Procedia Engineering

Volume 143, 2016, Pages 10–17

Advances in Transportation Geotechnics 3 . The 3rd International Conference on Transportation Geotechnics (ICTG 2016)

The Effect of Granulation Time of the Pan Granulation on the Characteristics of the Aggregates Containing Dunkirk Sediments

Hassane AZRAR1*, Rachid ZENTAR1 and Nor-Edine ABRIAK1 1École des Mines of Douai, Civil Engineering Department, 941, rue Charles Bourseuil, 59508 Douai Cedex, France [email protected], [email protected], [email protected]

Abstract The wet granulation process presents complex interactions between equipment variables as well as material properties making the outcome of a granulation process hard to predict. A frequently encountered difficulty is the process control for optimal condition of the granulation. This requirement depends largely on the operator and the desired properties of the final product. In this study, before the fabrication of aggregates by the pan granulation by associating the sediments with a specific hydraulic binder, the ingredients were characterised. Then, the evolution of the aggregate size with the granulation time has been explored. Finally, the physical and mechanical properties of artificial aggregates formulated by the pan granulation were discussed. The results of this study show firstly, that the use of marine sediments dredged from Dunkirk harbour in France in the production of artificial aggregates is a flexible and positive approach. Secondly, that the granulation time is an important parameter that controls the granulation by wet granulation plate.

Keywords: Dredged marine sediments, pan granulation, wet granulation, artificial aggregates, wetting liquid.

1 Introduction The wet granulation techniques are based on the setting in motion and the agitation of particles, followed by the introduction of the wetting liquid. The different methods of granulation are different mainly by the mode of contacting particles: pneumatic agitation (fluidized beds and their derivatives); agitation by rotation of the walls (pan granulation and rotating drum) and agitation by mechanical mobiles (mixer-granulator). From point of view of stresses exerted, these different modes of action correspond respectively to low shear rates, moderate shear rates and strong shear rates. The approaches to formulation of the solid by introducing the wetting liquid are based on models and experimental tests that remain to be validated for each type of desired functionality: the size, the shape, the mechanical properties of aggregates, etc. A frequently encountered difficulty is the process

10 Selection and peer-review under responsibility of the Scientific Programme Committee of ICTG 2016 c The Authors. Published by Elsevier B.V. doi: 10.1016/j.proeng.2016.06.002 The Effect of Granulation Time of the Pan Granulation on the Characteristics ... Azrar et al. control for optimal condition of the granulation. This requirement depends largely on the operator and the desired properties of the final product. The current regulations in environmental protection are increasingly restrictive, they represent an obstacle to the valorization of these waste. The research conducted in recent years are moving increasingly towards the valorization of dredging sediments for the use as a building material, also towards adapting the valorization in dredging projects and sediment management (Damidot, 2006). According to the physicochemical characteristics, geotechnical, mechanical and environmental dredging sediments, the valorization of these materials can be used in several areas such as road building (Azrar, 2014) ; (Kasmi, 2014) ; (Maherzi, 2013) ; (Liang, 2012) ; (Tran, 2009) ; (Dubois, 2006) ; (Colin, 2003) ; (Boutouil,1998) ; (Achour, al., 2014) ; (Dubois, al., 2008) ; (Zentar, al., 2008) ; (Wang, al., 2013), concrete (Azrar, 2014) ; (Achour, 2013); (Belas, al., 2011) ; (Zri, al., 2011), bricks (Chiang, al., 2008) ; (Samaraa, al., 2009) ; (Hamer, 2002), eco modeled landscape (Khezami, 2014) and artificial aggregates (Azrar, 2014). However, their use in artificial aggregates is not fully developed and deserving of special attention. This work is devoted to the study of the wet granulation by the pan granulation by associating the sediments with a specific hydraulic binder. This device works in continuous mode and allows carrying out the granulation by the rolling of particles over each other. In order to show the importance of granulation time on the aggregates growth and their final characteristics, the granulation was studied for four different times.

2 Materials and Methods

The studied marine sediments are dredged in 2012 in Dunkirk's Eastern Port located in Northern France were employed in these experiments. In order to reduce their water content and to control the liquid-solid mixing ratio, these materials were pre-dried in an oven at 60 °C. Their initial water content is 123 %. The cement used to improve the strength of the aggregates is denoted CEM I 52,5 N-Type SR3 CE PM-CP2 NF. It was chosen for its resistance to aggressive water, high sulphate resistance and good frost resistance. This cement is produced in the factory of Lägerdorf in Northern Germany and contains 65.5 % CaO, 21.7 % SiO2, 4.3% F2O3, 3.8 % Al2O3, 2.66 % SO3 and other minor components. The pan granulation consists of a flanged circular plate with relative low height (H / D < 0.2), which rotating about the central axis inclined from 30 to 70° relative to the horizontal (Figure 1). The angle and the speed of the pan granulation are adjusted to ensure a suitable rolling of aggregates. The particles are spread on the plate and the wetting liquid is dispersed continuously on the moving particles. A good wettability of the powder surface is a prerequisite for ensuring good adhesive bonding of aggregates. For this reason, the wetting position should be chosen and optimized according to the characteristics required for the aggregates. The addition of the wetting liquid leads to the growth of the aggregates by the mechanisms of nucleation and coalescence/consolidation. The preparation process of the materials used in this study consists, in the first step, in mixing 30 % cement and 70 % dredged sediments for one minute. In the second step, water is introduced to reach water content of 27 % which reduces the time required for the considered granulation. This mix is homogenized during three minutes. The obtained material is kept at constant water content in an airtight bag. The aggregates were manufactured using the pelletizer GTE of the company ERWEKA GmbH, Germany, as shown on Figure 1. The angle of plate inclination is set to 53° in the entire tests and the speed of rotation was varied from 12 to 28 rotations per minute. For each granulation, 300 g of the wet prepared mixture was introduced into the pan, after initiating the rotation of the plate, water is added using a peristaltic pump for the desired time of granulation. The added water during this operation represents 6 % to 9 % of the dry mix. This induces a final water content of the mix between 33 % and

11 The Effect of Granulation Time of the Pan Granulation on the Characteristics ... Azrar et al.

36 %. Aggregates obtained from these operations were kept in an airtight bag and cured for 24 hours in an oven maintained at 40 °C. This hardening phase promotes the hydrations and hardening of aggregate reactions. Finally, these aggregates were subjected to curing for 28 days at room temperature. On the artificial aggregates, the grain size distribution, the absolute density, the water absorption capacity, the wear resistance and the degradability were measured. The physical characteristics of dredged sediments and cement, like the absolute density, the grain size distribution and the specific surface, are determined according to European and French test standards and shown in Table 1. The beneficial use of dredged material in combination with specific cement has been proposed and the designed mixtures have led to the manufacture of spherical aggregates shown in Figure 1. To evaluate the physical and mechanical properties of manufactured aggregates, a series of tests like the grain size distribution, the absolute density, the water absorption capacity, the wear resistance and the degradability were measured in this study. The grain size distribution was carried out on all grains obtained during granulation according to the selected speeds and times. This test was performed at the end of the curing period mentioned above, according to the French standard NF P94-056. The determination of water absorption coefficient was conducted using the pycnometer method for aggregate particles passing the 31,5 mm test sieve and retained on the 4 mm test sieve according to NF EN 1097- 6. The minimum mass of test portion used in this test is 1000 g. The abrasion resistance (Micro-Deval) was determined according to the standard EN 1097-1. The mass of the sample was at least 2 kg of particles in the 10 mm to 14 mm size range. The test shall be carried out on aggregate passing the 14 mm sieve and retained on the 10 mm sieve. The test portion shall consist of two test specimens, each having a mass of 500 g. The degradability test determines the stability of the aggregates under conditions of immersion. The manufactured aggregates undergo 4 cycles of immersion/drying (immersion in water for 8h and drying in an oven for 16h). The aggregates fraction used in this test is 10/20 mm according to the French standard specification NF P94-067. Degradability coefficient is defined as the ratio of the diameter corresponding to 10 % of passing before and after the test.

3 Results 3.1 Raw Material Characterisation

The absolute density (ȡs) was determined using a Helium pycnometer. For the studied sediment, the average of one hundred and eighty measurements on two samples shows that, as expected, the measured values are lower than the known values for mineral particles (around 2.70 g/cm3). This difference is due mainly to the presence of organic matters of lower densities. As shown in Table 1, the fine particle size of raw dredged sediment and cement lead to a high specific surface area.

12 The Effect of Granulation Time of the Pan Granulation on the Characteristics ... Azrar et al.

Dredged sediment Specific cement Test standards

d10 1.40 1.04 NF P94-056

d50 13 8.94 NF P94-056

d90 194 27.40 NF P94-056

Specific surface (cm2/g) 8181 11019 ISO 9277

Absolute density (g/cm3) 2.52 3.10 NF EN ISO 18753

Table 1: Measured characteristics of raw dredged sediment and cement

In this study, tap water was used as the wetting liquid with pH 7.21 measured at 23.5 °C. This water is most commonly used in the wet granulation process to facilitate particle agglomeration. Appropriate granulation is only possible to predetermined water content experimentally. Beyond this water content, the granulation is going towards the production of one mud. For each tesst, 300 g of the prepared mixture was introduced in the pan granulation as shown in Figure 1. Aggregates production continues until the end of this mixture.

Figure 1: Pan granulation and the state of manufactured aggregates 3.2Evolution of the Aggregate Particle Size Distribution

In order to study the influence of the granulation time on the particle size distribution of the aggregates, after the introduction of the mixing and granulation with the addition of water during 2 min, the rotation is continued without addition of water for the other granulation time 5, 10 and 30 min. Under the effect of the hydraulic binder and of the rolling movement of particles, the agglomerates will attract each other and will grow progressively. Figure 2 shows a significant variation of the percentage of fine and coarse particles when increasing the granulation time. Indeed, the increase of the latter causes an increase in the aggregates

13 The Effect of Granulation Time of the Pan Granulation on the Characteristics ... Azrar et al. diameter. Similar conclusions have been fouund in the studies of the four granulation speeds tested (12, 18, 23 and 28 rotation per minute “rpm”). The decrease in the granulaation time leads to a reduction of the rate of larger particles size with an increasing fines content on the granulating plate, indicating that the aggregates diameter is closely linked to the granulation time. This conclusion is more pronounced for higher rotation speeds.

Figure 2: Influence of the granulation time on the aggregates-size distribution

14 The Effect of Granulation Time of the Pan Granulation on the Characteristics ... Azrar et al.

3.3 Aggregate Properties Figure 3 shows that the increasing of granulation time causes a gradual decrease of the water absorption after immersion for 24 hours and the abrasion resistance of the manufactured aggregates. Increasing the granulation time leads to a reduction of the porosity which improves the characteristics of aggregates. It seems that the time of 10 minutes is optimal in view of insignificant variation of results between 10 min and 30 min.

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for 24hours WA24 (%) for WA24 24hours ϮϬ ϮϬ Abrasion resistance (%) ϭϬ ϭϬ

Water absorption Water after immersion Ϭ Ϭ ϬϮϰϲϴϭϬϭϮϭϰϭϲϭϴϮϬϮϮϮϰϮϲϮϴϯϬ Granulation time (min)

Figure 3: Influence of granulation time on the aggregates properties

The degradability test consists to determine the stability of the aggregates under conditions of immersion. This test is performed on a fraction of 10/20 mm according to test standard NF P 94-067. In this test, aggregates undergo 4 cycles of immersion/drying as follows: immersion in water for 8 hours then drying in an oven for 16 h. The results of the performed tests on the different manufactured aggregates are shown on Figure 4. These tests were conducted on the aggregates made with the highest speed that was used namely 28 rotation per minute “rpm”. The results presented in Figure 4 allow concluding that the degradability of the manufactured aggregates is quite low. Table 2 shows that the degradability coefficient decreases with the increase of granulation time. Increasing granulation time leads to the improvement of the stability of the aggregates under conditions of immersion. These results open opportunities to explore the ability of these new aggregates to be used in maritime engineering.

15 The Effect of Granulation Time of the Pan Granulation on the Characteristics ... Azrar et al.

100

90 2min 5min 10min 30min D10 before D10 after Degradability

80 test test coefficient

70 28 rpm 10,7 6,5 1,65 60 (2min) 50 28 rpm 10,7 7,7 1,39

passing (%) passing 40 (5min) 30 28 rpm 10,7 9,0 1,19 20 (10min) 10 28 rpm 10,7 10,2 1,05 0 1234567891011121314151617181920 (30min) Particule diameter (mm)

Figure 4: Evolution of grain size distribution of Table 2: Degradability coefficient of manufactured the aggregates subject to immersion/drying test aggregates

4 Conclusion The results of this research work can provide a new method to reuse dredged sediments in marine works by using granulation technique. The data presented in this study shows that the combination between dredging sediment and cement can be used in the production of artificial lightweight aggregate by using pan granulation. Four granulation times with four rotation speeds were used to study the influence of the granulation time on the physical properties of aggregates. The evolution of physical characteristics shows that the granulation time is a key parameter that controls the wet granulation by the granulating plate. These results were encouraging for the potential utility of dredged sediments in the production of artificial lightweight aggregate. References Damidot, D. (2006). Guide technique régional relatif à la méthodologie de gestion des sédiments de dragage portuaire. Démarche PREDIS Nord Pas-de-Calais, p. 422 p. Azrar, H. (2014). Contribution à la valorization des sédiments de dragage portuaire : technique routière, béton et granulats artificiels, Thèse de doctorat, Mines Douai., p. 224. Kasmi, A. (2014). Prétraitement et traitement des sédiments fluviaux en vue d’une valorization en technique routière, Thèse de doctorat, Mines Douai, p. 174. Achour, R. (2013). Valorization et caractérisation de la durabilité d’un matériau routier et d’un béton à base de sédiment de dragage, Thèse de doctorat, Mines Douai, p. 194. Maherzi, W. (2013). Valorization des sédiments marins bruts et traités aux liants hydrauliques en technique routière, Thèse de doctorat, Université de Cean, p. 194. Liang, Y. (2012). Co-valorization de sédiments et de sols fins par apport de liants et de fibres, Thèse de doctorat, Université de Cean, p. 227. Tran, N. T. (2009). Valorization de sédiments marins et fluviaux en technique routière, Thèse de doctorat, Université d'Artois, p. 225. Dubois, V. (2006). Etude du comportement physico-mécanique et caractérisation environnementale des sédiments marins – Valorization en technique routière, Thèse de doctorat, Université d'Artois, p. 311. Colin, D. (2003). Valorization de sédiments fins de dragage en technique routière, Thèse de

16 The Effect of Granulation Time of the Pan Granulation on the Characteristics ... Azrar et al. doctorat, université de Caen-Basse-Normandie, p. 181. Boutouil, M. (1998). Traitement des vases de dragage par stabilisation et solidification à base de ciments additifs, Thèse de doctorat, Université du Havre, p. 279. Achour, R. ; Abriak, N.-E. ; Zentar, R. , Rivard P. et Gregoire, P. (2014). Valorization of unauthorized sea disposal dredged sediments as a road foundation material, environmental technology, vol. 35, pp. 1997-2007. Dubois, V. ; Abriak, N. E. ; Zentar, R. et Ballivyb, G. (2008). The use of marine sediments as a pavement base material, waste management, Conference: 5th Asian-Pacific Landfill Symposium Location: Sapporo, JAPAN, vol. 29, pp. 774-782, OCT 22-24. Zentar, R. ; Abriak, N. E. ; Dubois, V. (2008). Beneficial use of dredged sediments in public works, environmental technology: 12th International Symposium on Sediment Management Location: Lille, FRANCE, vol. 30, pp. 841-847, JUL 09-11. Wang, D. ; Abriak, N. E. ; Zentar, R. (2013). Strength and deformation properties of Dunkirk marine sediments solidified with cement, lime and fly ash, engineering geology, vol. 166, pp. 90- 99. Belas, N. ; Belaribi, O. ; Mebrouki, A. ; Bouhamou, N. (2011). Valorization des sédiments de dragage dans les bétons, INVACO2 : Séminaire International, Innovation & Valorization en Génie Civil & Matériaux de construction, p. 6. Zri, A. ; Abriak, N. E. ; Benzerzour, M. (2009). Valorization des sédiments dans le béton de sable à base du sable de dragage, SBEIDCO – 1st International Conference on Sustainable Built Environement Infrastructures in Developing Countries, p. 8. Chiang, K.-Y. ; Chien, K.-L. ; Hwang, S.-J. (2008). Study on the characteristics of building bricks produced from reservoir sediment, Journal of Hazardous Materials, Vols. %1 sur %2159, Issues 2–3, p. 499–504. Samaraa, M. ; Lafhaja, Z. ; Chapiseau, C. (2009). Valorization of stabilized river sediments in fired clay bricks: Factory scale experiment, Journal of Hazardous Materials, Vols. %1 sur %2163, Issues 2–3, p. Pages 701–710. Hamer, K. ; Karius, V. (2002). Brick production with dredged harbour sediments : An industrial-scale experiment, Waste Management, p. 521–530. Khezami, I. (2014). Approche expérimentale de valorization des sédiments de dragage dans des applications de Génie Civil, Thèse de doctorat, Mines Douai, p. 196.

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