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Microencapsulation of

n-hexadecane phase change


material by ethyl cellulose polymer

Hasanah (15020013)
Jantera Sekar Tirta (15020016)
Juan Prianto (15020017) 3K1 & 3K2
M. Ihsan Damhury (15020019) Textile Chemistry
M. Nur Hasan (15020043) Politeknik STTT Bandung

POLYMER BULLETIN (ISSN: 0170-0839) 71(12): 3289-3304 (2014)


DOI: 10.1007/s00289-014-1250-y
Introduction
Torza
Loxley
In ourand
andMason
study Vincentbriefly,
EC was [8] with
usedif for
droplets
the difference
of immiscible
embedding that relationship
liquids (phases
n-hexadecane PCMwas
by
1an
given
and for
3) are
onebrought
solid and
emulsion-solvent in two
contact
liquid
with
phases.
a third mutually
evaporation method immiscible
applying
liquid (phase 2),
PVA, Tween 80 the final equilibrium
or PMAA morphology
emulsifiers. can be yield,
Size, morphology,
deduced
PCM
Analyzing bythe
contentdetermining the
and thermal
interfacial various
tension interfacial
properties
between tensions
theof the between
core-oil forming
and the
the phasesaqueous
composite
various (γ12, γ23,were
particles and investigated.
γ13). as well as between the
surfactants
ethyl cellulose n-hexadecane
encapsulating polymer and the emulsifier solutions.

Emulsion-solvent evaporation method

PVA, Tween 80 or PMAA emulsifier


Emulsion-Solvent
Disadvantages Evaporation
Advantages Organic
OrganicPCMMethod
PCM
1. Low thermal
Non-corrosive
Advantages:
conductivities, Disadvantage:
1.
2. Simple
Chemically inert
Flammability 1. High organic solvent
2.
3. Easily
Stablechanges
High up-scalable
in volume
method demand
during phase change.
3.
4. High
Recyclable
yield
4.
5. and
Compatible
encapsulation
with numerous building materials.
efficiency
desirable cohesion
6. A high latent heat per unit weight
7. Low vapour pressure
8. No supercooling
9. Offer congruent melting and self-nucleation.
AnalysisMaterials
ofevaporation
Emulsion-solvent microcapsules
technique
Experiment 1
Yield Content
Thermal Properties
Size
1. Investigation
YieldDichloromethane
Determination
Content of interfacial tensions and spreading coefficients
stirred 150min
200 mg Ethyl
20 ml destilled with 800rpm
2. Emulsion:
Cellulose + 5 ml
Thermal Cycling Tests
filtration
dichloromethane
samples were weighed
Measured by
Stirred atMastersizer rinsing
2000 with
(Malvern
water Instruments,
three times cycled from 5 under
drying atdetermined using a
60°CμDSC3evo
into 100 Polymer
μL
+ 0.52 ml aluminium
gentlystirrer
(400 mg)films Malvern, UK)
magnetic operated distilled
pressed to the
upon water
laser 2 %to 35 °C, with
diffraction
containing a atmospheric
method extracted 3 Setaram
crucibles
n-hexadecane
-Polyvinyl alcohol (Mw=30,000-70,000,
bottom of the crucible
PVA
scanning rate of 0.6
emulsifier
microscope slide, 100 mg of °C/min.
87-90
pressure
times % at hydrolysed),
room
from
the
differential scanning
solution was
microcalorimeter
PCM
(4 % and a 5% (w/v)
rinsing with temperature
performed the
Morphology theInvestigation
warmed by a drying atcooled
(previously
60 down
cleaned
a 3each drained by 1 ml/min
content
solution of
filtration -Tween ethyl 80poly(methacrylic
distilled filtered acid
by sodium salt) (Mw=9500)
micropartic
consecutively
Experiment
cellulose polymer 2 in
Experiment
heating
water 1 °C with
to 9°C
mm bysample
ethanol)
cut-off a was
determination
les by each(five minuteswas )
- and poly(methyl
DCM.) circulator up methacrylate)Peltier (Mw~15,000)
weighed up to 1000 calculated
200 mg Ethyl Experiment 2 filter
20 ml distilled of 5yield
stirred
thermal
ml150min
n- and examined with a
Philips XL-30
Celulose from Sigma to 29 °C element hexane
centrifuging and
+ 5 ml
Melting/freezing Experiment Aldrich
and onset temperatures
3 onto
Stirred
were ata
determined
(Macherey-
by the drying
water
extracted 3 times
with
vacuum-coated
PCM
forcycles
800rpm
content.
3 under
environmental
The results were
redispersing the dropping Nagel containing
at room
640d) 2 %corresponding scanning
a 100 mg of eachby using the
processed
dichloromethane
enthalpies
3. were given
nhexadecane for magnetic stirrer
baseline from the min with
atmospheric
microparticles
+0.26 mlPCM
the total
in
content
(200 mg)
distilledmass of was was grid, purchased
integration method from
TweenMOL
temperature Hungarian
80 melting/freezing
mixture Oil
of goldat
pressure roomand Gas
electron Calisto
thermoanalyzer’s
water
n-hexadecane
microcapsules (EC+HD) microparticles
(Tangential sigmoid surfactantby enthalpies
and palladium sample was microscope
Processing (v1.12)
calculated
Company (Hungary). temperature (ESEM) at
software.25 kV.
baseline type). each 5 ml n-
measured by the
weighed
Experiment 3
4. Ethyl cellulose (viscosity: 4mPa
pendant hexanes, method
drop 5 wt% in 80:20 toluene/ethyl
using an FTA 1000 B dried overnight.
alcohol,
200 mg Ethyl
25 °C) was a kind gift
tensiometer
from
20 ml(First
Dow Ten
distilled
Deutschlandstirred 150min
with 800rpm
Anlagengesellschaft
Celulose
+ 5 ml Stirred at
mbH (Germany)
Angstroms, water
Inc., USA) under
dichloromethane magnetic stirrer
containing 1 % atmospheric
+0.26 ml (200 mg) PMAA pressure at room
n-hexadecane surfactant temperature
SEM observations (Fig. 2 a,c,f) confirmed what has already been pointed out at
Thermal Thermal
laser diffraction measurements:

A.
B. Size, Yield, PCM Content
Properties Properties
Fig. 4 DSC curves of ethyl
Morphology
Fig. 3 DSC curves of n-
cellulose–n-hexadecane hexadecane (A) and ethyl
composites manufactured cellulose-n-hexadecane
by PVA(A), Tween 80 (B) composites manufactured
and PMAA (C) surfactants F. using PVA (B), Tween 80 (C)
G.
after 1000 thermal cycles. and PMAA (D) surfactants.

C.
D.

Fig. 2 SEM images of fractured EC-


Fig. 2 SEM images of fractured EC-
HD microcapsules prepared by PVA
HD microcapsules prepared by PVA
(A), Tween 80 (C) and PMAA (F)
(B), Tween 80 (D) and PMAA (G)
Conclusions
Ethyl cellulose was found to be a suitable polymer to entrap n-
hexadecane phase change material by the emulsion-solvent
evaporation method using PVA, Tween 80 or PMAA emulsifier.
Both theoretically and in the experiments, composites prepared
with PMAA showed the most desirable
properties regarding the size and the latent heat storage
capacity, furthermore, there was no significant temperature
and enthalpy change observed after thermal cycling