inside the pores, shifting the boil
e place inside the heated castable. Although part of water to higher temperatures. This effect is dangerously enh
heat is conducted into the body through the solid during the time interval in which the discrepancy in the h
profiles inside the body is maintained, when the heatin
of it is also absorbed by the liquid water retained in
st enhancing evaporation under 100°C and then increases rapidly on the surface while water is still boiling
iling above that temperature. 9 center.
s in Fig. 4 indicate that these endothermic phase Figure 4(c) shows that, for the castable heated at 10°C/mi
sses are remarkably intense during the first and critical displacement interval refers to a temperature increase
ering peaks, causing a temporary slowdown in the 160°–220°C. According to Antoine’s equation, 4 this imp
nside the castable. This effect is further accentuated theoretical steam pressure buildup from 0.6 –2.3 MPa, whic
of steam leaving the body, which decreases the be sufficiently high to cause the explosion of a green ca
heat absorption and increases the thermal gradient These values obviously refer to the maximum pressure bu
achievable in the center of the body if no release is provid
body and the surrounding atmosphere. The result is
f both dewatering stages is immediately followed by steam. In practice, the castable’s permeability and the h
n of the castable heating rate. 9 schedule determine the amount of water retained in the pore
g schedule also has a marked effect on the thermal hence, the actual intensity of the pressure buildup. Neverth
e the castable, as can be observed in Fig. 4. For the the values calculated by Antoine’s equation for the critical
ested here, the furnace heat-up at 1°C/min is suffi- tering interval represent the upper limit for steam pressuri
to produce no important internal thermal gradient, and may be reasonably compared with the mechanical t
center and surface of the sample becoming equally strength of green castables with the purpose of evaluating th
the dewatering stages. of explosive spalling.
ior changes with heating rates of 5°C/min and
pecially during the second stage when there is a
crepancy between the heating profiles at the surface IV. Conclusions
This investigation demonstrated that the dewatering proc
a continuously heated high-alumina, ultra-low-cement ca
occurs in stages and in different temperature ranges. The tw
stages involve the removal of free water, first by evaporation
100°C and by ebullition thereafter. The third stage takes pl
higher temperatures and involves the elimination of hy
phases in the castable matrix. Thermal analysis revealed th
sample’s center and surface were both remarkably sensit
endothermic processes involving the conversion of wate
steam and to the heating schedule applied. The heating p
inside the castable is therefore clearly related to the dewa
stages, providing an indirect assessment of the maximum
pressure buildup developed inside the pores, thus guidin
choice of heating schedules that minimize the risk of exp
spalling.
References
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M. Velez, A. Erkal, and R. E. Moore, “Computer Simulation of the Dewat
Refractory Concrete Walls,” Taikabutsu Overseas, 20 [1] 5–9 (2000).
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R. E. Moore, J. D. Smith, W. L. Headrick Jr., and T. P. Sander, “Mo
Dewatering Theory Testing and Practice: New Challenges”; presented at t
Annual Symposium on Refractories, St. Louis, MO, Mar. 1996. American C
Society, St. Louis Section, 1996.
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M. D. M. Innocentini, C. Ribeiro, J. Yamamoto, A. E. M. Paiva, L.
Bittencourt, R. P. Rettore, and V. C. Pandolfelli, “Drying Behavior of Re
See all › See all › See all › Castables,”
4 Am. Ceram. Soc. Bull., 80 [11] 47–56 (2001).
D. A. Bell, “First Heat-up of Ladle citation
Linings”; pp. Share
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66 Citations 12 References 4 Figures Proceedings. American Ceramic Society, Westerville, OH, 1997.
5
P. Kalifa, F. D. Menneteau, and D. Quenard, “Spalling and Pore Pressure
at High Temperatures,” Cem. Concr. Res., 30, 1915–1927 (2000).
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G. W. Scherer, “Theory of Drying,” J. Am. Ceram. Soc., 73 [1] 3–14 (19
7
W. C. J. Wei and C. L. Hsieh, “Drying Kinetics of Ultrafine Alumina Ca
Drying Control Chemical (DCC),” J. Ceram. Soc. Jpn., 107 [4] 313–17 (19
8
K. Oda, H. Itoh, T. Matsumoto, and Y. Ono, “Drying Characteristic o
Dense Castable,” Taikabutsu Overseas., 13 [2] 21–28 (1992).
9
M. D. M. Innocentini, C. Ribeiro, L. R. M. Bittencourt, and V. C. Pan
“Fluid Dynamics and Thermal Aspects of the Dewatering of High-Alumina
tory Castables: Removal of Physically Absorbed Water,” J. Am. Ceram. Soc.,
ation found between the actual heating profiles inside the 2696 –98 (2001).
e dewatering stages for various furnace heating schedules 10
N. Schmitt, J. F. Hernandez, V. Lamour, Y. Berthaud, P. Meunier, and J.
e of 1°C/min, (b) heating rate of 5°C/min, and (c) heating “Coupling Between Kinetics of Dehydration, Physical and Mechanical Beha
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References (12)
and explosion resistance of cured samples was carried out in a device that simultaneously measured the
les and the samples' temperature [22] , when applying heating rates of 2, 5 and 20 °C/min up to 600 °C. On the other
s were conducted at room temperature [23] using samples obtained after drying at 110 °C/for 24 h and calcining at 200,
...
nd their evaluation for self-flowing refractory castables

le
la Da Luz · Victor C Pandolfelli
(heating rate = 5 °C/min) and explosion resistance (heating rate = 20 °C/min) of the cured castables were analyzed in
d for thermogravimetric analyses of refractory materials [21] . Cylindrical samples (d = 50 mm x height = 50 mm) were
le inserted approxi- mately in the middle of these specimens (in order to allow the detection of the sample's temperature
nts) and cured at 30 °C for 24 h. ...
ation of dense refractory castables by adding a permeability enhancing active compound
Murilo Henrique Moreira · Chistoph Wöhrmeyer · Victor C Pandolfelli
drying rate profiles of the castables (Fig. 4b), it was detected a first peak related to water evaporation and gel phases
0 °C), followed by a second one that corresponds to both vapor release and hydrate decomposition (∼280 °C) [27] . As
eak evaporation intensity for the TAB sample was higher than the corresponded one for TSZ castable, meaning that a
r was retained in the microstructure of the former, which could lead to higher potential of pressurization during ebullition
ing refractory castables bonded with calcium-free binders

le
Ana Paula Da Luz · Victor C Pandolfelli
o avoid such restrictions and to reduce the chances of explosive spalling [59][60] [61] [62][63] researchers contin- ued to
tent and finally cement free castables were developed [11,[64][65][66]. A number of cement-free bonding systems have
ave changed the castable properties significantly, and these include different colloidal systems like silica, alumina,
ratable alumina (HA); micro-silica; etc. ...
ctory
SeeCastables
all › — An
SeeOverview
all › See all ›
dry weight, P i (g) is the suspended weight and P u (g) is the saturated weight of the evaluated specimens.
asurements were carried out up to 600 °C using cylindrical specimens (40 mm × 40 mm, one specimen per composition)
in an apparatus developed to evaluate refractory materials [36] . A heating rate of 5 °C min −1 was used during these
e mass change and the derivative of the mass change was calculated as indicated in Eqs. ...
castables with enhanced explosion resistance due to in situ formation of phases with lamellar structure
or · Flávia G. Pinola · Ana Paula Da Luz · Victor C Pandolfelli
ture of stainless steel fibers application is about 1100 °C under oxidation and normal conditions (Lau, Anson 2006).
pylene, polyamide and others) are required for dense and deflocculated castables to facilitate the removal of water
tial heating (Innocentini et al. 2002;Leung, Balendran 2002;Peret et al. 2003) because castables are prone to explosive
ating (Innocentini et al. 2003a (Innocentini et al. , 2003bOlivier, Fabien 2014). These fibers shrink at a temperature
olve at ~150 °C, when the temperature is further increased. ...
polypropylene fibers on thermal shock resistance of the refractory castable
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on the Hydration Behavior of Calcium Aluminate Cement

le
hen · Xiangcheng Li · Boquan Zhu
ydration in refractory castables by using carboxylic acids

le
M SOC
or · J. dos Santos · Ana Paula Da Luz · Victor C Pandolfelli
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Heating of High-Alumina, Ultra-Low-Cement Refractory Castables

or C Pandolfelli Author content

Content uploaded by Victor C Pandolfelli Author content

J. Am. Ceram. Soc., 86 [7] 114

Murilo D. M. Innocentini, Fábio A. Cardoso, Mario M. Akyioshi, and Victor C. Pand

III. Results and Discussion

Drying Stages of High-Alumina, Ultra-Low-Cement Refractory Castables

ng as the transport forces maintain the flux of water

Journal of the American Ceramic Society—Innocentini et al. Vol. 86,

nd their evaluation for self-flowing refractory castables

la Da Luz · Victor C Pandolfelli

ation of dense refractory castables by adding a permeability enhancing active compound

Murilo Henrique Moreira · Chistoph Wöhrmeyer · Victor C Pandolfelli

ing refractory castables bonded with calcium-free binders

Ana Paula Da Luz · Victor C Pandolfelli

or · Flávia G. Pinola · Ana Paula Da Luz · Victor C Pandolfelli

polypropylene fibers on thermal shock resistance of the refractory castable

e with nano‐alumina and its effects on properties of corundum spinel castables

rfesten Gießmassen: Ein Überblick

on the Hydration Behavior of Calcium Aluminate Cement

hen · Xiangcheng Li · Boquan Zhu

ydration in refractory castables by using carboxylic acids

Y.-J. Song · S.-H. Meng · F.-D. Wang · [...] · Zhi-Cheng Tan

Thermal analysis on Na2B4O7-Na 2CO3 molten salt for boronizing

Y.-G. Huang · M.-D. Ren · Q.-Y. Li · H.-Q. Wang

Thermal decomposition kinetics of 2, 4, 6-triamino-3, 5-dinitropyridine-1-oxide and its moulding pow...

Aliye Arabacı · S. Kirtay · Nuri Solak

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