2700 Curing and Dryout

Abstract
This section tells what must be done to a lining after placement and before firing.
The terms “curing” and “dryout” are defined, and curing methods are given for
various refractory materials. Then dryout theories and procedures are discussed,
including advice on modifying start-up procedures after water washing, hydro-
blasting, etc. Typical dryout schedules are also given for five refractory lining
systems.

Contents Page

2710 Definitions 2700-2

2720 Curing 2700-2
2721 Hydraulically Bonded Castables
2722 Other Refractory Types
2723 Two-component Linings
2730 Dryout Theories 2700-4
2740 Dryout Procedures 2700-4
2741 Refractory Castable Linings
2742 Dryout of Type C Plastic Refractory
2743 Dryout of Two-component Linings
2744 Monitoring Dryout Temperature
2745 Shop Dryout
2746 Field Dryout
2747 Adjustment of Normal Dryout Procedure

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2700 Curing and Dryout Insulation and Refractory Manual

2710 Definitions
Curing is the initial ambient temperature holding period following placement. Not
all types of refractory material require a holding period before dryout.
Dryout (also called thermal curing) is the initial heating of refractory linings to
temperatures near their service temperature. The dryout procedure forces out any
remaining mechanically held water and also expels some chemically combined
water. If a controlled dryout is not accomplished, rapid heating may cause explosive
spalling or reduce the strength of the refractory. Dryout is completed according to a
time/ temperature schedule, and therefore is often done prior to startups of the unit
(or other equipment) to achieve better control of the operation.
With the exception of sprayable RCF, most RCF lining systems require neither
curing nor dryout.

2720 Curing

2721 Hydraulically Bonded Castables

Hydraulically bonded castables are cured in order to allow time for hydraulic
bonding to occur. It is important to prevent moisture loss from exposed surfaces
during curing so that an excess of water is available within the refractory to accom-
plish the various hydrating reactions which develop strength.
Membrane Curing Compound. Curing hydraulically bonded castables (Types A
and D through I) is best accomplished by applying a colored (often red) membrane
curing compound to the exposed surface. It is important that the compound be
applied as soon as practical after placement. This is usually after the material has
taken its initial set (about 1 hour). The objective is to minimize loss of moisture
from the castable by surface evaporation. Two coats of the curing compound are
preferable. This ensures complete coverage. Application is made with a pressure
tank garden sprayer. Only resin base curing compounds, such as Master Builder
Resin Base, should be used because they are less volatile.
For a minimum of 24 hours after placement, the refractory lining must be main-
tained between 50°F and 90°F to allow hydration reactions to occur and strength to
develop. Whatever happens, do not allow freshly installed refractory concrete
to freeze! Freezing virtually destroys the hydraulic bonding.
It is highly preferable that curing take place at temperatures greater than 70°F. The
reason for this involves highly technical cement chemistry. Basically, we wish to
minimize the formation of Al2O3 gel during hydration. Better (stronger) castables
are achieved when Al2O3 gel does not develop in the curing period.

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Insulation and Refractory Manual 2700 Curing and Dryout

Water Spray Curing. An alternative method (to using a curing compound) is to

keep the surface damp with a fine water spray, observing the following provisos:
1. Do not begin water spraying until the material has taken its initial set.
2. Spray the material at 2-hour intervals for a minimum of 24 hours after
installation.
Water spray curing is less satisfactory than curing compound. Because of the
multiple applications required, water spray curing is usually not done properly.

2722 Other Refractory Types

Type B Refractory. Allow material (such as Resco AA-22) to air dry for 24 hours
after installation at a temperature of 50°F to 90°F. Do not water spray or allow
water to contact the material. Do not apply a membrane curing compound.
Type C Refractory. Use the same procedure as for Type B (i.e., no compound or
water). Some of the erosion-resistant plastics tend to bloat during ambient curing,
creating a lamination 1/4 to 1/3 of the thickness below the surface. Fine grained
plastics tend to form a skin on the surface restricting water vapor transmission. This
tendency is minimized with newer “high-strength,” low-water-content plastics and
those with a fairly coarse grain structure. Bloating is definitely undesirable since
the delaminations spall off in service, decreasing the lining thickness. An interme-
diate temperature cure of about 125°F to 150°F for several days has been successful
in minimizing bloating.
Regular Plastic Refractory (material that might form the burner wall in a boiler).
The curing step should be skipped. If at all possible, the installation of the plastic
refractory should be delayed until the boiler or furnace can be fired immediately
upon completion of installation. If forms are involved, remove forms as soon as
plastic lining has hardened, usually in about 18 hours, and then begin the firing.
When it is impossible to fire the boiler right away, cover the plastic refractory
wall(s) with polyethylene film, held in place with nails, and keep all manways
closed. The objective is to minimize air drying and the formation of drying cracks
prior to dryout. Do not allow plastic refractory to freeze prior to dryout.

2723 Two-component Linings

No special considerations are involved when curing a two-component lining. Gener-
ally the time required for the back-up layer to set up (harden) and for the hot face
anchors to be installed is sufficient curing time before installation of the hot face
layer. No special hold times between installation of back-up and working lining are
required. Curing compound should be applied to all exposed refractory surfaces,
including the back-up layer, within one hour of placement.

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2700 Curing and Dryout Insulation and Refractory Manual

2730 Dryout Theories

The mechanism for dryout of a monolithic refractory lining involves applying heat
to the hot face and forcing the water to migrate out of the refractory. In early stages
of the dryout operation, more water may migrate towards the cooler steel shell than
to the hot face. Water that does reach the hot face is removed by evaporation.
As the dryout operation continues, the shell eventually reaches a temperature of
about 212°F. At this point, any condensed water begins to vaporize and is forced to
move (through small pores and capillaries) through the refractory to the hot surface.
Monolithic refractories contain both mechanically held and chemically combined
water. In general, the mechanical water is removed first (up to 212°F). As the lining
heats up further, above 220°F, the chemically combined water (or part of it, consid-
ering the temperature gradient through the thickness of the lining) is also removed.
The objective of the controlled dryout operation is to remove water from the lining
in such a way that steam or explosive spalling does not occur. Spalling occurs when
water flashes to steam and the resultant increase in volume fractures the refractory.
If dryout is too rapid the consequences can be catastrophic. If the lining is cured at
temperatures 70-90°F, steam spalling is less apt to occur even when the lining is
heated rapidly because of the creation of more permeable pore structures in this
temperature range.
Most refractory manufacturers promote the use of various organic fiber additives
(see Section 2130) that permit rapid firing (dryout) of installed castable linings. For
most types of castables, these organic fibers—which improve capillary structure in
the refractory and make it easier for water transport through the lining—may not be
required. For thick, dense refractory linings with low permeability and porosity,
Types A and D especially, organic fibers do provide a factor of safety during
dryout. When used, they lower the strength of the castable slightly. Also, these addi-
tives aren't useful in all situations. For example, in an FCC unit, other types of
refractory in the unit may limit the heat-up rate anyway.
Currently, several firms specialize in rapid controlled dryouts for new or repaired
linings. Their equipment consists of large volume gas fired air heaters and multi-
point recorders for monitoring temperature. Chevron has used these firms success-
fully on a number of jobs. Two companies that do this work are:
1. Hot Work, Inc. – (606) 276-1570
2. Cooperheat – (908) 981-0800

2740 Dryout Procedures

Dryout procedures that refractory manufacturers propose for monolithic refractory
linings are generally too conservative. The manufacturers are concerned that the
linings may be damaged during dryout by too rapid heating and that they will be
blamed for supplying inferior refractory products. The Company's recommended
rates are more practical and have proven safe when used with its refractory
specifications.

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Insulation and Refractory Manual 2700 Curing and Dryout

2741 Refractory Castable Linings

Dryout of refractory castable linings means heating the lining at a controlled rate to
a maximum temperature. The schedule may include one or more holding periods,
and the heat-up rate may increase as well.
Low-temperature Hold. The Company recommends a low-temperature hold
(250 to 300°F) for Types E and F semi-insulating castables. For Types A and D
erosion resistant castables the Company recommends a low-temperature hold at
325 to 375°F. [52, 63] These temperatures are hot gas temperatures and correspond
to about 225°F refractory hot face temperature. In either case the hold time should
equal one hour per inch of refractory thickness. The low-temperature hold must be
used in all refractory dryout procedures and is particularly important in fired
heaters and boilers, because furnace heatups are hard to control, with temperature
in different parts of firebox varying widely.
High-temperature Hold. The Company also recommends a holding period at
925 to 1000°F for one hour for types E and F semi-insulating castables. For Types
A and D, erosion resistant castables, the Company recommends a three hour hold at
1000°F. [62]

2742 Dryout of Type C Plastic Refractory

Although plastics have a much lower water content than hydraulically bonded casta-
bles, they go through some five phase changes before they reach the final reaction
at 932°F. They can be mechanically damaged until they reach about 230°F, and
they can rehydrate anytime before they reach 932°F. For this reason, the Company
recommends that in the field, where several types of refractory material are to be
used, Type C refractory work be done last (to prevent mechanical damage). For
shop-lined equipment, the Company recommends dryout (above 932°F) before it
goes to the field in case the lining should get wet before the equipment is installed.
Typical dryout schedules for monolithic refractory linings are shown in
Figure 2700-1.

2743 Dryout of Two-component Linings

When preparing a dryout schedule for a two-component lining (e.g., 3 inches of
dense 94% Al2O3 castable backed by 3 inches of insulating castable) the first thing
to calculate is whether or not the proposed schedule will remove all of the mechani-
cally held water from the back-up castable. Thermal conductivity calculations can
be used for this purpose. The lining should be held at the calculated temperature
long enough for the lining to reach equilibrium and the cold face temperature to
reach 230°F. Monitoring the cold face temperature is an additional way to monitor
dryout progress.
The other consideration is the heating rate to be used during dryout. Again, we
must control the heating rate to protect the refractory most apt to be damaged by
too rapid heat-up, in this case, the dense 90% Al2O3 castable. Too rapid heating
rates cause explosive spalling. (See Figure 2700-1 for a typical schedule.)

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2700 Curing and Dryout Insulation and Refractory Manual

Fig. 2700-1 Typical Dryout Schedules(1)

5" Vibration
5" Regenerator Cast Lining, 1" Cyclone 1" Cyclone Two-component
Parameters Lining, FCCU(2) Reactor Riser(3) Lining Lining Lining 6-8" thick
Monolithic “One-shot,” Erosion-resistant Chemical setting Chemical setting Typically 3-4" of
refractory semi-insulating castable, Type A erosion- erosion- 94% Al2O3
type (per castable, Type E or D resistant resistant plastic, (Type A) and 3-4"
GB-N1268) or F castable, Type B Type C insulating
(Type I)
Low-temp. Heat at 75°F/hr.; Heat at 50°F/hr.; Heat at 50°F/hr.; Heat at 50°F/hr.; Heat at 75°F/hr.;
Rate/Hold(4) Hold at 250-300°F Hold at 325-375°F Hold at 250-300°F Hold at 250-300°F Hold at 250-300°F
High-Temp. Continue at Continue at Raise rate to Continue at Continue at
Rate/Hold 75°F/hr.; Hold for 50°F/hr.; Hold 3 100°F/hr.; Hold 50°F/hr.; Hold at 75°F/hr. until
1 hr.; 925-1000°F; hrs.(5) at 1000°F.; at 650-700°F; 650-700°F; cold face
Ready to operate Ready to operate Ready to operate Continue heat- reaches 230°F;
up to 935°F Ready to operate
minimum; Ready
to operate
Remarks Dryout of lining Install TC's for Surface TC's for
is usually done shop dryout on shop dryout
during start-up refractory should be used
surface, & use to to make certain
monitor dryout refractory
reaches 935°F
(1) See text. Temperatures are “hot gas” temperatures with some exceptions. These schedules assume no credit for addition of organic
fibers.
(2) Refractory Types F, G, H and I follow approximately the same schedule.
(3) Refractory Types D2 and D3 follow approximately the same schedule.
(4) Holding time equals 1 hour per inch of thickness in all cases.
(5) If lining is being dried out by operations, eliminate hold and continue at 50°F/hr. to operating temperature.

2744 Monitoring Dryout Temperature

During dryout of a lining, it is desirable to measure the temperature of the refrac-
tory hot face as well as the temperature of the hot gas from the burners. It is prefer-
able that any temperature control (manual or automatic) of the dryout operation be
based on the hot-face temperature of the installed refractory rather than on the
temperature of the hot gas stream. There are two good reasons for this statement:
• The hot gas stream is typically hotter than the hot face of the refractory.
• If damage should occur to the refractory lining by too rapid heating, the
damage will be directly related to refractory temperature and not to the temper-
ature of the hot gas stream.
Unfortunately, it is often impractical to place thermocouples on the hot face of the
refractory. Also, dryout schedules proposed by the refractory manufacturers are
based on hot gas temperatures. For this reason, hot gas temperatures are given in
Figure 2700-1.

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Insulation and Refractory Manual 2700 Curing and Dryout

These schedules have a factor of conservatism built in and should be used to

monitor dryout of refractories when a process vessel or a fired heater is brought up
to operating temperature after a shutdown.
In the case of an FCC unit, there will be several repair/replacement areas involving
three or four different types of refractory. It is not feasible to have thermocouples
on the hot face of each refractory location. In this situation, use the slowest
schedule of those recommended for the refractory types involved (thickest, densest
refractory).

2745 Shop Dryout

It is important that dryout of shop fabricated equipment be accomplished before
shipment by heating in a fashion similar to how it is heated in service. Cyclones can
be heated from both the inside and the outside in an oven since they are hot wall
units. Transfer lines, vessels and other cold wall units should only be heated from
the hot face. If the cold (insulated) face is heated in an oven, the following may
occur:
1. The shell may be heated above its (metal) temperature limit.
2. Excessive thermal expansion of the shell may occur, causing anchors and/or
the shell to break loose from the refractory.
In the shop, it is usually feasible to place thermocouples on the hot surfaces of the
linings. These thermocouples should be used to control the dryout operation. A suit-
able “thermal curing” burner with adequate heat release is essential. In all cases, air
flow is extremely important. A cover plate, or damper, should be installed at the
equipment or vessel outlet for adjustment of hot flue gas flow.

2746 Field Dryout

It is very difficult to meet the dryout schedule and to hold temperatures constant
under field conditions. As an example, if you are drying out a fired heater by using
an existing burner(s), the temperature gradient throughout the heater may be signifi-
cant. In cases like this it may be better and less time consuming to contract the
dryout work to a firm which has the proper equipment. If practical, thermocouples
should be installed and connected to a field readout monitor after the refractory is
installed. These thermocouples must be tested prior to starting dryout so you know
they work and are accurate.
During dryout it is common to see a pattern of small (1/16-inch wide) cracks
develop in a monolithic refractory lining. These cracks are an expected result of
shrinkage and should not be considered a problem.

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2700 Curing and Dryout Insulation and Refractory Manual

2747 Adjustment of Normal Dryout Procedure

A few situations call for the normal dryout procedure to be modified. These situa-
tions develop from the following:
• Water washing of equipment in the early stages of an FCCU shutdown
• Hydrostatic testing of refractory-lined vessels
• Hydroblasting of a tube coil or other equipment during a shutdown
• Formation of ice crystals in linings (caused by sub-freezing weather during a
shutdown)
Except for the case of ice crystals, only minor modifications, if any, of the normal
dryout-startup procedure are needed to compensate for the extra water absorbed
into the lining. For example, if the normal startup procedure for an FCCU uses a
heating rate of about 100°F/hr with a hold period when torch oil is added, no extra
precautions are recommended. If the normal startup procedure is faster than that,
we recommend allowing a little extra time to dry out the lining.
If ice crystals have formed in the lining (ambient temperatures below 32°F), more
stringent precautions are required. Rapid heating of the lining must not occur until
all ice has been converted to water. (See Section 7 of IRM-MS-4786.)
Also, water washing of refractory linings should not start until the hot face tempera-
ture is below 350°F. This delay is rarely a problem, because most washing is done
by workers inside the unit which must be cool enough for personnel entry.
Rheniformer Lining with Shroud. No adjustment of the normal dryout schedule
is needed. The recommended schedules are conservative enough that the presence
of a stainless steel shroud has no practical effect on dryout.

March 1995 2700-8 Chevron Corporation