Journal of Highway and Transportation Research and Development VoL 7, No.

2 (2013) 1

Performance Optimization Method of Composite Modified Asphalt Sealant *

TAN Yi-qiu (i.�Hlfk) * *

,
GUO Meng (*�3'i) ,
ZHANG Lei (5*�) ,

CAO Li-ping (l!ri'Ji'J�)

(School of Transportation Science and Engineering, Harbin Institute of Technology, Harbin Heilongjiang 150090, China)

Abstract: Central composite design-response surface methodology was used to determine the best content of raw materials and

improve the performance of hot-poured bituminous sealant. Content range and process technology were studied through single
factor analysis method. Cone penetration, elastic recovery, creep strength, and creep strain rate " m" were analyzed by central
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composite model testing. The response surface of the overall desirability was established and the optimal content of raw materials
were determined and verified. Analyses of test results indicated that the optimal content of raw materials were as follows: rubber
powder -25%, additive -7%, SBS -5%, and SBR -3%. This paper proposes the application of central composite design in
the optimization of raw material dosage of hot-poured bituminous sealant.
Key words: road engineering; sealant; central composite design-response surface methodology; composite modified asphalt;

performance optimization

sealant, and easy removal of prefabricated rubber caulk­

1 Introduction
Cracking is a pnmary concern In pavement engI­
neering. Accelerated by temperature and traffic loading,
cracked pavements lose their carrying capacity as end re­
sult. Therefore, timely repair of cracks has significant
implications in pavement maintenance. Pouring sealant is
the most common for repair measure for cracks.
Various materials have been developed to aid the
cracking problem. Wu Zhen et al. have synthesized sin­
gle-component polyurethane caulking materials [I]. Zhang
Dong-chang et al. have developed a new type of long-life
2
sealant with organic silicon as the main component[ ].
Shou Chong-qi et al. have developed the silicon-modified
polyurethane prepolymers and two-component polyure­
thane sealant, and then prepared a composite sealant by
combining polyurethane sealant with organosilicone seal­
3
ant[ ]. Prefabricated rubber caulking strip-like materials
were developed for the Chinese National "8th Five-year
Plan" , where neoprene is the primary component. All
the sealants mentioned above cannot be used widely be­
4
cause of a number of drawbacks[ - 5] including the poor
durability of polyurethane, high cost of organosilicone
ing strips from slots. In the United States, the most pop­
ular sealants include rubber asphalt, PVC coal tar, poly­
sulfide, single-component and two-component polyure­
thane, and silicon rubber material. Rubber asphalt seal­
ant ranks first because of its excellent performance and
lower cost.
Traditional modified asphalts are usually modified
by adding polymers, such as poly ethylene (PE), pro­
pene polymer (PP), styrene-butadiene-styrene (SBS),
styrene-butadiene rubber (SBR), and ethylene vinyl ac­
etate ( EVA) [6 -9 ] . Each polymer has a unique effect on
the asphalt road performance. SBS improves the high­
temperature performance; SBR enhances the low-temper­
ature anti-cracking ability; and rubber powder improves
the elasticity of asphalt. Compared with single modifica­
tion, composite modification improves the overall per­
formance of the asphalt and excellent composite modified
asphalt can be used as hot-poured pavement sealant.
Composite modified asphalt additives, such as mul­
tiple polymers, are mixed into asphalt to produce com­
plex interaction [10]. Reasonable experimental design
method is needed to optimize the ratios of different addi-

Manuscript received October 21, 2012

• SuppOlted by the National Key Technologies R&D Program of China during 11 Ih Five-year Plan Period ( No. 2008BAGlOB02 ) and the
National Natural Science Foundation of China ( No. 51008099 )
• • E-mail address: yiqiutan@163. com

J. Highway Transp. Res. Dev. (English Ed.) 2013.7:1-7.

 2 Journal of Highway and Transportation Research and Development

tives. The existing design methods include factorial de­ 2.2 SBS

sIgn, uniform design, and orthogonal design. Factorial The SBS used in this paper is a star-type 3411 pro­
design requires too many tests, which needs large amount duced in Taiwan, whose basic properties are shown in ta­
of manpower, material resources, and time. The uniform ble 2.
design and orthogonal test design methods can obtain a Tab. 2 Physical properties of SBS

good point in the testing process, however, a number of 25% toluene

problem still exist: the test precision is not enough, the Specific Hardness Volatile matter Butadiene/ Ash conlent solution
Item
gravity (shore A) content (%) styrene (%) viscosiLy
test value is only close to the optimum value which is not
(MPa . s)
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the best accurate point, optimum conditions is empirical,

Test results 0.94 80 0.25 70/30 0.1 20 000
and the interaction among different factors cannot be in­
[II -12J 2.3 SBR
vestigated . Nowadays, most researchers use cen­
tral composite design and response surface methodology The SBR used in this paper is a powder modifier

for the experiments because of its less test number and which can improve low-temperature performance and

high test precision. ductility of the asphalt. The basic properties are shown in
table 3.
In this paper, central composite design and re­
Tab. 3 Physical properties of SBR
sponse surface methodology are used to design the com­
posite modified asphalt sealant. The contents of rubber Combined Rubber Mooney
Size Molecular weight
Item with stupid viscosity
powder, SBS, SBR, and a kind of additive were opti­ (mm) (ten thousand)
ethylene (%) [M . (l +4) 100 'C -I J
mized. Through the verification test, a composite modi­
fied asphalt sealant with high elasticity and excellent low­ Quality
0.425 20 - 30 21.5 - 35 48 - 66
index
temperature performance is obtained.
2.4 Rubber powder and additive
2 Materials and methods
The size of rubber powder used in this paper is be­
2. 1 Asphalt tween O. 3 mm and O. 15 mm, which were obtained by u­
The neat asphalt with the penetration grade of 90 sing the standard square mesh. The additive is a kind of
was used in this paper, whose basic properties are shown light oil, which affects the asphalt compliance.
in table 1. 2.5 Preparation technology

Tab.1 Physical properties of 90# Neat Asphalt A high-speed shear mixer was used in this study. To
Engineering achieve the same effect, faster stirring rate leaded to
Item Test results Test methods
requirements shorter mixing time. To find the reasonable mixing time,
Penetration ( 100 g, 5 s, this paper used a fixed speed of 4 500 Hz and a tempera­
80 - 100 83.0 JTJ T0604
25 'C)(O.I mm)
ture of 200 "C. Furthermore, 25 % rubber powder was
Ductility (5 cm/min,
> 100 JTJ T0605 added to the asphalt with constant speed stirring. Figure
10 'C) (cm)
1 shows the surface morphologies at 30, 60, 90, and 120
Ductility (5 cm/min,
1: 100 > 140 JTJ T0605
15 'C) (cm)
min, which were recorded using a digital camera.
Softening point TR&B Figure 1 shows that with increased stirring time,
42 -52 46.3 JTJ T0606
('C) rubber powder was more equally distributed in the as­
Solubility ( trichloroeth­ phalt . On the contrary, the particle state appears easily
99.0 99.5 JTJ T0607
ylene) (%) on the asphalt with short stirring period. After repeated
Flashing point (COC ) 13J
230 3 10 JTJ T0609 experiments and referring literature [ , the final process
(%)
is shown in figure 2.
Density ( 15 'C) Actual
1. 009 JTJ T0603 2.6 Test methods
(g . cm -3 ) measurement
Paraffin content ( distil­ Various test methods were used in this paper, inclu­
1.5 JTJ T06 15
lation) ( %) ding conditional asphalt tests, conditional sealant tests,

J. Highway Transp. Res. Dev. (English Ed.) 2013.7:1-7.

 TAN Yi-qiu. et al: Performance Optimization Method of Composite Modified Asphalt Sealant 3

sults are shown as follows.

( a) 30min ( b) 60min
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Fig. 3 Uniform state

( c) 90min ( d) 120min

Fig.1 Relationship between surface morphologies and

stirring time

Fig. 4 Particle state

Mix with Mix with
Heat asphalt
to 200'C f==:> additive for � rubber Figure 5 shows that the penetration value decreases
10min powder for 2 h
with higher rubber powder content. When the content of
II rubber powder is 25% , saturated condition is observed.
Decrease the temperature Decrease the temperature
to 15 0 'C, and mix with
f: to 170 'C, and mix with Stirring strongly for 2 hours to 3 hours can disperse the
SBR for 2h SBS for 2 h
rubber powder uniformly ( figure 3). Particle state ap­
Fig. 2 Preparation process of sealant pears when the content is more than 30% ( figure 4).

and tests for stiffness and m-value. Stiffness and m-value ( Note: all contents mentioned in this paper are the per­
were obtained by Bending Beam Rheometer at - 30 "C. centages of asphalt )

During the test, the bitumen beam was placed uncon­ 38

strained on two supports ( distance between supports was
E 37
101. 6 mm ) and loaded with 100 g mass. The applied E

load was measured by a load cell and the deflection was e 36

"
.g 35
tested using a high precision Linear Variable Differential g'"
"
Transformer six times within a period of 4 min (8, 15, "
0..
34

30, 60, 120, and 240 s ) . The data obtained were trans­ 33 •

mitted to a personal computer. The flexural creep modu­ 24 26 28 30 32 34 36

lus 5 ( t) was calculated on the basis of stress a and The content of rubber powder (%)

strain B ( t) in the outer fibre at midspan. The calcula­ Fig. 5 Effects of rubber powder content on cone

tions were based on the elementary Bernoulli-Euler theo­ penetration value ( without other modifiers)

ry of bending[ 14] . 3.2 The effect of SBR content

To study the effect of SBR powder on composite

3 Results and discussion
3. 1 The effect of rubber powder content
The dispersed state and penetration values of differ­
ent contents were analyzed to study the effect of rubber
powder content on the performance of sealant. The re-
modified asphalt, modified asphalt with different contents
of SBR were tested, which are shown in table 4.
Table 4 shows that the asphalt which was modified
by SBR meets the specification requirements, and its
high-temperature performance is improved significantly.

J. Highway Transp. Res. Dev. (English Ed.) 2013.7:1-7.

 4 Journal of Highway and Transportation Research and Development

Table 4 also shows that with the increase of SBR, the
penetration of asphalt decreases and ductility and softing
point increases. When the increase of SBR is 4. 5 % , the
softing point and ductility of asphalt increase by 28 %
and 932% , respectively, while the penetration decreases
by 44% .
Tab. 4 Test results of SBR powder modified 90# asphalt
Modified asphalt
JTJ036 - 98
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Figure 6 shows that the additive can adjust the soft­
ness of asphalt. The higher content of additive leads to
bigger penetration and smaller viscosity. Finding the best
content which can balance the softness and high-tempera­
ture performance of asphalt is the key to optimize the
sealant. Figure 6 shows that SBR powder can decrease
the penetration of asphalt, and figure 7 shows that both
SBR and additive have little effect on the elastic recovery

90# Neat with different of asphalt.

Item SBR category
asphalt contents of SBR
3.4 The content optimization of experimental mate­
2.5% 4.5% 6% II-A II-B II-C
rials
Penetration
3.4. 1 Experimental design
(25 "C. 100 g. 82 72 46 43 ",100 ",80 ",60
5 s) (0.1 mm) The reasonable scope of various modifier contents
Softing point ("C ) 47 54 60 63 ;;.45 ;;.48 ;;.50 can be determined through the previous single factor a­
Ductility (15 "C ) nalysis test. This study used Design-Expert Software
> 140 > 140 > 140 > 140
(cm) 7. 0, which is widely used in food biology and engineer­

Ductility (5 "C) ing, to aid the design of response surface experiment.

6.3 44 65 80 ;;.60 ;;.50 ;;.40
( cm) The response surface experiment of four factors and five
levels including 30 experimental points (6 center points)
3.3 The effect of additive content
was designed by the central composite model. The 30
To study the effect of additive content on the per­
test points were divided into two categories. First, facto­
formance of asphalt, two asphalts were selected as sam­
rial point with a total number of 24 and variable values in
ples. The composites are as follows: Neat asphalt +
the three-dimensional vertex formed. The second catego­
25% rubber powder; Neat asphalt + 25% rubber pow­
ry has zero as the center of the region, and the experi­
der + 5% SBR. The contents of additive are 3% , 7% ,
ment was repeated six times to estimate the experimental
10% , and 12% . The tests results are shown in figure 6
error[ 15 -17]. This experiment took residual strain, elastic
and figure 7.
ratio and creep stiffness, and creep strain rate" m value"
160
140 -+- Without SBR
as analysis indexes. Each index was standardized at a
?
E 120 --With%SBR normalized value between 0 and 1. The geometric mean
S 100 of these indexes was calculated to obtain the overall de­
"
.g 80
�'" sirability (OD) [18]. The formula is shown as follows:
60
"'"
0.. 40
(1)
20
0 where k is index number.
0 5 10 15
The content of additive (%) We used a mathematical transformation method
Fig. 6 Effects of additive content on cone called Hassan to deal with the value dmin and dmax' The
penetration value
smaller dmin and larger dmax lead to a better performance.
� 70 The formulas are as follows:
•
C 60
'";>
0 50
:
-+- WithoutSBR
� dmin = ( 'Ymax - 'Yi)/( 'Ymax - 'Yrnin) , (2)
�
u

40 --With 5%SBR
u

.t; dmax (Yi -Ymin)/(Ymax -Ymin), (3)

'" 30
u:l 0 5 10 15
where, 'Y refers to the value of indicators; i refers to the
The content of additive (%)

Fig. 7 Effects of additive content on elastic

test number; 'Ymax refers to the maximum value of indica­
recovery rate value. tors; and 'Ymin refers to the minimum value of indicators.

J. Highway Transp. Res. Dev. (English Ed.) 2013.7:1-7.

 TAN Yi-qiu, et al: Performance Optimization Method of Composite Modified Asphalt Sealant 5

The levels of response surface experimental factors 3.4.2 Tests results analysis

are shown in table 5, and the experimental data of re­ Based on least squares method, this study took the
sponse surface are shown in table 6. content of the four modifiers as factors, and took penetra­
Tab. 5 Levels of response surface experimental factors tion, elastic recovery, creep stiffness, m-value, and o­
Factors -2 -I o 2 verall desirability as indexes to execute quaternary quad­
Xl(%) 15.0 18.0 21.0 24.0 27.0 ratic polynomial fitting using SPSS software. The least
X2(%) 3.0 6.0 9.0 12.0 15.0 significant items were successively removed until all re­
X3 (%) 0.0 2.5 5.0 7.5 10.0 maining items were significant. The results are shown as
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X4(%) 2.0 4.0 6.0 8.0 10.0 tables 7 -9.

Tab. 7 Summary of OD regression model
Note: Xl - content of rubber powder, X2 - content of additive, X3 -
2
Model R Adjustive R Standard error of estimate
content of SBS, X4 - content of SBR) .

Tab. 6 Experimental data of response surface 0.830 0.689 0.608 0.142 21

Elastic Creep Tab. 8 Analysis of OD regression variance

Pe netra tio n m-
Set Type Xl X2 X3 X4 recovery stiffness OD
( 0.I mm) value Model
Quadratic Degree of Mean
F Prob > F
(%) (MPa) sum freedom square
4 Fact -I -I 92.5 55.9 249.7 0.25 0.29
Regression 1.030 6 0.172 8.492
17 Axial -2 0 0 0 59.3 59.3 277.2 0.27 0.40
Residual 0.465 23 0.020
ract -I -I -I -I 59.0 52.3 142.5 0.36 0.52
Gross 1.495 29
5 Fact -I -I -I 45.3 61.3 113.8 0.31 0.65
Tab.9 Coefficients of OD regression equation
21 Axial 0 0 -2 0 87.3 59.8 355.6 0.24 0.00

18 Axial 2 0 0 0 67.3 67.7 Ill.8 0.33 0.70 Unstandardized

16 Fact 64.5 63.7 90.7 0.38 0.76 coefficients Standardized

Model T Prob > t
28 Center 0 0 0 0 61.3 57.3 123.I 0.29 0.54 Standard coefficients
B
9 ract -I -I -I 65.0 54.3 246.2 0.24 0.29 error

15 Fact -I 81.0 63.3 125.3 0.31 0.58 Constant -l. 018 0.316 - 3.217 0.003 8
20 Axial 0 2 0 0 73.0 58.3 213.6 0.27 0.42 0.023 0.010 0.274 2.354 0.027 5
2 Fact -I -I -I 79.3 63.0 82.I 0.33 0.64 0.128 0.058 I . 540 2.219 0.036 6
25 Center 0 0 0 0 68.3 68.3 90.9 0.27 0.59
0.137 0.038 l. 368 3.621 0.001 4
13 ract -I -I 53.0 65.7 122.3 0.28 0.62
- O. 009 0.003 - 2.046 - 3.161 0.004 4
19 Axial 0 -2 0 0 47.3 60.3 248.3 0.22 0.00
0.008 0.003 0.850 2.363 0.027 0
Fact -I -I -I 123.3 47.3 144.1 0.33 0.00
- 0.012 0.006 - 0.916 - 2.069 0.050 0
30 Center 0 0 0 0 69.2 65.8 96.3 0.31 0.67

14 Fact -I 53.7 66.8 97.9 0.32 0.73

The primary and secondary order for influence factors
6 ract -I -I 53.3 66.3 158.6 0.31 0.66 is as follows: X3 > Constant > X2X2 > X2X4 > XI > X2 >

10 Fact -I -1 71.7 59.8 174.0 0.27 0.47 X3X4•

26 Center 0 0 0 0 69.2 65.8 92.3 0.29 0.62 The regression equation for OD is as follows:
II ract -I -I 85.7 67.3 125.4 0.30 0.58
OD = - 1. 018 + O. 023XI + O. 128X2 + O. 137X3 -
24 Axial 0 0 0 2 59.2 65.0 144.I 0.29 0.61
0. 009X2X2 + O. 008X2X4 - O. 012X3X4•
27 Center 0 0 0 0 68.3 72.7 82.2 0.31 0.72

22 Axial 0 0 2 0 70.5 75.7 47.3 0.36 0.85 Figure 8 shows the relationship between additive,
23 Axial 0 0 0 -2 89.3 79.5 145.I 0.29 0.61 rubber powder, and OD when the content of SBS is 5 %
29 Center 0 0 0 0 78.7 65.0 llO.3 0.33 0.64 and the content of SBR is 3% .
7 Fact -I -I 59.3 78.7 120.3 0.30 0.75 Figure 8 shows that the higher rubber powder con­
Fact -I 79.0 77.3 87.7 0.35 0.78 tent leads to the higher OD value, which can subsequent­
12 Fact -I 88.0 75.0 85.2 0.33 0.70 ly improve the overall performance. However, too much

J. Highway Transp. Res. Dev. (English Ed.) 2013.7:1-7.

 6 Journal of Highway and Transportation Research and Development

3. 4. 3 Model validation
0.8
0.6 This study tested the above formula. The actual val­
0.4
ues were compared with the calculated values obtained
0.2
o
through the mathematical model. The results are shown
-0.2 in table 10.
-0.4 Tab.10 Validation test
-0.6
Low-
-0.8
Elastic temper- Stiffness
Fluidity Penetration m-
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[tern recovery ature modulus OD

(mm) (O.lmm) value
(%) tensile (MPa)
Fig. 8 Response surface of OD effected by rubber
(mm)
powder and additive
Predicted value 73.1 7 0.6 85.31 0.35 0. 745

rubber powder makes dispersal difficult. The maxImum Actual value 0 67.3 67.7 >15 1 11.76 0.37 0.752

critical value is 25% . The effect of additive on OD value Deviation 8.6% 4.3% -23.7% -5.4% -0.9%
follows a parabolic trend, and the optimal content is 7 %
Table 10 shows that the deviations of individual in­
to 8% .
dicators are large, but on the whole, the forecasting
Figure 9 shows the relationship between SBS, SBR,
model is accurate. The deviation is within the actual al­
and OD value when the content of rubber powder is 25 %
lowable range and can be applied into practice.
and the content of additive is 7 % .
4 Conclusions

Based on the testing and analysis presented, the

conclusions of the study are summarized as follows:
(1) An environment-friendly sealant with high elas­
ticity and excellent high-temperature and low-temperature
performance was obtained with the 25 % rubber powder,
5 % SBS, 3 % SBR, and 7 % additive adding into neat
asphalt.
Fig.9 Response surface of OD effected by SBS and SBR
(2) Central composite design-response surface meth­

Figure 9 shows that the increase of low content SBS odology and overall desirability effectively optimize the

corresponds with the increase in OD value. When the formulation of composite modified asphalt sealant.

content of SBS is more than 5 % , the increase in SBS (3) Higher rubber powder content increases the e­

content corresponds with the decrease in OD value. lasticity of asphalt.

When the content of SBS is lower than 5% , the increase (4) SBR improves the mid-temperature and high­

in SBS significantly improves the performance of asphalt.
However, too much SBS induces the interaction among
different additives. The optimal content of SBS is 5 % .
Figure 9 shows that SBR has a little effect on the OD val­
ue, thus only a small amount of SBR is needed in actual
temperature shear deformation resistant ability, as well as
the low-temperature cracking resistant ability.
(5)The additive, as a kind of cosolvent, enhances
the compliance of the composite modified asphalt.
References

practice to play a role in complex modification with other

modifiers. The value determined in this paper is 3 % .
From the above analysis, we can draw a conclusion
that the best OD value can be obtained through the fol­
lowing modifier content: 25% rubber powder, 7% addi­
tive, 5% SBS, and 3% SBR.
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