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Construction and Building Materials 347 (2022) 128531

Contents lists available at ScienceDirect

Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Effects of the chemical structure of curing agents on rheological properties

and microstructure of WER emulsified asphalt
Yan Kezhen a, b, Shi Junyi a, Shi Kaixin a, Wang Min a, *, Li Goukai a, Hong Zhe a
a
College of Civil Engineering, Hunan University, Changsha 410082, China
b
Key Laboratory for Green & Advanced Civil Engineering Materials and Application Technology of Hunan Province, College of Civil Engineering, Hunan University,
Changsha 410082, China

A R T I C L E I N F O A B S T R A C T

Keywords: Current researches in the pavement engineering field are neglecting the influence of the chemical structure of
Curing agent curing agents on rheological properties of waterborne epoxy resin (WER) emulsified asphalt. The length of
WER molecular chain and the number of active groups will affect the rigidity and flexibility of WER emulsified asphalt.
Emulsified asphalt
In this study, three curing agents (TETA\DETA\593) with obvious differences in molecular chain length and
Rheological properties
Microstructure
number of active groups were selected to modify emulsified asphalt. The three kinds of WER emulsified asphalt
were subjected to the conventional properties, DSR, BBR, SEM and FITR test. The research has found that the
addition of WER system makes emulsified asphalt produce three-dimensional network structure, which signifi­
cantly improves the high-temperature performance and temperature sensitivity of emulsified asphalt. Whereas,
the low-temperature performance of WER emulsified asphalt deteriorates. This indicates that the high-
performance of WER emulsified makes it more suitable for the adhesive of micro surfacing or cold mix
asphalt used in heavy-load traffic in medium and high temperature areas. Curing agent TETA has the greatest
impact on WER emulsified asphalt at high-temperature while 593 has the least adverse influence on the low-
temperature performance. The results demonstrate that the more active groups in the curing agent, the higher
the crosslinking degree and complexity of the three-dimensional network structure in WER emulsified. And it
will lead to the better high-temperature performance of WER emulsified. The longer the molecular chain of
curing agent, the more flexible chains in WER emulsified. And it will lead to better flexibility of WER emulsified.

1. Introduction rubber emulsified asphalt [12]. Additionally, WER-EA is the most

affordable option in terms of the bonding layer of road and bridge deck
1.1. Research background [13,14].

The surge of traffic flow and wheel load has raised the demands of
1.2. Research scope
high-performance asphalt pavement [1–5]. Moreover, to achieve the
goal of peak emissions by 2030 and carbon neutral by 2060, it is
Waterborne epoxy resin (WER) and curing agent are the main
required to increase the service life of asphalt pavement. Thus, relying
components of WER-EA. For WER, it is a stable dispersion system with
on high-performance asphalt material for achieving sustainable devel­
epoxy resin dispersed in water in the form of particles or droplets
opment in pavement engineering field is an important issue to current
[15,16]. On the one hand, WER has the same excellent properties as
study [6]. Previous work has confirmed that waterborne epoxy resin
traditional epoxy resin, such as fantastic adhesion and splendid thermal
emulsified asphalt (WER-EA) not only has high-performance to resist
stability. On the other hand, WER has advantages of low volatile organic
polytropic road diseases [7], but also has a positive effect on environ­
compounds (VOC), low cost, good workability and safety [17]. Previous
mental protection [8–11]. The shear strength and tensile strength of
work has confirmed that WER cured material filled in asphalt with a
WER-EA is superior than styrene–butadienestyrene/styrene–butadiene
three-dimensional structure made asphalt has excellent high-

* Corresponding author.
E-mail addresses: yankz@hnu.edu.cn (Y. Kezhen), SJY@hnu.edu.cn (S. Junyi), wangmin19@hnu.edu.cn (W. Min), lgk@hnu.edu.cn (L. Goukai), hzhe@hnu.edu.cn
(H. Zhe).

https://doi.org/10.1016/j.conbuildmat.2022.128531
Received 14 May 2022; Received in revised form 2 July 2022; Accepted 18 July 2022
Available online 26 July 2022
0950-0618/© 2022 Elsevier Ltd. All rights reserved.
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Y. Kezhen et al.
Fig. 1. Reaction equation of epoxy resin with curing agent.
Fig. 2. The schematic of the cross-linking of WER-EA.
temperature deformation resistance [18,19]. For curing agent, an
indispensable part of WER system, it can react with WER to form the
highly cross-linked three-dimensional reticular spatial structure in
modified asphalt system [20]. The chemical structure of curing agent
determines the chemical and physical properties of epoxy curing prod­
ucts to a great extent. The longer the molecular chain of the curing
agent, the better the adhesion and ductility of the curd WER. The greater
the amount of active hydrogen atoms in the curing agent, the higher its
reaction activity, and the higher the three-dimensional structure cross­
linking degree of the cured WER, which will make the high-temperature
performance of the cured WER better. There are many kinds of curing
agents, among which aliphatic amine curing agents have the advantages
of good miscibility with WER, simple curing process and high-
performance of cured products, which make them the most widely
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Construction and Building Materials 347 (2022) 128531
used in road engineering [21]. The amine/WTR system has higher glass
transition temperature (Tg) and elastic modulus, and lower thermal
expansion coefficient (CTE) [22]. The combination of bisphenol–A WER
and alicyclic amine curing agent has been proved to have the best
comprehensive property [21]. Nowadays, the modification technology
of aliphatic amine curing agent is more mature [23–25], so the perfor­
mance of modified aliphatic amine 593 (obtained from the addition of
diethylenetriamine and butyl glycidyl ether) is more stable, making it
more widely used. As a result, aliphatic amine curing agent is the top
choice in the pavement engineering field.
The modification process of WER-EA is gradually carried out with
the evaporation of water. In this process, WER and amine curing agent
constantly solidify through chemical reaction or physical cross-linking
to form a stable three-dimensional reticular spatial structure. From a
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Y. Kezhen et al. Construction and Building Materials 347 (2022) 128531

Fig. 3. Chemical formula for (a) Modified Diethylenetriamine (5 9 3), (b) Diethylenetriamine (DETA) and (c) Triethylenetetramine (TETA).

1.3. Research status

Table 1
Physical properties of base asphalt.
It can be seen that the different molecular chain length or the amount
Index Unit Requirements Test result of active hydrogen atoms of curing agent will lead to different cross­
Penetration (25 ◦ C) 0.1 mm 60–80 68.3 linking degree and stereoscopic degree of three-dimensional structure in
Softening point ◦
C 44–54 47.2 WER-EA, which ultimately makes WER-EA show differences in high-
Ductility (15 ◦ C) cm 126.0
≥100
temperature performance or ductility [33,34]. However, current re­
Viscosity (135 ◦ C) Pa⋅s <3 0.46
searches in the pavement engineering field are neglecting the influence
of the chemical structure of curing agents on rheological properties of
WER-EA [21,35], which leads to the dosage large range of WER system
Table 2
in different studies. Gu et al. have proved that the stability of WER-EA
Physical properties of emulsified asphalt.
was the most remarkable at high temperature when the dosage of
Index Unit Requirements Test result amine/WER system is between 20 % and 25 % [36]. Wang et al. found
Particle charge — + + that the combination of alicyclic amine curing agent TETA and WER
Demulsification speed — Slow or Slow improved the high-temperature performance of emulsified asphalt.
moderate demulsification Meanwhile, when the dosage of WER system ≥ 10 %, the low-
demulsification
1.18-mm screen residues % ≤0.1 0.04
temperature performance of WER-EA reduced [8]. Therefore, it is
Solid content of emulsified % ≥55 63 essential to compare the influence of different curing agents on the
asphalt performance of WER-EA and find out their modification mechanism
Mixing stability in water — Uniformity Uniformity under the same evaluation system, which will make WER further
Storage stability at 1 day % 0.55
≤1
popularized and applied in the road field.
room temperature 5 ≤5 3.17
days
Residue Penetration (25 C)◦
0.1 45–150 64.2 1.4. Research purpose
mm
Residue Softening point ◦
C — 48.5 The purpose of this paper is to evaluate the influence of the chemical
Residue Ductility (15 ◦ C) cm 80.3
structure of curing agents on rheological properties and microstructure
≥40

of WER-EA. Modified Diethylenetriamine (593), Diethylenetriamine

molecular point of view, the epoxy group can react with the primary
amine groups (–NH2) and secondary amine groups (–NH–) on the amine
curing agent molecule chains [26,27] (Fig. 1). During curing, the epoxy
group is opened and carbon atoms replace the hydrogen atoms to con­
nect to the amine group. Thus, each curing agent molecule can form a
node of epoxy resin three-dimensional reticular spatial structure [28]. It
can be seen that the molecular chain length of the curing agent and the
amount of active hydrogen atoms involved in the reaction will affect the
stereoscopic degree and crosslinking degree of the three-dimensional
structure. WER molecules dispersed in asphalt also react with asphalt
molecules to form chemical crosslinking bonds. In addition, under the
dual action of external machinery and molecular movement, asphalt and
cured WER interweave with each other, forming thousands of physical
cross-links in the system [29]. The cross-linked reticular spatial struc­
ture is still very stable under high temperature and pressure, because it
can act like a “skeleton” to hinder the free flow of asphalt and resist the
deformation of asphalt [30,31]. However, when the dosage of WER
system is too high, the solidified product will agglomerate, which will
negatively affect the performance of WER-EA [32] (Fig. 2).
(DETA) and Triethylenetetramine (TETA), which are widely used
aliphatic amine curing agents, can endow WER-EA cured products with
good mechanical properties, heat resistance and water resistance. These
three kinds of curing agents have similar functional groups but signifi­
cantly different molecular chain lengths and number of active groups
(593 has the longest molecular chain while the number of active groups
of TETA is the largest) (Fig. 3). Therefore, 593, DETA and TETA were
selected to prepare WER-EA named W5, WD, WT, respectively. The
high- and low-temperature rheological properties were explored by
Dynamic shear rheometer (DSR), Multiple stress creep recovery (MSCR)
and Bending beam rheometer (BBR) tests. Moreover, the Fourier trans­
forms infrared (FTIR) spectroscopy and scanning electron microscopy
(SEM) were employed to analyze the micro-chemical interaction be­
tween WER systems and emulsified asphalt. It will provide scientific
basis for the systematic research and engineering application of WER-
EA.

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Y. Kezhen et al. Construction and Building Materials 347 (2022) 128531

Table 3 showed the physical properties of these materials. The properties of base
Performance parameter of WER. asphalt and emulsified asphalt meet specification (JTG E20-2019)
Index Appearance Epoxy Epoxy value Solid requirements.
equivalent content
weight 2.1.2. WER and curing agent
Measured Milky white 223 g/mol 0.41–0.47 50 ± 2 % Tables 3 and 4 summarizes the essential properties of WER and
values uniform liquid eq/100 g curing agents, which are provided by the supplier.

2. Materials and methods 2.2. Preparation of WER modified emulsified asphalt and its evaporation
residue
2.1. Raw material
2.2.1. Preparation of WER-EA
2.1.1. Emulsified asphalt Previous studies have shown that the appropriate dosage of WER
Cationic emulsified asphalt was used in the experiment. And emul­ system can significantly improve the high-temperature performance of
sified asphalt is prepared from 70# base asphalt. Table 1 and Table 2 emulsified asphalt while reduce its negative impact on low-temperature
performance [37]. Referring to the existing research results, the dosages

Table 4
Performance indicators of curing agents.
Index Unit Test result

Modified DETA Diethylenetriamine (DETA) Triethylenetetramine

(593) (TETA)

Appearance — Light-colored transparent liquid Light yellow transparent liquid Light yellow
viscous liquid
Molecular weight — 217.13 103.17 146.23
Amine value mgKOH/g 603.5 1617.8 1498.0
Solid content % >99 >99 >99
Density g 0.985 0.960 0.982
Boiling point ◦
C 170 207 278

Fig. 4. Preparation of WER-EA and its evaporation residue.

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Fig. 5. Test results for penetration (a), softening point (b) and ductility (c).
of WER used in this experiment are 0 %, 5 %, 10 %, 15 % and 20 % of the
mass of emulsified asphalt. In addition, the preparation scheme
(including the addition sequence of WER and curing agent, stirring
speed, etc.) selected by referring to the existing research results and
actual laboratory conditions is as follows [8,36,38]:
1. WER was added in different dosages to emulsified asphalt at room
temperature. Blend the mixture containing emulsified asphalt and
WER with a blender of 1000r/min. Semi-finished modified emulsi­
fied asphalt was obtained after stirring for 10 min.
2. Adding the curing agent in an amount of 20 % of the mass of the WER
into the semi-finished product prepared in the first step. The WER-EA
sample was obtained after stirring at the same speed (1000r/min) for
3 min.
2.2.2. Preparation of evaporation residue samples
Due to the performance of emulsified asphalt is reflected through its
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Construction and Building Materials 347 (2022) 128531
evaporation residue [8], it is necessary to prepare the evaporation res­
idue of WER-EA before testing its performance. The evaporation residue
preparation steps are as follows (Fig. 4):
1. Take 200 g WER-EA in the electric stove and control the surface
temperature of electric furnace 200–250 ◦ C, and stir continuously for
30 min until the water in WER-EA completely evaporates. Stop
heating when the evaporation residue temperature reaches about
160 ◦ C. In this process, it is necessary to ensure that the evaporation
residues have good fluidity, otherwise the failed sample needs to be
prepared again.
2. Put the prepared WER-EA evaporation residue into a 163 ◦ C oven
and keep it warm for 3–5 min. When there is no bubble in the
evaporation residue, the preparation is successful.
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Y. Kezhen et al.
Fig. 6. Test results for penetration (a), softening point (b) and ductility (c) after 24 h.
2.3. Test methods
2.3.1. High- and low-temperature performance test
The three fundamental indexes including penetration (25 ◦ C), soft­
ening point and ductility (15 ◦ C) were evaluated to explore the physical
properties of WER-EA evaporation residue.
DSR test (including temperature sweep and MSCR test) and BBR test
were employed to analyze the high-and low-temperature rheological
properties of WER-EA evaporation residue, respectively [39–41]. And
multiple stress creep and recovery (MSCR) test was utilized to evaluate
the viscoelastic behaviors of WER-EA evaporation residue [42–44].
In addition, three parallel pieces were employed for each test.
2.3.2. Microstructure test
Fourier transform infrared (FTIR) has been an effective method to
evaluate the composition and phase state of substances, study the
intermolecular interaction and identify substances qualitatively and
quantitatively [45,46]. Before the test, dissolve the WER-EA evaporation
residue with carbon disulfide (CS2). The FTIR test can be carried out
only when the solution with the volume of 1 mm3 is distributed in po­
tassium bromide (KBr) tablet [47].
The micro morphological and characteristics of WER-EA evaporation
residue were observed and analyzed by Scanning electron microscopy
(SEM) test [48].
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3. Results and discussion
3.1. Conventional properties test
In this part, base emulsified asphalt evaporation residue (EA), based
asphalt (70#) and three kinds of WER-EA evaporation residues (W5,
WD, and WT stands for WER-EA of 593, DETA, and TETA, respectively)
were evaluated to explore the conventional physical properties. The
addition dosages of WER system in EA are 5 %, 10 %, 15 % and 20 %,
respectively. The results are showed in Fig. 5. From Fig. 5, it can be
inferred that base emulsified asphalt evaporation residue has slightly
lower penetration (25 ◦ C)/ductility (15 ◦ C) and slightly higher softening
point compared with base asphalt. This is because the emulsifier and
other materials used in the preparation of emulsified asphalt have a
certain influence on asphalt. With the increase of dosage, penetration
(25 ◦ C)/ductility (15 ◦ C) of the three WER-EA evaporation residues
decrease significantly and the softening point increases significantly.
These results indicate that the three WER systems can significantly
improve the high-temperature performance of emulsified asphalt.
However, the addition of the WER systems reduce the ductility of the
emulsified asphalt especially when dosages were above 10 %, which
means the low-temperature performance of WER-EA decreases.
Fig. 5(a)-(b) shows that the three WER systems have the greatest
influence on emulsified asphalt when the dosage is 20 %. And the
penetration (25 ◦ C) of evaporation residues decreases by 51.8 % (W5),
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Y. Kezhen et al. Construction and Building Materials 347 (2022) 128531

Fig. 7. PI of the three kinds of WER-EA with different dosages.

Fig. 8. G* and δ of the three kinds of WER-EA with different dosages.

40.3 % (WD) and 53.7 % (WT), respectively compared with 70# base
asphalt, meanwhile, their softening point increases by 68.2 % (W5),
58.3 % (WD) and 86.9 % (WT). It can be seen that the addition of TETA
has the greatest influence on the penetration (25 ◦ C) and softening point
of WER-EA evaporation residue, while the influence of the addition of
DETA curing agent is minimal. That is, the addition of TETA has the best
positive influence on the high-temperature property of WER-EA. Addi­
tionally, Fig. 5(c) shows that the addition of 593 had the least adverse
influence on the low-temperature property of WER-EA.
The properties of WER-EA can only be reflected after complete
curing. Conventional properties of WER-EA evaporation residues ob­
tained by the same preparation scheme were tested after being placed
for 24 h to prove that the curing level of evaporation residues had met
the requirements of road asphalt. By comparing Fig. 5 and Fig. 6, it is
observed that the trends and data of the three indexes of WER-EA
evaporation residues measured before and after 24 h are similar. This
suggests that the above conclusions are reliable.
3.2. Penetration index (PI)
It can be seen from the above experiments that the addition of WER
system will reduce the temperature sensitivity of WER-EA. The perme­
ability index (PI) value (Eq. (3.1)) is commonly utilized to evaluate the
temperature sensitivity of asphalt [49]. The calculation results are
shown in the Fig. 5.

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Y. Kezhen et al. Construction and Building Materials 347 (2022) 128531

Fig. 9. G*/sinδ of the three kinds of WER-EA with different dosages.

Fig. 10. Jnr0.1 and Jnr3.2 the three kinds of WER-EA with different dosages at 58 ◦ C (a), 64 ◦ C (b) and 70 ◦ C (c).

1952 − 500log(Pen25) − 20 × SP lower the temperature sensitivity of WER-EA evaporation residue. In

PI =
50log(Pen25) − SP − 120
where Pen25 is the penetration (25 ◦ C) and SP is the softening point of
WER-EA evaporation residue (Fig. 7).
The higher the PI value, the lower the temperature sensitivity of
asphalt. Fig. 1 shows that the higher the dosage of WER system, the
(3.1)
addition, the temperature sensitivity of WT was significantly lower than
that of the other two materials, indicating that the higher the amount of
active hydrogen atoms in the curing agent, the more stable the three-
dimensional structure in the cured product. The three-dimensional
structure can improve the high-temperature deformation resistance of
WER-EA evaporation residue.

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Fig. 11. R100 and R3200 of the three kinds of WER-EA with different dosages at 58 ◦ C (a), 64 ◦ C (b) and 70 ◦ C (c).
3.3. Temperature sweep test
Temperature sweep test characterizes high-temperature and visco­
elastic properties in terms of Complex modulus (G*) and phase angle (δ)
[50]. Strain control model is utilized in this experiment. The shear strain
remains at 2 %. The size of samples is: diameter = 25 mm, thickness = 1
mm. The test temperature was 30-90 ◦ C. The temperature increment was
1 ◦ C and the test frequency was 1.59 Hz (10 rad/s). The test results are
presented in Fig. 8.
Fig. 8(a)-(b) shows the effects of curing agents (593\DETA\TETA) on
G* and δ of WER-EA. It shows that with the rise of temperature, G* of
asphalt decreases and δ increases, which means that the state of asphalt
gradually changes from glassy state to flowing state, and the material
begins to change from elastic to viscous elastic. In addition, the G* and δ
of the three kinds of WER-EA are larger and smaller than those of the
base asphalt, respectively. This shows that the WER-EA has good shear
deformation resistance.
The high-temperature performance of the three kinds of WER-EA has
a similar trend with the change of dosage. At the same temperature, the
G* of the WER-EA evaporation residue gradually increases and the δ
gradually decreases with the increase of the dosage. This shows that the
addition of three WER systems improves the high-temperature perfor­
mance and the elastic behavior of emulsified asphalt, and in the mean­
time, the viscosity of WER-EA increases and the plasticity gradually
weakens. This is because a cross-linking reaction occurs within WER-EA,
and the resulting three-dimensional reticular spatial structure improves
the modulus of asphalt [35,51–53]. When the dosage is fixed, with the
increase of temperature, the δ of WER-EA evaporation residue increases
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Construction and Building Materials 347 (2022) 128531
first and then decreases, especially when the temperature is higher than
60 ◦ C. This indicates that the use of the three WER systems will harden
the WER-EA evaporation residue and reduce its low-temperature per­
formance. This is because the higher the temperature, the more obvious
the effect of WER on emulsified asphalt. WER cured products are ther­
mosetting and prone to brittle fracture. The increase of elastic response
at high temperature (the reduction of δ) can be attributed to the loss of
light components and the decrease of viscous components in asphalt.
Under this condition, the influence of the elastic network generated in
WER-EA on the mechanical properties of the evaporation residue
increases.
G* of the three kinds of WER-EA has the following quantitative
relationship: WT > W5 > WD when the dosage is 5 %; W5 > WT > WD
when the dosage is 10 %; when the dosage of WER system is 15 %, the
performance law of G* is consistent with that of 5 %; WT > W5 > WD
when the dosage is 20 % and the test temperature is less than 58 ◦ C；W5
> WT > WD when the dosage is 20 % and the test temperature>58 ◦ C. δ
of the three kinds of WER-EA has the following quantitative relation­
ship: WT < WD < W5. Under the same conditions, the peak temperature
of δ of W5 appears later, while the other two kinds of WER-EA are
similar. Moreover, the temperature corresponding to the peak value of δ
tends to a fixed value when the dosage reaches 15 %. Overall, the G* of
WT is higher and the δ of WT is lower, so WT is better at high temper­
atures. This indicates that the greater the amount of active hydrogen
atoms in the aliphatic amine curing agent, the higher the crosslinking
degree of the three-dimensional network structure, which means that
the higher the high-temperature deformation resistance of WER-EA.
Rutting factor (G*/sinδ) calculated by complex shear modulus (G*)
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Y. Kezhen et al.
Fig. 12. m of the three kinds of WER-EA with different dosages at − 6 ◦ C (a), − 12 ◦ C (b) and − 18 ◦ C (c).
and the phase angle (δ) is an index utilized to characteristic the ability to
resist permanent deformation of asphalt. The DSR test results are pre­
sented in Fig. 9.
With the increase of temperature, G*/sinδ shows a decreasing trend.
It indicates that the plastic rheological property of WER emulsified
asphalt evaporation residues increases and the bond behavior de­
teriorates with the increase of temperature. The G*/sinδ of the three
kinds of WER-EA evaporation residues gradually increases with the in­
crease of the dosage. It indicates that the addition of WER can signifi­
cantly improve the rutting resistance of WER-EA. The higher the dosage,
the gentler the curve of G*/sinδ. It’s because WER has the less sensitivity
to temperature, and emulsified asphalt is more significantly affected by
WER system with the increase of dosage. The G*/sinδ of the three kinds
of WER-EA exhibits similar laws to G*.
3.4. MSCR test
The viscoelastic properties of WER emulsified asphalt evaporation
residues at high temperature were studied by MSCR test [54]. The test
results at the stress level of 0.1 kPa reflect the linear viscoelasticity of the
asphalt. In addition, the test results at 3.2 kpa stress level reflect the
nonlinear viscoelasticity of asphalt [55]. The evaluation indexes of un­
recoverable creep compliance (Jnr) and creep recovery rate (R) can be
obtained by performing 10 creep stress cycles (including 1 s creep and 9
s recovery) at 0.1/3.2 kpa with a specimen of the same size as the
temperature sweep test used [56]. Calculation methods of Jnr and R are
given in Eqs. (3.2) and (3.3).
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γnr − γ0
Jnr = (3.2)
τ
R =
γ 1 − γnr
(3.3)
γ1 − γ0
where γ 0 is the initial strain of each creep recovery period at each stress
level; γnr is residual strain after recovery stage; γ 1 is the total strain at
creep stage; τ is creep stress.
With the increase of Jnr, the elastic deformation of asphalt decreases
and the residual deformation increases, which indicates the deformation
resistance of asphalt becomes worse under high temperature conditions.
On the contrary, the high-temperature deformation resistance of asphalt
becomes stronger with the decrease of Jnr. Similarly, the larger R, the
larger the proportion of elastic deformation of asphalt in the total
deformation, and the smaller the proportion of unrecoverable defor­
mation. This shows that the residual deformation of the asphalt will be
reduced at high temperature. The unrecoverable creep compliance and
creep recovery rate under two stresses (0.1 kPa, 3.2 kPa) were repre­
sented by Jnr0.1, Jnr3.2 and R100, R3200. Yan et al. [4] and Hong et al. [3]
found that the temperature of asphalt pavement can reach 60 ◦ C or
more, especially in summer, which can cause pavement damage due to
softening. Therefore, test samples were tested at 58 ◦ C, 64 ◦ C, and 70 ◦ C.
The results are presented in Figs. 10 and 11.
By contrasting with Fig. 10(a)-(c), it is found that with the increase of
temperature and pressure, Jnr of emulsified asphalt evaporation residues
increases. With the increase of WER system dosage, Jnr of the three WER-
EA decreases, and Jnr tend to be the same when dosage greater than 15
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Y. Kezhen et al.
Fig. 13. S of the three kinds of WER-EA with different dosages at − 6 ◦ C (a), − 12 ◦ C (b) and − 18 ◦ C (c).
%. Fig. 10(a) shows that at 58 ◦ C, Jnr of W5 is significantly higher than
that of WD and WT, meanwhile, Jnr of WD and WT is similar. Fig. 10(b)
shows that when the dosage is less than 20 %, Jnr of W5 is significantly
higher than that of WD and WT. However, when it reaches 20 % and the
pressure is 3.2 Pa, Jnr of WD tends to be larger than that of W5 and WT.
Fig. 10(c) shows that at 70 ◦ C, Jnr has a significant pattern when the
dosage is less than 10 %: W5 > WD > WT. But when the dosage is 15 %
or higher, Jnr of WD was significantly higher than that of W5 and WT.
By contrasting with Fig. 11(a)-(c), it is found that R decreases with
temperature and pressure increasing. With the increase of WER system
dosage, R of the three WER-EA increases. At 58 ◦ C, 64 ◦ C and 70 ◦ C, the
R100 of W5 is significantly higher than that of WD and WT, meanwhile,
R of WD and WT is similar. In addition, the pattern of R3200 is WT > W5
> WD. However, when the dosage is 5 %, R3200 of WT is less than W5,
which may be caused by experimental error.
The above tests provide reference for the viscoelastic properties of
WER-EA at different temperatures and pressures. On the whole, Jnr of
WT is lower and R of WT is higher. This means that WT has better
deformation resistance and smaller proportion of unrecoverable defor­
mation. This is because TETA contains more active hydrogen atoms, so
the three-dimensional structure produced by adding TETA to WER-EA is
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Construction and Building Materials 347 (2022) 128531
more stable.
3.5. BBR test
Flexural stiffness modulus (S) and creep rate (m) are essential in­
dexes of low-temperature property of asphalt samples. Under the same
test conditions, high S value means high brittleness of asphalt samples.
In addition, it means that asphalt samples have insufficient deform­
ability. Similarly, high m means strong stress relaxation capacity of
asphalt samples. The Bending Beam Rheometer test is used to obtain the
S/m value of WER-EA evaporation residues. The size of the samples used
is: length = 127 ± 2 mm, width = 12.70 ± 0.05 mm, thickness = 6.35 ±
0.05 mm. The test pieces are insulated with ethanol, and the load is 980
± 50 mN [57]. The results are presented in Figs. 12 and 13.
According to Figs. 12 and 13, it is found that when the temperature
decreases from − 6◦ C to − 12 ◦ C or from − 12 ◦ C to − 18◦ , S of all asphalt
increases in different degrees, while the m decreases. It indicates that the
brittleness and hardness of the material increases as temperature de­
creases, in the meantime the likelihood of low-temperature fracture
increases. The m of EA is larger than base asphalt, and the S of EA is
smaller than base asphalt. It indicates that the low-temperature property
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Y. Kezhen et al.
Fig. 14. FTIR of the three kinds of WER-EA samples (a) W5, (b) WD and (c) WT at 20% dosage.
of base asphalt can be improved by the addition of emulsifier. However,
the S and m of WER-EA were smaller than EA and larger than EA,
respectively. It shows WER systems reduce the low-temperature prop­
erty of emulsified asphalt. And the effect of higher dosage is more
obvious. At a given temperature, as the dosage of WER system increases,
the S of the WER-EA increases, and the m gradually decreases. It shows
that as WER system dosage increases, the strength modulus of WER-EA
evaporation residues increases, while the relaxation ability of the WER-
EA evaporation residues obviously decreases. In the meantime, the crack
resistance performance at low-temperatures deteriorates. This is
because the cured WER is thermosetting and becomes hard and brittle,
which leads to an increase in WER-EA evaporation residue stiffness
modulus and a decrease in low-temperature crack resistance of WER-EA
evaporation residue [58].
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Construction and Building Materials 347 (2022) 128531
Creep rate (m) of three kinds of WER-EA has a significant pattern:
WT > W5 > WD. Flexural stiffness modulus (S) of three kinds of WER-EA
has a significant pattern: W5 < WD < WT. Through the comprehensive
analysis of BBR test, it is found that the addition of 593 had the least
adverse influence on the low-temperature performance of WER emul­
sified asphalt. This indicates that the longer the molecular chain of
aliphatic amine curing agent, the higher the proportion of flexible seg­
ments generated in WER-EA, which means that the lower the adverse
influence of WER system on the low-temperature crack resistance of
emulsified asphalt.
3.6. FTIR test
Previous research has proved that FTIR spectrum can clearly explore
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Y. Kezhen et al.
Fig.15. SEM images of the three kinds of WER-EA samples with different dosages (a) 5%, (b) 10%, (c) 15% and (d) 20%.
the changes of functional groups in asphalt. It can be seen from the
above experiments that the WER system with 20 % dosage has the
greatest impact on the performance of emulsified asphalt, which in­
dicates that the change of functional groups is the most obvious under
this condition. Therefore, the evaporation residues of emulsified asphalt
with 20 % WER system dosage are analyzed. The result is shown in
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Construction and Building Materials 347 (2022) 128531
Fig. 14.
Fig. 14 shows that there are C–H tensile vibration peaks at 813 cm− 1
and 2862 cm− 1. The generated 1369 cm− 1 peak represents the charac­
teristic absorption peak of C–N of alicyclic amine. The characteristic
absorption peak of C–O at 1242 cm− 1 indicates the carbon chain sub­
stitution of hydroxyl group. The peak at 1462 cm− 1 is the stretching
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Y. Kezhen et al.
vibration of benzene ring (C–– C). The absorption peak of WT has higher
intensity and larger area, which indicates that TETA can improve the
performance of WER-EA more obviously.
It can be seen from Fig. 14(a)-(c) that there is no characteristic ab­
sorption peak of epoxy group near 910 cm− 1, indicating that the epoxy
group in WER completely reacts with N–H in curing agent [59].
3.7. SEM test
The three kinds of WER-EA with different dosages (5 %, 10 %, 15 %,
20 %) were sampled. The structure formed by solidification in WER-EA
evaporation residues was showed by SEM (scanning electron micro­
scope) test. The SEM images are showed in Fig. 15.
It can be seen from Fig. 15 that irregular and dispersed three-
dimensional reticular spatial solidified materials are formed after the
ring-opening reaction of WER system occurs in emulsified asphalt
evaporation residue. After the reaction, WER system is permeated with
asphalt. The cured resin blocks the flow of asphalt by forming a three-
dimensional structure. Therefore, the high-temperature property and
bonding property of WER-EA are better than base asphalt and emulsified
asphalt.
By contrasting with Fig. 15(a)–(d), it is found that when the WER
system dosage up to 5 %, the three-dimensional reticular spatial struc­
ture formed is sparse and linear. With the increase of the amount of WER
resin system, the three-dimensional reticular spatial structure formed by
WER system is more three-dimensional and the linear connections are
stronger. When the WER system dosage reaches 15 %, the skeleton
structure is the most obvious. However, when the dosage of WER system
reaches 20 %, the compatibility between the reticular structure and
asphalt deteriorates, and the phenomenon of solidified substance ag­
gregation appears. Therefore, high dosage has a negative effect on
emulsified asphalt. Macroscopically, the storage stability and the
fluidity plasticity of WER-EA evaporative residue become worse.
Compared with the other two curing agents, the addition of TETA
can make the skeleton structure of WER-EA more solid, uniform and
stable. In addition, WT has basically formed a comprehensive three-
dimensional reticular spatial structure when the dosage is 5 %. How­
ever, WD has the weakest skeletal structure connection under the same
conditions. Therefore, the curing agent TETA is more favorable to the
formation of WER-EA skeleton structure, while WD has the least impact.
4. Conclusion
In this study, three WER emulsified asphalts were prepared with
three different curing agents. The effects of curing agents on high-
temperature and low-temperature rheological properties of WER-EA
were studied by conventional properties test (permeability, ductility
and softening point), DSR and BBR tests. In addition, the microstructure
of WER-EA emulsified asphalt evaporation residue were studied by SEM
and FTIR. The following conclusions are drawn:
1. The addition of three WER systems can significantly improve the
high-temperature deformation resistance of emulsified asphalt, effec­
tively reduce the stress sensitivity under high shear stress level while
have adverse influence on its low-temperature performance, indicating
that WER-EA is fit for heavy-load traffic in medium and high tempera­
ture areas.
2. DSR test results show that the addition of curing agent TETA
makes WER-EA have better high-temperature performance and smaller
unrecoverable deformation ratio. The BBR test results indicate that the
addition of 593 has the least effect on the low-temperature performance
of WER emulsified asphalt.
3. SEM images show that the three-dimensional network structure
was formed in the WER-EA evaporation residue. Under the same con­
ditions, the addition of TETA can make the skeleton structure of WER-EA
more solid, uniform and stable.
The experimental results show that the high strength of WER-EA
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Construction and Building Materials 347 (2022) 128531
makes it more suitable for heavy-load traffic in medium and high tem­
perature areas. So WER-EA can be used as a binder for micro surfacing or
cold mix asphalt.
Furthermore, it is found that the more active groups in the curing
agent, the higher the crosslinking degree and complexity of the three-
dimensional network structure in WER-EA, which will lead to the
stronger high-temperature deformation resistance of WER-EA. The
longer the molecular chain of curing agent, the more flexible chains in
WER-EA, which will lead to better flexibility of WER-EA. This provides a
new reference for road workers in selecting materials, which enables
them to select the curing agent with appropriate chemical structure
according to the performance requirements of WER-EA.
CRediT authorship contribution statement
Yan Kezhen: Conceptualization, Funding acquisition, Methodology,
Resources, Supervision, Writing – review & editing. Shi Junyi:
Conceptualization, Data curation, Formal analysis, Investigation,
Methodology, Writing – original draft, Writing – review & editing. Shi
Kaixin: Conceptualization, Formal analysis, Investigation, Supervision,
Writing – original draft, Writing – review & editing. Wang Min: Data
curation, Investigation, Supervision, Formal analysis, Writing – review
& editing. Li Goukai: Data curation, Formal analysis, Investigation,
Supervision, Writing – review & editing. Hong Zhe: Data curation,
Formal analysis, Investigation, Supervision, Writing – review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
No data was used for the research described in the article.
Acknowledgments
The authors would like to show gratefulness for the financial sup­
ported by the National Natural Science Foundation of China (NSFC, No.
51778224).
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