Asphalt modified with superfine electric arc furnace steel dust (EAF dust) with high zinc oxide content

Construction and Building Materials 145 (2017) 538–547

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Construction and Building Materials journal homepage: www.elsevier.com/locate/conbuildmat

Asphalt modified with superfine electric arc furnace steel dust (EAF dust) with high zinc oxide content Alexandra Loaiza a, Sergio Cifuentes b, Henry A. Colorado a,⇑ a b

CCComposites Lab, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín, Colombia Conasfaltos S. A, Medellín, Colombia

h i g h l i g h t s
In this research a particular EAF dust with high ZnO is evaluated as an admixture for asphalt up to 50 wt%.
In addition to a very complete characterization, an analysis of an asphalt mechanism modified by chemical means was carried out.
The particle distance was calculated using the composite materials theory, and other variables were analyzed in terms of these estimations.

a r t i c l e

i n f o

Article history: Received 1 January 2017 Received in revised form 10 March 2017 Accepted 5 April 2017

Keywords: Asphalt Electric arc furnace dust Waste

a b s t r a c t Electric arc furnace (EAF) dust is a complex ceramic-type hazardous waste generated by the metallurgical industry and produced worldwide in millions of tons. In this research EAF dust is evaluated as an admixture for asphalt up to 50 wt%. The microstructure was analyzed by optical and scanning electron microscopy. Fourier transform infrared spectra, penetration, softening point and viscosity tests were conducted for all compositions. The results show the penetration point increases until 10 wt% of waste and it then decreases. Conversely, the softening point, penetration index (PI) and viscosity, decrease after 5 wt% and reaches a minimum at 10 wt%. The particle distance was calculated using the composite materials theory, and other variables were analyzed in terms of inter-particle distance estimations. Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction Electric arc furnace dust (EAF dust) is a byproduct produced by the electric arc furnace in the steel making industry. This waste is considered hazardous by the EPA (United States Environmental Protection Agency) [1], as it is dangerous for water sources if not well treated or stored. EAF dust is formed in the electric arc furnace at approximately 1600 °C. Elements such as Zn, Cd and Pb present in the scrap are volatilized and then condensed as soon as the temperature drops in the outlet of the furnace [2]. The waste is then typically disposed of in baghouse systems. Fig. 1 shows a representation of EAF dust formation in the furnace. According to the World Steel Association [3], the annual production of steel is approximately 1,600,000 tons. Of this, 33% is produced by electric arc furnaces. EAF dust makes up about 1–2% of the load in the furnace [4]. This means that annually 16,000 to 32,000 tons of EAF dust are generated worldwide. Reported uses

⇑ Corresponding author at: Universidad de Antioquia, Facultad de Ingeniería, Bloque 20, Calle 67 No. 53-108, Medellín, Colombia. E-mail address: [email protected] (H.A. Colorado). http://dx.doi.org/10.1016/j.conbuildmat.2017.04.050 0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.

of EAF dust include bricks [5], recycling of metals [4], Portland cement [6] and phase change materials [7]. Asphalt bitumen is used as a binder for EAF dust due to the fact that the solidification process is inexpensive and suitable for stabilizing such waste. EAF dust has been put into asphalt cement and asphalt concrete in order to use this waste for road infrastructure and to decrease the pollution of water resources [8–10]. Vahcˇicˇ et al. [11] evaluated the leachability of EAF dust in asphalt concrete to determinate its environmental impact. Another waste that has been used more extensively in asphalt concrete is steel slag from the electric arc furnace [12,13] and steel slag from the basic oxygen furnace [7,14,15]. Many diverse methods had been developed for treating the byproducts of pyrometallurgical and hydrometallurgical processes. However, these have only been partially successful because the recovery of metals is not fully efficient and typically generates more pollutant byproducts [4], which means the applied solution can also produce hazardous waste itself. Fortunately, there are more options coming from the asphalt industry, such as the solidification/stabilization (S/S) technology, a method of mixing a waste with a binder in order to immobilize the pollutant agents found in industrial wastes [16]. S/S is an economical and simple process to

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Fig. 1. EAF dust formation in the furnace and the furnace mechanism.

stabilize hazardous wastes when compared with other methods [17], and when asphalt is used as a binder, properties like impermeability and stability in water are maximized. Moreover, if the waste is mixed with asphalt and aggregates in an asphalt concrete, it can be used worldwide for building infrastructure, not only because of its low cost but also because its processing is quite simple and only requires basic technology found in all countries. Furthermore, perhaps the most important feature is that this method has a significant impact on the environment as tons of waste can be consumed and the waste is easily stabilized [18]. This paper shows an economical and viable alternative to improve asphalt performance and stabilize the ZnO content of hazardous waste from the steel making industry. Alsheyab & Khedaywi [8] evaluated the effect of EAF dust on an asphalt matrix. However, in this paper EAF dust with a higher ZnO content is assessed, which is a different material to what is presented before and therefore shows unique results. The waste and its asphalt composite were characterized using several methods, including particle size distribution, optical (OM) and scanning electron (SEM) microscopy, Fourier transform infrared spectroscopy (FTIR), penetration, softening point, and viscosity tests. In addition, an analysis of an asphalt mechanism modified by chemical means was carried out. The poor use of EAF waste is a worldwide problem. Huge quantities of unused dust are formed and little research has been done on the subject. This paper attempts to look at new applications for such waste. 2. Experimental phase Asphalt grade 60–70 was supplied by the Ecopetrol Colombian national oil company and its properties appear in Table 1. The waste EAF dust was generated in the steelmaking process at

Ternium S.A company. EAF dust composition was measured with an X-ray fluorescence Thermo model Optim’x and this is summarized in Table 2. It can be seen that the main components are iron oxide (Fe2O3 = 21.5%) and zinc oxide (ZnO = 50.4%). Waste granulometry was done using a #200 sieve. Asphalt mixes were prepared as follows: 0.0 (neat asphalt) 1.0, 50, 10.0, 15.0, 20.0, 30.0 and 50.0 wt% of EAF dust. Mixing was conducted in a Velp Scientifica mechanical stirrer for 1 h at 155 °C and 200 rpm in order to guarantee a good powder distribution and liquid asphalt impregnation in the waste particles. Powder distribution was observed with a Leica optical microscope. The mix was then deposited in a glass slide and observed in transmission mode. For SEM-EDS examinations, samples were mounted on a glass slide and sputtered in a Hummer 6.2 system (15 mA AC for 30 s) creating a film of gold approximately 1 nm thick. The SEM used was a JEOL JSM 6490LV in high vacuum mode. Powder size distribution was obtained from the analysis of the SEM images using the Image-J software. FTIR spectra were collected in a Shimadzu apparatus with wave numbers ranging from 500 to 3500 cm1. Potassium bromide (KBr) powder was used for this test. Penetration tests were conducted following the ASTM D5 standard at 25 °C using a Controls type penetrometer. Softening point tests were done following the ASTM D36 standard using a standard ring and ball apparatus. Viscosity tests were carried out in a rotational Brookfield viscometer at 60 °C in order to assess the high temperature workability of different samples. The penetration index was estimated from the penetration and softening point results using the corresponding equations [19]. The asphalt-waste particle system follows Stoke’s law, which uses gravitational and floatability forces, and density and particle

Table 1 Asphalt properties as supplied by Ecopetrol. Test

Units

Result

Viscosity at 60 °C Viscosity at 80 °C Viscosity at 100 °C Viscosity at 135 °C Viscosity at 150 °C Ductility Gravity API Density at 15 °C Penetration at 25 °C Penetration index Mass loss (RTFO) Softening point Flame point Solubility in trichloroethylene

cP cP cP cP cP cm Grados API kg/m3 mm/10 N/A g/100 g °C °C %

242,000 21,750 3725 395 217.5 140 6.9 1021.7 60 1 0.48 49.2 294 99.7

Other information

100

60–70 1.0 45–55 232 99.0

Methods ASTM D 4402 ASTM D 4402 ASTM D 4402 ASTM D 4402 ASTM D 4402 Asfalto VENT ASTM D 4052 ASTM D 4052 Asfalto VENT Asfalto VENT Asfalto VENT Asfalto VENT ASTM Asfalt VENT

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Table 2 XRF results for the EAF dust, with loss of ignition of 11%. Oxide

ZnO

Fe2O3

Na2O

MgO

Mn3O4

SiO2

SO3

K2O

CaO

Al2O3

SrO

wt%

50.40

21.54

3.38

2.55

2.43

2.12

1.90

1.32

1.20

0.77

0.004

Oxide

BaO

Cr2O3

P2 O5

CuO

HfO2

TiO2

PbO

NiO

V2O5

ZrO2

LOI

wt%

0.472

0.26

0.172

0.19

0.115

0.035

0.025

0.020

0.006

0.001

11

Fig. 2. SEM images and particle size distribution obtained from them for EAF dust as received.

Fig. 3. Optical microscopy images for asphalt with EAF dust.

size are key factors [20]. Therefore, in this research the velocity for EAF dust particle drop was estimated. In order to estimate the stiffness modulus for all mixtures at a specific temperature and loading time, the Van der Poel nomograph [21] was used, which employs

the penetration index and the softening point. In this investigation, the stiffness modulus was calculated at a temperature of 25 °C and a loading time of 0.002 s, which corresponds to a typical vehicle speed between 30 and 40 mph [22,23]. The particle distance was

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also calculated using the composite materials theory for particle reinforced composites [24]. The penetration, softening point, stiffness modulus and viscosity were analyzed in terms of interparticle distance estimations. 3. Results Fig. 2 shows scanning electron microscopy (SEM) images of the EAF dust. Fig. 2a shows that the waste particles are small and have a very narrow particle size distribution, and some even go down to the nanoscale (see Fig. 2b). This indicates that the particles are not only hazardous because of their chemical composition, but also because of their reactivity and potential to pollute the air, mainly while they are being produced in the steel making process Fig. 2c shows the particle distribution and demonstrates that many particles are below 1 mm. Fig. 2b supports the distribution

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characterization since in that image most of the grains are very close to 0.5 mm. Fig. 2c shows that about 50% of the particles are smaller than the mean. In addition, the distribution is heterogeneus, which has been reported before for similar waste particles [25]. Table 2 summarizes the composition of the EAF dust obtained with XRF. The main component by amount is ZnO, with 50.48 wt %. Fe2O3 is also present in a significant quanity, making up 21.15 wt%. These composition types are typical when galvanized scrap is processed for making new steel. Fig. 3 summarizes optimal images showing the EAF dust particle distribution in the asphalt binder. In all samples with the different waste contents studied in this research, the distribution was homogenous. This result was expected because the hot asphalt was very good at impregnating the particles. It confirms that even though the process is inexpensive, it effectively impregnates particles without particle agglomeration. This decreases the material properties related to strength and durability. The softening point, penetration and penetration index for asphalt with EAF dust are shown in Fig. 4a, b and c respectively. In general, asphalt mixes increase the softening point as the EAF dust content increases. Only at 10 wt% is there a significant decrease in the softening point. An increase in quantity of this ceramic waste increases the temperature of the softening point in general, which can be very good for applications involving higher temperatures. However, 10 wt% of waste is the critical amount that breaks the trend. This is important because it shows that at 10 wt% there is another complex mechanism involved, in addition to the effect of the harder particle reinforcement itself, in the mechanical and thermal properties of the mix. As expected, the penetration results from Fig. 4b show the opposite trend, i.e. the higher the softening point, the shorter the penetration. The penetration index (PI) was found with Eq. (1) [19], and the corresponding results are shown in Fig. 4c, where P is the penetration and SP is the softening point.

PI ¼

1952  500  LogðPÞ  20  SP 50  LogðPÞ  SP  120

ð1Þ

The trend given by the viscosity tests was expected. As the ceramic waste increases, viscosity also increases, as seen in Fig. 5. However, at 10 wt% waste content, the viscosity is reduced, and from 10 to 20 wt% there is an important increase in the viscosity values. In fact, it was not possible to conduct viscosity tests for samples with more than 20 wt% of waste. These results also support that fact that at 10 wt% waste the asphalt mix properties are changed significantly. In order to see the differences, SEM images were analyzed for different compositions. In particular, samples were taken from the surface of the mixes and prepared for the optical microscope.

Fig. 4. Samples with different contents of EAF dust: a) softening point, b) penetration, and c) penetration index.

Fig. 5. Viscosity tests for asphalt with different EAF dust contents at 60 °C. The procedure indicated by the ASTM D4402 standard was followed.

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They showed important topographic changes on the binder matrix, as seen in Fig. 6. For samples with 1.0 wt% of waste, the surface is relatively smooth (Fig. 6a), while for 10 wt% the surface shows flow lines (Fig. 6b). This is a qualitative result that shows that the asphalt binder is changed to make particle-particle interaction possible, which has a critical value at 10 wt%. Fig. 7 shows EDS-SEM maps for different elements taken from a sample with 10 wt% of EAF dust. All maps correspond to the image located in the top-right. The corresponding quantitative compositions are summarized in Table 3.

From these maps, it can be seen that the Zn and Fe contents are very high. All elements are distributed relatively homogeneusly, supporting a good particle distribution, but perhaps some signals are from the disolution of the metal elements in the liquid asphalt. SEM resolution cannot solve this because it is beyond the scale limits and may be hidden or mixed with nanoparticle signals (and most of the characterization technique limits). However, this is an important consideration to evaluate in the future since if the resulting ions form the disolution in the asphalt, they could have an important effect on the thermomechanical behavior of the

Fig. 6. SEM images for asphalt with steel slag.

Fig. 7. EDS-SEM for asphalt with EAF dust.

Table 3 EDS-SEM results. Element

C

O

Mg

Al

Si

S

Cl

K

Ca

Mn

Fe

Zn

Total

Weight% Atomic%

81.52 92.19

4.73 4.02

0.24 0.13

0.18 0.09

0.49 0.24

1.86 0.79

0.38 0.15

0.36 0.12

0.32 0.11

0.28 0.07

2.52 0.61

7.11 1.48

100 100

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matrix. The carbon and sulfur peaks in the spectrum are from the asphalt composition. The most significant result from this analysis is that the most hazardous elements such as Pb and Cr, found with XRF and reported in Table 2 for the raw EAF dust, are not found in the modified asphalt sample. This suggests that asphalt masks their effect at levels not detectable by the SEM-EDS. Fig. 8 summarizes all FTIR spectra. FTIR data for samples with 0.0, 1.0, 10.0 and 20.0 wt% of EAF dust show that when the EAF is added, a new signal appears at about 2727 cm, which corresponds to vibration of the CAH bond stretching from the RC@OH

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molecule [26]. This is an important result because it proves that the asphalt binder chemically interacts with the waste and supports the data presented before regarding the mechanical and thermal properties. 4. Analysis and discussion The interaction between the EAF dust and asphalt is governed by the chemical and physical properties given by the bond, composition, particle morphology and size, and perhaps by other factors

Fig. 8. FTIR for asphalt with EAF dust.

Fig. 9. Asphalt microstructure as a colloidal system. a) Sol type asphalt, b) gel type asphalt.

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such as ion dissolution in the liquid asphalt. The morphology of the EAF dust particles, their size distribution and the surface area available for adsorption have the most important effect on the mechanical and thermal properties, which were indirectly tested by the penetration, softening and viscosity tests. Some of these considerations have already been reported [20] for other modified asphalts, which can lead to acid-basic Lewis reactions and may be associated to covalent bonds, which in addition to the particle surface variations can decrease the interfacial tension in the liquid producing a better stabilization of the waste. Several authors have described the physicochemical interactions between asphalt and fillers and have reported a more complex interaction than that of the particle-asphalt interaction [27,28,29,30,31]. In this research we propose that there are potential particle-particle interactions, for instance due to the iron powder having ferromagnetic effects, and some possible ion dissolution in the liquid asphalt. Future fundamental modeling such as molecular dynamics may give some clues about this complex phenomena. It is well-known that asphalt has a complex composition that includes asphaltenes and maltenes. Maltenes can be divided into saturates, aromatics and resins. A common 60/70 asphalt has 2% of saturates, 73% of aromatics, 7% of resins and 18% of asphaltenes [32]. Asphaltene is the most viscous and is polar, maltene is the least viscous and is non-polar, and the resin has both characteristics [33]. This complex composition has an intricate effect on the mix of particles used in this research-a ceramic type waste with a very diverse amount of oxides. Each of the particle types may have a very distinctive interaction in the asphalt liquid. For the different curves we observed, at around 10 wt% of asphalt there is a mix of all these complex interactions. Looking at the type of bonding alone, we can see that the diverse oxides have different potentials and therefore distinct interactions with the asphalt. Moreover, asphalt is considered to be a colloidal material mixture, with asphaltenes as the disperse phase and maltenes as the continuous phase. According to its microstructure, asphalt can be divided into two types: gel and sol, both of which are represented in Fig. 9. In the sol asphalt, asphaltenes are well dispersed in the maltenes, while in the gel asphaltenes they are not well dispersed and tend to agglomerate in the maltenes continuum. This is because the amount of saturates and aromatics are different. As the amount of aromatics increases, the asphaltene dispersion increases as well, because aromatics form a stabilizing layer around the asphaltenes. The saturates have little effect on the asphaltenes and that is why the asphaltenes tend to agglomerate and form a gel structure [34]. The asphalt used here has a large amount of aromatics and is therefore a sol type asphalt. Asphalt with EAF dust particles forms a composite material itself, where asphalt is the matrix and EAF dust particles are the filler or the reinforcing material. Three main reinforcement mechanisms have been defined [28]: volume-filling reinforcement,

physiochemical reinforcement, and particle interaction reinforcement. One of the most significant asphalt-particle interactions is described by the adhesion theory, where polar components in asphalt are adhered to the particle surface [31]. Polar asphalt’s components are asphaltenes, which are the most viscous part of the mix. They adhere to the waste particles’ surface and make the matrix less viscous [27,28,29,31,33,35]. The penetration results in this investigation support previous research, where penetration increases as the EAF dust content increases to 10 wt%, which must be connected with the viscosity increase with more than 10 wt% of waste, see Fig. 5, which most likely is due to the shear thinning originated in the orientation of neighboring macromolecules and their entanglement and immobilization given by the solvent, [36,37]. Fig. 10a represents the mechanism that occurs. As the content of EAF dust increases, the particle-particle interaction increases and some particles even attach themselves to each other. This limits asphalt impregnation in the particle-particle interface, as seen in Fig. 10b. The interparticle distance was calculated following the interparticle distance equation for particle reinforced composite materials [24]. The relationship is summarized in Eq. (2), where s is the interparticle distance, d is the particle diameter, and up is the filler content. As expected, when the waste content increases, the interparticle distance decreases, as shown later in Fig. 12a.

2

s ¼ d4

p 6up

!1=3

3

 15

ð2Þ

On the other hand, the morphology of the particles is an important parameter that contributes to the asphalt-EAF dust interaction. Particles with an angular surface have better compatibility with a polymeric matrix. The angularity of the particles can be seen in Fig. 2. In addition, the asphalt-particle system follows Stoke’s law [20]. The effect of gravitational and buoyancy forces and density and particle size are the key features, as seen in Eq. (3):

V ¼ 2ðqo  q1 Þgr2 =9g

ð3Þ

where qo is the density of asphalt, which is 1.02 g/cm3, q1 is the density of EAFD, which is 4.93 g/cm3 [38], g is the gravitational force constant, r is the average radius of the EAF dust particles, which is 0.27 mm, and g is the viscosity of the base asphalt. The decreasing velocity of the particles reaches as low as about 2.66  1010 cm/s. The penetration index is a quantitative measurement of how the viscosity changes with temperature. Table 4 summarizes typical values with their respective interpretation. The mixtures fabricated in this research can be applied to the construction of roads because all values follow in the 2 to +2 interval. Only the mix

Fig. 10. EAF dust particle surrounded by the interface layer and asphalt: a) less than 10 wt% of EAF dust, b) more than 10 wt% of particles.

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Fig. 11. a) Van Der Poel nomograph, b) Stiffness modulus calculated from Van Der Poel nomograph.

with 10 wt% of EAF dust can be lower than 2 in some cases, simply because of its high variability in PI. However, its mean value is in the recommended interval. The stiffness modulus is another key parameter to determinate the behavior of asphalt on the road. This was estimated from the Van der Poel nomograph [21], as seen in Fig. 11, and was calculated for 25 °C of temperature and 0.02 s of loading time. The loading

time of 0.02 s approximately corresponds to 30–40 mph of a typical vehicle speed [22,23]. Finally, Fig. 12 summarizes the estimation of interparticle distance for several parameters. First, Fig. 12a shows that as particle content increases, the interparticle distance increases from about 3 mm for 1.0 wt% to 0.5 mm for 50 wt%. Also, for 10 wt% of waste, the interparticle distance is 1.0 mm. Correspondingly, Fig. 12a

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waste), the viscosity has a breaking value which separates the different compositions into two very different regions: below 10 wt% (1.0 wt% waste) with a high viscosity and over 10 wt% with a low viscosity. A 1.0 mm interparticle distance (1.0 wt% waste) gives a minimum value for the stiffness modulus, confirming the results discussed above. 6. Conclusions In conclusion, EAF dust has a very complex and multiparameter effect on the performance of asphalt due to the complex physical-chemical interactions of these two very complex materials, each a multi-composite material itself. The penetration index is 2 to 2 in all cases, which enables all mixes to be used for road construction. EAF waste is harmful to the environment because of its hazardous metal content, but this toxicity can be stabilized using asphalt thereby allowing for the widespread use of this material in infrastructure. Acknowledgements The authors wish to acknowledge the Research office of the Universidad de Antioquia for supporting this research. References

Fig. 12. Interparticle distance relationships with a) waste contents, b) penetration and softening point, c) viscosity and stiffness modulus.

Table 4 Typical values of PI in asphalt cement. Asphalt type

Penetration index

Blown asphalt Conventional road pavement asphalt Temperature susceptible asphalt

>2 2 to +2 <2

shows that for 1.0 mm interparticle distance (1.0 wt% waste), the penetration reaches a maximum and the softening point reaches a minimum, and for interparticle distances large than that, the two variables stabilize. However, the most significant result is shown in Fig. 12c. For a 1.0 mm interparticle distance (1.0 wt%

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