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Separation of Zno from the Stainless Steelmaking Dust and Graphite Mixture by Microwave Irradiation

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Separation of Zno from the Stainless Steelmaking Dust and Graphite Mixture by Microwave Irradiation High Temp. Mater. Proc. 2015; 34(2): 177–184 Yun Zhou, Liushun Wu*, Jue Wang, Haichuan Wang and Yuanchi Dong Separation of ZnO from the Stainless Steelmaking Dust and Graphite Mixture by Microwave Irradiation Abstract: In this study, microwave was used to treat stain- been developed to process ZnO-bearing dust [1–5]. The less steelmaking dust containing zinc oxide. The effects methods can be classified into three groups: physical of heating time, carbon content and zinc oxide content method, wet process (acid process and alkaline process), on the removal efficiency of zinc oxide and the reduction pyrogenic process. Physical method, including magnetic efficiency of iron oxide were investigated. Experimental separation, floatation separation and gravity concentra- results show that, for the sample with 16% (mass percent, tion has been developed in early years. After the dust is the same below) graphite heated for 10 minutes by 10 kW processed by physical method, the removal efficiency of power microwave, the removal efficiency of zinc oxide is zinc oxide is between 50%–60% (mass percent, the same between 80% and 90% and the metallization ratio of iron below) [6], and part of zinc oxide still remains in the dust. oxide is between 40% and 60%; Initial zinc oxide content The removal efficiency of zinc oxide doesn’t reach expec- has a slight effect on the removal efficiency of zinc oxide. tation. Besides, lots of water is required for its effective The results indicate microwave treatment is one of the fea- operation. For wet process, the essence of ZnO removal is sible ways to process metallurgical solid waste containing that zinc oxide in the dust reacts with acid or base to form the metal with low boiling point. the compounds dissolved into solution, and then the solu- tion is separated from residual by filtration. However, Keywords: microwave heating, stainless steelmaking during zinc oxide leaching, a great deal of iron oxide dust, carbon thermal reduction, zinc removal becomes soluble iron, which leads to low utilization of iron in dust (the part of iron can’t be recycled by steel PACS® (2010). 05.70.-a, 07.57.-c plant), so this technique is not suitable for the dust with low content of ZnO [7–9]. For low-grade ZnO-bearing dust DOI 10.1515/htmp-2013-0118 with high content of carbon, pyro-metallurgy technique Received November 22, 2013; accepted April 26, 2014; which is based on carbothermic reduction reaction is the published online May 28, 2014 most common way [10]. The technique can be subdivided into three groups: rotary hearth furnace, fluidization and rotary kiln which is a representative of pyro-metallurgy process. However, the methods share a disadvantage – 1 Introduction high energy consumption. To develop an environment-friendly and low energy During the smelting of stainless steel, dust generates inev- consumption technique, recently some researchers suc- itably. The dust is mainly composed of iron oxide, zinc cessfully separated zinc oxide from Zn-bearing dust using oxide, chromium oxide, calcium oxide, silica, and so on. the microwave processing [11–17]. Compared with other Except for zinc oxide, the other oxides are effective consti- heating methods, microwave have better heating proper- tutes for stainless smelting. Therefore the removal of zinc ties, such as fast heating rate, selective heating. Besides, oxide from the dust makes it possible to recycle in stain- the microwave heating overcomes the barrier of tradi- less steel mill. In recent decades, some methods have tional heating model-heat transmission from external to internal. In addition, the microwave heating has two ad- vantages in the processing of ZnO-bearing stainless steel *Corresponding author: Liushun Wu: School of Metallurgical dust: rapid heating (Since the dust contains some magnet, Engineering, Anhui University of Technology, Maanshan, Anhui it has a strong ability to absorb microwave) and lower 243002, China. E-mail: [email protected] Yun Zhou, Jue Wang, Haichuan Wang, Yuanchi Dong: School reduced processing temperature (It is generally believed of Metallurgical Engineering, Anhui University of Technology, that microwave heating may lower reaction activation Maanshan, Anhui 243002, China energy [18].) 178 Y. Zhou et al., Separation of ZnO from the Stainless Steelmaking Dust Table 1: Chemical compositions of EAF dusts (mass%) Table 2: Particle sizes of Zn-bearing stainless steelmaking dust (μm) Oxides Carbon steel Stainless steel Cumulative percent Particle size dust (EAF) dust (EAF) D10 8 Fe2O3 56.83 48.69 D25 16 FeO 4.58 9.85 D50 37 MFe – – D75 68 ZnO 4.86 3.45 D90 95 CaO 14.72 12.06 Note: D10, D25, D50, D75, D90 and Dav are cumulative SiO 5.19 4.06 2 percentages of particle sizes at 10%, 25%, 50%, 75%, 90% Al O 1.27 – 2 3 and average particle size, respectively. MgO 6.46 – Cr2O3 – 16.66 NiO – 2.96 Others 6.09 2.27 Table 3: The ratio of the dust to graphite in mixture (mass%) EAF dust Graphite 92% 8% 88% 12% The above mentioned researches focused on the con- 84% 16% ventional Electric Arc Furnace (EAF) steelmaking dust. Compared with the conventional EAF steelmaking dust, the stainless steelmaking dust has a higher content of 2+ 3+ Cr2O3 and a better ratio of Fe and Fe which is closer to 76 μm. Besides, the screen underflow was also analyzed 2+ 3+ the ratio of Fe and Fe in Fe3O4 (see Table 1). The iron by a Laser Granulometer (S3500, American Microtrac oxide combines with ZnO or Cr2O3 to form spinel (the Company). Table 2 shows the size distribution of screen mineral has a high melting point), and the difference in underflow. The sizes of the particles are between 37 μm to the ratio of Fe2+ and Fe3+ may means the difference in the 68 μm. content of Fe3O4 (Fe3O4 shows excellent heating behavior To study the effect of graphite content on the removal than FeO or Fe2O3, as seen in Table 5). This may lead to efficiency of ZnO, graphite was added to the dust to obtain the difference in heating and reduction behavior of the different graphite-dust mixtures. To study the effect of stainless steelmaking dust from that of the conventional zinc oxide content on the removal efficiency of ZnO, the EAF steelmaking dust. Therefore, the heating and reduc- different ZnO-graphite-dust mixtures were prepared by tion behavior of the stainless steelmaking under micro- mixing the graphite-dust mixture and different amount of wave irradiation will be investigated in this study. The zinc oxide. study will give guidance for effective utilization of stain- In a general run, a predetermined amount of graphite less steelmaking dust containing zinc oxide. (<76 μm) was added into the stainless steelmaking dust (the ratios of the dust to graphite are shown in Table 3) or a predetermined amount of zinc oxide was added into the 2 Experimental graphite-dust mixture. The mixture (50 g) was well mixed in a pot mill. After dried for 4 hours, the mixture in a The chemical composition of the stainless steelmaking quartz crucible (inner diameter: 50 mm, height: 60 mm) dust and carbon steel dust from Bao Steel Co. Ltd. in China was heated in a microwave furnace (maximum power: was analyzed by an ISP Emission Spectrum (type: Thermo 10 kW, frequency: 2450 MHz). Figure 1 shows a schematic Elemental-IRIS Intrepid) and titration (Analysis result is diagram of the microwave furnace. Nitrogen gas was shown in Table 1). The morphology and mineral structure used as protection gas to enhance reduction atmosphere of the dust were analyzed by a Scanning Electron Micro- (0.1 L/min). A double platinum rhodium thermocouple scope (JSM-6490LV) equipped with an Energy Dispersive (Pt – 6% Rh / Pt – 30% Rh) was inserted into the sample to X-ray Spectroscopy (EDX). measure temperature. The thermocouple was protected To determine the distribution of particle size, the by two layer pipes: inner layer of alumina pipe and outer dust was screened by a sieve with 200 meshes, and 85% layer of stainless steel (Type: 316L) pipe. Since stainless of samples passed through the mesh. The result indi- steel had a strong ability to reflect microwave, the protec- cates that 85% of particles in the dust are smaller than tive pipe could effectively protect the interruption on the Y. Zhou et al., Separation of ZnO from the Stainless Steelmaking Dust 179 Fig. 1: Schematic diagram of microwave furnace temperature measurements by the microwave. After pro- 3 Results and discussion cessing, shutting off the furnace and increasing the flow rate of nitrogen gas (5 L/min), and then moving the sample Figure 2 presents SEM image of the dust and Table 4 shows along with the crucible out of the furnace to quench. the chemical compositions of the particles in the dust. As Usually, the sample could be cooled to 800 K in 2 minutes. shown in Fig. 2 and Table 4, iron oxide exists in most of The quenched sample was collected for analysis. the particles in the dust and its content is above 30%. Zinc The phases in the sample were analyzed by a Scanning oxide only exists in the big particles in the dust. The differ- Electron Microscope. The amount of metallic iron in the ence in the distribution of the oxides may be caused by the sample was analyzed by potassium dichromate titration difference in the source of the oxides. During EAF smelt- (Metallic iron was leached using CuSO4 solution or FeCl3 ing, due to the splashing of liquid iron, a few liquid iron solution, and leach solution and residual were separated is oxidized on the surface of EAF to form iron oxide. Then by filtration.
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