基于活性焦改性协同脱除二氧化硫和汞机理研究
摘要
在各种燃煤烟气污染物排放控制技术中,采用多种污染物综合控制技术实现二氧化硫和汞排放协同控制是当今污染物控制领域的重要发展方向。但由于目前还未有一种完善的控制体系能达到SO2与汞同时高效脱除,究其原因是缺乏对相关机理的深入了解。本文结合相关国家项目的支持,对协同脱除SO2与汞的反应特性及反应机理进行了深入系统的试验和机理研究。
本文从单种污染物脱除机理入手,以活性焦为研究对象,综合采用固定床活性焦S02与汞协同脱除机理试验台及热重分析对活性焦对SO2与汞协同吸附及再生过程进行了系统的实验研究。通过试验研究表明,活性焦脱硫脱汞主要是通过活性焦表面带有的含氧官能团作为氧化吸附汞和SO2的活化中心,烟气中的O吸附到活性焦表面形成化学吸附态O可以使Hg0氧化成HgO,SO2氧化成S03,在有水分的条件下形成硫酸而易被脱除。但SO2与汞会在活性焦表面产生竞争吸附,高浓度的SO2会导致脱汞效率的降低。
通过以上研究发现,O2是SO2与汞的吸附氧化过程中举足轻重的反应组分,当反应系统中氧气浓度较低时,SO2与汞吸附效率较低。因此,在实际工业应用中,SO2与汞的协同吸附效率受到烟气中氧含量的限制,而烟气中的氧含量较低,一般仅为4%-5%,因而十分有必要开发对O2依赖性较弱的新型吸附剂。同时,急需解决高浓度的SO2条件下低汞吸附性能问题。
采用浸渍法制备了改性活性焦吸附剂——Ce02/AC催化吸附剂,通过BET、XRD、SEM等吸附剂表征,发现制备的吸附剂具有较大的比表面积,其中负载5%Ce02的活性焦表面负载的Ce分散度较高,活性组分与载体之间相互作用较强。负载过程可以氧化AC表面,生成更多内酯和羰基官能团。改性后的活性焦即使在低浓度氧的情况下也能保有较高SO2和汞吸附效率,主要是因为Ce02有着很强的储存和释放O的能力。同时,在SO2存在的条件下,Ce02可以很大地增强活性焦的汞吸附效率,SO2浓度为500ppm时,Ce02/AC比新鲜活性焦的Hg0脱除效率提高了50%。这是因为SO2在Ce02的催化氧化下生成了适宜吸附零价汞的含硫官能团,可以与部分吸附态的Hg生成HgSO4,增强了Hg的氧化吸附。基于以上结论,进一步得出吸附剂表面发生的汞与SO2吸附氧化主要发生在吸附态的Hg0、吸附态的SO2和吸附态的O2之间。
基于试验研究结果,结合机理分析,针对固定床反应器,运用气固催化反应动力学方法进行分析研究,考虑多种污染物协同脱除的主要影响因素,根据吸附理论、扩散传质、质量平衡、吸附速率等方面的内容建立了固定床吸附剂协同脱除SO2和Hg反应器内浓度分布的数学模型。结果表明,SO2和Hg吸附过程既包括化学吸附,也包括物理吸附。SO2和Hg协同吸附的关键步骤是吸附剂对烟气中O的捕捉能力。SO2的反应速率常数要比Hg的反应速率常数大一个数量级,这也导致了SO2和汞在吸附剂表面形成竞争吸附,而SO2更易被吸附剂捕捉。为了获得较大的反应速率,高效的汞和SO2协同脱除吸附剂对反应组分应具有较强的吸附能力,以减少吸附剂的使用量。
以负载CeO2的活性焦为研究对象,采用热脱附为再生手段,通过热重分析,考察了热脱附再生对Ce02/AC性能的影响以及SO2和Hg的解吸附规律。结果表明：Ce02/AC再生后释放出的气体形态为SO2和Hg0,最佳联合再生温度应定在320℃以上。但再生温度越高,二次汞吸附效率就越低。根据Ce02/AC表面化学性质检测,其二次脱硫脱汞效率随再生次数以及再生温度的增加而降低的原因可以归为AC表面的碳在再生过程中受到烧蚀和氧化而,致使表面活性成分Ce02减少以及表面酸性官能团分解。
In different kinds of environmental pollution control technologies in coal-fired flue gas, the combined removal SO2/Hg technology in a complete single process is considered to be the potential developing direction. Howerver, it hasn't been well developed for the combined removal SO2/Hg technology with high efficiency. The reason is the lack of understanding of relevant mechanisms. In this paper, with the support of relevant national projects, the character and michanism of combine SO2/Hg control technology have been researched systematicly.
At the first, single plutant removal mechanism of activated coke (AC) was researched using SO2/Hg combine control fixed-bed system. And then the SO2/Hg regeneration mechanism of AC was researched using TG analysis. The results showed that the key step of Hg capture was the oxidation of Hg0. The O2containing functional group and chemi-adsorbed O2on the surface of AC was the activation center for Hg0oxidation, which can oxidize SO2and Hg0to SO3and HgO. There would be competitive adsorption between SO2and mercury on the surface of AC, high concentration of SO2could cause low Hg0removal efficiency.
From these results above, O2is considered to be the essencial reaction component during SO2and Hg0oxidation and adsorption. SO2and Hg0removal efficiency was low with the low concentration of O2, which means the SO2and Hg0removal efficiency is limited by the O2concentration in flue gas. The O2concentration in flue gas is4%～5%. It's necessary to develop the new sorbent for SO2and Hg0removal, which is efficient under low O2concentration. Moreover, the problem of low Hg0removal efficiency under the high concentration of SO2should be solved.
Cerium oxide supported on AC (CeO2/AC) were synthesized by an impregnation method for SO2and Hg0removal in simulated coal-fired flue gas. The sorbents were characterized by BET, XRD and SEM. The sorbents have large surface ares and the5%CeO2impregnated AC with highly dispersed cerium oxides can be obtained. The CeO2impregnation method could oxdize the AC surface and bring large amount of oxygen surface groups. CeO2/AC has the high SO2and Hg0removal efficiency even under low O2concentration due to its storing or releasing O2ability. Moreover, the results showed that SO2had great promotion on Hg0removal efficiency with the existence of CeO2. The Hg0capture capability of CeO2/AC was50%higher than that of AC when the SO2concentration was500ppm. In the case of CeO2/AC, the interaction between SO2and CeO2/AC is mainly chemisorption due to the catalysis of CeO2.The formed sulfur groups on the CeO2/AC surface favor the absorbtion of Hg0to form HgSO4, which inhance the oxidation of Hg0. Base on the conclusion above, the SO2and Hg0adsorption and oxidation on the surface of AC is among the adsorbed Hg0/adsorbed SO2and adsorbed O2.
Based on the experimental results, a model of SO2and Hg0adsorption process based on adsorption theory, diffusion mass transfer, mass balance, the adsorption rate over CeO2/AC was developed. The results implies that both chemisorption and physisorption played an important role in removing SO2and Hg0. The key step of simutanious SO2and Hg0adsorption is the ability to O2capture in flue gas. The reaction rate constant of SO2is one order bigger than that of Hg0, which lead to the competitive adsorption between SO2and Hg0on the surface of sorbent and SO2was easier to capture. Efficient adsorbent for SO2and Hg0removal should have a strong adsorption capacity for each component in order to get a larger reaction rate, which can reduce the use of adsorbent.
The characteristic of SO2and mercury desorption of CeO2/AC was investigated during heating regeneration process in N2atmosphere though TG analysis. The results showed the best regeneration temperature of SO2and Hg0should be set above320℃. The mercury removal efficiency decreased with increasing regeneration times and temperature due to CeO2loss during the carbon ablation and oxidation as well as desorption of surface acid functional group during the regeneration.
本文从单种污染物脱除机理入手,以活性焦为研究对象,综合采用固定床活性焦S02与汞协同脱除机理试验台及热重分析对活性焦对SO2与汞协同吸附及再生过程进行了系统的实验研究。通过试验研究表明,活性焦脱硫脱汞主要是通过活性焦表面带有的含氧官能团作为氧化吸附汞和SO2的活化中心,烟气中的O吸附到活性焦表面形成化学吸附态O可以使Hg0氧化成HgO,SO2氧化成S03,在有水分的条件下形成硫酸而易被脱除。但SO2与汞会在活性焦表面产生竞争吸附,高浓度的SO2会导致脱汞效率的降低。
通过以上研究发现,O2是SO2与汞的吸附氧化过程中举足轻重的反应组分,当反应系统中氧气浓度较低时,SO2与汞吸附效率较低。因此,在实际工业应用中,SO2与汞的协同吸附效率受到烟气中氧含量的限制,而烟气中的氧含量较低,一般仅为4%-5%,因而十分有必要开发对O2依赖性较弱的新型吸附剂。同时,急需解决高浓度的SO2条件下低汞吸附性能问题。
采用浸渍法制备了改性活性焦吸附剂——Ce02/AC催化吸附剂,通过BET、XRD、SEM等吸附剂表征,发现制备的吸附剂具有较大的比表面积,其中负载5%Ce02的活性焦表面负载的Ce分散度较高,活性组分与载体之间相互作用较强。负载过程可以氧化AC表面,生成更多内酯和羰基官能团。改性后的活性焦即使在低浓度氧的情况下也能保有较高SO2和汞吸附效率,主要是因为Ce02有着很强的储存和释放O的能力。同时,在SO2存在的条件下,Ce02可以很大地增强活性焦的汞吸附效率,SO2浓度为500ppm时,Ce02/AC比新鲜活性焦的Hg0脱除效率提高了50%。这是因为SO2在Ce02的催化氧化下生成了适宜吸附零价汞的含硫官能团,可以与部分吸附态的Hg生成HgSO4,增强了Hg的氧化吸附。基于以上结论,进一步得出吸附剂表面发生的汞与SO2吸附氧化主要发生在吸附态的Hg0、吸附态的SO2和吸附态的O2之间。
基于试验研究结果,结合机理分析,针对固定床反应器,运用气固催化反应动力学方法进行分析研究,考虑多种污染物协同脱除的主要影响因素,根据吸附理论、扩散传质、质量平衡、吸附速率等方面的内容建立了固定床吸附剂协同脱除SO2和Hg反应器内浓度分布的数学模型。结果表明,SO2和Hg吸附过程既包括化学吸附,也包括物理吸附。SO2和Hg协同吸附的关键步骤是吸附剂对烟气中O的捕捉能力。SO2的反应速率常数要比Hg的反应速率常数大一个数量级,这也导致了SO2和汞在吸附剂表面形成竞争吸附,而SO2更易被吸附剂捕捉。为了获得较大的反应速率,高效的汞和SO2协同脱除吸附剂对反应组分应具有较强的吸附能力,以减少吸附剂的使用量。
以负载CeO2的活性焦为研究对象,采用热脱附为再生手段,通过热重分析,考察了热脱附再生对Ce02/AC性能的影响以及SO2和Hg的解吸附规律。结果表明：Ce02/AC再生后释放出的气体形态为SO2和Hg0,最佳联合再生温度应定在320℃以上。但再生温度越高,二次汞吸附效率就越低。根据Ce02/AC表面化学性质检测,其二次脱硫脱汞效率随再生次数以及再生温度的增加而降低的原因可以归为AC表面的碳在再生过程中受到烧蚀和氧化而,致使表面活性成分Ce02减少以及表面酸性官能团分解。
In different kinds of environmental pollution control technologies in coal-fired flue gas, the combined removal SO2/Hg technology in a complete single process is considered to be the potential developing direction. Howerver, it hasn't been well developed for the combined removal SO2/Hg technology with high efficiency. The reason is the lack of understanding of relevant mechanisms. In this paper, with the support of relevant national projects, the character and michanism of combine SO2/Hg control technology have been researched systematicly.
At the first, single plutant removal mechanism of activated coke (AC) was researched using SO2/Hg combine control fixed-bed system. And then the SO2/Hg regeneration mechanism of AC was researched using TG analysis. The results showed that the key step of Hg capture was the oxidation of Hg0. The O2containing functional group and chemi-adsorbed O2on the surface of AC was the activation center for Hg0oxidation, which can oxidize SO2and Hg0to SO3and HgO. There would be competitive adsorption between SO2and mercury on the surface of AC, high concentration of SO2could cause low Hg0removal efficiency.
From these results above, O2is considered to be the essencial reaction component during SO2and Hg0oxidation and adsorption. SO2and Hg0removal efficiency was low with the low concentration of O2, which means the SO2and Hg0removal efficiency is limited by the O2concentration in flue gas. The O2concentration in flue gas is4%～5%. It's necessary to develop the new sorbent for SO2and Hg0removal, which is efficient under low O2concentration. Moreover, the problem of low Hg0removal efficiency under the high concentration of SO2should be solved.
Cerium oxide supported on AC (CeO2/AC) were synthesized by an impregnation method for SO2and Hg0removal in simulated coal-fired flue gas. The sorbents were characterized by BET, XRD and SEM. The sorbents have large surface ares and the5%CeO2impregnated AC with highly dispersed cerium oxides can be obtained. The CeO2impregnation method could oxdize the AC surface and bring large amount of oxygen surface groups. CeO2/AC has the high SO2and Hg0removal efficiency even under low O2concentration due to its storing or releasing O2ability. Moreover, the results showed that SO2had great promotion on Hg0removal efficiency with the existence of CeO2. The Hg0capture capability of CeO2/AC was50%higher than that of AC when the SO2concentration was500ppm. In the case of CeO2/AC, the interaction between SO2and CeO2/AC is mainly chemisorption due to the catalysis of CeO2.The formed sulfur groups on the CeO2/AC surface favor the absorbtion of Hg0to form HgSO4, which inhance the oxidation of Hg0. Base on the conclusion above, the SO2and Hg0adsorption and oxidation on the surface of AC is among the adsorbed Hg0/adsorbed SO2and adsorbed O2.
Based on the experimental results, a model of SO2and Hg0adsorption process based on adsorption theory, diffusion mass transfer, mass balance, the adsorption rate over CeO2/AC was developed. The results implies that both chemisorption and physisorption played an important role in removing SO2and Hg0. The key step of simutanious SO2and Hg0adsorption is the ability to O2capture in flue gas. The reaction rate constant of SO2is one order bigger than that of Hg0, which lead to the competitive adsorption between SO2and Hg0on the surface of sorbent and SO2was easier to capture. Efficient adsorbent for SO2and Hg0removal should have a strong adsorption capacity for each component in order to get a larger reaction rate, which can reduce the use of adsorbent.
The characteristic of SO2and mercury desorption of CeO2/AC was investigated during heating regeneration process in N2atmosphere though TG analysis. The results showed the best regeneration temperature of SO2and Hg0should be set above320℃. The mercury removal efficiency decreased with increasing regeneration times and temperature due to CeO2loss during the carbon ablation and oxidation as well as desorption of surface acid functional group during the regeneration.
引文
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