A low MgO content in sinter is conducive to reduce the MgO content in blast furnace slag. This study investigated the effect of MgO content in sinter on the softening–melting behavior of the mixed burden based on fluxed pellets. When the MgO content increased from 1.31wt% to 1.55wt%, the melting temperature of sinter increased to 1521°C. Such an increase was due to the formation of the high-melting-point slag phase. The reduction degradation index of sinter with 1.31wt% MgO content was better than that of others. The initial softening temperature of the mixed burden increased from 1104 to 1126°C as MgO content in sinter increased from 1.31wt% to 1.55wt%, and the melting temperature decreased from 1494 to 1460°C. The permeability index (S-value) of mixed burden decreased to 594.46 kPa·°C under a high MgO content with 1.55wt%, indicating that the permeability was improved. The slag phase composition of burden was mainly akermarite (Ca2MgSiO7) when the MgO content in sinter was 1.55wt%. The melting point of akermarite is 1450°C, which is lower than other phases.
To maintain the normal pressure difference of blast furnace smelting and avoid hanging and developing gas–solid reduction of the mixed burden in the upper part of the blast furnace, certain requirements on the performance of the cohesive zone for blast furnace smelting, especially the position and permeability of the cohesive zone, must be fulfilled [1–2]. The properties of the cohesive zone are mainly affected by the metallurgical performance of the mixed burden and the properties of the slag phase.
MgO content in sinter is increased to improve slag fluidity for ensuring the good fluidity and desulfurization capacity of blast furnace slag [3–4]. Many studies have investigated the softening–melting properties of the mixed burden under different MgO contents [5–9]. Umadevi et al. [10] studied the difference of tumbler index (TI), reduction degradation index (RDI), and reduction index (RI) when the MgO content in high silicon- and low silicon-sinter increased from 1.40wt% to 3.20wt%; the results indicated that the MgO content in sinter should be less than 2.80wt%, and SiO2 content in sinter should be less than 6.0wt%. Jiang et al. [11] examined the effect of MgO on the blast furnace cohesive zone. They found that when the MgO content in sinter was reduced from 3.0wt% to 1.3wt%, the cohesive zone gradually narrowed, thus reducing the pressure difference of the charge and improving the permeability of the cohesive zone. The effect of MgO on the softening–melting properties of burden, which contains vanadium, titanium, and chromium, was also studied. Zhou et al. [12] and Zheng et al. [13] investigated the influence of MgO content on the phase structure of titanium-containing sinter and discussed the effects of different MgO contents on the high temperature properties of titanium-containing burden, such as softening temperature, melting temperature, and maximum pressure difference. The softening–melting behavior was also analyzed when the sinter with different MgO contents was mixed with chrome vanadium–titanium magnetite. The result showed that the high-melting-point component of slag augmented when the MgO content increased, thereby reducing the gas permeability of the mixed burden [1].
Many studies on the softening–melting behavior of burden under different MgO contents in sinter have been conducted and have great significance in improving the permeability of the blast furnace cohesive zone. However, the studied MgO contents in sinter in previous research are relatively high. On the basis of ensuring the smelting of the blast furnace, the MgO content in sinter can be further reduced. Pellets in the mixed burden are generally acidic pellets with a low calcium content. Few studies on the softening–melting behavior of the mixed burden, which is based on calcareous flux pellets and under different MgO contents in sinter, have been performed. Research on the phase composition of the integrated charge slag when the calcium content of the pellet is high is also scarce.
Therefore, this study mainly investigated the metallurgical properties of sinter and the softening–melting behavior of the mixed burden when the pellet alkalinity was 0.94 and the MgO content in sinter was 1.04wt%, 1.31wt%, and 1.55wt%. The influence of the comprehensive charge slag on the permeability index of the cohesive zone was also analyzed.
2.
Experimental
2.1
Materials
The pellets used in this experiment were flux pellets with a binary alkalinity of 0.94. The total Fe (TFe) content of pellets was approximately 65.65wt%, and the CaO content was 2.35wt%. The sinter was prepared by laboratory sintering pot. The main difference among the three kinds of sinter was the MgO content (1.04wt%, 1.31wt%, and 1.55wt%). The composition of iron-containing raw materials used in the experiment is shown in Table 1. The particle size of the various materials used in the experiment ranged from 10 to 12.5 mm.
Table
1.
Chemical composition of raw materials
Material
Composition / wt%
R2
MgO
TFe
FeO
CaO
SiO2
Al2O3
TiO2
Sinter 1#
1.04
57.96
9.13
9.74
5.26
1.66
0.14
1.85
Sinter 2#
1.31
58.06
10.40
9.34
4.95
1.71
0.12
1.88
Sinter 3#
1.55
57.15
7.39
9.79
5.49
1.74
0.10
1.78
Pellets
0.73
65.65
1.38
2.35
2.50
0.23
0.11
0.94
Lump
0.79
62.86
0.48
0.06
3.67
0.05
0.04
0.016
Note: R2 represents the mass ratio of CaO to SiO2 in raw material.
To simulate the position of the blast furnace cohesive zone, the charge structure adopted in this experiment is presented in Table 2. The softening–melting experimental device of the mixed burden is shown in Fig. 1. The materials used in the experiment were dried in an oven at 105°C for 2 h, and then uniformly mixed according to the ratio of the burden structure (Table 2). First, 20 g of coke with a diameter of 10–12.5 mm was taken into a graphite crucible with an inner diameter of 75 mm to simulate the coke in the cohesive zone of the blast furnace. Second, 500 g of the mixed burden was placed on the upper part of the coke, and another 20 g of coke was placed on top of the mixed burden. The heating system and gas flow settings during the experiment are shown in Fig. 2.
Table
2.
Proportion of the mixed burden used in tests wt%
In the softening–melting test of the charge, its initial softening temperature (T10) is the temperature at which the charge shrinkage reaches 10%, and the final softening temperature (T40) refers to the temperature at which the charge shrinkage reaches 40%. The initial melting temperature (Ts) indicates the temperature at which the pressure difference of the charge sharply rises, and the temperature at the end of melting (Td) is the temperature at which iron starts to drip. The characteristic curve is illustrated in Fig. 3. The permeability index (S-value) of the charge was calculated according to Eq. (1), where ΔP means the pressure drop of the charge in softening–melting test.
Fig.
3.
Experimental curve of softening–melting characteristics.
3.1
Microstructure of sinter with different MgO contents
To study the influence of MgO content on the phase structure of sinter, scanning electron microscope (SEM) was used for observing the microstructure of sinter. Through SEM characterization, the sinter was found to be mainly composed of hematite, magnetite, calcium ferrite, and silicate. As shown in Figs. 4(a) and 4(b), when the MgO content in sinter was 1.04wt%, the sinter contained additional hematite and composite calcium ferrite phases. Hematite, magnetite, and calcium ferrite were intertwined. When the MgO content in sinter was 1.31wt%, hematite and calcium ferrite in the sinter had an intertwined structure (Figs. 4(c)). The sinter had additional magnetite phases with MgO content of 1.31wt%, as shown in Fig. 4(d), and energy dispersive spectroscopy (EDS) results indicated that a certain amount of Mg existed in the magnetite. Because the ion radius of Mg2+ and Fe2+ is similar, substitution reaction is easily to undergo to form (Mg,Fe)O·Fe2O3. In addition, Mg–O bonds are shorter than Fe–O bonds and have large bond energy, which can stabilize the magnetite lattice [14–15]. The grain size of magnetite was significantly increased with the increase of MgO concent from 1.04wt% to 1.55wt%, as displayed in Fig. 4. When the MgO content in sinter increased to 1.55wt%, (Mg,Fe)O·Fe2O3 and (Fe,Mg)O·Fe2O3 formed partial segregation in sinter, resulting a certain amount of liquid phase in other areas, and intertwined calcium ferrite dendrites are finer, as shown in Fig. 4(e). The quality of the sintered ore was improved.
Fig.
4.
Micrographs of the sinter with different MgO contents and the EDS results of some points in the micrographs: (a, b) 1.04wt%; (c, d) 1.31wt%; (e) 1.55wt%; (P1–P4) EDS maps of points P1–P4. H is hematite, M represents magnetite, SFCA is composite calcium ferrite, P is hole, and S indicates silicate phase.
3.2
Properties of the sinter with different MgO contents
The reduction and softening–melting behavior of sinter are quite complex processes in the blast furnace. The RI and RDI are important properties for the improvement of sinter quality. The RI of the sinter was determined by the ISO test under 900°C, and the RDI was tested under 500°C, followed by a drum test. Reduction degradation index (RDI or RDI+3.15) means the mass proportion of sinter with a particle size above 3.15 mm after dtum test. The Fig. 5 shows the RI and RDI of the sinter with different MgO contents. Its RI was the lowest when the MgO content was 1.31wt%, which was only 76.72%. Meanwhile, the RDI was the highest, which was 83.58%. Reduction degradation is mainly caused by the lattice expansion of Fe2O3 to Fe3O4 during the reduction. According to the microstructure of the sinter with different MgO contents, additional magnetite grains are found in the sinter with 1.31wt% MgO content, which was difficult to reduce. The RDI result of sinter with MgO content of 1.31wt% is attributed to the wide distribution of magnetite grains. The magnetite grains of the sinter with 1.55wt% MgO content were not well dispersed, as shown in Fig. 4, resulting in a lower RDI than that of the sinter with 1.31wt% MgO content.
Fig.
5.
RI and RDI of the sinter with different MgO contents.
The softening–melting results of the sinter with different MgO contents are presented in Fig. 6. Fig. 6(a) shows that when the MgO content in sinter was increased from 1.04wt% to 1.55wt%, its T10 increased from 1112 to 1125°C, and its T40 increased from 1205 to 1232°C, with the softening interval widened by 14°C. The increase of MgO raised the softening temperature and softening interval of the sinter. The sinter with 1.55wt% MgO content had the best reduction performance. A dense metal iron shell was easily formed in the surface during the reduction process, resulting in high strength. Therefore, T10 and T40 were the highest.
Fig. 6(b) illustrates that when the MgO content in sinter was increased to 1.55wt%, its Ts was increased by 9°C, and its Td was gradually increased from 1513 to 1521°C. During the reduction reaction process, most MgO in the iron phase continuously entered the slag phase; caused the high MgO content in the slag phase; and increased the magnesia sulfate, calcium forsterite, and magnesium aluminum in the slag phase. The amount of high-melting-point minerals, such as spinel, was increased and thus increased Td.
Fig.
6.
Softening–melting behaviors of the sinter with different MgO contents: (a) initial softening temperature T10 and final softening temperature T40; (b) initial melting temperature Ts and melting temperature Td; (c) shrinkage ratio and its magnified curve of shrinkage near 1350°C; (d) pressure drop.
The pressure difference of the sinter with 1.04wt% MgO content showed a second sudden increase at the end of the experiment, thereby decreasing the shrinkage curve near 1350°C, as shown in Figs. 6(c) and 6(d). When the MgO content was 1.31wt%, the pressure difference of the sinter was low, and the pressure difference was continuously lowered after rising.
3.3
Softening–melting behavior of the mixed burden
The softening–melting performance of the mixed burden affects the smooth operation of the blast furnace [16–21]. Specifically, the permeability of the blast furnace and the location of the cohesive zone have significant impacts on the production of the blast furnace [22]. Fig. 7 shows the shrinkage curve and pressure difference curve of the mixed burden in the softening–melting test with low-magnesium sinter. The MgO content in sinter was 1.04wt%, 1.31wt%, and 1.55wt%, respectively. Table 2 presents the charge structure. Fig. 7(a) shows a certain negative growth phenomenon in the shrinkage curve under different integrated charge structures in the early stage of the experiment, and the mixed burden gradually shrank when temperature exceeded 1000°C. By amplifying the “a” region, when the MgO content was 1.55wt%, the expansion ratio of the mixed burden was the largest after 650°C. The reasons are because the FeO content in the sinter with 1.55wt% MgO content; and a large amount of Fe2O3, which caused lattice expansion during the reduction process, existed and further improved the expansion ratio of the mixed burden. As the temperature gradually increased above 1000°C, the integrated charge surface was reduced to metal iron shell, and the melt that contains FeO gradually oozed out. The material layer began to deform and shrink. The Ts and Td were obtained by amplifying the “b” region.
Fig.
7.
Shrinkage curve (a) and pressure difference curve (b) under the mixed burden.
Fig. 7(b) shows the pressure difference curves of the mixed burden with different MgO contents in sinter. When the MgO content in sinter was 1.04wt%, the pressure difference of the mixed burden sharply decreased twice during the experiment. The maximum pressure difference was 7.70 kPa, and the calculated S-value was 1074.18 kPa·°C. When the MgO content in sinter increased to 1.31wt%, only one steep significant rise occurred during the experiment, after which the pressure difference gradually decreased. The maximum pressure difference decreased to 7.42 kPa, and the S-value was 940.26 kPa·°C. When the MgO content in sinter was further increased to 1.55wt%, the maximum pressure difference of the mixed burden decreased to 4.71 kPa, and the S-value decreased to 594.46 kPa·°C. Moreover, the permeability of the mixed burden was the best when the MgO content in sinter ranged from 1.04wt% to 1.55wt%.
Fig. 8 shows the softening–melting characteristics of the mixed burden with different MgO contents in sinter. Fig. 8(a) illustrates the softening characteristic values. When the MgO content in sinter was 1.55wt%, the T10 and T40 of the mixed burden were the highest, and the softening interval was the narrowest. Fig. 8(b) displays the melting droplet characteristic value. When the MgO content in sinter increased from 1.04wt% to 1.55wt%, the Td of the mixed burden gradually decreased from 1494 to 1464°C. Fig. 8(c) shows the cohesive zone location of the mixed burden; when the MgO content in sinter gradually increased from 1.04wt% to 1.55wt%, the position of the cohesive zone in the blast furnace decreased, and the cohesive zone became thin. Therefore, when the MgO content in sinter increased from 1.04wt% to 1.55wt%, the melting behavior of the mixed burden was improved.
Fig.
8.
Effect of MgO content in sinter on the softening–melting property of the mixed burden: (a) softening characteristics; (b) melting characteristics; (c) temperature range of cohesive zone.
The main phases of the slag system in the blast furnace cohesive zone are different, which lead to a large difference in metallurgical properties and cohesive zone material properties. To investigate the influence of the cohesive zone slag on the melting performance of the mixed burden based on low-magnesium sinter, XRD analysis was performed on the slag formed by the mixed burden after the softening–melting experiment, as shown in Fig. 9. The contents of the main slag phase are shown in Table 3. When the MgO content in sinter was 1.04wt%, a 47.99wt% Ca3Mg(SiO4)2 phase was found in the slag. The remaining phases were Ca2Al(AlSi)O7 and Ca2MgSi2O7. The Ca2MgSi2O7 phase content of the slag increased from 16.79wt% to 28.60wt% as the MgO content in sinter increased from 1.04wt% to 1.31wt%. The slag phase contained 55.47wt% Ca2MgSi2O7 when the MgO content in sinter was 1.55wt%. The rest were Ca3Mg(SiO4)2 and Ca2Al(AlSi)O7. These three kinds of mixed burden slag phases also contained C and other element oxides, and the contents were relatively low. In the slag phase, the melting point of Ca2Al(AlSi)O7 is 1593°C, the melting point of Ca3Mg(SiO4)2 is 1550°C, and the melting point of Ca2MgSi2O7 is 1450°C. Ca3Mg(SiO4)2 is close to the primary crystal region of periclase (MgO) in phase diagrams that has a high melting point. Thus, when the MgO contents in sinter were 1.04wt% and 1.31wt%, the melting temperature of the mixed burden was higher than that when the MgO content was 1.55wt%. The S-value of the mixed burden, when the MgO contents in sinter were 1.04wt% and 1.31wt%, was large with poor permeability. When the MgO content in sinter was 1.55wt%, there are fewer high melting point slag phases and lower S-value during softening–melting test, which increased the permeability of the cohesive zone in the blast furnace. The high-melting-point Mg–Al spinel phase was not analyzed in these three kinds of comprehensive charge materials. Therefore, the pressure difference and S-value of the mixed burden were low, and the Td did not exceed 1500°C.
Fig.
9.
X-ray diffraction patterns of the slag with different MgO contents: (a) 1.04wt%; (b) 1.31wt%; (c) 1.55wt%.
This study investigated the metallurgical properties of the sinter with different MgO contents, which range from 1.04wt% to 1.55wt%, and the softening–melting behavior and permeability index of the mixed burden based on low-magnesium sinter and fluxed pellets.
(1) When the MgO content in sinter ranges from 1.04wt% to 1.55wt%, the softening interval of the sinter increases from 93 to 107°C. The increase of MgO content in sinter results in the presence of a high-melting-point material during test, which further causes the increase of Td from 1513 to 1521°C.
(2) Based on the same ratio of fluxed pellets, when the MgO content in sinter increases from 1.04wt% to 1.55wt%, the T10 of the burden increases from 1104 to 1126°C, and Td decreases from 1494 to 1460°C. The S-value decreases from 1074.18 to 594.46 kPa·°C. The position of the cohesive zone is lowered, and the permeability is improved when the MgO content in sinter is increased to 1.55wt%.
(3) When the MgO content in sinter is 1.04wt%, the slag phase of the burden is mainly Ca3Mg(SiO4)2. The Ca2MgSi2O7 phase content of the slag increases from 16.79wt% to 28.60wt% as the MgO content in sinter increases from 1.04wt% to 1.31wt%. The slag contains 55.47wt% of Ca2MgSi2O7 when the MgO content in sinter is 1.55wt%, which could decrease Td and S-value, and can improve the permeability of the burden. The slag phase of these three kinds of burden contains a small amount of other impurity oxides.
Acknowledgements
This work was financially supported by the Fundamental Research Funds for the Central Universities, China (No. 06500170) and the Guangdong Basic and Applied Basic Research Foundation, China (No. 2020A1515111008)
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