USE OF REJUVENATORS IN RECLAIMED ASPHALT PAVEMENT

AND AGED BITUMEN

SEMINAR REPORT

Submitted in partial fulfilment of the requirements

for the award of M.Tech Degree in

Civil Engineering (Traffic and Transportation Engineering) of the

Dr. A P J Abdul Kalam Technological University

Submitted by

DEEPU R

M1 Traffic and Transportation Engineering

Roll No:

DEPARTMENT OF CIVIL ENGINEERING

COLLEGE OF ENGINEERING

TRIVANDRUM

2015
 DEPARTMENT OF CIVIL ENGINEERING
COLLEGE OF ENGINEERING
TRIVANDRUM

CERTIFICATE

This is to certify that this seminar report entitled Use of Rejuvenators in

Reclaimed Asphalt Pavement and Aged Bitumen is a bonafide record of the seminar
presented by Deepu R (M1 Traffic And Transportation Engineering) in partial fulfilment
of the requirements for the award of M.Tech Degree in Civil Engineering (Traffic and
Transportstion Engineering) of the Dr. A P J Abdul Kalam Technological University
during the year 2015.

Guided by PG Professor

Prof. Anil R Prof. A K Sheeja

Associate Professor Professor

Department of Civil Engg Department of Civil Engg

College of Engineering College of Engineering

Trivandrum Trivandrum
 ACKNOWLEDGEMENT

I express my heartfelt gratitude to my guide Prof. Anil R, Associate Professor,

Department of Civil Engineering, College of Engineering, Trivandrum for his valuable
guidance and suggestions in preparing and completion of this seminar report.

I would also like to thank Dr. M Satyakumar, Professor and Head of

Department, Department of Civil Engineering, Prof. Loui T R and Prof. Preethi P,
seminar coordinators, Dr. Satheesh Chandran R, Staff Advisor for their advice and
support.

I also express my sincere gratitude to my family and friends who encouraged

and supported to complete this work.

Above all I thank Lord Almighty for blessing me to complete this seminar report
on time.

DEEPU R
 ABSTRACT

Recycling asphalt pavement creates a cycle of reusing materials that optimizes

the use of natural resources. Reclaimed asphalt pavement (RAP) is a useful alternative
to virgin materials because it reduces the need to use virgin aggregate, which is a scarce
commodity. But the asphalt obtained from this RAP is aged and its properties will be
entirely different from that of a virgin binder. To modify these properties and make them
fit for use in constructions, rejuvenators have to be used.

Rejuvenator is a kind of asphalt additives to soften the stiffness of the oxidized

asphalt mixtures. Typically, rejuvenators contain a high proportion of maltenes
constituents that help re-balance the composition of the aged binders that lost its
maltenes during construction and field service.

In this seminar, the effects of adding rejuvenators on the reclaimed asphalt

pavement and aged bitumen are studied. The diffusion and distribution of rejuvenator
also affects the properties. Making rejuvenators into microcapsules is a new field of
study which will have a great effect on construction of bituminous pavements in coming
years. Various tests like penetration tests, dynamic shearing rheometer test are studied
and reported in this paper.
 CONTENTS

TOPIC PAGE NO:

1. INTRODUCTION

1.1 General 1

1.2 Reclaimed Asphalt Pavement 1

1.2.1 Advantages of RAP 3

1.3 Rejuvenators 3

1.3.1 Criteria for a Rejuvenator 4

1.3.2 Working Mechanism 6

1.3.3 Uses of Rejuvenators 6

1.3.4 Commonly Used Rejuvenators 7

2. CASE STUDIES

2.1 Effect of Rejuvenators on RAP 8

2.1.1 Material Selection 8

2.1.2 Hamburg Wheel Tracking Test and Associated Results 9

2.1.3 Overlay Tests and Associated Results 10

2.2 Evaluation of Diffusion and Distribution of 12

on Aged Bitumen and RAP

2.2.1 Materials 12

2.2.2 Test for Diffusivity of Rejuvenators 13

i. Diffusion Penetration Test and Associated Results 13

ii. Diffusion DSR Test and Associated Results 14

2.2.3 Test for Distribution of Rejuvenators 16

2.3 Self Healing of Aged Bitumen Using Microcapsules of Rejuvenators 17

2.3.1 Principle and Working of Microcapsules 17

2.3.2 Tests on Microcapsules 18

i. Characterization of Microcapsules 18

ii. Thermal Stability of Microcapsules 19

3. CONCLUSION 20
 LIST OF FIGURES

TITLE PAGE NO:

Fig. 1 Milled RAP 2

Fig. 2 Components of Asphalt 5

Fig. 3 Overlay Test Results 12

Fig. 4 Diffusion Penetration Test 14

Fig. 5 Diffusion DSR Test 15

Fig. 6 DSR Tests for Outer Layer and Inner Layer Asphalts 17

Fig. 7 ESEM Morphologies of Microcapsules Containing 19

Rejuvenator Fabricated Under Emulsion Rates of

(a) 1000 r min-1 (b) 2000 r min-1 (c) 3000 r min-1

Fig. 8 Optical Morphologies of Microcapsules in Melting 19

Bitumen under Different Temperatures

 1. INTRODUCTION

1.1 GENERAL

Recycled materials, such as recycled asphalt shingles (RAS) and reclaimed asphalt
pavement (RAP), have been widely used in asphalt paving industry, and the trend seems
to use more and more, which can save taxpayer dollars, preserve energy and protect the
environment. However, these recycled materials are often highly aged and cause
potential durability issue for asphaltic layers. The use of more RAP and RAS often
makes asphalt mixtures too stiff, and consequently less workable and difficult to
compact in the field, which may ultimately lead to premature field failure. To balance
out the impact of stiff binder of recycled materials, rejuvenators have been recently
evaluated.

Every year about 95% of the almost 100 million tonnes of bitumen is applied in the
paving industry where they essentially act as a binder for mineral aggregates to form
asphalt. One important issue needed to be considered is the ageing of bitumen from
climate and traffic in service life. After years of usage, the stiffness of asphalt concrete
increases while its relaxation capacity decreases, the binder becomes more brittle
causing development of micro-cracks and ultimately cracking of the interface between
aggregates and binder occurs. The ageing problem of bitumen leads to pavement failure
including surface ravelling and reflective cracking. It will increase the expense of
maintaining bituminous pavements. An increase in the application of a higher
percentage of the preservation and renovation of asphalt pavement is achievable using a
rejuvenator. It is the only one method that can restore the original properties of the
pavements. The most important goal of utilizing rejuvenator products is to restore the
asphaltenes/maltenes ratio. Rejuvenating agents have the capability of reconstituting the
binders chemical composition and consist of lubricating and extender oils containing a
high proportion of maltene constituents.

1.2 RECLAIMED ASPHALT PAVEMENT

Existing asphalt pavement materials are commonly removed during resurfacing,

rehabilitation, or reconstruction operations. Once removed and processed, the pavement
1
 material becomes RAP, which contains valuable asphalt binder and aggregate (see
figure 1). Every year, over 80 percent of RAP is recycled, making asphalt the most
frequently recycled material. RAP is most commonly used as an aggregate and virgin
asphalt binder substitute in recycled asphalt paving, but it is also used as a granular base
or sub-base, stabilized base aggregate, and embankment or fill material. It can also be
used in other construction applications. RAP is a valuable, high-quality material that can
replace more expensive virgin aggregates and binders.

Fig. 1 Milled RAP

(Source: Stephen J Cooper (2011))

There are four major asphalt production cost categories: (1) materials, (2) plant
production, (3) trucking, and (4) lay down (i.e., construction). Materials are the most
expensive production cost category, comprising about 70 percent of the cost to produce
HMA. The most expensive and economically variable material in an asphalt mixture is
the asphalt binder. It is most commonly used in the intermediate and surface layers of
flexible pavement to provide tensile strength to resist distortion, protect the asphalt
pavement structure and subgrade from moisture, and provide a smooth, skid-resistant
riding surface that withstands wear from traffic. As a result, the most economical use of
RAP is in the intermediate and surface layers of flexible pavements where the less
expensive binder from RAP can replace a portion of the more expensive virgin binder.

2
1.2.1 Advantages of RAP

With increased demand and limited aggregate and binder supply, HMA
producers have begun using reclaimed asphalt pavement (RAP) as a valuable
component in HMA. As a result, there has been renewed interest in increasing the
amount of RAP used in HMA. While several factors influence the use of RAP in asphalt
pavement, the two primary factors are economic savings and environmental benefits.
RAP is a useful alternative to virgin materials because it reduces the use of virgin
aggregate and the amount of virgin asphalt binder required in the production of HMA.
The use of RAP also conserves energy, lowers transportation costs required to obtain
quality virgin aggregate, and preserves resources. Additionally, using RAP decreases the
amount of construction debris placed into landfills and does not deplete non renewable
natural resources such as virgin aggregate and asphalt binder. Ultimately, recycling
asphalt creates a cycle that optimizes the use of natural resources and sustains the
asphalt pavement industry.
The use of more RAP often makes asphalt mixtures too stiff, and consequently
less workable and difficult to compact in the field, which may ultimately lead to
premature field failure. Some serious problems, such as low early stiffness, cracking,
ravelling and short durability, are also commonly observed for hot recycling asphalt
pavement during use in the field.

1.3 REJUVENATORS

Rejuvenator is a kind of asphalt additive to soften the stiffness of the oxidized

asphalt mixtures. Typically, rejuvenators contain a high proportion of maltenes
constituents that help re-balance the composition of the aged binders that lost its
maltenes during construction and field service. Recently, rejuvenating agents have been
receiving attention from the pavement research community because they can improve
the engineering properties of asphalt mixtures containing high content recycled
materials.

3
1.3.1 Criteria for a Rejuvenator

Asphalt binders cannot be represented by a single chemical formula. The

American Society of Testing and Materials (ASTM) defines it as "a dark brown to black
cementitious material in which the predominating constituents are bitumen which occur
in nature or are obtained in petroleum processing." Asphalt binders are, however,
fractionated into two subdivisions, i.e., asphaltenes and maltenes. Asphaltenes (A) is
defined as that fraction of the asphalt insoluble in n-pentane. The function of the
asphaltenes is to serve as a bodying agent. Maltenes is the collective name for the
remainder of the asphalt material left after precipitation of the asphaltenes. Four
principle bodies of maltenes have been identified and each has a specific function.
These four bodies are:
Polar compounds or Nitrogen bases (N) - components of highly reactive resins, which
act as a peptizer for the asphaltenes.
First acidiffins (A1) - components of resinous hydrocarbons which function as a
solvent for the peptized asphaltenes.
Second acidiffins (A2) - components of slightly unsaturated hydrocarbons that also
serve as a solvent for the peptized asphaltenes.
Saturated hydrocarbons or paraffins (P) components of hydrocarbons, which
function as a jellying agent for the asphalt components.

The cementing agent in an asphalt pavement, the asphalt binder (normally 4-7%
by weight) represents the component that experiences premature hardening as a result of
oxidation. Asphalt pavements, which are structurally sound, deteriorate as a result of
oxidation and occasionally as a result of incorrect design or improper construction
practice. The first phenomena that of oxidation, is prevalent in all asphalt pavements.

It is reported that the "A" and "P" asphalt components are the most stable; and the "N",
"A1", and "A2" components are more subject to oxidation in descending order,
respectively. Consequently, during oxidation the "N" components convert to "A"
components rapidly while the conversion process for the "A1" and "A2" components
proceed at a slower rate. This process results in an increase in the "A" fraction of
4
 asphalt with time, and decreases the "N", "A1", and "A2" components. It is also
reported the "the maltenes parameter (N+A1)/(P+A2), the ratio of chemically more
active to less reactive components present in the asphalt binder, is a measure of
predictable durability."
During the process of weathering or oxidation, the ratio of maltenes to
asphaltenes is reduced with the result being a dry and brittle pavement. Therefore, if a
rejuvenator is to successfully resurrect an aged facility, it must be able to penetrate the
pavement and to a limited depth improve or restore the maltenes to asphaltenes balance.
A reasonable measure of the ability of a rejuvenator to improve a pavement's durability
can be had:
By comparing the penetration at 250C (770F) of the asphalt binder extracted from
untreated and treated cores.
By comparing the viscosity at 60 0C (1400F) of the asphalt binder extracted from
untreated and treated cores.
By comparing the percentage loss of aggregate when untreated and treated samples are
subjected to a pellet abrasion test.
In summary, the criteria for a rejuvenator must involve two phenomena:
First, the product must contain maltenes fractions of asphalt in order to improve and
balance the maltenes to asphaltenes ratio.
Secondly, a test method must be employed to measure improved durability of a
pavement; e.g., an asphalt penetration, viscosity, or abrasion loss test.

Fig. 2 Components of Asphalt

(Source: Robert E Boyer (2000))

5
1.3.2 Working Mechanism

The working mechanism (or diffusion process) of a rejuvenator consists of the

following four steps:
I. The rejuvenator forms a very low viscosity layer that surrounds the asphalt-coated
aggregate which is highly aged binder layer.
II. The rejuvenator begins to penetrate into the aged binder layer, decreasing the amount
of raw rejuvenator that coats the particles and softening the aged binder.
III. No raw rejuvenator remains, and the penetration continues, decreasing the viscosity
of the inner layer and gradually increasing the viscosity of the outer layer.
IV. After a certain time, equilibrium is approached over the majority of the recycled
binder film.

1.3.3 Uses of Rejuvenators

All rejuvenators are applied in the same way by spraying the chemical onto the
pavement surface with an asphalt distributor. However, the procedures may slightly vary
because of the different products and because of the different end results desired.
Discussion of the use of rejuvenators can be considered in three separate categories;
new construction, maintenance, and re-construction.

Using a rejuvenator on new construction does not seem to be logical at first

glance. However, it has been established that the greatest change in composition of an
asphalt binder takes place during the manufacture of the hot mix asphalt (HMA).
Applying a rejuvenator to a new surface a few weeks after it has been laid does several
things to the pavement. Besides restoring the original asphalt properties that were lost in
the HMA manufacture, the chemical assists in sealing the pavement as well as in
improving the durability of the surface course.
Maintenance can be subdivided into preventive and corrective maintenance.
Preventive maintenance should be applied to pavements at the first signs of aging of the
surface course, pitting, ravelling, shrinkage, and cracking. Some pavement experts
maintain that preventive maintenance should begin before any of these described signs
occur. However, to do this, there must be a certain amount of clairvoyance involved in
determining the right time before these conditions show up. Starting a maintenance
6
program too early can become a costly item. Nonetheless, applying the rejuvenator at
periodic intervals can restore the asphaltene-maltene balance which is so essential to
maintain a ductile, pliable pavement.
Corrective maintenance involves reworking and salvaging existing road mixes.
Using a rejuvenator in this type of maintenance can facilitate scarifying and mixing. It
will aid in re-plasticizing old asphalt and improve its durability. This form of
maintenance should be considered when the road mix surface appears weathered and
crusted and cannot be restored by applying only a rejuvenator.
The third category of rejuvenator use is that of re-construction. This involves
more than applying a rejuvenator emulsion onto the surface and rolling the treated
pavement. Work in the category is undertaken when the pavement has outlived its life;
when preventive maintenance has failed to stop the pavement deterioration; or when a
HMA overlay is to be placed over the existing pavement. The overlayment may be due
to a need for increased structural strength, or it may be necessitated by failure of the old
surface to respond to normal maintenance.
If the existing pavement possesses good structural qualities and the overlay is
being placed to increase its strength, a rejuvenator can be applied to the old surface
several days before the overlay is constructed. This application will cause the existing
surface to soften, regain some of its original ductility, and will promote a good bond
between the old and new surfaces.

1.3.4 Commonly Used Rejuvenators

The following is a listing of the rejuvenator materials which are commonly

available. The listing includes the product name and the classification of the base
material:
1. Asphalt Rejuvenator 2000 (AR 2000); Coal-Tar Based Material.
2. Asphalt Pavement Rejuvenator (APR-100); Petroleum-Based Material.
3. Bituminous Concrete Rejuvenator (BCR 2000); Coal-Tar Based Material.
4. Bituminous Concrete Rejuvenator (BCR 3000); Coal-Tar Based Material (with
proprietary rejuvenating oils).
5. CBRT-SO; Coal-Tar Based Material.
6. CPR - Conditioning Pavement Rejuvenator; Coal-Tar Based Material.
7
7. GSB - Modified; Petroleum-Based Material; Emulsified Asphalt (with proprietary
rejuvenating oils and gilsonite).
8. Reclamite; Petroleum-Based Material.
9. RejuvaSeal N; Coal-Tar Based Material.
10. RejuvaSeal 50; Coal-Tar Based Material (with proprietary rejuvenating oils).
11. RejuvaSeal 500; Coal-Tar Based Material (with proprietary rejuvenating oils).

2. CASE STUDIES

2.1 EFFECT OF REJUVENATORS ON RAP

This study evaluated the impacts of three commercial rejuvenators on

performance and engineering properties of mixtures containing recycled materials (i.e.,
RAP and RAS) in terms of moisture resistance, cracking resistance, dynamic modulus,
and rutting resistance. The three rejuvenators were designated as R1, R2 and R3.

2.1.1 Material Selection

Three different control mixtures containing RAS only, RAP and RAS, and RAP
only, respectively, were produced to compare the mixture performance and engineering
properties to those of mixtures incorporated with three different commercial
rejuvenators. Local aggregates used at three different field projects were collected to
produce asphalt mixtures in the laboratory. Each mixture contains different contents of
RAP and/or RAS (i.e., 5% RAS, 13% RAP plus 5% RAS, and 19% RAP, respectively).
A PG 64-22 asphalt binder was used to produce each mixture, and binder contents for
different mixtures, 5.2%, 5.1%, and 4.8%, were determined as appropriate values that
satisfy all key volumetric characteristics of asphalt mixtures.
Three different commercial rejuvenators were chosen in this study. The dosage
of each rejuvenator was recommended by each specific manufacturer. Two of them (R1
and R2) were directly added to the virgin binder, while the other one (R3) was blended
into the recycled materials. The following is a short summary of the information on the
8
rejuvenators used in this study:
R1: directly added to virgin binder (0.6% of total asphalt binder by weight).
R2: directly added to virgin binder (1.5% of total asphalt binder by weight).
R3: dry recycled materials were mixed with a moisture content of 1% by weight
and then 2% agent (by dry weight) heated at 65 0C directly was blended with wet
recycled materials.

2.1.2 Hamburg Wheel Tracking Test and Associated Results

Hamburg Wheel Tracking Test (HWTT) was conducted at a temperature of 50 0C

in accordance with TEX-242-F, Test Procedure for Hamburg Wheel-Tracking Test
(HWTT). A Super pave gyratory compactor was used to mould cylindrical specimens
with a diameter of 150 mm and a height of 62 mm. A masonry saw was used to cut
along the edge of the cylindrical specimens. The target air void of specimens was 7
1%. To evaluate the rutting susceptibility and moisture resistance, specimens were
submerged under water at a temperature of 500C during the test, and a linear variable
differential transducer (LVDT) device measured deformations of specimens. The stop
criterion was rut depth of 12.5 mm or 20,000 passes.
Table 1 summarizes the rut depths from each test at different passes. The
observations are discussed below:
For the 5% RAS mixtures, as shown in Table 1, R2 and R3 rejuvenating agents
significantly improved the rutting/moisture resistance of the mixtures, while the
performance of the mixture with R1 rejuvenating agent was similar to the 5%
RAS control mixture.
For the 13% RAP/5% RAS mixtures, all rejuvenated mixtures were not better
than the control mixture.
For the 19% RAP mixtures, R1 and R2 rejuvenating agents improved HWTT
results but not significantly.
In summary, based on the test results obtained from this study, the incorporation of
rejuvenators with RAP and/or RAS improved the rutting resistance and moisture
susceptibility of HMA mixtures, although a clear trend from all three mixtures was not
observed.
9
Table 1 Hamburg Testing Results
 Mix Type Passes Control Mix R1 R2 R3
5000 3.40 5.08 2,59 3.48
10000 6.23 9.73 3.14 4.29
5% RAS
15000 12.33 12.82 3.56 5.42
20000 N/A N/A 4.02 9.88
13% RAP 5000 1.97 5.12 3.81 3.07
10000 11.22 12.65 12.71 11.91
Plus 5%
15000 12.60 N/A N/A 12.61
RAS 20000 N/A N/A N/A N/A
5000 12.55 9.54 6.05 12.54
10000 N/A 12.71 13.00 N/A
19% RAP
15000 N/A N/A N/A N/A
20000 N/A N/A N/A N/A
(Source: Soohyok Im et.al. (2014))

2.1.3 Overlay Test and Associated Results

The overlay test was used to evaluate the cracking resistance of the asphalt
mixtures. This test procedure is described in TEX-248-F, Test Procedure for Overlay
Test (OT). Five trimmed specimens from each mixture targeting air void of 7 1% were
prepared. Before testing, individual OT specimens were conditioned in an
environmental chamber with a target temperature of 250C. The sliding block applied
tension in a cyclic triangular waveform to a constant maximum displacement of 0.06
cm. The sliding block reached the maximum displacement and then returned to its initial
position in 10 s. The time, displacement, and load corresponding to a certain number of
loading cycles were recorded during the tests. The number of cycles to failure is
reported at the end of the test. The larger the OT cycles, the better cracking resistance is.
The average OT cycles of the five specimens from each mixture tested is presented in
Fig. 3. For the 5% RAS mixtures, R1 rejuvenating agent exhibited the best performance,
followed by the R2 rejuvenating, and then R3 rejuvenating agent. The control mixture
showed the lowest value of cracking life. Similar results were observed for both the
13% RAP/5% mixtures and the 19% RAP mixtures, but the performance

10
ranking of the rejuvenators were changed as shown in Fig. 3. In summary, all the
mixtures with rejuvenators exhibited higher OT cycles (approximately from 110% to
300% improvements) than the control mixtures.
 20
18
16
14
12
10
8
6
OT Cycles to Failure
4
2
0

(a) 5% RAS Mixtures

16

14

12

10

8
OT Cycles to Failure
6

0
Control Mixture With R2

(b) 13% RAP/ 5% RAS Mixtures

11
 100
90
80
70
60
50
40
OT Cycles to Failure 30
20
10
0

(c) 19% RAP Mixtures

Fig. 3 Overlay Test Results

(Source: Soohyok Im et.al. (2014))

2.2 EVALUATION OF DIFFUSION AND DISTRIBUTION OF

REJUVENATORS ON AGED BITUMEN AND RAP

There are currently no standard test procedures to evaluate the real blending status
of the rejuvenator and aged asphalt in a recycled asphalt mixture. Laboratory tests were
designed in this study to reveal the diffusion and distribution of the rejuvenator in the
aged asphalt of the RAP. The influences of the diffusion and distribution of the
rejuvenator on the performance of the recycled asphalt mixture were also evaluated.
2.2.1 Materials
Four different rejuvenators, named A, B, C and D, were used in this study.
Rejuvenators A and B have much lower viscosity than rejuvenators C and D because
rejuvenators A and B are mainly composed of light oils, whereas rejuvenators C and D
are composed of light oils and tackifying resins. Clearly, after aging via the thin film
oven test (TFOT), rejuvenators A and B have higher residual viscosity ratios and quality
changing percentages than rejuvenators C and D. Therefore, the thermal stability and
aging resistance of rejuvenators A and B are worse than those of rejuvenators C and D.
12
 Artificial RAP was prepared by blending aged asphalt with aggregates and then
cured in an oven at 1000C for 12 h. Two different types of artificial RAP were prepared.
One type is artificial RAP with graded aggregates, which was prepared based on the
previous mix design for a virgin asphalt mixture. Aged asphalt was used instead of
virgin asphalt to mix with the graded aggregates to obtain the artificial RAP. The other
type is artificial RAP with single-size aggregates, which was prepared by blending aged
asphalt with 4.75-mm aggregates and mineral fillers. For each sample, 500 g of 4.75-
mm aggregates, 10 g of mineral fillers and 9.6 g of aged asphalt were used to obtain the
artificial RAP. Meanwhile, aggregates with size of 13.2 mm were prepared as new
aggregates.

2.2.2 Test for Diffusivity of Rejuvenators

To evaluate the diffusivity of the rejuvenator in the aged asphalt, diffusion tests,
named the diffusion-penetration test and the diffusion-DSR test, were designed
based on the penetration test and the dynamic shearing rheometer (DSR) test,
respectively.

i. Diffusion Penetration Test and Associated Results

During the diffusion-penetration test, the penetration test sample of aged asphalt
was prepared. Next, 10% of the rejuvenator by weight of the aged asphalt sample was
poured into the penetration mould to form a rejuvenator layer on the top surface of the
aged asphalt sample. The penetration sample was cured in an oven at 100 0C for different
times of 0.5, 1, 2, 3 and 4 h. After curing and cooling down the sample, the rejuvenator
remaining on the top surface of the aged asphalt sample was rinsed. The penetration test
was then conducted on the final sample at 250C.

The average penetrations of the samples with different rejuvenators at different

oven curing times are shown in Fig. 4. The penetration is found to increase with
increasing curing time. This result indicates that, with increasing curing time, the
rejuvenators continue to diffuse into the aged asphalt and lower the viscosity of the aged
asphalt. This result also shows that, for all of the four rejuvenators, the amounts of
13
 penetration increase rapidly during the first hour and then increase slowly with
increasing curing time. With the rejuvenator diffusing into the aged asphalt, the
concentration of the rejuvenator decreases and the viscosity difference between the
rejuvenator and the aged asphalt decreases; it becomes increasingly difficult for the
rejuvenator to further diffuse into the aged asphalt. Based on Fig. 4, at the same curing
time, a rejuvenator with lower viscosity is found to lead to higher penetration of the
asphalt sample.

120

100

80

60 A
Penetration(0.1mm)
B
40 C
D
20

0
0 0.5 1 2 3

Time

Fig. 4 Diffusion Penetration Test

(Source: Tao Ma et.al. (2015))

ii. Diffusion DSR Test and Associated Results

During the diffusion-DSR test, the DSR test sample of the aged asphalt was
prepared. Next, 10% of the rejuvenator by weight of the aged asphalt sample was
dropped onto the top surface of the aged asphalt sample to form a rejuvenator film. The
DSR sample was cured in oven at 1000C for 4 h. After curing and cool down, the
rejuvenator remaining on the top of the aged asphalt sample was rinsed. The DSR test
was then conducted to measure the G/sin of the final sample at 520C.
14
 To conduct a comparative analysis, each rejuvenator was also used to fully blend
with the aged asphalt to obtain the recycled asphalt named as mix-recycled asphalt. The
average G/sin values via the DSR test for diffusion-recycled asphalt and mix-recycled
asphalt with different rejuvenators are shown in Fig. 5. During the diffusion test, it is
expected that, if the rejuvenator is fully diffused into the aged asphalt, then the
diffusion-recycled asphalt should have the same G/sin as the mix-recycled asphalt;
otherwise, the G/sin of diffusion-recycled asphalt should be greater than that of the
mix-recycled asphalt. From Fig. 5, the G/sin of the mix-recycled asphalt and the
diffusion-recycled asphalt are found to be close to each other for rejuvenators A and B.
This result indicates that all of the rejuvenators have diffused into the aged asphalt.
Meanwhile, for both rejuvenators C and D, the G/sin values of diffusion-recycled
asphalt are obviously smaller than that of the mix-recycled asphalt. Compared to the
light oil components, the diffusivity of the tackifying resin components is much weaker.
Thus, one of the possible reasons for the observed difference is that the light oil
components of rejuvenators C and D fully diffused into the aged asphalt, while the
tackifying resin components of rejuvenators C and D did not fully diffuse into the aged
asphalt. The loss of tackifying resin components can lead to a lower G/sin of the
recycled asphalt.

10
9
8
7
6
5
G/sin
4 Mix Recycled Asphalt
3 Column1
2
1
0
A B C D

Rejuvenators

Fig. 5 Diffusion DSR Test

(Source: Tao Ma et.al. (2015))
15
2.2.3 Test for Distribution of Rejuvenators

The phased extraction and recovery test was designed to evaluate the
distribution of the rejuvenator in the aged asphalt of the RAP. For each test sample, 1.5
kg of artificial RAP with graded aggregates was prepared and then blended with the
rejuvenator at 1500C for 1 min to obtain the recycled asphalt mixture. After cooling
down, the recycled asphalt mixture was placed into a net basket and immersed in 1500
ml of trichloroethylene solvent for 45 min. Based on the trial tests, approximately half
of the recycled asphalt was dissolved in the trichloroethylene solvent; this dissolved
asphalt is considered as the outer-layer asphalt surrounding the aggregates in the
recycled asphalt mixture. Next, the recycling asphalt mixture was immersed again in a
new trichloroethylene solvent for another 45 min to dissolve the remaining recycling
asphalt. This dissolved asphalt is considered as the inner-layer asphalt surrounding the
aggregates in the recycled asphalt mixture. A glass microfiber filter was used to
eliminate the fine aggregates and the mineral fillers in the trichloroethylene-asphalt
solutions. Subsequently, the recovery test was performed by using a rotary vacuum
evaporator to obtain the outer-layer and inner-layer asphalt from the trichloroethylene-
asphalt solutions separately. The DSR tests were conducted to measure the G/sin of the
outer-layer asphalt and the inner-layer asphalt.

The value of G/sin of the outer-layer and inner-layer asphalts for the RAP
without the rejuvenator and the recycled asphalt mixtures with different rejuvenators are
shown in fig 6. Clearly, without the influences of the rejuvenator, the values of G/sin
of the outer-layer and inner-layer asphalts of the RAP are similar to each other. It is
expected that, if the rejuvenator mixes well with the aged asphalt in the recycling
asphalt mixture, then the G/sin of the outer-layer and inner-layer asphalts of the
recycled asphalt mixture should also be similar to each other. However, for each
rejuvenator, the G/sin of the outer-layer asphalt is found to be much smaller than that
of the inner-layer asphalt. This result proves that, during a short blending process, it is
difficult for the rejuvenator to diffuse and mix well with the aged asphalt. Most of the
rejuvenator may just remain in the outer layer of the aged asphalt.

16
 12

10

6
G/sin
Inner Layer
4
Column1
2

0
Non A B C D
Rejuvenators

Fig. 6 DSR Tests for Outer-Layer and Inner-Layer Asphalts

(Source: Tao Ma et.al. (2015))

2.3 SELF HEALING OF AGED BITUMEN USING MICROCAPSULES OF

REJUVENATORS

An increase in the application of a higher percentage of the preservation and renovation

of asphalt pavement is achievable using a rejuvenator. It is the only one method that can
restore the original properties of the pavements. When applying these materials, the
road must be closed for some time after their application. The rejuvenator, at the same
time, will cause a high reduction of surface friction of pavement for vehicles. Moreover,
an important aspect of these rejuvenators is that they may be dangerous to the
environment. Encapsulation rejuvenator inside-usage in asphalt may be an alternative
approach. These microcapsules had satisfactory thermal stability in bitumen and reliable
mechanical properties resisting the mixing process and temperature changes. It had been
proved that this product was environmental-friendly powder encapsulating suitable size
rejuvenator.

2.3.1 Principle and Working of Microcapsules

Monomer is encapsulated and embedded within the matrix materials. When the
crack gets to the microcapsule, the capsule breaks and the monomer bleeds into the

17
crack, where it can polymerize and mend the crack. Microcapsules in bitumen can be
broken by micro-cracks, then the released rejuvenator seals the micro-cracks and
permeate surrounding bitumen. With the help of capillarity, rejuvenator flows into
narrow micro-cracks without the assistance of, and in opposition to, external forces. As
bitumen acts as thin layers between aggregates which are usually less than 50 m, size
of microcapsules containing rejuvenators should be smaller than 50 m to avoid being
squeezed or pulverized during asphalt forming. The shell thickness must be controlled
to make sure that the microcapsules have excellent thermal stability. Thicker shell will
enhance the mechanical properties of microcapsules, but the micro-cracks may not be
able to break these microcapsules. It must be prevented that the micro-cracks
propagation will go round the shells.

2.3.2 Tests on Microcapsules

The shell material was commercial pre-polymer of melamineformaldehyde

modified by methanol. The core material used as rejuvenator is dense, aromatic oil
obtained from Petro plus Refining Antwerp. A small percentage of the anhydride groups
have been established with a low molecular weight alcohol and it is fine, off-white, free
flowing powder with a faint, aromatic odour. The bitumen used in this study was 80/100
penetration grade obtained from Kuwait Petroleum. The aged bitumen 40/50 penetration
grade was artificially produced by thin film oven test.

i. Characterization of Microcapsules

The mean size is an important parameter for microcapsules containing

rejuvenator influencing their application possibility in asphalt. Too tiny size will limit
the encapsulated content of rejuvenator. In another case, large microcapsules may be
broken in mixing with asphalt concrete. Figure. 7 shows the Environmental Scan
Electron Microscopy (ESEM) morphologies of microcapsules (core/shell ratio of 3/1)
with different mean sizes fabricated under emulsion stirring rates of 1000, 2000 and
3000 r min-1. It can be seen that the mean sizes decreased sharply with the decreasing of
stirring rates because higher stirring rates will smash the oily rejuvenator into smaller
droplets.
18
 Fig. 7 ESEM Morphologies of Microcapsules Containing Rejuvenator Fabricated
Under Emulsion Rates of (a) 1000 r min-1 (b) 2000 r min-1 (c) 3000 r min-1

ii. Thermal Stability of Microcapsules

To verify the thermal stability of microcapsules in bitumen, the microcapsules

were mixed with melting bitumen under various temperatures for 30 min. Then shape of
microcapsules was observed by an optical microscope. The microcapsules had an
average size of about 16 m which were fabricated under core material stirring rate of
3000 r min-1(core/shell ratio of 2/1). In Fig. 8 (a), it can be seen that microcapsules
survived in bitumen under temperature 1400C. With the increasing of temperature to
1600C(Fig. 8(b)), 1800C(Fig. 8(c)) and 2000C(Fig. 8(d)), the microcapsules still kept
their global shape without crack and thermal decomposition. These results indicate that
microcapsules can resist the thermal effect of bitumen in application.

Fig. 8 Optical Morphologies of Microcapsules in Melting Bitumen under Different

Temperatures
19
 3. CONCLUSION

The following generic conclusions were drawn based on the literatures studied and case
studies reported.
Use of rejuvenators in reclaimed asphalt pavement materials improved the
cracking resistance and reduced the stiffness of aged binder.
Moisture susceptibility and rutting resistance of mixtures containing recycled
materials are improved by the incorporation of rejuvenators.
The use of rejuvenated RAP can be a competitive solution for reducing
environmental impacts related to virgin material extraction and waste disposal.
The complete diffusion of the rejuvenator into aged asphalt of the RAP is found
to be difficult to achieve. To improve the distribution of rejuvenator in the
recycled asphalt, it is important to reduce viscosity, enhance thermal stability
and guarantee the content of the rejuvenator.
The microcapsules of rejuvenator can survive in melting bitumen with a good
thermal stability.
The microcapsules can be broken by micro-cracks and leaked the oily liquid
rejuvenator into micro-cracks. This rejuvenator will mend the crack.
With the help of penetration of rejuvenator, the aged bitumen has a trance to
recover its virgin properties.

20
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3. Jun-Feng Su, Erik Schlangen, Ying-Yuan Wang (2015)," Investigation the self healing
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4. Robert E Boyer (2000)," Asphalt Rejuvenators -Fact or Fable.

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