基于产物资源化的湿式镁法烟气脱硫技术研究
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摘要
湿式镁法烟气脱硫技术在国内经过十多年的研究和发展,其技术的可靠性、建造和运行的经济性以及脱硫副产物资源化的可行性已获得了广泛认同,有希望成为我国未来的主导脱硫技术之一。本文基于循环经济理念,着重探讨了湿式镁法烟气脱硫过程中亚硫酸镁的氧化和抑制氧化过程,并对不同反应器中的湿式镁法烟气脱硫过程进行了系统研究,根据实验结果探索了亚硫酸镁氧化和二氧化硫吸收过程的反应机理,为其工业化应用提供理论依据。主要内容如下：
通过间歇式密闭均相反应器,研究了亚硫酸钠在不同水质中的本征氧化动力学,并建立了相应动力学方程,证实亚硫酸钠的氧化过程对于水质变化十分敏感；通过曝气搅拌反应器,研究了亚硫酸镁的宏观氧化动力学,建立了相应的动力学方程,证实氧的扩散是亚硫酸镁氧化的速率控制步骤。通过间歇式密闭均相反应器,研究了不同抑制剂存在时亚硫酸钠的本征氧化动力学,建立了相应动力学方程；最终确定硫代硫酸钠作为脱硫产物的最佳抑制氧化剂；通过曝气搅拌反应器,研究了各参数对硫代硫酸钠抑制条件下亚硫酸镁氧化过程的影响,并建立了反应动力学方程；实验证明硫代硫酸钠对亚硫酸镁的氧化具有良好的抑制效果,在其浓度为6.67mmol/L时,抑制氧化效率高达92.8%。
通过鼓泡反应器,研究了不同参数条件对产物常规氧化的湿式镁法烟气脱硫过程的影响,结果表明鼓泡反应器能适应各参数变化对脱硫率的冲击；烟气量、烟气SO2浓度、烟气O2含量和MgSO4浓度都能影响MgSO3占产物比值；反应过程中浆液pH值的变化可分为稳定阶段、缓慢下降阶段和快速下降阶段三个部分,当pH值低于5.0左右后,脱硫率迅速下降。通过鼓泡反应器,研究了不同参数条件对产物抑制氧化的湿式镁法烟气脱硫过程的影响,结果表明鼓泡反应器能适应各参数变化对脱硫率的冲击；较小的烟气量、较低的烟气O2含量和较高的Na2S2O3浓度有助于提高MgSO3占产物比值,而烟气SO2浓度的变化对其影响不大；反应过程中浆液pH值的变化同样分为三个阶段,当pH值低于5.5左右后,脱硫率迅速下降。
通过喷淋塔反应器,研究了不同参数条件对产物常规氧化的湿式镁法烟气脱硫过程的影响,确定了最佳操作条件为：烟气量为20Nm3/h,烟气S02浓度为1000～2000mg/Nm3,液气比为8L/Nm3,以及使用较高位置的1“喷嘴；浆液提浓实验表明当MgSO4浓度接近饱和时浆液利用率和脱硫率最高,其最佳pH值操作范围为5.3-5.8。通过喷淋塔反应器,研究了不同参数条件对产物抑制氧化的湿式镁法烟气脱硫过程的影响,确定了最佳操作条件为：烟气量为20Nm3/h,烟气S02浓度为2000mg/Nm3,液气比为8L/Nm3,使用3#单层喷嘴,抑制剂浓度为20mmol/L,浆液pH值为6.5-7.0左右；为使MgSO3占产物比值高于90%,Na2S2O3与MgSO3的摩尔比应维持在1：4以上。基于SO2的气液平衡、气侧传质、液侧传质和SO2的外部传质四个部分建立了喷淋塔湿式镁法烟气脱硫传质模型,结果表明此模型能够较好的模拟正常操作条件下产物常规氧化和抑制氧化的湿式镁法烟气脱硫过程,同时证实了8O2的吸收过程受气膜扩散控制。
对不同浆液条件下的镁法脱硫产物进行了分析,结果表明产物组成与终止pH值有关,而与Mg(OH)2初始浓度无关；通过热重分析,获得了外部水和结构水去除、亚硫酸镁热解、亚硫酸氢镁热解和硫酸镁热解四个阶段的最大失重温度依次为100℃左右、540℃左右、640℃左右和990℃左右；通过抽滤与离心分离的比较,发现两者组分和浓度差异并不明显,说明固液分离方法对产物的影响不大。
After more than10years of research and development of the magnesium-based wet flue gas desulfurization technology in China, the reliability of the process, the economy of the construction and operation as well as the feasibility of desulfurization byproducts resources have been widely recognized, which is expected to become the dominant desulfurization technology in our country in the future. This paper is based on the concept of circular economy, focused on the oxidation and oxidation inhibition processes of magnesium sulfite in the magnesium-based wet flue gas desulfurization process, systematically studied the magnesium-based wet flue gas desulfurization process in different reactors, and explored the reaction mechanism of magnesium sulfite oxidation and sulfur dioxide absorption process based on the experimental results, which provided the theoretical basis for the industrial application of the magnesium-based wet flue gas desulfurization technology. The main contents are as follows:
Using the intermittent airtight homogeneous reactor, the intrinsic oxidation kinetics of sodium sulfite under different water quality has been studied and the corresponding kinetic equations have been established. The results confirmed that the sodium sulfite oxidation process is very sensitive to the water quality. Using the aeration stirred reactor, the macroscopical oxidation kinetics of magnesium sulfite has been studied and the corresponding kinetic equation has been established. The results confirmed that the oxygen diffusion is the controlling step of the magnesium sulfite oxidation. Using the intermittent airtight homogeneous reactor, the intrinsic oxidation kinetics of sodium sulfite under the presence of different inhibitors has been studied and the corresponding kinetic equations have been established. Sodium thiosulfate was determined as the optimal oxidation inhibitor for the desulfurization product. Using the aeration stirred reactor, the impact of various parameters on magnesium sulfite oxidation process under oxidation inhibition condition with sodium thiosulfate has been studied and the corresponding kinetic equation has been established. The results confirmed that sodium thiosulfate has a good inhibition effect on the magnesium sulfate oxidation and the oxidation inhibition efficiency could reach92.8%with a concentration of6.67mmol/L of sodium thiosulfate.
Using the bubbling reactor, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with conventional oxidation of the product has been studied. The results confirmed that the bubbling reactor could adapt to the impact of various parameters on the desulfurization efficiency and the flue gas flow rate, the flue gas SO2concentration, the flue gas O2content and the slurry MgSO4concentration could affect the MgSO3content in the product. The slurry pH value which changes during the reaction process can be divided into three parts, the stable stage, the slow decline stage and the rapid decline stage, respectively. The desulfurization efficiency began to fell rapidly when the pH value was less than5.0. Using the bubbling reactor, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with oxidation inhibition of the product has been studied. The results confirmed that the bubbling reactor could adapt to the impact of various parameters on the desulfurization efficiency and the lower flue gas flow rate, the lower flue gas O2content and the higher Na2S2O3concentration could improve the MgSO3content in the product while the flue gas SO2concentration has less impact on it. The slurry pH value changes during the reaction process can also be divided into three parts and the desulfurization efficiency began to fell rapidly when the pH value was less than5.5.
Using the spray scrubber, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with conventional oxidation of the product has been studied. The optimum operating conditions were determined as follows:flue gas flow rate as20Nm3/h, flue gas SO2concentration as1000-2000mg/Nm3, liquid-gas ratio as8L/Nm3, and using the1nozzle which located in the higher position. The slurry enrichment experiment indicated that the slurry utilization efficiency and the desulfurization efficiency could reach the highest level when MgSO4concentration was close to the saturation state and the optimal operation pH value range was5.3-5.8. Using the spray scrubber, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with oxidation inhibition of the product has been studied. The optimum operating conditions were determined as follows:flue gas flow rate as20Nm3/h, flue gas SO2concentration as2000mg/Nm3, liquid-gas ratio as8L/Nm3, using the3#nozzle, inhibitor concentration as20mmol/L, and pH value around6.5-7.0. The molar ratio of Na2S2O3to MgSO3should be maintained above1:4in order to maintain the MgSO3content in the product above90%. The magnesium-based wet flue gas desulfurization mass transfer model in spray scrubber has been established based on the four parts of gas-liquid equilibrium of SO2, gas side mass transfer, liquid side mass transfer and external mass transfer of SO2. The results confirmed that the model can be reasonable simulate the magnesium-based wet flue gas desulfurization process with conventional oxidation or oxidation inhibition of the product under normal operating conditions and the SO2absorption process was found to be controlled by gas-film diffusion.
The analysis results of the magnesium-based wet flue gas desulfurization products under different slurry conditions showed that the product composition was related to the terminate pH value and was independent to the initial Mg(OH)2concentration. Using the thermogravimetric analysis method, the maximum mass loss temperature of the removal of external water and structural water, the thermal decomposition of magnesium sulfite, the thermal decomposition of magnesium bisulfite, and the thermal decomposition of magnesium sulfate were obtained as100℃,540℃,640℃and990℃, respectively. The difference of the desulfurization products components from air pump filtration and centrifugal separation was not significant, which indicated that the solid-liquid separation method has less impact to the product.
通过间歇式密闭均相反应器,研究了亚硫酸钠在不同水质中的本征氧化动力学,并建立了相应动力学方程,证实亚硫酸钠的氧化过程对于水质变化十分敏感；通过曝气搅拌反应器,研究了亚硫酸镁的宏观氧化动力学,建立了相应的动力学方程,证实氧的扩散是亚硫酸镁氧化的速率控制步骤。通过间歇式密闭均相反应器,研究了不同抑制剂存在时亚硫酸钠的本征氧化动力学,建立了相应动力学方程；最终确定硫代硫酸钠作为脱硫产物的最佳抑制氧化剂；通过曝气搅拌反应器,研究了各参数对硫代硫酸钠抑制条件下亚硫酸镁氧化过程的影响,并建立了反应动力学方程；实验证明硫代硫酸钠对亚硫酸镁的氧化具有良好的抑制效果,在其浓度为6.67mmol/L时,抑制氧化效率高达92.8%。
通过鼓泡反应器,研究了不同参数条件对产物常规氧化的湿式镁法烟气脱硫过程的影响,结果表明鼓泡反应器能适应各参数变化对脱硫率的冲击；烟气量、烟气SO2浓度、烟气O2含量和MgSO4浓度都能影响MgSO3占产物比值；反应过程中浆液pH值的变化可分为稳定阶段、缓慢下降阶段和快速下降阶段三个部分,当pH值低于5.0左右后,脱硫率迅速下降。通过鼓泡反应器,研究了不同参数条件对产物抑制氧化的湿式镁法烟气脱硫过程的影响,结果表明鼓泡反应器能适应各参数变化对脱硫率的冲击；较小的烟气量、较低的烟气O2含量和较高的Na2S2O3浓度有助于提高MgSO3占产物比值,而烟气SO2浓度的变化对其影响不大；反应过程中浆液pH值的变化同样分为三个阶段,当pH值低于5.5左右后,脱硫率迅速下降。
通过喷淋塔反应器,研究了不同参数条件对产物常规氧化的湿式镁法烟气脱硫过程的影响,确定了最佳操作条件为：烟气量为20Nm3/h,烟气S02浓度为1000～2000mg/Nm3,液气比为8L/Nm3,以及使用较高位置的1“喷嘴；浆液提浓实验表明当MgSO4浓度接近饱和时浆液利用率和脱硫率最高,其最佳pH值操作范围为5.3-5.8。通过喷淋塔反应器,研究了不同参数条件对产物抑制氧化的湿式镁法烟气脱硫过程的影响,确定了最佳操作条件为：烟气量为20Nm3/h,烟气S02浓度为2000mg/Nm3,液气比为8L/Nm3,使用3#单层喷嘴,抑制剂浓度为20mmol/L,浆液pH值为6.5-7.0左右；为使MgSO3占产物比值高于90%,Na2S2O3与MgSO3的摩尔比应维持在1：4以上。基于SO2的气液平衡、气侧传质、液侧传质和SO2的外部传质四个部分建立了喷淋塔湿式镁法烟气脱硫传质模型,结果表明此模型能够较好的模拟正常操作条件下产物常规氧化和抑制氧化的湿式镁法烟气脱硫过程,同时证实了8O2的吸收过程受气膜扩散控制。
对不同浆液条件下的镁法脱硫产物进行了分析,结果表明产物组成与终止pH值有关,而与Mg(OH)2初始浓度无关；通过热重分析,获得了外部水和结构水去除、亚硫酸镁热解、亚硫酸氢镁热解和硫酸镁热解四个阶段的最大失重温度依次为100℃左右、540℃左右、640℃左右和990℃左右；通过抽滤与离心分离的比较,发现两者组分和浓度差异并不明显,说明固液分离方法对产物的影响不大。
After more than10years of research and development of the magnesium-based wet flue gas desulfurization technology in China, the reliability of the process, the economy of the construction and operation as well as the feasibility of desulfurization byproducts resources have been widely recognized, which is expected to become the dominant desulfurization technology in our country in the future. This paper is based on the concept of circular economy, focused on the oxidation and oxidation inhibition processes of magnesium sulfite in the magnesium-based wet flue gas desulfurization process, systematically studied the magnesium-based wet flue gas desulfurization process in different reactors, and explored the reaction mechanism of magnesium sulfite oxidation and sulfur dioxide absorption process based on the experimental results, which provided the theoretical basis for the industrial application of the magnesium-based wet flue gas desulfurization technology. The main contents are as follows:
Using the intermittent airtight homogeneous reactor, the intrinsic oxidation kinetics of sodium sulfite under different water quality has been studied and the corresponding kinetic equations have been established. The results confirmed that the sodium sulfite oxidation process is very sensitive to the water quality. Using the aeration stirred reactor, the macroscopical oxidation kinetics of magnesium sulfite has been studied and the corresponding kinetic equation has been established. The results confirmed that the oxygen diffusion is the controlling step of the magnesium sulfite oxidation. Using the intermittent airtight homogeneous reactor, the intrinsic oxidation kinetics of sodium sulfite under the presence of different inhibitors has been studied and the corresponding kinetic equations have been established. Sodium thiosulfate was determined as the optimal oxidation inhibitor for the desulfurization product. Using the aeration stirred reactor, the impact of various parameters on magnesium sulfite oxidation process under oxidation inhibition condition with sodium thiosulfate has been studied and the corresponding kinetic equation has been established. The results confirmed that sodium thiosulfate has a good inhibition effect on the magnesium sulfate oxidation and the oxidation inhibition efficiency could reach92.8%with a concentration of6.67mmol/L of sodium thiosulfate.
Using the bubbling reactor, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with conventional oxidation of the product has been studied. The results confirmed that the bubbling reactor could adapt to the impact of various parameters on the desulfurization efficiency and the flue gas flow rate, the flue gas SO2concentration, the flue gas O2content and the slurry MgSO4concentration could affect the MgSO3content in the product. The slurry pH value which changes during the reaction process can be divided into three parts, the stable stage, the slow decline stage and the rapid decline stage, respectively. The desulfurization efficiency began to fell rapidly when the pH value was less than5.0. Using the bubbling reactor, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with oxidation inhibition of the product has been studied. The results confirmed that the bubbling reactor could adapt to the impact of various parameters on the desulfurization efficiency and the lower flue gas flow rate, the lower flue gas O2content and the higher Na2S2O3concentration could improve the MgSO3content in the product while the flue gas SO2concentration has less impact on it. The slurry pH value changes during the reaction process can also be divided into three parts and the desulfurization efficiency began to fell rapidly when the pH value was less than5.5.
Using the spray scrubber, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with conventional oxidation of the product has been studied. The optimum operating conditions were determined as follows:flue gas flow rate as20Nm3/h, flue gas SO2concentration as1000-2000mg/Nm3, liquid-gas ratio as8L/Nm3, and using the1nozzle which located in the higher position. The slurry enrichment experiment indicated that the slurry utilization efficiency and the desulfurization efficiency could reach the highest level when MgSO4concentration was close to the saturation state and the optimal operation pH value range was5.3-5.8. Using the spray scrubber, the impact of various parameters on the magnesium-based wet flue gas desulfurization process with oxidation inhibition of the product has been studied. The optimum operating conditions were determined as follows:flue gas flow rate as20Nm3/h, flue gas SO2concentration as2000mg/Nm3, liquid-gas ratio as8L/Nm3, using the3#nozzle, inhibitor concentration as20mmol/L, and pH value around6.5-7.0. The molar ratio of Na2S2O3to MgSO3should be maintained above1:4in order to maintain the MgSO3content in the product above90%. The magnesium-based wet flue gas desulfurization mass transfer model in spray scrubber has been established based on the four parts of gas-liquid equilibrium of SO2, gas side mass transfer, liquid side mass transfer and external mass transfer of SO2. The results confirmed that the model can be reasonable simulate the magnesium-based wet flue gas desulfurization process with conventional oxidation or oxidation inhibition of the product under normal operating conditions and the SO2absorption process was found to be controlled by gas-film diffusion.
The analysis results of the magnesium-based wet flue gas desulfurization products under different slurry conditions showed that the product composition was related to the terminate pH value and was independent to the initial Mg(OH)2concentration. Using the thermogravimetric analysis method, the maximum mass loss temperature of the removal of external water and structural water, the thermal decomposition of magnesium sulfite, the thermal decomposition of magnesium bisulfite, and the thermal decomposition of magnesium sulfate were obtained as100℃,540℃,640℃and990℃, respectively. The difference of the desulfurization products components from air pump filtration and centrifugal separation was not significant, which indicated that the solid-liquid separation method has less impact to the product.
引文
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