Startseite Dependence of Temperature and Slag Composition on Dephosphorization at the First Deslagging in BOF Steelmaking Process
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Dependence of Temperature and Slag Composition on Dephosphorization at the First Deslagging in BOF Steelmaking Process

  • Chao-gang Zhou EMAIL logo , Jing Li , Cheng-bin Shi , Wen-tao Yu , Zhi-ming Zhang , Zhi-ming Liu und Chang-fu Deng
Veröffentlicht/Copyright: 17. Juli 2015
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High Temperature Materials and Processes
Aus der Zeitschrift High Temperature Materials and Processes Band 35 Heft 4

Abstract

Effects of temperature and slag composition on dephosphorization in a 120 ton top-bottom combined blown converter steelmaking process by double slag method were studied. The slag properties were determined by scanning electron microscope- energy dispersive spectrometry (SEM-EDS), X-ray diffraction (XRD). The results show that the transition oxidation temperature between dephosphorization and decarbonization Tf is not the favorable temperature for the first deslagging. The optimum first deslagging temperature is confirmed to be approximately 1,673 K which is about 70 K higher than Tf. High melting temperatures phases (such as 3CaO·SiO2) in the slag with high basicity and MgO content are unfavorable to the dephosphorization. The optimum process condition for dephosphorization at the first deslagging in present work is approximately 1,673 K in temperature, 2.0 in slag basicity, 6 and 17 mass% in MgO and T.Fe content, 6 mass% ≤ MnO content.

Keywords: dephosphorization; temperature of the first deslagging; thermodynamic analysis; slag composition

Introduction

High phosphorus content in final steel products usually cause embrittlement largely induced by the segregation of phosphorus at grain boundaries [1], and low ductility, poor mechanical and welding performances [2]. The demand on low phosphorus content is more and more critical for pipeline steel and marine ship steel. For example, pipeline steels of high grades require phosphorus content less than 0.01 mass%, in particular, the phosphorus content in the 9 mass% Ni steel grade is demanded lower than 0.004 mass% [3]. Thus, the efficient phosphorus removal is increasingly needed, double slag operation combined with remaining slag method is widely applied in many steel plants. Many researchers [4–7] reported the efficiency of this method for dephosphorization and proposed that the temperature, slag basicity and FeO content should be properly controlled in order to obtain the favorable dephosphorization condition. But due to their trial conditions difference, the parameters proposed by different researchers based on their industrial trial vary in a large range.

It takes advantage of low temperature at the first stage of double slag method, which favors dephosphorization; thus, it is essential to confirm the favorable temperature of the first deslagging for dephosphorization. Some researchers [8, 9] proposed that the transition temperature for the selective oxidation reaction Tf should be the admirable temperature for the first deslagging temperature based on the selected deoxidation theory. The other researchers [10, 11] calculated Tf based on this viewpoint are approximately 1,573 K. Thus, the proper temperature for the first deslagging should be further understood from thermodynamic. Properties and compositions of slag for dephosphorization are extremely concerned by the researchers and some works [12, 13] have done for this, but slag structures and thermodynamic properties for dephosphorization also need to be further understood.

In the present study, based on the industrial trial results, the admirable the first deslagging temperature was analyzed from the thermodynamic. In addition, to understand effects of slag on the reaction process of dephosphorization, the structure and properties of slag were analyzed by scanning electron microscope-energy dispersive spectrometry (SEM combined EDS) and X-ray diffraction (XRD).

Experimental

Twenty industrial trials were carried out in a 120-ton top-bottom combined blown steelmaking converter. Double slag operation was carried out in the converter for dephosphorization. The composition and temperature of the hot mental are shown in Table 1.

Table 1:

Composition and temperature of the hot metal in the present study.

Hot metal composition (mass %)Temperature/°C
CSiMnPS
4.1–4.80.39–0.730.27–0.460.10–0.140.030–0.0451,279–1,325

After the hot metal and scrap (16% of the total load) was loaded in the BOF, blowing of oxygen into the converter from the top lance was started. After 1 min, the first patch of lime along with certain amount of iron ore, fluorite and burn dolomite were added into the converter to form slag. The blowing of oxygen was stopped after about 5–6 min. The converter was then tilted for deslagging and about 50–70% of P2O5-rich slag is removed out of the BOF. The slag at this stage is called first slag. After removing the slag as much as possible, the converter was put into normal standing position again. This was followed by the addition of the second patch of lime, iron ore, fluorite and burnt dolomite. Lime was used to adjust the slag basicity while iron ore was charged to improve the dissolution of lime into slag and to simultaneously control the proper temperature, carbon and phosphorus contents for tapping. The total amount of the slag is about 14–18 ton. To get good mass transfer, bottom blowing was adopted throughout the whole process.

Steel samples and slag samples were taken in each heat. The time of the sampling was during the first deslagging process. A steel spoon was used for sampling. The steel sample was obtained about 0.8 m below the surface of the molten bath. The slag attached on the steel rod was employed as slag sample. Thereafter, the slag composition was analyzed by X-ray fluorescence (XRF). The FeO contents in the slags were analyzed by chemical analysis. The thermodynamic calculation software FactSage 6.4, SEM combined EDS and XRD were applied to analyze structures and properties of slag to understand how the slag affects to dephosphorization.

Results and discussion

Temperature for dephosphorization at the first deslagging

Figure 1 shows the dependence of dephosphorization rate on temperature of first deslagging. As shown in Figure 1, with the increase in temperature at first deslagging, the dephosphorization rate increases firstly, and thereafter decrease after the temperature over approximating 1,673 K. The experimental results show that the favorable temperature for the first deslagging should be approximately 1,673 K. Many researchers [14–18] proposed that the favorable first deslagging temperature should be about 1,573 K.

Figure 1: Dependence of dephosphorization rate on temperature of the first deslagging.
Figure 1:

Dependence of dephosphorization rate on temperature of the first deslagging.

To deeply understand the favorable dephosphorization condition, the thermodynamic analysis was performed. At the slag–steel interface, the dephosphorization reaction takes place as follows:

(1)2[P]+5(FeO)=(P2O5)+5[Fe]
(2)ΔG1θ=−27763.3561+255.2313T19−21(J⋅mol−1)
(3)ΔG1=ΔG1θ+RTlnaP2O5×aFe5aFeO5×aP2J⋅mol−1

Decarbonization reaction happens as eq. (4), completing with the dephosphorization reaction.

(4)[C]+(FeO)=CO+[Fe]
(5)ΔG2θ=98799−90.76T19−21(J⋅mol−1)
(6)ΔG2=ΔG2θ+RTlnaCO×aFeaC×aFeOJ⋅mol−1

The following reaction can be obtained through eqs (1)–(4):

(7)2[P]+5CO=(P2O5)+5[C]
(8)ΔG3θ=−521758.3561+709.0313T19−21(J⋅mol−1)
(9)ΔG3=ΔG3θ+RTlnaP2O5×aC5aP2×PCO5J⋅mol−1

where aP2O5 and aFeO are the activities of P2O5 and FeO in slag, respectively; aFe, aP, and aC are the activities of Fe, P, and C, respectively; PCO is the partial pressure of CO. Reaction (7) is the selective oxidation reaction between carbon and phosphorus. The transition temperature for the selective oxidation reaction Tf can be calculated by ΔG3=0. When temperature is higher than Tf in the bulk, the decarbonization reaction will take place prior to dephosphorization reaction in thermodynamics. Consequently, it is extremely significant to confirm Tf to obtain the optimum temperature at the first deslagging.

To obtain the Tf, the activity coefficient of P2O5 in slag is calculated by eq. (10) [19–21], and the activity coefficients of C and phosphorus in liquid metal are calculated by eqs (11) and (12). In the calculations, the slag composition at the first deslagging is taken the average as: 42.87 CaO, 9.03 mass% MgO, 22.09 mass% SiO2, 6.31 mass% FeO, 7.39 mass% MnO, 2.29 mass% P2O5. The molten steel composition and the temperature for the first deslagging are taken as, C 3.26 mass%, Si 0.0278 mass%, Mn 0.1328 mass%, P 0.0543 mass%, S 0.0313 mass%, T = 1,674 K. The activity interaction coefficients of C and P are listed in Table 2:

(10)lgγP2O5=−1.12[22XCaO+15XMgO+13XMnO+12XFeO−2XSiO2]−44600T+23.8
(11)lg fC=eCC[%C]+eCSi[%Si]+eCMn[%Mn]+eCP[%P]
(12)lg fP=ePC[%C]+ePSi[%Si]+ePMn[%Mn]+ePP[%P]
Table 2:

Activity interaction coefficient of elements in molten steel [19–21].

eCCeCSieCMneCPePCePSiePMnePP
0.140.08−0.0120.0510.130.1200.062
Figure 2: Gibbs free energy as a function of temperature.
Figure 2:

Gibbs free energy as a function of temperature.

As shown in Figure 2, the transition temperature Tf is about 1,599 K, which is somewhat lower than the favorable temperature for the first deslagging as shown in Figure 1. The temperature range shown in Figure 2 can be divided into three regions according to the Gibbs free energy variation. In region (I) (T < Tf), ΔG1<ΔG2<0, ΔG3<0, the dephosphorization reaction occurs prior to decarbonization reaction. But it should be noted that the Gibbs free energy change for reaction (7) is also negative, thus it can also take place in this region. In fact, during the first deslagging period the carbon content decreases from about 4 mass% to 3 mass% that supports the analysis. In region (II), ΔG2<ΔG1<0, ΔG3>0, the decarbonization reaction occurs prior to dephosphorization reaction. It is generally thought that Tf should be the favorable temperature at the first deslagging since dephosphorization is not the main reaction above this temperature. But in this region, the Gibbs free energy is also much lower than 0, i.e. the dephosphorization reaction can also take place. At the temperature Tf, rephosphorization reaction (7) just starts to take place, thus, it can be easily deduced, the increase rate of phosphorus content is lower than its removal rate and the process still appear dephosphorization. With the temperature increase, the phosphorus removal rate will slow down and the rephosphorization rate will speed up. Only at certain temperature, the phosphorus removal rate equals its increasing rate, the phosphorus content will not decrease any more. According to the analysis, this temperature, which is higher than Tf should be the favorable temperature at the first deslagging. Present trials results show that the favorable temperature should be about 1,673 K at the first deslagging, about 70 K higher than Tf.

Mineral phase of dephosphorization slag

Slag compositions influence the activity coefficient of P2O5 and the activity of CaO, which directly affect dephosphorization reaction. CaO–SiO2–FeO ternary phase diagram was calculated by Factsage6.4 (FToxid database) at 1,673 K at the first deslagging as shown in Figure 3. The compositions of BOF slag at first deslagging were presented in CaO–SiO2–FeO ternary phase diagram at 1,673 K. As shown in Figure 3, the composition mainly locate in the region of liquid and the 2CaO·SiO2 (s)-bearing region, which means the precipitation of 2CaO·SiO2 at the temperature.

Figure 3: Composition of the slag at first deslagging in CaO–SiO2–FeO ternary phase diagram at 1,673 K.
Figure 3:

Composition of the slag at first deslagging in CaO–SiO2–FeO ternary phase diagram at 1,673 K.

In order to further understand how the slag composition and its structure effect on the dephosphorization, SEM-EDS and XRD are applied to detect the slag properties. Two heats of first slag are selected for the examination to understand their differences, one heat is poor (1#) and the other is admirable (2#) for dephosphorization, phosphorus content and dephosphorization rate at the first deslagging of two selected heats are listed in Table 3.

Table 3:

Phosphorus content and dephosphorization rate at the first deslagging of two selected heats/mass%.

Heat no.Initial PPDephosphorization rate
1#0.1140.05551.75
2#0.1310.03275.57

As shown in Figure 4(a), the phase particles of 1# heat are very non-uniform in size and morphology. Figure 4(b) shows that particles is a type of calcium silicate, and the phosphorus content in this particle is relative low, about 2.26 mass%. Figure 4 shows that the matrix is composed of calcium silicate containing some FeO and MnO; the phosphorus distributes mainly in these region. Whereas some iron spinel particles composed of MgO and FeO + MnO, wrapped by the matrix, are observed. In these spinel regions, the phosphorus is nearly absent that means these particles can hardly dephosphorize.

Figure 4: SEM images and EDS analysis results of the first deslagging of 1# heat: (a) SEM image, (b) EDS spectra.
Figure 4:

SEM images and EDS analysis results of the first deslagging of 1# heat: (a) SEM image, (b) EDS spectra.

In contrast, as shown in Figure 5(a), the slag particles of 2# heat are generally uniform in size and morphology. Figure 5(b) shows that particle is a type of calcium silicate composed of CaO-SiO2-FeO-(MnO) multi-component phase. Figure 7(b) shows the mineral phase of 2# heat are 2CaO·SiO2 and 3CaO·P2O5, and the phosphorus content in this particle is rich, about 9.73 mass%. In addition, the calcium silicate is as 2CaO·SiO2-based phase. Sasaki et al. [22] found that a 2CaO SiO2 phase capable of fixing P existed in regions where dephosphorization efficiency was high. As shown in Figure 6, it can be seen that the slag is divided into two phase, the first type is calcium silicate, mainly composed of CaO and SiO2; and the other is calcium ferrite, which is composed of mainly silicate and phosphate. Phosphorus distributes nearly uniform in the two phases, indicating both phases have well ability of favorable dephosphorization.

Figure 5: SEM images and EDS analysis results of the first deslagging for 2# heat: (a) SEM image, (b) EDS spectra.
Figure 5:

SEM images and EDS analysis results of the first deslagging for 2# heat: (a) SEM image, (b) EDS spectra.

Figure 6: SEM-mapping photos result in the first deslagging of 2# heat: (a) SEM image, (b) to (g) element mappings.
Figure 6:

SEM-mapping photos result in the first deslagging of 2# heat: (a) SEM image, (b) to (g) element mappings.

Figure 7 shows the XRD analysis results of mineral phase of 1# heat and 2# heat at the first deslagging. Figure 7(a) shows that the mineral phase of 1# heat the first deslagging is 3CaO·SiO2. Figure 7(b) show the mineral phase of 2# heat are 2CaO·SiO2 and 3CaO·P2O5, which is favorable for dephosphorization. It can be concluded that the 2# heat slag could dephosphorization very well.

Figure 7: XRD analysis results of mineral phase of the 1# heat and 2# heat at the first deslagging.
Figure 7:

XRD analysis results of mineral phase of the 1# heat and 2# heat at the first deslagging.

Effect of slag composition on dephosphorization

Figure 8 shows the effects of the basicity of slag at the first deslagging on the dephosphorization rate. As shown in Figure 8, dephosphorization rate increase with the increase of slag basicity at the first deslagging, and then decreases when slag basicity is greater than 2. The dephosphorization rate increases with the increase of slag basicity at the initial stage of converter steelmaking process when the slag basicity is less than 2. Because the steelmaking temperature is relatively low at the initial stage of converter steelmaking process, the excessive addition of lime lead to the decrease of slag fluidity, resulting in the decrease of dephosphorization rate when the slag basicity is more than 2.

Figure 8: Effect of the slag basicity in slag on the dephosphorization rate at the first deslagging.
Figure 8:

Effect of the slag basicity in slag on the dephosphorization rate at the first deslagging.

Figure 9 presents the effects of the total iron content in slag at the first deslagging on dephosphorization rate. It can be seen from Figure 9 that dephosphorization rate increases with the increase of total iron content at the first deslagging when total iron content of slag dephosphorizationat the first deslagging is lower than 19.74 mass%. This is because the slag oxidation increases with the increases of FeO content, higher FeO content of slag favors the dissolution of lime. As dephosphorization product, 3FeO·P2O5 is less stable than calcium phosphate. A part of slag containing 3FeO·P2O5 which is not reduced as calcium phosphate can be removed at the first deslagging.

Figure 9: Effect of the total iron content in slag on dephosphorization rate at the first deslagging.
Figure 9:

Effect of the total iron content in slag on dephosphorization rate at the first deslagging.

As shown in Figure 10, with the MgO content at the first deslagging increase, the phosphorus content in liquid steel decreases at first. But the phosphorus content in liquid steel increases when the MgO content is more than 6 mass%. This is because when the MgO content is too high, iron spinel phase generates which not only consumes the FeO content that should be used for dephosphorization, but also worsen the dephosphorization kinetic conditions. Some works [23, 24] reported that MgO content increased within 6 mass%, the melting temperature of slag decrease, but melting temperature increased when it is higher than 6 mass%, thus it also confirmed the present viewpoint.

Figure 10: Effect of the MgO content in slag at the first deslagging on the phosphorus content in bulk metal.
Figure 10:

Effect of the MgO content in slag at the first deslagging on the phosphorus content in bulk metal.

The effect of MnO on dephosphorization rate at the first deslagging is shown in Figure 11. It can be seen that the dephosphorization rate decreases with increasing MnO content. The dephosphorization rate of slag is larger when the MnO content is smaller than 6 mass% under this condition, the dephosphorization rate at the first deslagging is larger than 68.99 mass%. This is because the increase of MnO content leads to the decrease of the relative contents of CaO and T.Fe, which is unfavorable for dephosphorization, resulting in the decrease of dephosphorization rate. Therefore, the MnO content should be smaller than 6 mass% to keep the dephosphorization rate at the first deslagging larger than 68.99 mass%.

Figure 11: Effect of the MnO content in slag at the first deslagging on the phosphorus content in bulk metal.
Figure 11:

Effect of the MnO content in slag at the first deslagging on the phosphorus content in bulk metal.

Conclusion

On the basis of industrial trials and theoretical analysis of dephosphorization by double slag method in BOF aiming to produce low phosphorus steel, the following conclusions are obtained.

  1. Transition oxidation temperature between dephosphorization and decarbonization Tf is not the favorable temperature for dephosphorization at the first deslagging. The optimum the first deslagging temperature is confirmed to be approximately 1,673 K, approximately 70 K higher than Tf.

  2. High melting temperatures phases (such as 3CaO·SiO2) are unfavorable for dephosphorization in the slag with high basicity and high MgO content.

  3. The optimum process condition for dephosphorization at first deslagging in a 120 ton top-bottom combined blown converter steelmaking process by double slag method is approximately 1,673 K in temperature, 2.0 in slag basicity, 6 and 17 mass% in MgO and T.Fe content, 6 mass% ≤ MnO content, respectively.

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Received: 2014-10-21
Accepted: 2015-4-9
Published Online: 2015-7-17
Published in Print: 2016-4-1

©2016 by De Gruyter

This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

Artikel in diesem Heft

  1. Frontmatter
  2. Research Articles
  3. Effects of Cations on Corrosion of Inconel 625 in Molten Chloride Salts
  4. Thermodynamic Analysis on the Minimum of Oxygen Content in the Deoxidation Equilibrium Curve in Liquid Iron
  5. Air Oxidation Behavior of Two Ti-Base Alloys Synthesized by HIP
  6. Generation of Constant Life Diagram under Elevated Temperature Ratcheting of 316LN Stainless Steel
  7. Effect of c-BN Size and Content on the Self-Propagating High-Temperature Synthesis of c-BN Composites Bonded with Ti-Al-C System Multiphase Products
  8. Effect of Welding Speeds on Mechanical Properties of Level Compensation Friction Stir Welded 6061-T6 Aluminum Alloy
  9. Simulation of Thermo-viscoplastic Behaviors for AISI 4140 Steel
  10. Transition Metal Nitrides: A First Principles Study
  11. The Constitutive Relationship and Processing Map of Hot Deformation in A100 steel
  12. Preparation of Granular Red Mud Adsorbent using Different Binders by Microwave Pore – Making and Activation Method
  13. On the Structure and Some Properties of LaCo Co-substituted NiZn Ferrites Prepared Using the Standard Ceramic Technique
  14. Effect of MgO and MnO on Phosphorus Utilization in P-Bearing Steelmaking Slag
  15. Dependence of Temperature and Slag Composition on Dephosphorization at the First Deslagging in BOF Steelmaking Process
https://doi.org/10.1515/htmp-2014-0187
Schlagwörter für diesen Artikel
dephosphorization; temperature of the first deslagging; thermodynamic analysis; slag composition
Creative Commons
BY-NC-ND 3.0

Artikel in diesem Heft

  1. Frontmatter
  2. Research Articles
  3. Effects of Cations on Corrosion of Inconel 625 in Molten Chloride Salts
  4. Thermodynamic Analysis on the Minimum of Oxygen Content in the Deoxidation Equilibrium Curve in Liquid Iron
  5. Air Oxidation Behavior of Two Ti-Base Alloys Synthesized by HIP
  6. Generation of Constant Life Diagram under Elevated Temperature Ratcheting of 316LN Stainless Steel
  7. Effect of c-BN Size and Content on the Self-Propagating High-Temperature Synthesis of c-BN Composites Bonded with Ti-Al-C System Multiphase Products
  8. Effect of Welding Speeds on Mechanical Properties of Level Compensation Friction Stir Welded 6061-T6 Aluminum Alloy
  9. Simulation of Thermo-viscoplastic Behaviors for AISI 4140 Steel
  10. Transition Metal Nitrides: A First Principles Study
  11. The Constitutive Relationship and Processing Map of Hot Deformation in A100 steel
  12. Preparation of Granular Red Mud Adsorbent using Different Binders by Microwave Pore – Making and Activation Method
  13. On the Structure and Some Properties of LaCo Co-substituted NiZn Ferrites Prepared Using the Standard Ceramic Technique
  14. Effect of MgO and MnO on Phosphorus Utilization in P-Bearing Steelmaking Slag
  15. Dependence of Temperature and Slag Composition on Dephosphorization at the First Deslagging in BOF Steelmaking Process
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