Original Article

High Performance Polymers

2014, Vol. 26(8) 900–905
Synthesis of polystyrene nanolatexes via ª The Author(s) 2014
Reprints and permission:

emulsion polymerization using sodium sagepub.co.uk/journalsPermissions.nav

DOI: 10.1177/0954008314533979
hip.sagepub.com
dodecyl sulfonate as the emulsifier

Liyan Yang and Yangchuan Ke

Abstract
Polystyrene (PS) nanolatexes were successfully prepared via emulsion polymerization using sodium dodecyl sulfonate as the
emulsifier. The effects of emulsifier concentration, initiator concentration, polymerization reaction time, and polymerization
reaction temperature on particle size and size distribution of PS colloidal spheres were investigated, respectively. The
particle size of the diluted polymer emulsion was about 20 nm, as determined by laser scattering. These obtained PS particles
were also characterized using Fourier transform infrared spectroscopy and scanning electron microscopy.

Keywords
Polystyrene nanolatexes, emulsion polymerization, sodium dodecyl sulfonate

Introduction Suspension polymerization is a kind of precipitation poly-

merization. Kim et al16 synthesized PS particles by the
Polymer nanoparticles (PNPs) have attracted much atten-
reverse iodine transfer polymerization -suspension polymer-
tion over recent decades in the field of material and colloi-
ization ranging approximately from 100 nm–200 mm with
dal science. During the past decades, PNPs are widely used in
broad size distribution. Although this system uses water as
many fields, such as electronics, paint coatings, optics, cata-
polymerization medium which is nonflammable and non-
lysis, diagnostics, therapeutics, and so on.1–6 These particles
toxic, the average particle diameter and the size distribution
can be made from large numbers of materials, such as metals,
of PS particles are large, broad, and polydisperse. Microe-
metal oxides, inorganic materials, polymeric materials, and mulsion polymerization is a new and effective approach for
so on.7–10 The diameter of these particles can range from sev-
preparing nanoscaled polymer particles and has attracted
eral to several hundreds of nanometers. Among these parti-
significant attention. However, the commercial use of this
cles, polystyrene (PS) nanolatexes are one of the most
process has been limited because typical polymer formula-
promising materials due to their monodispersity, strong
tions are diluted and require a large ratio of surfactant com-
adsorption ability, uniform particle size, large specific surface
pared with monomer. The surfactant concentrations usually
area,11–14 and so on. More and more attention has been paid to
exceed the amount required for polymer stability.21
the study of PS in many countries.
To overcome the disadvantages as mentioned previ-
Several methods for production of the PS nanolatexes ously, emulsion polymerization is generally used to prepare
have been developed, such as emulsion polymerization,
PS nanoparticles.15 Over the past decades, emulsion poly-
suspension polymerization, microemulsion polymeriza-
merization has been used for the production of polymers.
tion, cationic polymerization, and dispersion polymeriza-
To date, it is employed for the polymerization of a variety
tion.15–19 In general, dispersion polymerization technique
has been widely used to produce monodisperse micron-
sized polymer particles directly in the size range of approx-
imately 0.5–20 mm. Hou et al.20 synthesized five kinds of State Key Laboratory of Heavy Oil Processing, College of Science, China
PS microspheres of approximately 4–6 mm in diameter University of Petroleum, Beijing, China
bearing different surface functional groups by dispersion
Corresponding author:
copolymerization of styrene and various vinyl comono- Yangchuan Ke, State Key Laboratory of Heavy Oil Processing, College of
mers. Although this method is simple and practicable, the Science, China University of Petroleum, Beijing 102249, China.
average particle diameter of the copolymer is large. Email: kyc01@sohu.com
Yang and Ke 901

of monomers such as styrene, graphene, methyl metacry-

late, isoprene, butadiene, and so on.22–24 Emulsion poly-
merization is the most successful industrial methods.
Regarding the most commonly used organic solvent-
based systems, water as polymerization medium exhibits
unique properties such as high heat capability and high
polarity.25 Generally, high-molecular-weight polymers and
narrow size distribution particles are easy to be obtained in
emulsion polymerization.26,27 Recently, the micro-sized PS
nanoparticles were successfully prepared by emulsion
polymerization and the average diameter is 60 nm.15 Kim
et al.28 synthesized unmodified and modified PS nanoparti-
cles with hydrophilic end group on surface by emulsion
polymerization for adsorption of a protein (immunoglobu-
lin G, IgG). The presence of formed IgG-PS particle com-
plex was confirmed by dynamic light scattering
measurement which shows the increased size of particle
(approximately178 and 220 nm) after IgG immobilization.
Therefore, emulsion polymerization has been widely
applied in the design and preparation of functional polymer
materials with special function, such as block copolymers,
surface-modified emulsion, and responsive particles, or
with fancy morphologies such as core–shell structure parti-
cles and natural material-coated emulsions. 29–32
In this study, small-sized PS nanolatexes with uniform
distribution via emulsion polymerization using sodium
dodecyl sulfonate (SDSN) as the surfactant have been suc-
cessfully prepared. The effects of emulsifier concentration,
initiator concentration, polymerization reaction time, and
polymerization reaction temperature on particle size and
size distribution of PS colloidal spheres were investigated,
respectively. The particle size of the diluted polymer emul-
sion was about 20 nm, as determined by laser scattering.
These obtained PS particles were also characterized by
Fourier transform infrared spectroscopy (FTIR) and scan-
ning electron microscopy (SEM).
Experimental
Materials
Styrene (St) from Tianjin Guangfu Chemical Reagents
Company (China) was vacuum distilled to remove trace
inhibitor prior to use. Divinylbenzene (DVB), SDSN, and
potassium peroxydisulfate (KPS) from Beijing Chemical
Reagents Company (China) were used as received.
Synthesis of the PS nanospheres
H
CH CH2
SDSN, initiator C CH2
n
water, 70°C
O O
S
SDSN: O O– Na+
Figure 1. Chemical reaction and the chemical structure of the
emulsifier.
Typically, the emulsifier was dissolved in deionized water
in a 250-mL flask and agitated at around 400 r min1 with a
magnetic stirrer for 15 min. A condenser pipe was used to
prevent evaporation during polymerization. After homoge-
nization, the solution was purged with nitrogen (N2) for 45
min to remove the dissolved oxygen; meanwhile, the reac-
tor temperature was brought to 70 C. St monomer, DVB,
and KPS were added into the reaction system under N2
protection. Afterward, the system was obturated, and the
solution was stirred for 16 h. Then, the solution was natu-
rally cooled and demulsified by the addition of alcohol;
finally, the PS nanospheres were collected and washed
three times with deionized water and then dried at 50 C
in the oven for 24 h. PS spheres of different particle sizes
were synthesized by changing the experiment conditions.
The emulsion polymerization mechanism follows Harkins
theory.33 The chemical reaction and the chemical struc-
ture of the emulsifier is shown in Figure 1.
Characterization
The PS particle size and size distribution were determined
by laser scattering using a Malvern Mastersizer 2000
(Malvern Instruments, Malvern, UK) at 25 C. Before
analysis, the latexes were diluted with deonized water to
minimize the particle–particle interactions. The determina-
tion of PS size and size distribution is derived from Eshuis
et al.34 The number-average, volume-average, and weight-
average diameters (i.e., Dn, Dv, and Dw, respectively) are
defined as usual.35 If one were to assume a single-sized pop-
ulation following a Gaussian distribution, then the polydis-
persity index (PDI) related to the standard deviation () of
the hypothetical Gaussian distribution is shown below:
P 
Ni Di
Dn ¼ P ð1Þ
Ni

PS nanolatexes were successfully prepared via emulsion P 1=3

Ni D3i
polymerization. A typical emulsion recipe, consisting of Dv ¼ P ð2Þ
Ni
0.1 wt% SDSN, 0.01 wt% KPS, 0.01 wt% DVB, 20 mL
St, and 100 mL water, was employed. It was performed P 1=3
in a three-necked flask immersed in an oil bath controlled Ni D6i
Dw ¼ P ð3Þ
at 70 C. KPS was selected as a water-soluble initiator. Ni D3i
902
35
30
Dv (nm)
25
20
15
0.1 0.2 0.3 0.4 0.5 0.6
SDSN (wt%)
Figure 2. Effect of SDSN concentration on volume–average
particle diameter of polystyrene nanolatexes. A nonlinear
decrease in particle size was observed with increasing concen-
tration of SDSN, meanwhile, initiator concentration and volumes
of styrene and of aqueous continuous phase were kept constant.
SDSN: sodium dodecyl sulfonated.
2
PDI ¼ ð4Þ
ZD2
where Ni is the number of particles having diameter Di.
FTIR spectra of PS nanolatexes were obtained using an
FTS-3000 spectrophotometer (Digilab Inc, Marlborough,
MA, USA). FTIR spectra were obtained at wave numbers
ranging from 4000 cm1 to 400 cm1. The measured wafer
was prepared by potassium bromide (KBr) pellet with a 1/
100 weight ratio of sample to KBr. The resolution was set
at 2 cm1 for all measurements.
SEM analysis was measured using a field-emission
scanning electron microscope Quanta 200F(FEI Corpora-
tion, Hillsboro, Oregon, USA) with an accelerating voltage
of 20 kV.
Results and discussion
Effect of reaction conditions on particle size of PS
nanolatexes
Effect of SDSN concentration. As is well documented, particle
size decreases with increasing emulsifier concentration.36
Figure 2 demonstrates the effect of SDSN concentration
on Dv of PS nanolatexes. Variation of SDSN concentration
was found to be an effective method for obtaining average
diameters in the range of approximately 10–30 nm, while
keeping constant initiator and total monomer concentration.
Dv of PS nanolatexes curve shows that with an increas-
ing SDSN concentration, the volume-average particle size
decreased. This can be attributed to variations in the num-
ber of the loci. A higher concentration of surfactant gener-
ated and stabilized larger number of PS nanolatexes; the
High Performance Polymers 26(8)
27
26
25
Dv (nm)
24
23
22
21
20
0.01 0.02 0.03 0.04 0.05 0.06
KPS (wt%)
Figure 3. Effect of KPS concentration on volume–average parti-
cle diameter of polystyrene nanolatexes. A nonlinear decrease in
particle size was observed with increasing concentrations of KPS,
meanwhile, surfactant concentration and volumes of styrene and
aqueous continuous phase were kept constant. KPS: potassium
peroxydisulfate.
speed of reaction also accelerated. However, when the
SDSN concentration was higher than 0.4 wt%, reaction rate
and viscosity of the system increased rapidly, some PS
nanolatexes coalesced into larger particles, and the particle
size did not decrease but rather increased slightly.
Effect of KPS concentration. The effect of KPS concentration
on Dv of PS nanolatexes is shown in Figure 3. The curve
shows that with an increasing concentration of KPS, from
0.01 wt% to 0.04 wt%, based on monomer weight, the Dv
of PS nanolatexes decreased. This result can be explained
as follows: higher initiator concentration generated more
free radicals and formed more activated micelles. More-
over, the decomposition of initiator can play a part in in situ
co-emulsifying effect. In addition, increasing the concen-
tration of KPS enhanced the in situ co-emulsifying effect
and stabilized the formed particles easily. However, when
the KPS concentration was higher than 0.04%, Dv of PS
nanolatexes increased slightly. This is because the emulsi-
fier in the system could not stabilize such more free radicals
simultaneously generated by higher initiator concentration
and increased the probability of aggregation. Thus, the par-
ticle size increased.
Effect of polymerization reaction time. Figure 4 exhibits the
effect of reaction time on Dv of PS nanolatexes; mean-
while, other parameters are fixed. Clearly, the particle size
grows as the polymerization time increases.
From Figure 4, the reaction can be divided into three
stages. In the first stage, more polymer nuclei are rapidly
produced, and the system becomes unstable. In the second
stage, they gradually come together to form larger size par-
ticles and increase to 20.62 nm average within 6 h. In the
Yang and Ke 903

25 35

20
30

15
Dv (nm)

Dv (nm)
25
10

20
5

0 15
0 2 4 6 8 10 12 14 16 18
60 65 70 75 80
t (h)
T (°C)
Figure 4. Effect of polymerization reaction time on volume–
Figure 5. Effect of reaction temperature on volume–average
average particle diameter of polystyrene nanolatexes.
particle diameter of polystyrene nanolatexes.

Table 1. Average particle size of polystyrene nanolatexes via emulsion polymerization with different emulsifier concentration.

Concentration (wt%) Dn (nm) Dw (nm) Dw/Dn PDI (101)

0.10 28.42 27.59 1.03 0.72

0.20 26.53 26.01 1.02 0.57
0.30 22.47 21.61 1.04 0.39
0.40 20.39 20.19 1.01 0.25
0.50 23.72 23.25 1.02 0.46
0.60 28.67 27.84 1.03 0.83
Dn: number-average diameter; Dw: weight-average diameter; PDI: polydispersity index.

last stage, as the reaction time increases, the growth of the

polymer sphere particle size almost never changes.
Effect of polymerization reaction temperature. The relation
2844.5

1604.5
Transmittance (%)

between the particle sizes of PS nanolatexes and reaction

3446.2

752.1
temperature of the system is illustrated in Figure 5. It is
1452.2
3027.7

1492.7
2921.7

clear that Dv of PS decreases with the increasing tempera-

ture at first and then increases when the temperature is
higher than 70 C. The reason is that when the temperature
was higher than 70 C, the decomposition rate of initiator
increased, and the stability of PS nanolatexes decreased.
Particles should gather together to improve the surface
698.1

charge density so as to improve the stability of PS nanola-

texes. The aggregation of PS nanolatexes generated more
4000 3500 3000 2500 2000 1500 1000 500
number of larger size particles. Thus, the optimal reaction
Wavenumber (cm–1)
temperature is 70 C.
Particle size distribution of PS nanolatexes. The particle size Figure 6. FTIR spectra of the polystyrene spheres. FTIR: Fourier
transform infrared.
distribution of PS nanolatexes was measured by Malvern
Mastersizer 2000 (Malvern Instruments). The particle size
of PS nanolatexes via emulsion polymerization with differ- FTIR analysis. Figure 6 illustrates the IR absorption spectra
ent emulsifier concentration was measured and is listed in of the PS spheres. Obviously, there are several absorption
Table 1. From Table 1, it can be seen that Dw/Dn < 1.05, peaks within the involved wave number range. The absorp-
indicating that PS nanolatexes are of narrow and small size tion bands at 3027.7 and 2921.7 cm1 correspond to aro-
distribution. matic C–H stretching vibration absorption, and there are
904
Figure 7. SEM images of polystyrene nanoparticles with different emulsifier concentration (a) 0.4 wt% SDSN and (b) 0.6 wt% SDSN.
SEM: scanning electron microscopic; SDSN: sodium dodecyl sulfonated.
three absorption peaks at 1604.5, 1492.7, and 1452.2 cm1
that correspond to aromatic C¼C stretching vibration
absorption. These absorption peaks indicate the existence
of benzene rings. The absorption peaks at 752.1 and
698.1 cm1 correspond to C–H out-of-plane bending vibra-
tion absorption and indicate that there is only one substitu-
ent in the benzene ring. Figure 6 also shows the absorption
peaks at 2921.7 and 2844.5 cm1, corresponding to the
existence of methylene. In addition, the absorption peaks
at 3446.2 cm1 correspond to O–H stretching vibration
absorption indicating the existence of hydroxyl.
These FTIR results have confirmed that the polymeriza-
tion reaction of St has occurred. There is no absorption peak
at approximately 1680–1620 cm1 or 970–800 cm1corre-
sponding to olefin C¼C stretching vibration absorption or
olefin hydrogen bending vibration, which is a further indica-
tion that the polymerization reaction occurred. Obviously,
FTIR characterization results of PS are in accord with the
standard spectrum diagram indicating that the product is
pure PS.
SEM morphology. The SEM images of PS nanolatexes with
different emulsifier concentration are shown in Figure 7.
It is confirmed that PS nanolatexes with uniform size
were successfully prepared via emulsion polymerization.
In Figure 7(a), the nanospheres were perfect spheres with
a very smooth surface and well dispersed. Figure 7(b) indi-
cates that when the emulsifier concentration was 0.6 wt%,
higher than 0.4 wt%, some PS particles aggregated to gen-
erate larger particles, and the particle size distribution was
not homogenous anymore.
Conclusions
PS nanolatexes were successfully prepared via emulsion
polymerization using SDSN as the emulsifier. The effects
of emulsifier concentration, initiator concentration, poly-
merization reaction time, and polymerization reaction tem-
perature on particle size and size distribution of PS
High Performance Polymers 26(8)
colloidal spheres were investigated, respectively. The par-
ticle size of the diluted polymer emulsion was about 20
nm, as determined by laser scattering. These obtained PS
particles were also characterized by FTIR and verified that
the polymerization reaction of St occurred. SEM results
also showed that the nanospheres were perfect spheres with
a very smooth surface and were well dispersed.
Funding
This report was supported by National Major Project
(2011ZX05009-005), Financial Supports of Forward-Looking
Guidance Project of China University of Petroleum (Beijing)
(QZDX-2010-04), Natural Science Foundation of China (no.
21076229), PRP/open-1105, the Foundation for Innovative
Research Groups of the National Natural Science Foundation of
China (grant no. 51221003), and Science Foundation of China
University of Petroleum, in Beijing (no. KYJJ2012-06-30).
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