Sustainable Production of WMA with Pine Gum Wax Modification: Physical and Rheological Evaluation

doi:10.21203/rs.3.rs-3549860/v1

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Sustainable Production of WMA with Pine Gum Wax Modification: Physical and Rheological Evaluation

https://doi.org/10.21203/rs.3.rs-3549860/v1

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Warm mix asphalt (WMA) produced with (S®), which is a common organic additives, (S®-WMA) shows an over-rising softening point value and a decrease in stripping resistance. These two shown behavior of S®-WMA are seen some problems that need to be solved. Because they adversely affect the structural performance of the pavement and therefore, this study is established to evaluate the possible solutions to these two problems by one more modification processes. It was investigated in this study whether modifying S®-WMA by using pine gum wax (PGW), which is a product that has not been investigated before, be a solution to the aforementioned problem. In this context, WMA was produced with S® at 1%, 2% and 3% (by bitumen mass) in 1% increments. Since PGW was not previously used as an additive to modify S®-WMA, it was added within a limit as 1% (by mass of bitumen). Physical and rheological standard tests were performed on each sample in order to demonstrate the variation in the properties of the produced S®-WMA with 1% PGW compared to S®-WMA. The results showed that the addition of 1% PGW to S®-WMA caused significant reduction in the softening point and an improvement in stripping resistance compared to S®-WMA. Thus, it shows that the use of PGW can be a potential solution for the two mentioned problems. It can also be emphasized that S®-WMA sample can be an efficient, economical and environmentally friendly solution by modifying it with PGW without compromising its properties. However, more in-depth research is required due to the use of a limited PGW contribution rate.

Warm mix asphalt

Sasobit®

Pine Gum Warm Wax

Softening Point

Stripping Resistance

Bitumen is a valuable and versatile building material due to its sensitivity to heat and its properties such as being both viscous and elastic under thermal changes, as well as having a sticky and oily structure [1]. It consists of hydrocarbon molecules, which can be obtained naturally and/or artificially after the processing of crude oil [2]. Owing to the aforementioned properties, it is used as binder in the construction of flexible pavements in the transportation sector, which are mainly constructed with hot mix asphalt (HMA). Although it constitutes about 5–8% of the HMA by mass, it has a significant impact on the structural and functional performance of HMA [3]. With technological advancements, highway pavements are exposed to harsh environmental conditions and increased traffic loads due to the varying combination of vehicles. In order to develop a durable and flexible pavement throughout its service life, there is a need to improve bitumen properties without compromising its current performance [4]. To achieve this, bitumen has been modified for many years with different natural, chemical, commercial and industrial or municipal waste products [5].

HMA causes environmental pollution by generating high amounts of greenhouse gas emissions during the production and construction process. It also jeopardizes occupational health and safety due to its high operating temperature. During the production and construction processes, HMA requires high temperatures such as 150°C and above, and significant amounts of heat energy, which is usually derived from fossil fuels [6]. Environmental pollution caused by the high amount of emission gases from fossil fuels, one of the main sources of global warming, has led researchers to search for solutions to high-temperature HMA production. In addition, increasing social environmental awareness and sensitivity has accelerated this solution process. In this context, scientists have been in a long-standing effort to produce HMAs at lower temperatures on the basis of energy efficiency, economy and environmental friendliness [7]. Therefore, researchers have developed a new asphalt technology called warm mix asphalt (WMA) for the production and construction of a sustainable, economical, ecological and energy efficient flexible pavement, as well as providing technical benefits. Over time, the use of HMA technology is gradually being replaced by WMA technology[8].

WMA technology aims to improve workability by reducing viscosity and reduce fuel consumption by lowering the processing temperature. Compared to HMA, WMA allows processing at lower mixing and compression temperatures, such as between at 100–135°C or may be lower than that of them [9]. Thus, it protects the environment by reducing greenhouse gas emissions and contributes to occupational health and safety by providing a lower working temperature in the workplace [10].

Today, there are several widely used WMA technologies with different levels of effectiveness for a common purpose [8]. These are classified as (1) chemical, (2) foaming and (3) organic warm mix technologies [11]. There are a large number of additives developed for use in WMA production. Some of these might be as Revix, Evotherm, Cecabase RT, Interlow, ZycothermTM Rediset ® LQ for chemical techniques; Licomont ® BS, Asphaltan A, Asphalt B, Sasobit ® and Ecoflex for organic warm mix ones, and Advera®, Zeolite, Aspha-min for foaming ones [12]. The organic WMA technologies used in this study are mostly used in the transportation industry [13, 14]. This technology aims to significantly reduce the viscosity of the binder by mixing WMA additives with some modified bitumen or HMA [15–17]. In this technology, after the additive is added to the bitumen, it crystallizes during cooling, resulting in a harder binder. This is because the most well-known and widely used organic additive used in this study is Sasobit®, which is produced by the Fisher-Tropsch (FT) process [18], where FT is produced by a process using natural gas [19].

Instead of presenting a detailed individual literature summary, we highlight the outputs of the review articles, where hundreds of studies are cited within it to provide a broad perspective on WMA characteristic properties. Some of the evaluated review papers can be exemplifedi with the ones presented by Cheraghian, et al. [20], Diab, et al. [21] Farooq and Mir [22], Prakash and Suman [23], Abdullah, et al. [24], Guo, et al. [26]. All of these presented the advantages and disadvantages of WMA technology and they divided the advantages under the environmental, economic and technical categories. Using of WMA technology is mainly associated with environmental benefits that including reducing energy use and greenhouse gases amount due to lower heat processing compared to HMA. It has been determined that with the use of WMA, greenhouse gases (Carbon dioxide, Sulphur dioxide, Nitrous oxide, Carbon monoxide, etc.) emitted from the use of fossil fuels can be reduced by about 10–70% and the amount of energy used in WMA production can be about 20% less than that used in HMA processes. Therefore, depending on parameters such as the technology, type and quantity of product, a reduction in WMA production and pavement construction costs of between 10% and 40% can be achieved. Cost savings can be achieved by improving occupational health and safety by working at lower temperatures and subsequently increasing the performance of employees. Besides the environmental benefits, there are also some technical benefits, which can be expressed as follows: (1) Improved workability throughout the entire construction phase; (2) Extending the construction season and making it possible to work in cold weather conditions; (3) Shortening the time required to open the pavement to traffic by providing faster curing following pavement construction; (4) Ability to allow longer distances and haulage times between the construction site and bitumen plants due to low temperature operation; (5) Ability to show significant enhancement or reduction in binder and mixtures performances.

The occurrence of excessive increase in softening point and low moisture resistance are the two problem for (S®-WMA). In light of numerous available studies [5, 13, 27–35], solutions can be on basis of modifying WMA with additional additives. To overcome these problems, S®-WMA was prepared with S® in a 1% increase from 1–3% (by weight of bitumen). Pine Gum Wax (PGW), which is not used before in any kind of WMA preparation is used for modification of S®-WMA. Besides being an organic product like S®, the main reason behind the use of PGW is that it exhibits some physical and mechanical properties similar to bitumen. Accordingly, to make a preliminary on the use of PGW, only 1% (by weight of bitumen) was added to each S®-WMA produced at each rate of S® for modification purpose. Finally, the properties of new S®-WMA were analyzed a series of physical and rheological test methods.

3.1. Materials

Base bitumen with a 70/100 penetration grade was used to produce S®-WMA and PGW modified S®-WMA samples. Moreover, aggregate used in this study is basalt to examine the stripping resistance of the produced WMA samples. The properties of base bitumen and aggregate are presented in the Table 1 and Table 2.

Table 1

Properties of bitumen.
Test methods	Unit	Standard	Results
Penetration	0.01 mm	EN 1426	85.7
Softening Point	°C	EN 1427	50.5
Flashing Point	°C	EN 22592-b	240.0
Ductility (at 25°C)	cm	EN 13589	103.8
Viscosity (135°C)	cP	ASTM D4402	405.6
Viscosity (165°C)	cP	ASTM D4402	112.3
Solubility	%	EN 12592	99.4
Penetration Index	-	-	0.34
Density	g/cm³	EN 1087	1.032

Table 2

Properties of basalt
Test methods	Unit	Standard	Results
Water Absorption (Coarse)	%	EN 1097-6	2.22
Water Absorption (Fine)	%	EN 1097-6	8.79
Unit Weight (Coarse)	g/cm³	EN 1097-6	2.63
Unit Weight (Fine)		EN 1097-6	3.08
Unit Weight (Filler)		EN 1097-7	2.72
LA Fragmentation Resistance	%	EN 1097-2	18.95
Weathering Resistance		EN 1367-1	8.15
Micro-Deval Abrasion Resistance		EN 1097-1	9.94
Polish Stone Value	PSV	EN 1097-8	56.79
Flakiness Index	%	EN 933-3	11.92
Mytilene Blue	MB	EN 933-9	1.75
Stripping Test	%	EN 12697-11	40–45

All results are presented for each test sample taking into account a set of nomenclature according to the principle given below.

Base Bitumen: BB
Sasobit® S
Pine Gum Warm Wax: PGW
Modified Bitumen with S + X (%): S-X
Modified Bitumen with PGW + X (%): PGW -X
Modified Bitumen with combination of S and PGW + X (%): SPGW-X

where,

X is the rate of Sasobit® as a percentage by mass of bitumen.

The following bitumen modification procedure was determined in the light of previous studies [13, 21, 30–33, 36–38].

The bitumen needs to be made viscous and in this context, the base bitumen was heated at 160 ± 5 °C for 60 minutes.
500 grams of heated bitumen was transferred into metal cans.
The cans filled with bitumen samples were placed separately on a heater operating at 140 ± 5 °C.
The additives, S® and PGW, were added to the bitumen based on the determined rate and mixed for 30 minutes with a propeller mixer operating at 500 rpm.
The modified bitumen was mixed again for the next 10 minutes with the mixer running at 100 rpm to ensure the success of the bitumen modification by means homogeny.
Finally, the modified bitumen samples were transferred for testing.

3.2. Methods

3.2.1. Physical test methods

Within the scope of physical test methods, penetration, softening point, rotational viscometer tests and Nicholson stripping tests were conducted on bitumen samples. Besides, thermal sensitivity of each sample using the penetration index that is developed based on the penetration and softening point test results was determined.

Penetration test method

The test helps researchers to ensure adequate consistency of bituminous binder. It is used to determine the hardness or consistency of bitumen. The EN 1426 standard [39] was followed to perform the test on test samples in this study.

Softening point test method

The test helps researchers to ensure adequate fluidity before it is used for a variety of road applications. It is used to determine the temperature at which the bituminous binder reaches a certain softening phase. EN 1427 standard [40] was followed to test samples in this study.

Determining of the thermal sensitivity level of each test sample is done with the penetration index developed based on the penetration and softening point test results. The following Eq. (1) is used to determine the index value [41].

PI = \(\frac{1952 - 500\text{l}\text{o}\text{g}\text{P}\text{e}\text{n} - 20\text{S}\text{P}}{50\text{l}\text{o}\text{g}\text{P}\text{e}\text{n} - \text{S}\text{P} - 120}\)(1)

where,

PI refers to the penetration index and is unitless,

Pen refers to the penetration value obtained at 25°C and

SP refers to the softening point value.

Rotational viscometer test method

The test helps researchers to measure the apparent viscosity of bituminous binders at different temperatures. The test is applied under controlled temperature provided by thermal chamber and rotational rate. The tests were conducted on the samples according to ASTM D 4402 standard [42].

Considering the viscosity data provided at different temperatures, usually 135 and 165℃, it is possible to estimate the mixing and compaction temperatures of asphalt binders. In this study, viscosity tests were carried out for each unaged sample at the specified temperatures. The viscosity values defined for the determination of mixing and compression temperatures of bitumen samples are 170 ± 20 centipoise (cP) and 280 ± 30 cP, respectively [43].

Nicholson stripping test method

This test is based on coating a defined size and quantity of aggregate with a certain amount of bitumen and keeping the test specimens prepared in this way in water at a constant temperature for a certain period of time to determine whether they strip or not by visual analysis. The EN 12697-11 standard [44] was followed for implementing the test in this study.

3.2.2. Rheological test methods

The rheological properties of bituminous binders are presented in the Superior Performance Asphalt Pavements (SuperPAVE) system developed by the Strategic Highway Research Program [45]. The test methods that measure the rheological properties of bitumen samples within the test defined in the SuperPAVE system. This test methods are: (1) Dynamic Shear Rheometer-DSR, (2) Bending Beam Rheometer-BBR, (3) Rolling Thin Film Oven-RTFO for short-term aged samples and (4) Pressure Aging Vessel-PAV for long-term aged samples [46].. With this system, it is possible to classified bitumen samples based on resistance to high and low temperature performance that are identified with DSR and BBR test method, respectively. To make a representation of classification for any type of bitumen samples, (XX-YY) is used, where XX refer to highest temperature and the lowest temperature -YY [47]. All the test methods mentioned above are briefly described the following.

Dynamic Shear Rheometer-DSR

It is one of the main test used in the SuperPAVE system. The test is performed within a uniquely designed logical framework and analyzed with a specific software program. The test is applied on unaged, short and long-term aged bitumen samples. The two parameters, complex shear modulus (G*) and phase angle (δ°) are the parameter derived from the test. The phase angle means that bitumen samples are elastic as it approach 0° while it is viscous as approaching 90°. The relationships developed between G* and δ° provide information about the structural performance of the bituminous binder including rutting and fatigue resistance. The rutting factor is determined by G*/Sin(δ°), while the fatigue factor is calculated by G*.Sin(δ°). The SuperPAVE system sets limit values taking into account different aging conditions. These limit values are defined as 1000 Pa (1 kPa) and 2200 Pa (2.2 kPa) in the relationship G*/Sin(δ°) for unaged and short-term aged specimens, respectively, and 5 × 10⁶ Pa (5000 kPa) for G*.Sin(δ°) for long-term aged specimens. The DSR test was performed on the samples with following the EN 14770 standard [48].

Bending Beam Rheometer-BBR

The test is used to determine low temperature properties by means of or thermal cracking and relaxation. The test is applied to long term aged bitumen samples specimens. The BBR test has two test parameters, creep stiffness (St) and m-value. St refers to the quotient of flexural stress and flexural strain under specified load, while m-value refers to the slope of creep hardness at 60 seconds. As in DSR, limit values are defined for St as maximum 300 MPa and for m-value as minimum 0.300. The test temperature that satisfies both of these two limit values is called as the low temperature resistance or thermal cracking. The test is applied to the specimens according to the EN 14771 standard.

Rolling Thin Film Oven-RTFO

Bitumen undergoes some aging during mixing, transportation and compaction that is called short-term aging. Under laboratory conditions, it is possible to simulate the aging using the Rolling Thin Film Oven (RTFO) test method. The test system includes a specially designed rotary oven, standard open-ended glasses and an air supply compressor. The test is performed under the defined speed and temperature while exposing the specimens spread in the glass as a thin film by blowing hot dry air from the open end to the specimen. The test is performed according to EN 12607-1 standard [49].

Pressure Aging Vessel-PAV

The aging occurs through the period starting from the production to the end of their service life of bitumen samples refers to the long-term aging. As in RTFO, it is possible to gather long-term aged bitumen samples under laboratory conditions. The test systems include a vessel, a dry air supply compressor and a set of sample plates. The test can be performed at 90, 100, 110°C under a pressure of 2.1 kPa. In this study, the test is performed according to EN 14769 standard [50].

4.1. Physical test methods

The results of bitumen physical tests such as penetration, softening point tests, and accordingly penetration index analysis. Besides, mass loss of base and short-term aged specimens are presented in Table 3.

Table 3

Physical test results
Test method	OB	S-1	S-2	S-3	PGW	SPGW-1	SPGW-2	SPGW-3
Penetration (0.01. mm)	85.7	58.1	49.5	49.0	81.5	58.0	51.8	50.8
Softening Point (℃)	50.5	72.5	77.1	78.0	51.4	61.8	65.6	66.7
Penetration Index	0.34	3.64	3.89	3.99	0.42	1.77	2.18	2.32
Penetration (dmm) (After short-term Aging)	60.2	50.0	44.8	30.6	45.7	36.3	35.7	29.2
Softening Point (℃) (After short-term Aging)	59.3	75.5	59.6	81.0	62.0	72.3	77.7	84.5
Mass Loss (%) (After short-term Aging)	0.45	0.25	0.30	0.40	0.60	0.71	0.43	0.60

According to the results in Table 3, it can be said that the penetration value of the samples decreases as the rate of S® increases significantly. Although the addition of 1% of PGW (by weight of bitumen) reduces penetration, the rate of reduction is much lower than the ones with S®. However, the combined use of both additives in bitumen caused a slight increase in the penetration of the samples. On the other hand, the addition of to the base bitumen increased the softening point value, significantly. However, the addition of PGW produced a significant decrease compared with the other. This prevent the over-rising of softening point the seen for the S®-WMA samples. The penetration index values showed that the S® additive makes the bitumen more sensitive to thermal changes, but the sensitivity decreases when PGW is added to the S®-WMA samples. For all specimens, the mass loss after prolonged aging is below the permissible limit of 1%. Short-term aging leads to an increase in hardness, which causes a significant decrease in penetration value and a significant increase in softening point value.

The rotational viscosity test results were determined at two temperatures, 135℃ and 165℃, and the calculated mixing and compression temperature ranges are given in Table 4.

Table 4

Viscosity and mixing-compaction temperature results
Samples	Viscosity (cP)		Mixing Temperature (℃)	Compaction Temperature (℃)
Samples	135 ℃	165 ℃	Mixing Temperature (℃)	Compaction Temperature (℃)
OB	405.6	112.3	157.1-161.1	144.8-150.9
S-1	345.4	101.1	154.1–159.0	139.3-146.7
S-2	284.8	95.5	150.0-156.4	131.0-140.5
S-3	252.5	81.6	146.0-153.0	124.9-135.4
PGW	366.4	100.8	154.9-159.4	141.4-148.1
SPGW-1	309.6	96.1	151.8-157.4	134.9-143.4
SPGW-2	344.8	89.5	153.2-157.9	139.1-146.1
SPGW-3	355.6	88.3	153.6-158.1	140.1-146.9

From the data given in Table 4, it is obvious that the S® modification decreases the viscosity and therefore the mix operating temperatures. PGW shows similar effect due to its adhesive properties. However, the SPGW samples reflect both cases, giving results close to the average result found for S® and PGW modification separately. This can be attributed to their engineering properties and compatibility with each other.

As mentioned before, the second motivation that led to the creation of this study was to overcome the problem of stripping of S®-WMA samples. To overcome this situation, PGW additive was added to S®-WMA due to certain properties inherent in bitumen, such as stickiness, oily structure and temperature sensitivity. The stripping resistances of both S®-WMA and SPGW bitumen samples are presented and the results and post-test sample images are given in Fig. 1.

It can be seen from Fig. 1 that the S® modification decreases stripping resistance of the base bitumen as the rate increases. But, the addition of PGW significantly improved the stripping resistance of the base bitumen. Based on these results, it can be shown that the addition of PGW at 1% is effective in improving the stripping resistance of S®-WMA.

4.2. Rheological test results

Under constant and/or variable loading and elevated temperature conditions, The unaged, short-term and long-term aged samples are analyzed with DSR. However, BBR tests applied on long-term aged samples at specified temperature. Besides, RTFO and PAV tests are used. to provide short and long term aged samples, respectively.

The DSR test results for all specimens under different aging conditions are given in Fig. 2, 3, and 4.

The DSR test results presented in the Figs. 2 and 3 showed rutting resistance performances of the bitumen samples. The rutting resistance of the samples increased with S® modification and the highest one is determined for the highest content rate in the additive. However, the addition of PGW also decrease the rutting resistance. The lower rutting resistance performance of SPGM bitumen samples is determined for SPGW-1 and rutting resistance increases while the S® rate increses.

DSR results given at Fig. 4 shows the fatigue resistance of samples. The fatigue resistance of modified bitumen decreases with addition of S® and this is more obvious as the rate increase. However, that of PGW modified one has a change, which is not change significantly the performance. On the other hand, decrease in the fatigue performance of bitumen is more significant for SPGW samples.

Throughout the study, BBR tests were performed at -18℃, only. Because, it is the temperature at which all specimens met the requirements specified at SuperPAVE system. The test results are presented at Fig. 5.

As can be seen from the Fig. 5, all samples met the minimum St and m-value criteria. Therefore, further testing at different temperatures was not required to ensure sufficient test temperature that meet both parameters.

The SuperPAVE system based classification is determined on the failure temperatures that are determined on DSR test applied on unaged and short-term aged bitumen samples and the temperature established by the BBR test, that applied on long-term aged samples. Table 6 shows the SuperPAVE based classification of each bitumen sample.

Table 6

SuperPAVE classification for each bitumen samples
Samples	Failure Temperature (℃)	High-temperature Grade	Low Temperature Grade (℃)	SuperPAVE Classification
OB	70	64	− 18	64 − 18
S-1	76	70	− 18	70 − 18
S-2	82	76	− 18	76 − 18
S-3	82	76	− 18	76 − 18
PGW	70	64	− 18	64 − 18
SPGW-1	76	70	− 18	70 − 18
SPGW-2	82	76	− 18	76 − 18
SPGW-3	88	82	− 18	82 − 18

In this study, a solution to two common problems in S®-WMA bitumen (excessive increase in softening point and decrease in peel resistance) was investigated. In this context, different S®-WMA bitumen samples were modified by using 1% PGW, a commercial industrial product, which has not been studied before, as far as can be seen from the available literature. In this context, Sasobit® additives were used in 1% increments up to 3% (by weight of bitumen) to modify base bitumen with 70/100 penetration for WMA production. A number of physical and rheological properties of the bitumen samples were determined by standard test methods. As a result, the following can be highlighted.

A significant decrease in penetration results occurred with the S® modification, but the decrease in penetration occurred with the addition of PGW.

The softening point results showed an extreme increase with S® modification, but a significant decrease in softening point obtained with the addition of PGW.

The lower stripping resistance caused by the S® modification was increased by the addition of PGW.

Decrease in viscosity was detected with the addition of PGW to S®-WMA and hence increase at compaction and mixing temperatures.

SPGW samples perform better than S®-WMA samples in terms of rutting resistance.

PGW modified S®-WMA reduced fatigue resistance more than Sasobit® modification

The low temperature cracking resistance performance of SPGW samples hows better than that of S®-WMA ones.

Overall, this study shows that the addition of 1% PGW additive to S(R)-WMA can be an innovative, effective, environmentally friendly and economical solution to overcome the excessive increase in softening point and low stripping resistance.

As far as can be seen from the available studies, PGW has not been used before in WMA production, especially in WMA produced with S®. Therefore, as a preliminary study, the PGW utilization rate was kept low at 1%. Accordingly, the scope of future studies may include the use of higher proportions of PGW. The analyses in the study were limited to a series of physical and rheological tests and analysis methods. It is recommended to expand the study in the future to include chemical, image processing and/or microscopic analyses for an in-depth understanding of the relationship between the materials. Furthermore, the production of WMA mixture specimens was excluded from the scope of the present study. Therefore, future studies are needed to investigate the structural and functional performance of WMA mix samples within the parameters defined in this study.

Acknowledgements

The authors would like to thank the department of Chief Engineering of Research and Development of 5th and 9th Regional Directorate of Highways and 97th (Batman) Chief of Bitumen for providing some of the test samples and for their assistance. The authors also thank Assist. Prof. Dr. Murat Vergi TACİROĞLU for editing and transferring the DSR test results taken from the program database.

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No competing interests reported.

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Sustainable Production of WMA with Pine Gum Wax Modification: Physical and Rheological Evaluation

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Abstract

Figures

1. Introduction

2. Objective and Scope of Study

3. Materials and Methods

3.1. Materials

3.2. Methods

3.2.1. Physical test methods

3.2.2. Rheological test methods

4. Results and Discussion

4.1. Physical test methods

4.2. Rheological test results

5. Summary and Conclusions

6. Limitations and Recommendations

Declarations

Acknowledgements

References

Additional Declarations

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