Minerals Engineering 23 (2010) 5457

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

Technical Note

Effect of grinding aids on the grinding energy consumed during grinding of calcite in a stirred ball mill
H. Choi a,*, W. Lee a, D.U. Kim a, S. Kumar a, S.S. Kim b, H.S. Chung b, J.H. Kim c, Y.C. Ahn d
School of Nano and Advanced Materials Engineering, Changwon National University, Changwon, Republic of Korea Department of Precision and Mechanical Engineering and Eco-Friendly Heat and Cooling Energy Mechanical Research Team, BK21, Gyeongsang National University, Tongyoung, Republic of Korea c Department of Quantum Science and Energy Engineering, Tohoku University, Aramaki Aza Aoba, Aoba-ku, Sendai, Miyagi, Japan d School of Architecture College of Engineering, Pusan National University, Busan, Republic of Korea
b a

a r t i c l e

i n f o

a b s t r a c t
A series of wet-grinding experiments has been carried out on inorganic powders by a stirred ball mill to systematically investigate the grinding characteristics. The grinding power consumed for a given grinding time was considered, as well as the effect of grinding aids on particle size. The grinding energy consumed, dened as the integral of the grinding power over time, was also investigated. The grinding aids were found to inuence the product size and decrease the grinding energy. This is attributed to the prevention of agglomeration and coating of the sample powder onto the ball and grinding chamber wall. The grinding process seemed to be controlled by the force of agglomeration of the ground products. It was demonstrated that the particle size and grinding consumption energy could be decreased by the addition of grinding aids. 2009 Elsevier Ltd. All rights reserved.

Article history: Received 10 July 2009 Accepted 17 September 2009

Keywords: Comminution Grinding Mineral processing Fine particle processing

1. Introduction Recently, attention has been drawn to ultra-ne grinding in the sub-micron range, in the wake of the development of new functional materials, such as new ceramics and electronic materials, in various industrial elds. Stirred ball mills have been used in recent years for grinding particles to sub-micron sizes due to their easier operation, simpler construction, higher grinding rate and lower energy consumption compared with other ne grinding machines (Choi, 1996; Bernhart et al., 1999; Shinohara et al., 1999; Choi and Wang, 2007; Choi et al., 2007; Shi et al., 2009; Stamboliadis et al., 2009). Furthermore the grinding energy efciency is an important parameter that affects the amount of energy used during grinding. It is affected by the mechanical energy transition, the breakage mode, and the energy lost in elastic and permanent deformation when the solid particles are broken. Gao et al. (1996) found that increasing the power consumed during grinding dramatically accelerated the size reduction, with only a small change in the energy efciency of the process. In an experiment using a stirred ball mill and grinding aids (Paramasivam and Vedaraman, 1992; Sureshan and Moothedath, 1992; Fuerstenau, 1995; Wang and Forssberg, 1995; Hasegawa et al., 2001; Oettel and Husemann, 2004), Paramasivam and Vedaraman (1992) studied the effect of the physical properties of liquid additives on dry grinding and found that additives increased the neness of the
* Corresponding author. Tel.: +82 55 213 3889; fax: +82 55 261 7017. E-mail address: hkchoi99@changwon.ac.kr (H. Choi). 0892-6875/$ - see front matter 2009 Elsevier Ltd. All rights reserved. doi:10.1016/j.mineng.2009.09.011

ground particles and the powder ow. Fuerstenau and Hasegawa et al., reviewed the use of chemical additives for improving the efciency of both wet and dry pulverization. The effects of grinding aids, i.e. dispersants or additives, on grinding have been mainly explained by two mechanisms. One is the alteration of the surface and mechanical properties of individual particles, such as a reduction of surface energy, and the other is the change in arrangement of particles and their ow in suspensions (Bernhart et al., 1999; Garcia et al., 2002, pp. 1317). Bernhart et al. (1999) also showed that the slurry concentration has an important effect on grinding efciency. In particular, the improvement of experimental conditions was very important for the increase of grinding efciency. Clearly it would be useful if the grinding behaviour could be quantitatively correlated with the grinding efciency. In this study, the behaviour of inorganic powders ground into sub-micron particles in a wet-grinding process in a stirred ball mill has been investigated by examination of the grinding power consumed, which is the main parameter affected by the grinding aids and slurry concentration. The average grinding power consumed based on the measured power is discussed. And the effect of grinding aids on average grinding power consumed is investigated. 2. Experiment 2.1. Equipment The grinding tests were performed in a vertical stirred media mill KMD-1B manufactured by Korea material development Co.,

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Ltd., the same equipment used in previous papers (Choi et al., 2007b). The net volume of the milling chamber was 0.95 l. The grinding media used were alumina 1 mm balls produced by Nikkato Co., Ltd., Japan, 99.9% pure and density 3.60 g cm3. The devices used to measure the energy consumption consisted of an automatic voltage regulator, GPA 100SS AVR (Sung Sin Electronic. Co., Ltd., Korea) and a detection circuit constructed in our laboratory. The torque of the stirrer was measured using an A/D converter (AX5210, Axiom Technology Inc., Taiwan) and interface card (ACL-8112PG, AD Link Technology Inc. UK) with data recorded on-line by a PC using turbo C++ software written in our laboratory (A/D Link Technology Inc., 1998). The particle-size distribution of the ground products was analyzed by a Mastersizer microplus (Malvern Co., LTD., UK), in which the detection method is based on laser diffraction and scattering. The homogenizer US-300T (Nihonseiki Kaisha Ltd., Japan) was used as a dispersion device. The grinding materials, calcite (CaCO3, S500, density = 2.72 g cm3), were produced by Wang Pyo Chemicals Co., Ltd., Korea. Grinding aids were based on poly-acrylic acid (CH2CHCOOH)n. Table 1 shows the physical property of grinding aids.

power consumed at different grinding times another series of experiments was carried out. Slurry of the sample that included 0.2 wt.% grinding aids was ground for an initial period of 13 min and then 1.0 wt.% grinding aid was fed continuously into the grinding chamber from 14 to 73 min. During the last 2 min, the grinding operation took place without feeding grinding aids. An investigation of the effects of slurry concentration on the particle-size distribution of the products for different grinding times was carried out as follows. The power consumption during grinding was recorded every 2 min for 30 min grinding and every 5 min thereafter. 3. Results and discussion Fig. 1 shows the cumulative particle-size distribution of the products obtained after various grinding times without (Fig. 1a) and with grinding aids (Fig. 1b). Whether grinding aids were added or not, the tendencies of changes in particle-size distribution were similar to those shown in Fig. 1. However, the addition of grinding aids resulted in differences in the size of the nal product. It is known that grinding aids are absorbed on the particle surfaces, and then prevent or reduce the agglomeration of ne particles due to van der Waals forces or cold welding. In the absence of agglomeration, grinding can proceed to a ner state, since the limit of grinding is shifted towards the ner region as shown in Fig. 1 (Choi et al., 2009). In Fig. 2, in addition to the benecial effect of the grinding aids, it is also seen that the grinding power consumed is dependent on the slurry concentration. In the present case, a lower slurry concentration, i.e. Cs = 60 wt.%, results in more nely ground particles for a given set of experimental conditions. Furthermore, the addition of the grinding aids results in a smaller power ground, as compared to a case without the grinding aids. In general, the penetration of water and grinding aids into a crack within a particle can promote propagation of the crack, resulting in easier breakage of the particle. With the benecial role of the grinding aids in preventing agglomeration of the particles and the lower slurry concentrations accelerating particle breakage, the combination of lower slurry concentrations and addition of grinding aids should provide optimum conditions for ne grinding for a given consumption of grinding energy. The effects of the grinding aid and the slurry concentration on the grinding power consumed are now explored. The falling off of the grinding power consumed is due to two factors: the larger particles are not readily nipped between the balls, and they tend to be cushioned by a layer of ne particles. The grinding behaviour is often explained in terms of the grinding power and the energy consumed during the grinding process (Choi

2.2. Methods The stirrer was rotated with a constant gap of 5 mm between the bottom and the end of the stirrer. When the stirrer started rotating, the measurement of the grinding power consumed was begun with the on-line data acquisition system. The total charged weights of balls for each value of the ball-lling ratio, J, was 1380 kg (70 vol.% of chamber) for J = 0.7. The slurry concentration was changed between 60.0 and 70.0 wt.%. The grinding experiment was carried out using a batch process of sampling from the pot at the determined grinding time interval. In order to investigate the effect of stirrer speed, ball size and sample size on the grinding

Table 1 The physical property of grinding aids. Grinding Grinding aids of surfactant system 1. Atomic compound 2. Aliphatic compound (a) Aim (b) Alcohol (c) Glycol 3. Resin Grinding aids of solid inserted 1. Carbon material system (a) Carbon black (b) Graphite (c) Lime 2. Mineral (a) Talc (b) Clay

Fig. 1. The frequency particle-size distribution of feed and ground products for experimental conditions: n = 700 rpm, J = 0.7 (), dB = 1.0 mm, Cs = 60 wt.%. (a) Without grinding aids and (b) with grinding aids.

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Fig. 2. (a) The grinding power consumed P and the grinding time as a function of experimental conditions. (b) The grinding energy consumed Ei and the grinding time as a function of experimental; sample: calcite, experimental conditions: n = 700 rpm, J = 0.7 (), dB = 1.0 mm, Cs = 60 wt.% and 70 wt.%, Caids = 1.2 wt.%.

et al., 2007). The average grinding powers consumed for each combination of experimental condition are shown in Fig. 3 (Choi et al., 2007). The reduce rate of the grinding energy consumed, illustrated by the slope of the curve in Fig. 3, decreases gradually with higher slurry concentration. Comparison of the slopes of the curves in Fig. 3a and b also suggests that better grinding energy efciency is expected, i.e., the plateau of the decrease in the slope is reached at lower grinding consumption energy, when high slurry concentration is used. It can be seen that the grinding power consumed, Paveg, decreases with the use of a grinding aid. For Cs = 60 wt.%, Paveg is improved by 31.61% with the use of a grinding aid, whereas it is improved by 37.27% with the use of a grinding aid when Cs = 70 wt.%. Therefore, it is suggested that grinding aids have an important effect on decreasing the grinding power consumed, especially when the slurry concentration is high. These results show that the main benecial effect of grinding aids for a high slurry concentration is to permit full utilization of the grinding medium inside the mill through a reduction of slurry viscosity in the wet-grinding processes. Grinding aids appear to serve the function of preventing re-agglomeration by adsorption onto the external particle surface (Garcia et al., 2002; Wang and Forssberg, 2007, pp. 1617). Some more points about the role of grinding aids can be drawn from the results of this study. Reduction in the attractive forces causes better dispersion of the ne particles, which subsequently results in easier particle ow, and reduction or prevention of the coating of the balls and the chamber wall with powder. Furthermore, it should be noted that the specic surface area did not

reach the grinding limit when grinding aids were used. Therefore, it is conrmed that grinding aids are very effective in the range of sub-micron grinding. 4. Conclusions A series of wet-grinding experiments using inorganic powders has been carried out in a vertical stirred ball mill. The results of these experiments can be summarised as follows. The effects of grinding aids on the grinding power consumed were examined. The grinding power consumed using grinding aids was decreased by 31.6% and 37.2% for 60 and 70 wt.% slurry concentrations, respectively, compared with those without the addition of grinding aids. Thus, it is conrmed that the grinding rate constant improved with the addition of grinding aids, and that they are very effective for ne grinding. Acknowledgement The authors wish to thank an Emeritus Professor Woosik Choi of the Interdisciplinary Program Powder Technology in Pusan National University for advice on this study. References
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Fig. 3. The average grinding power consumed and the slurry concentration as a function of experimental conditions; sample: calcite, experimental conditions: n = 700 rpm, J = 0.7 (), dB = 1.0 mm, Cs = 60 wt.% and 70 wt.%, Caids = 1.2 wt.%.

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