4 Dissertation
4 Dissertation
4 Dissertation
INTRODUCTION
Thin film Intumescent coatings are increasingly used because they provide a high
standard of finish, quality and reliability. They can be applied on or off-site and can be
used on structures to provide protection for the steel. These coatings are from organic
materials and are inert at low temperatures[1]. They swell (or intumesce) to provide a
charred layer of low conductivity foam when exposed to high temperatures[1]. This char
layer reduces the rate of temperature rise in the steel and prolongs the steels load bearing
capacity[1]. Intumescent coatings foam and bubble when subjected to high temperatures
and create multicellular cushions which prevent (a) heat from penetrating into the
substrate and (b) flames from spreading along the surface. [2]
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Figure 1: Swollen intumescent coating[2]
1.1.1 GLASSWOOL
Glasswool is an insulating material, made from fibre glass, arranged into a texture
similar to wool. Glass wool is produced in rolls or in slabs, with different thermal and
mechanical properties. Glasswool is a thermal insulation that consists of intertwined and
flexible glass fibres, which causes it to "package" air, resulting in a low density that can
be varied through compression and binder content. It can be a loose fill material, blown
into attics, or, together with an active binder sprayed on the underside of structures,
sheets and panels that can be used to insulate flat surfaces such as cavity wall insulation,
ceiling tiles, curtain walls as well as ducting. It is also used to insulate piping and for
soundproofing[11].
1.1.2 ROCKWOOL
Rockwool products are robust insulation material suitable for hot surfaces up to 650°C.
Rockwool are made from long fine fibres spun from natural rock bonded with a
thermosetting resin. Rockwool products are easy to install and they come in the form of
blankets, slabs and pipe sectionals.
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1.2 Problem statement
Most structures are steel-based structure. Intumescent coatings are used to protect these
structures from the damage of fire. The basic intumescent coating is quite fragile and
cannot stand high temperature. Rockwool and glasswool are two high temperature
resistance materials. Incorporating these fibers into intumescent coating might improve
thermal performance of the coating. However, appropriate fiber content is among the
key element of an effective coating fiber.
SCOPE OF STUDY
a) Research on the formulation of the intumescent coating, glasswool and rockwool
b) Study on the composition of intumescent coating with glasswool and rockwool
c) The samples will gone through laboratory test to obtain its thermal performance
d) Analysis will be done due to the data attained
e) Report of the project is then been established based on the result gained
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CHAPTER 2
LITERATURE REVIEW
Components;
Ammonium Polyphosphate (APP) as the acid source
Melamine (MEL) as the blowing agent
Pentaerythritol (PER) as the carbon agent
Hardener
Epoxy resin
Boric acid
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The mechanism of intumescence is usually described as follow;
1) Acid source breaks down to yield a mineral acid
2) Then it takes part in the dehydration of the carbonization agent to yield the
carbon char
3) Blowing agent decomposes to yield gaseous products
4) The latter causes the char to swell and hence provides an insulating multicellular
protective layer
5) This shield limet the heat transfer to substrate and the mass transfer from the
substrate to the heat source resulting in a conservation of the underlying material
[6]
The invention features a fire-retardant and heat-resistant coating applied by first coating
the surface to be protected with a protective composition comprising (1) an intumescent
paint consisting essentially of a volatile liquid vehicle, 35 to 150 parts by weight of a
resinous film-forming binder, and 120 to 475 parts by weight of a solid spumific agent
which when heated to 400°C causes a dried film of the paint to increase in thickness at
least 4 times, and (2) 2 to 30% by weight (exclusive of the weight of any organic
coating on the fibers), based on the remaining ingredients of the paint, of glass fibers;
and overlaying this protective composition with a protective layer comprising a flexible,
surface-conformable fabric sheet, e.g., a textile fabric, having sufficient strength and
permeability to unite with a paint applied therewith. The coating may be dried either
before or after applying the protective layer. In preferred embodiments, this protective
layer may consist of an incombustible fabric, such as fiber glass cloth; a combustible
fabric coated with an overcoating of intumescent paint; or an incombustible fabric
coated with an overcoating of intumescent paint. The overcoating intumescent paint
may, but need not also be combined with glass fibers. Also, 10% or more of the fibers in
the protective composition may be glass fibers precoated with polyvinyl chloride. [3]
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2.1.2 GLASSWOOL
Centrifugal glass wool is a silk-like material made by fiberization and spraying of
thermosetting resin. Glass wool is non-combustible, non-toxic, and resistant to
corrosion. It has low weight by volume, low thermal conductivity, stable chemical
property, and low moisture absorption rate due to its excellent hydrophobicity. Due to
its intertwined flexible fibers, glass wool is the best insulating material against noise,
cold and heat and also offers excellent fire-resistant properties. The panel, felt, and pipe
products made of glass wool have been used in the industries of construction, chemical,
electronic, energy, metallurgy and communication[13].
The basic raw materials are natural sand, to which recycled glass and fluxing agents like
soda ash are added. Use of recycled glass coming from buildings flat glass, car glass and
containers, is steadily increasing. Its share may represent up to 80 % of the batch. Glass
batch is made of ground particles with a very precise sieve analysis. In addition, the mix
of components is quite accurate in order to get an homogeneous batch to be melted in an
optimal way[14].
2.1.3 ROCKWOOL
In the other hand, one of the most vital properties of Rockwool is its ability to withstand
temperatures of more than 1000°C. Properly used, Rockwool acts as a fire resistant
barrier, which can provide those vital extra minutes for rescuing people.
This insulating material is made from waste products namely, bottom ash, cement kiln
dust, slag, and waste from mineral wool production. These materials, along with a
binder, are homogenized into a mixture. Thereafter, the process includes briquetting the
mixture into agglomerated pieces. The agglomerates are then melted in a cupola furnace
and the molten agglomerate is discharged into a receiver. Hot combustion gases are then
passed into the melt or molten agglomerate to chemically homogenize the melt and heat
the melt to a preselected temperature. Thereafter, the melt is converted into fibers using
conventional practices[4]. The final product is a mass of fine, intertwined fibres with a
typical diameter of 6 to 10 micrometers. Rockwool may contain a binder, often food
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grade starch, and an oil to reduce dusting. Though the individual fibres conduct heat
very well, when pressed into rolls and sheets their ability to partition air makes them
excellent heat insulators and sound absorbers[11].
The paper demonstrates the benefits of Lapinus' fibres when used in simplified
intumescent coating formulations and their effect on the performance and hence the
protective efficiency of said coatings.
7
The figures show the influence of the presence of Lapinus' fibres on the protective
properties of the char layer of both PVA based system and a 2K epoxy system. Not only
does the temperature of the substrate remain lower for a longer period of time (up to
more than 120 min for the 2K epoxy) when fibres are used, but also the strength of the
char layer is improved which is beneficial for the performance during raging fire. The
results obtained with Lapinus' fibres are better than the results obtained with the
competitor fibre type.
It is shown that the performance of both a waterborne PVA and 2K epoxy based
simplified
intumescent coating can be improved using Lapinus' fibres:
• The temperature reached at the coating/ substrate interface is lower and remains lower
when Lapinus' fibres are used. The most suitable fibre grade depends on the binder
used;
• The strength of the char layer is increased, while the integrity remains. As a result, the
char
layer is more stable and longer lasting (> 120 min) compared to the other tested systems.
- From the research paper above, it is proven that the addition of fibre into the
intumescent coating will improve the performance of intumescent coating in
term of thermal performance. Briefly explaining, Lapinus Fibres is the world's
largest producer of precision-engineered mineral fibre products.
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2.1.5 THERMAL PERFORMANCE TEST STANDARD
The thermal performance test that will be going through to test the intumescent coatings
resistance to fire resembles the standardized test from ASTM Standard.
The test will obey the Standard WK12643, Test Method for Slug Calorimetry. The
proposed standard is under the jurisdiction of Subcommittee E37.05 on Thermophysical
Properties.
From the above picture, assembled slug calorimeter specimen ready for testing in the
furnace. The coating shown is an organic intumescent material, surrounded by a high
temperature microsilica thermal insulation, with the assembly being held together by
two retaining plates.
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Below is the figure that shows the cone calorimeter. Cone calorimeter resembled the
usage of bunser burner for direct burning.
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CHAPTER 3
METHODOLOGY
Make analysis and discussions with the reference to the data gained
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3.3 SAMPLE PREPARATIONS
Weighted stirring
Epoxy-hardener
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3.4 SAMPLE ANALYSIS
The development of the Scanning Electron Microscope in the early 1950's brought with
it new areas of study in the medical and physical sciences because it allowed
examination of a great variety of specimens.
As in any microscope the main objective is for magnification and focus for clarity. An
optical microscope uses lenses to bend the light waves and the lenses are adjusted for
focus. In the SEM, electromagnets are used to bend an electron beam which is used to
produce the image on a screen. By using electromagnets an observer can have more
control in how much magnification he/she obtains. The electron beam also provides
greater clarity in the image produced.
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3.4.2 THERMAL TEST
To test the performance of the intumescent coating applied, the mild steel
substrate coated with applied intumescent coating will be fired up using Bunsen burner.
At the same time, a digital thermocouple will be attached at the opposite side of the
substrate to take the value of temperature vs. time. Here is the setup:
Figure 6: Direct burning setup for measuring the temperature of back steel
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CHAPTER 4
RESULTS AND DISCUSSION
Table 3 shows the results of the height before the fire burning test. While Table 3 shows
the results of the samples height after the fire burning test. From the results gained, the
best sample is determined.
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Table 3: Height before burnt
Samples h1 (mm) h2 (mm) h3 (mm) h4 (mm) h5 (mm) h6 (mm) Avg (mm)
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Table 4: Height after burnt
Samples h1 (mm) h2 (mm) h3 (mm) h4 (mm) h5 (mm) h6 (mm) Avg (mm)
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Before burning test samples
Note:
*the dimension for the steel plate is 5mm x 5mm
*only for direct burnt test, 10mm x 10mm steel plate being used
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FORMULATION 3
Fig.10: N3
FORMULATION 4 Fig.11: N4
FORMULATION 5 Fig.12: N5
FORMULATION 6 Fig.13: N6
FORMULATION 7 Fig.14: N7
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FORMULATION 8 Fig.15: N8
FORMULATION 9 Fig.16: N9
FORMULATION 12
Fig.19: N12
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FORMULATION 13 Fig.20: N13
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4.1.2 SCANNING ELECTRON MICROSCOPE (SEM) FOR NORMAL
FORMULATION
Fig. 21 and 22 are the SEM image of the normal formulation chosen, formulation N8.
Fig.21(a) & (b) shows its outer image. There are some pores seen. Fig. 22(a) & (b)
shows the inner image of N8 samples, which we can see there are many flakes there.
N8
Fig. 21: (a): Outer image-magnification 100; (b): Outer image-magnification 300
Fig. 22: (a): Inner image-magnification 100; (b): Inner image-magnification 300
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4.1.3 RESULTS & DISCUSSION OF FIBRE REINFORCED INTUMESCENT
COATINGS
Table 6 and 7 shows the results of the samples reinforced glasswool and rockwool with
its description. For glasswool samples, the swelling is quite good, yet some of the
samples are not uniformly swell. In the other hand, for rockwool samples, the there are
not much swell as compared with the glasswool samples, but the chat is quite hard and
not easily broken.
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Table 8: Intumescent coating with reinforced rockwool
Formula Fibre Height Description Top view Cross section
-tion percent- Before After
age (%) burnt burnt
R0.5 2.08 2.35 6.63 Not swell Fig.26: R0.5
much, hard,
not smooth
outer layer
R0.24 1 2.41 7.02 Swell a bit Fig.27: R0.24
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4.1.4 SCANNING ELECTRIC MICROSCOPE (SEM) FOR FIBRE
REINFORCED INTUMESCENT COATINGS
As can be seen from the SEM results of the intumescent coatings reinforced fibres as
compared to the normal formulations, the fibre are strongly attached with the
intumescent formulation, resulting in a better coatings’ char, providing a better layer to
protects from fire attack.
R0.5
Fig. 29: (a): Outer image-magnification 100; (b): Outer image-magnification 300
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G0.5
Fig. 31: (a): Outer image-magnification 100; (b): Outer image-magnification 300
Fig. 32: (a): Inner image-magnification 100; (b): Inner image-magnification 300
26
G0.24
Fig. 33: (a): Outer image-magnification 100; (b): Outer image-magnification 300
Fig. 34: (a): Inner image-magnification 100; (b): Inner image-magnification 300
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4.1.4.1 ANALYSIS AND DISCUSSION FOR SEM
Samples N8 R0.5 G0.5 G0.24
Characteristics
Outer char Smooth outer Smooth outer A lot of pores A lot of pores
char layer, not char layer, not and fibres
much pores much pores
Inner Char A lot of flakes Lesser flakes Lesser flakes Much flakes
than N8 and a than N8 and a than R0.5 and
lot of fibres lot of fibres G0.5, but
lesser fibre
Viscosity Low viscosity, Less than Very high Less than
easy to apply G0.5, not too viscosity, G0.5
hard to apply sticky and
very hard to
apply
The charring layer protects the matrix materials, and its protective property depends on
the physical and chemical structure of the charring layer. Researches indicate that there
are other elements in the charring-layer structure. But the non-charring element is easy
to be oxygenated and very unstable on chemistry aspects. There are two ideal typical
charring structures listed as follows. There are a great deal of integrated closed
honeycomb pores in Fig. 6(a); such structure can form adequate temperature grads in the
charring layer and protect the molten mass and matrix below. But the other structure is
nonideal; there are many channels and apertures, and the gas and molten mass of
polymers can overflow to the entry of the flame-region. Thus the isolation effect of heat
transfer is inferior [8]. The physical structure of the charring layer plays a very
important role in the performance of the flame retardant [8]. The formation of the final
charring layer and their morphological structures is studied by SEM. If the structure of
the charring layer inclines to be more compact and more homogeneous, the intension of
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charring layer improves largely, and the effect of the flame retardant is better. The
irregular mini-pore structures of spongy foams in the charring layer explains the
dehydration charring of PER and frothing of Mel proceeds in the range of rather
appropriate temperature. Moreover, the intumescent layer is compact and spongy, and
the heat insulation effect. The different aperture surface tensions in the course of gas
cavities lead to the asymmetry of abscess, and the surface tension relies on the viscosity
and symmetry of the coating. The intumescent charring layer with many mini-pores acts
as the effect of the flame retardant, heat insulation and protecting inner matrix materials.
Direct fire test, using Bunsen burner is used to determine the value of back steel during
the burning. The temperature data taken using digital thermocouple.
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R0.5 TEMPERATURE vs. TIME
300
250
200
Temperature
150
(°C)
100
50
0
0 10 20 30 40
Time (min)
30
G0.24 TEMPERATURE vs. TIME
250
200
Temperature 150
(°C) 100
50
0
0 20 40 60 80
Time (min)
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4.1.5.1 ANALYSIS AND DISCUSSION
From the direct fire test, the back steel temperature of sample N8 is proved to have the
highest value of temperature when directed with fire. The intumescent coating
reinforced rockwool and glasswool have a better resistance to fire, therefore protects the
steel from high temperature. From the graph of sample N8, it is shown that the value of
temperature of the back steel plate is higher than 300°C in average. As compared with
reinforced intumescent coatings, those are having quite low value of back steel
temperature which is mostly below 300°C. From the experiment done, the best
formulation is formulation G0.24. It has good structure inside and out, and easier to
apply as compared with G0.5 which is quite sticky.
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CHAPTER 5
Conclusion and recommendation
5.1 CONCLUSION
Intumescent coating consists of 3 main components which are acid source, carbon
source and blowing agent. The right amount of those 3 components results in a good
sample of intumescent coating. Other than that, fibre reinforcement is a good way in
improving the intumescent coating. The fibre which is having high thermal resistance
somewhat is a medium for the coatings components to attached and bonded with. The
fibre makes the char structure tougher. Different fibre has different properties. In this
project, two different fibres are used; rockwool and glasswool. Rockwool has a higher
density value as compared to glasswool. So, it is quite hard to apply the intumescent
coating reinforced glasswool of higher amount as compared to rockwool. The best
formulation is formulation G0.24 as it has good structure inside and out, and easier to
apply as compared with G0.5 which is quite sticky. In direct fire test also, it has quite
good resistance to fire.
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5.2 RECOMMENDATION
i. instead of using Bunsen burner which result in not uniform result, a proper
calorimeter should be prepared to obtain the back steel temperature of the
sample.
iii. APP, PER and MEL are the common basic components for acid source, carbon
source and blowing agent. More research can be done to obtain a better
component to replace those remaining components for a better improvement in
intumescent coatings
iv. Other tests like DSC and TGA can be done to study more on the thermal
performance of the intumescent coatings.
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APEENDIXES
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REFERENCES
[1] Intiumescent Coating, Structural Fire Design: Off-site Applied Thin Film
Intumescent Coatings (2nd ed), SCI P160,The Steel Construction Institute. 2007
[2] Intumescent coatings and their uses, J. A. Rhys, Fire and Materials, 2004
[4] Controlled process for making a chemically homogeneous melt for producing
mineral wool insulation, United States Patent 4617045
[6] Development of Intumescent Formulations for Fire Protection in Oil and Gas
Industry, Mohd Halim Hasni b Hasan
[7] Relative Short Fibre Content Measurement Using Premier aQura and its Influence
on Yarn Quality, By: Mr. V.Srinivasan, Head BU-Lab, Premier Evolvics Pvt Ltd
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Internet sources:
[10] http://www.astm.org/SNEWS/DECEMBER_2006/slug_dec06.html
[11] http://en.wikipedia.org
[12] http://www.refracon.com.my
[13] http://www.tlimpex.com/glasswool.html
[14] http://www.isover.co.uk/about_glasswool.asp
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