抗结皮复合镁铝尖晶石浇注料的研究
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摘要
水泥工业是国民经济的支柱产业，同时也是典型的高能耗行业。通过科技的发展和技术的进步，预分解窑逐渐取代了立窑等落后技术，不仅使水泥产质量显著提高，而且取得了巨大的节能减排效果。然而，预分解窑中仍存在传热分解效率较低的堆积态传热，增大了生产能耗。短流程预烧成技术通过提高入窑物料温度，强化悬浮态下的传热过程，提高换热效率，大幅度降低能耗，是水泥窑炉技术的一大进步。但是，短流程预烧成窑的入窑物料温度由900℃提高至1200℃，并且能够造成窑中碱氯硫环境的改变，更易造成结皮堵塞等问题，因此，对短流程预烧成窑用耐火材料的抗结皮性、抗热震性、耐高温性等提出了更高的要求。
本课题是基于国家“973”计划项目《水泥低能耗制备与高效应用的基础研究》的第二课题《熟料分段烧成动力学及过程控制》的重要研究内容之一，目的是针对短流程预烧成窑工况条件和使用要求，开发新型的抗结皮耐火浇注料，并获得最优配方，为工业生产奠定基础，主要研究内容包括以下几个方面：
（1）设计了新型抗结皮耐火浇注料的矿物组成。针对短流程预烧成窑工况条件及其对浇注料抗结皮性、抗热震性、抗硫碱侵蚀性和耐高温性等使用性能的要求，通过材料性能对比和分析，选择具有优异抗硫碱侵蚀性和抗结皮性的镁铝尖晶石相作为主晶相，选择具有优异抗热震性能的堇青石相作为次晶相，以MgO-Al_2O_3-SiO_2-H_2O作为结合相，并根据MgO-Al_2O_3-SiO_2三元相图，确定结合相的平衡组成位于镁铝尖晶石（MA）和堇青石（M_2A_2S_5）的连线附近。
（2）建立了新的耐火材料抗结皮性能测试方法。针对现行的抗结皮性能试验标准《抗结皮耐火浇注料抗结皮性试验方法》的不足，即只能定性分析浇注料是否有抗结皮性，无法定量分析和比较各材料之间的抗结皮性能优劣，参考《普通混凝土力学性能试验方法》，设计了劈裂抗拉强度试验方法，实现了浇注料抗结皮性能的定量分析；利用该法测试了4种“三明治试样”的抗结皮性能，得到其抗结皮性的优劣顺序，即MA_2> MA_1>50S≈13NL；并通过单因素方差分析，对4种试样的劈裂抗拉强度试验结果进行组内和组间对比，证明了试样劈裂抗拉强度存在的显著性差异是由浇注料的种类不同引起的，验证了劈裂抗拉试验的合理性。
（3）优化了新型抗结皮耐火浇注料的配方。在前期研究基础上，通过黑箱原理、四次性能优化试验，对抗结皮复合镁铝尖晶石浇注料进行了配方优化设计，研究各种配料掺量等条件对浇注料各项性能的影响，并最终获得了抗结皮复合镁铝尖晶石浇注料的最优配方。
（4）系统测试了抗结皮复合镁铝尖晶石浇注料最优配方的抗结皮性、抗热震性、抗侵蚀性等性能，结果表明该浇注料的各项性能明显优于13NL、50S等浇注料。通过TG/DTA、XRD、SEM等测试手段对结合相的热稳定性、矿相组成、微观形貌等进行表征，初步分析了最优配方性能提高的原因。
Cement manufactory is the pillar industry of domestic economy and a typicalhigh energy consumption industry. The ultilization of precalciner, which replaced thebackwardness technologies, not only improved the qulity and quantity of cement, butalso reduced the energy consumption and pollutant emission. However, the heattransfer of accumulation in the precalciner brought about higher practical energyconsumption. Short process precementation technology can obviously enhance theheat transfer process and efficiency and reduce energy consumption by increase thetemperature of raw meal. The temperature of raw meal in short processprecementation kiln was increased from900℃to1200℃, which would cause thevariation of alkali-chlorine-sulfur environment, leading to such problems as crust andblock. Therefore, the refractories used in short process precementation kiln shouldhave excellent crust-resistance, thermal shock-resistance, and hightemperature-resistance.
This dissertation is one important research of "kinetics study and process controlof clinker sectional burning", based on the "973" national projects “fundamentalresearch on cement production with low energy consumption and high efficientapplication”, aimed to develop anti-crust refractory castable and its optimal formula,which suit to the condition and requirement of the short process precementation kiln.The main contents include the following aspects:
(1) According to the requirement of short process precementation kiln, theMagnesia-Alumina Spinel with excellent sulfur alkali corrosion-resistance andtemperature-resistance property was used as main crystal. The cordierite with highthermal shock-resistance was chosen as the secondary crystalline phase and theMgO-Al_2O_3-SiO_2-H_2O was selected as the combined phase. Based on theMgO-Al_2O_3-SiO_2three ternary phase diagram, the equilibrium composition can belocated at the connected line of the spinel (MA) and cordierite (M_2A_2S_5).
(2) In view of disadvantagement of the current anti-crust performance test standard,the split tensile strength method was designed for quantitative analysis ofcrust-resistance. Four Sandwich specimens was tested by this method. The resultsshowed the order of their crust-resistance performance, i.e. MA_2> MA_1>50S=13NL.Meanwhile, the single factor analysis of variance was carried out to compare the test results within groups and between groups. The results proved that the significantdifferences between the split tensile strength were caused by different species, andalso verified the rationality and accuracy verification of the method.
(3) The optimum formula of the composite Magnesia-Alumina Spinel castable wasobtained through the black-box principle and four orthogonal experiments. The effectof the ingredient content on the performance of castable was also obtained.
(4) The crust-resistance, thermal shock-resistance, and corrsion-resistanceperformance of optimum formula of the composite Magnesia-Alumina Spinel castablewere systemically studied, which was much higher than13NL and50S. The thermalstability, mineral composition, morphorgy, et. al of the combined phase werecharacterized by methods like TG/DTA, XRD, SEM. Moreover, the reasons for theimproved performance of optimal formula were also anylized.
本课题是基于国家“973”计划项目《水泥低能耗制备与高效应用的基础研究》的第二课题《熟料分段烧成动力学及过程控制》的重要研究内容之一，目的是针对短流程预烧成窑工况条件和使用要求，开发新型的抗结皮耐火浇注料，并获得最优配方，为工业生产奠定基础，主要研究内容包括以下几个方面：
（1）设计了新型抗结皮耐火浇注料的矿物组成。针对短流程预烧成窑工况条件及其对浇注料抗结皮性、抗热震性、抗硫碱侵蚀性和耐高温性等使用性能的要求，通过材料性能对比和分析，选择具有优异抗硫碱侵蚀性和抗结皮性的镁铝尖晶石相作为主晶相，选择具有优异抗热震性能的堇青石相作为次晶相，以MgO-Al_2O_3-SiO_2-H_2O作为结合相，并根据MgO-Al_2O_3-SiO_2三元相图，确定结合相的平衡组成位于镁铝尖晶石（MA）和堇青石（M_2A_2S_5）的连线附近。
（2）建立了新的耐火材料抗结皮性能测试方法。针对现行的抗结皮性能试验标准《抗结皮耐火浇注料抗结皮性试验方法》的不足，即只能定性分析浇注料是否有抗结皮性，无法定量分析和比较各材料之间的抗结皮性能优劣，参考《普通混凝土力学性能试验方法》，设计了劈裂抗拉强度试验方法，实现了浇注料抗结皮性能的定量分析；利用该法测试了4种“三明治试样”的抗结皮性能，得到其抗结皮性的优劣顺序，即MA_2> MA_1>50S≈13NL；并通过单因素方差分析，对4种试样的劈裂抗拉强度试验结果进行组内和组间对比，证明了试样劈裂抗拉强度存在的显著性差异是由浇注料的种类不同引起的，验证了劈裂抗拉试验的合理性。
（3）优化了新型抗结皮耐火浇注料的配方。在前期研究基础上，通过黑箱原理、四次性能优化试验，对抗结皮复合镁铝尖晶石浇注料进行了配方优化设计，研究各种配料掺量等条件对浇注料各项性能的影响，并最终获得了抗结皮复合镁铝尖晶石浇注料的最优配方。
（4）系统测试了抗结皮复合镁铝尖晶石浇注料最优配方的抗结皮性、抗热震性、抗侵蚀性等性能，结果表明该浇注料的各项性能明显优于13NL、50S等浇注料。通过TG/DTA、XRD、SEM等测试手段对结合相的热稳定性、矿相组成、微观形貌等进行表征，初步分析了最优配方性能提高的原因。
Cement manufactory is the pillar industry of domestic economy and a typicalhigh energy consumption industry. The ultilization of precalciner, which replaced thebackwardness technologies, not only improved the qulity and quantity of cement, butalso reduced the energy consumption and pollutant emission. However, the heattransfer of accumulation in the precalciner brought about higher practical energyconsumption. Short process precementation technology can obviously enhance theheat transfer process and efficiency and reduce energy consumption by increase thetemperature of raw meal. The temperature of raw meal in short processprecementation kiln was increased from900℃to1200℃, which would cause thevariation of alkali-chlorine-sulfur environment, leading to such problems as crust andblock. Therefore, the refractories used in short process precementation kiln shouldhave excellent crust-resistance, thermal shock-resistance, and hightemperature-resistance.
This dissertation is one important research of "kinetics study and process controlof clinker sectional burning", based on the "973" national projects “fundamentalresearch on cement production with low energy consumption and high efficientapplication”, aimed to develop anti-crust refractory castable and its optimal formula,which suit to the condition and requirement of the short process precementation kiln.The main contents include the following aspects:
(1) According to the requirement of short process precementation kiln, theMagnesia-Alumina Spinel with excellent sulfur alkali corrosion-resistance andtemperature-resistance property was used as main crystal. The cordierite with highthermal shock-resistance was chosen as the secondary crystalline phase and theMgO-Al_2O_3-SiO_2-H_2O was selected as the combined phase. Based on theMgO-Al_2O_3-SiO_2three ternary phase diagram, the equilibrium composition can belocated at the connected line of the spinel (MA) and cordierite (M_2A_2S_5).
(2) In view of disadvantagement of the current anti-crust performance test standard,the split tensile strength method was designed for quantitative analysis ofcrust-resistance. Four Sandwich specimens was tested by this method. The resultsshowed the order of their crust-resistance performance, i.e. MA_2> MA_1>50S=13NL.Meanwhile, the single factor analysis of variance was carried out to compare the test results within groups and between groups. The results proved that the significantdifferences between the split tensile strength were caused by different species, andalso verified the rationality and accuracy verification of the method.
(3) The optimum formula of the composite Magnesia-Alumina Spinel castable wasobtained through the black-box principle and four orthogonal experiments. The effectof the ingredient content on the performance of castable was also obtained.
(4) The crust-resistance, thermal shock-resistance, and corrsion-resistanceperformance of optimum formula of the composite Magnesia-Alumina Spinel castablewere systemically studied, which was much higher than13NL and50S. The thermalstability, mineral composition, morphorgy, et. al of the combined phase werecharacterized by methods like TG/DTA, XRD, SEM. Moreover, the reasons for theimproved performance of optimal formula were also anylized.
引文
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