活性焦的制备及其烟气脱硫的实验研究
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摘要
活性焦(AC)烟气脱硫是一种可资源化烟气脱硫工艺,该工艺不但可以脱除烟气中的S02,还可实现硫资源回收,是当前研究的重要脱硫方法。本文以粘结性煤为原料,通过简化生产工艺(原煤破碎、预氧化、炭化和活化)制备活性焦,将此活性焦分别作为吸附剂和催化剂载体用于烟气脱硫和再生实验并进行了相关研究,最后进行了活性焦烟气脱硫中试研究。
将粘结性煤破碎后在空气中氧化,通过炭化、活化制备活性焦。结果表明,粘结性煤经过氧化后,可降低煤的粘结性,增加煤的孔隙率；氧化温度越高、氧化时间越长,煤的粘结性越低,孔隙率越高。与煤未氧化得到的炭化料和活性焦相比,煤氧化后得到的炭化料和活性焦的比表面积、微孔容积和总孔容积有明显的提高。煤在270℃氧化1h后制备活性焦的最佳工艺条件为：炭化温度600℃、炭化时间1h、活化温度900℃、活化时间1.5h、水蒸气流量406mL·min-1。在此条件下制得的活性焦的机械强度为95.2%,硫容为65.8mg·g-1。
利用固定床反应器,将活性焦作为吸附剂进行烟气脱硫实验,考察空速、床层温度、SO2浓度、O2浓度、水蒸气浓度和活性焦的表面性质对活性焦脱硫性能的影响。结果表明,空速越小、SO2浓度越低、O2浓度和水蒸气浓度越高,活性焦的脱硫效率越高,烟气脱硫床层温度80℃～100℃较适宜。活性焦的比表面积、微孔容积和总孔容积越大,活性焦的硫容越大,活性焦表面碱性基团浓度越高,活性焦的硫容越大。在实验数据基础上,建立了烟气脱硫动力学方程和数学模型,用其参数设计并建立了烟气量为1000Nm3·h-1的移动床活性焦脱硫中试装置,设计值与实验结果基本吻合。
将活性焦作为催化剂载体制备CuO/AC,在工业锅炉排烟温度下直接脱硫,考察空速、床层温度、S02浓度、02浓度、水蒸气浓度和载铜量对CuO/AC脱硫性能的影响。结果表明,空速越小、床层温度越高、SO2浓度越低,CuO/AC的脱硫效率的越高,O2浓度对CuO/AC脱硫性能无影响,而水蒸气不参与脱硫反应。CuO/AC的硫容随载铜量的增加先增加后减小,综合考虑CuO/AC的硫容和活性组分CuO的利用率,负载5%-10%的铜较适宜。硝酸处理活性焦载体后制得的CuO/AC,其硫容明显提高。在实验数据基础上,建立CuO/AC烟气脱硫动力学模型方程,利用模型方程模拟Cu/S摩尔比随时间变化,模拟结果与实验测定基本一致。
分别将饱和的活性焦和失活的CuO/AC在惰性气氛下加热再生,在400℃下,SO2再生较完全,再生后的活性焦和CuO/AC用于烟气脱硫,其脱硫性能几乎没有变化。升高再生温度、降低载气流量可提高再生气中SO2的浓度。
Flue gas desulfurization by activated coke is a resourceable technology that can not only remove SO2, but also recover sulfur element. Therefore, many researches have been done about flue gas desulfurization by activated coke. The key factors for applicating this technology are desulfurization and regeneration of activated coke. Broken activated coke was prepared with caking coal by simplifying the production process, which including coal crushing, preoxidation, carbonization and activation. The production process of preparing the broken activated coke overcame the complex production process of traditional activated coke. Experiments of flue gas desulfurization were conducted with broken activated coke as adsorbent and catalyst carrier respectively on a fixed-bed reactor. The effect of surface properties of activated coke and process conditions on desulfurization efficiency and sulfur capacity research was studied. And the regeneration characteristics of adsorbent and catalyst of activated coke after desulfurizaion was also studied. Finally pilot study was conducted.
The effect of preoxidation of caking coal on the property of coal, char and activated coke was studied. The caking index of coal decreased and the porosity of coal increased after preoxidation of coal. Specific surface area, micropore volume and total pore volume of char increased with preoxidation of coal, compared to the char carbonizated without preoxidation of coal. With increasing preoxidation time, specific surface area, micropore volume and total pore volume of activated coke enhanced significantly, but mechanical intensity of activated coke decreased. After preoxidation of coal at 270℃for 1h, the best conditions for preparing activated coke was as follows:carbonization temperature is 600℃, carbonization time is 1h, activation temperature is 900℃, the activation time is 1.5h and the flow of steam is 406 mL·min-1. On these conditions, specific surface area, micropore pore volume, total pore volume mechanical strength and sulfur capacity of is 245.20m2·g-1,0.0968m3·g-1,0.1183m3·g-1, and 95.2% respectively. The sulfur capacity of activated carbon is 65.8mg·g-1.
Experiments of desulfurization were conducted with activated coke as adsorben. The results show that activated coke has higher sulfur capacity and longer breakthrough time under lower inlet concentration of SO2, higher concentration of O2 and steam. Reducing the flow also can increase breakthrough time of activated coke. Reaction temperature of 80℃～100℃is suitable. Specific surface area, micropore volume and total pore volume of activated coke were greater, sulfur capacity is bigger. Surface basictiy concentration of activated coke was higher, sulfur capacity is bigger. Based on experimental data, dynamics equation and mathematical model of flue gas desulfurization by activated coke were established. Mobile bed desulfurization tower of dealing with the flow of 1000Nm3·h-1 was designed and established according to the parameter, the experimental results agreed well with the designed results.
CuO/AC catalyst was prepared with activated coke, Experiments of desulfurization were conducted with CuO/AC. The results show that activated coke has higher sulfur capacity and longer breakthrough time under lower inlet concentration of SO2 and lower flow velocity in oxygen gas environment. Steam didn't participate in the reaction of flue gas desulfurization. Reaction temperature of 200℃-240℃is suitable. The sulfur capacity of CuO/AC first increases then decreases with increasing copper loading on activated carbon. Considering the sulfur capacity of CuO/AC and the utilization of copper, copper content of 5%～10% is prefer. CuO/AC was prepared by activated coke treated by nitric acid, the sulfur capacity of CuO/AC is improved obviously. Based on the experiment data, dynamics model of flue gas desulfurization by CuO/AC was established, Cu/S mole ratio of the simulation results and experimental results are almost the same using this model.
Saturated activated coke and deactivated CuO/AC were regenerated at 400℃under inert atmosphere, the regeneration efficiency is close to 100%. The sulfur capacity of activated coke and CuO/AC has no change almost after several desulfurization-regeneration cycles. SO2 concentration of regeneration gas are higher at higher temperature or under smaller flow of carrier gas.
将粘结性煤破碎后在空气中氧化,通过炭化、活化制备活性焦。结果表明,粘结性煤经过氧化后,可降低煤的粘结性,增加煤的孔隙率；氧化温度越高、氧化时间越长,煤的粘结性越低,孔隙率越高。与煤未氧化得到的炭化料和活性焦相比,煤氧化后得到的炭化料和活性焦的比表面积、微孔容积和总孔容积有明显的提高。煤在270℃氧化1h后制备活性焦的最佳工艺条件为：炭化温度600℃、炭化时间1h、活化温度900℃、活化时间1.5h、水蒸气流量406mL·min-1。在此条件下制得的活性焦的机械强度为95.2%,硫容为65.8mg·g-1。
利用固定床反应器,将活性焦作为吸附剂进行烟气脱硫实验,考察空速、床层温度、SO2浓度、O2浓度、水蒸气浓度和活性焦的表面性质对活性焦脱硫性能的影响。结果表明,空速越小、SO2浓度越低、O2浓度和水蒸气浓度越高,活性焦的脱硫效率越高,烟气脱硫床层温度80℃～100℃较适宜。活性焦的比表面积、微孔容积和总孔容积越大,活性焦的硫容越大,活性焦表面碱性基团浓度越高,活性焦的硫容越大。在实验数据基础上,建立了烟气脱硫动力学方程和数学模型,用其参数设计并建立了烟气量为1000Nm3·h-1的移动床活性焦脱硫中试装置,设计值与实验结果基本吻合。
将活性焦作为催化剂载体制备CuO/AC,在工业锅炉排烟温度下直接脱硫,考察空速、床层温度、S02浓度、02浓度、水蒸气浓度和载铜量对CuO/AC脱硫性能的影响。结果表明,空速越小、床层温度越高、SO2浓度越低,CuO/AC的脱硫效率的越高,O2浓度对CuO/AC脱硫性能无影响,而水蒸气不参与脱硫反应。CuO/AC的硫容随载铜量的增加先增加后减小,综合考虑CuO/AC的硫容和活性组分CuO的利用率,负载5%-10%的铜较适宜。硝酸处理活性焦载体后制得的CuO/AC,其硫容明显提高。在实验数据基础上,建立CuO/AC烟气脱硫动力学模型方程,利用模型方程模拟Cu/S摩尔比随时间变化,模拟结果与实验测定基本一致。
分别将饱和的活性焦和失活的CuO/AC在惰性气氛下加热再生,在400℃下,SO2再生较完全,再生后的活性焦和CuO/AC用于烟气脱硫,其脱硫性能几乎没有变化。升高再生温度、降低载气流量可提高再生气中SO2的浓度。
Flue gas desulfurization by activated coke is a resourceable technology that can not only remove SO2, but also recover sulfur element. Therefore, many researches have been done about flue gas desulfurization by activated coke. The key factors for applicating this technology are desulfurization and regeneration of activated coke. Broken activated coke was prepared with caking coal by simplifying the production process, which including coal crushing, preoxidation, carbonization and activation. The production process of preparing the broken activated coke overcame the complex production process of traditional activated coke. Experiments of flue gas desulfurization were conducted with broken activated coke as adsorbent and catalyst carrier respectively on a fixed-bed reactor. The effect of surface properties of activated coke and process conditions on desulfurization efficiency and sulfur capacity research was studied. And the regeneration characteristics of adsorbent and catalyst of activated coke after desulfurizaion was also studied. Finally pilot study was conducted.
The effect of preoxidation of caking coal on the property of coal, char and activated coke was studied. The caking index of coal decreased and the porosity of coal increased after preoxidation of coal. Specific surface area, micropore volume and total pore volume of char increased with preoxidation of coal, compared to the char carbonizated without preoxidation of coal. With increasing preoxidation time, specific surface area, micropore volume and total pore volume of activated coke enhanced significantly, but mechanical intensity of activated coke decreased. After preoxidation of coal at 270℃for 1h, the best conditions for preparing activated coke was as follows:carbonization temperature is 600℃, carbonization time is 1h, activation temperature is 900℃, the activation time is 1.5h and the flow of steam is 406 mL·min-1. On these conditions, specific surface area, micropore pore volume, total pore volume mechanical strength and sulfur capacity of is 245.20m2·g-1,0.0968m3·g-1,0.1183m3·g-1, and 95.2% respectively. The sulfur capacity of activated carbon is 65.8mg·g-1.
Experiments of desulfurization were conducted with activated coke as adsorben. The results show that activated coke has higher sulfur capacity and longer breakthrough time under lower inlet concentration of SO2, higher concentration of O2 and steam. Reducing the flow also can increase breakthrough time of activated coke. Reaction temperature of 80℃～100℃is suitable. Specific surface area, micropore volume and total pore volume of activated coke were greater, sulfur capacity is bigger. Surface basictiy concentration of activated coke was higher, sulfur capacity is bigger. Based on experimental data, dynamics equation and mathematical model of flue gas desulfurization by activated coke were established. Mobile bed desulfurization tower of dealing with the flow of 1000Nm3·h-1 was designed and established according to the parameter, the experimental results agreed well with the designed results.
CuO/AC catalyst was prepared with activated coke, Experiments of desulfurization were conducted with CuO/AC. The results show that activated coke has higher sulfur capacity and longer breakthrough time under lower inlet concentration of SO2 and lower flow velocity in oxygen gas environment. Steam didn't participate in the reaction of flue gas desulfurization. Reaction temperature of 200℃-240℃is suitable. The sulfur capacity of CuO/AC first increases then decreases with increasing copper loading on activated carbon. Considering the sulfur capacity of CuO/AC and the utilization of copper, copper content of 5%～10% is prefer. CuO/AC was prepared by activated coke treated by nitric acid, the sulfur capacity of CuO/AC is improved obviously. Based on the experiment data, dynamics model of flue gas desulfurization by CuO/AC was established, Cu/S mole ratio of the simulation results and experimental results are almost the same using this model.
Saturated activated coke and deactivated CuO/AC were regenerated at 400℃under inert atmosphere, the regeneration efficiency is close to 100%. The sulfur capacity of activated coke and CuO/AC has no change almost after several desulfurization-regeneration cycles. SO2 concentration of regeneration gas are higher at higher temperature or under smaller flow of carrier gas.
引文
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