改性多孔材料常温下吸附分离密闭空间二氧化碳
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摘要
在密闭空间中,如载人航天飞行器、空间站和潜艇等,CO2去除是环境控制与生命保障系统的重要任务之一,其浓度过高将直接危害人体健康。密闭空间中CO2去除技术首先要求高效、稳定和安全,其次是装置体积小、重量轻、能耗低、寿命长,以及操作和维护简便。本论文围绕上述目标,基于吸附法效率高、可再生、低能耗和工艺相对简单等优势,选用新型多孔材料SBA-16和碳纳米管(CNTs)为载体、富氨基材料为改性剂开发制备新型CO2吸附剂。通过表面分析和性能测试对所合成吸附剂进行优选,并在模拟密闭空间条件下对优选出的固体胺吸附剂进行性能研究,并设计比较最佳脱附工艺,为实际应用奠定理论研究基础。得到以下一些结论：
以多孔材料SBA-16、NTs为载体,四乙烯五胺(TEPA)、三乙烯四胺(TETA)为氨基改性剂,采用浸渍法合成新型CO2吸附剂。研究结果表明,吸附剂通过浸渍改性后均保持了原有主孔道结构。吸附剂的比表面积、孔容以及孔径随着TETA或TEPA浸渍量的增加而减小。改性后SBA-16和CNTs吸附剂的CO2吸附量随着TETA或TEPA浸渍量的升高而增加,并存在最佳浸渍量,均为30wt%左右。改性后SBA-16和CNTs吸附剂的C02吸附量随着吸附温度(288-308K)的升高而增大,在308K时,样品CTP-30和CTT-30表现出较高的吸附容量,分别为3.37mmol·g-1和2.65mmol·g-1。经过5次的吸附脱附循环再生,改性后SBA-16和CNTs吸附剂均表现出较为稳定的吸附性能。
固定床动态吸附实验表明,在实际密闭空间温度范围内(283-313K),随着温度的升高,样品CTP-30的CO2动态吸附量从2.52mmol·g-1升至3.56mmol·g-1,其吸附C02过程以化学吸附为主,在283～313K之间,CTP-30的化学吸附量qec占吸附量q的比例达到74%以上。CTP-30对CO2的吸附等温线(283～313K)属于Ⅰ型吸附等温线。利用Langmuir方程模拟实验所得结果,相关系数均大于0.99,其平均等量吸附热为32.68kJ·mol-1
气体中一定量水分的存在能提高CTP-30的CO2吸附量。在298K时,随着混合气体中水汽含量由0%升至2%,吸附量由2.97mmol·g-1增加到3.87mmol·g-1。但随着水汽含量继续增加到7%,吸附量逐渐下降,基本保持在2.67mmol·g-1。采用半吸附时间作为衡量手段,考察改性CNTs在密闭空间环境下对低浓度CO2的吸附动力学。在模拟密闭空间环境空气条件下,CTP-30吸附剂具有良好的吸附再生稳定性。经过20次的循环吸附脱附实验后,CO2的吸附容量有所下降,但吸附容量仍维持在3.68mmol·g-1以上。利用失活动力学模型对CTP-30在不同反应条件下的CO2吸附穿透曲线进行模拟分析。结果证明,模拟曲线与实验结果的相关系数R2均大于0.99。
CTP-30吸附剂具有良好的脱附再生性能。TPD实验结果发现CTP-30存在两个明显的强弱脱附峰,其脱附温度分别为313K和358K。采用真空加热耦合脱附技术后,CTP-30可以在较低温度下(353K)实现脱附,脱附效率达到95%以上。而在5kPa压力,373K温度的脱附条件下实验所得初始最高脱附速率明显高于其它条件下的脱附速率,达到了0.7mmol·min-1,且在15min内达到基本完全脱附。根据实验结果,设计空间站小型改性碳纳米管两床式CO2清除概念装置,要求吸附脱附过程同时交替进行,单位操作时间为30min。吸附床层总容积为0.06m3,装置的处理量为0.3m3·h-1,最低耗能约为22.9kWh·kg-1CO2,可支持空间站内10名宇航员同时工作,同时将密闭舱室CO2浓度控制在03%以下。本研究对烟气中CO2的捕集也有借鉴意义。
CO2would be harmful and needs to be removed in confined space, such as submarines and space capsules. A key function of environment control and life support system is the removal of metabolic CO2from the atmosphere in the living quarters. The system needs indicate that any future CO2sequestration technologies must be high efficiency, stable and secure, and then the device must be small, light, low energy consumption, durable and easy operation. In this paper, according to the advantages of adsorption method, we developed a series of solid amine adsorbents by impregnating TEPA and TETA into SBA-16and CNTs porous material support. This material removed CO2at a low concentration at ambient temperature, similar to cabin atmosphere conditions. The adsorption and desorption performance of the adsorbent was investigated at a fixed-bed column. The main conclusions are as follows:
The solid amine adsorbents for CO2removal were developed by SBA-16and CNTs impregnated with TEPA or TETA. After impregnation, the shapes, fundamental channels and pore structures of adsorbents were not changed. But the surface area and pore volumn decreased remarkably with the increasing amine loading amounts. And the CO2adsorption capacity was changed with a contrary tendency.The maximum amount of amine loading in the pore channel was about30wt.%. After modification, the CO2adsorption capacity improved with the temperature (288-308K). When the temperature reached308K, the maximum capacity was3.37and2.65mmol·g-1fo CTP-30and CTT-30, respectively. The adsorption performance of modified SBA-16and CNTs was relatively stable afer5adsorption/desorption cycles.
The CO2adsorption capacity of CTP-30was remarkably improved with the increasing temperature from2.52to3.56mmol·g-1with the increasing temperature from283to313K. And the adsorption of CO2on CTP-30was mainly chemisorption. The ratio of chemisorption capacity was no less than74%of total adsorption capacity. The shapes of the adsorption isotherms of for CTP-30corresponded to type I at various temperatures. The average isosteric heat of adsorption is32.68kJ·mol-1.
The adsorption capacity was also influenced by moisture.It increased significantly from2.97to2.88mmol·g-1as the water vapor increased from0to2%but began to decrease from3.88to2.67mmol·g-1as the water vapor further increased from2to7%. As a preliminary assessment of the adsorption kinetics of these materials under low CO2concentration, the adsorption half time was measured using the fixed-bed column. The CTP-30also exhibited a relatively stable CO2regeneration performance in adsorption capacity after20cycles, which remained around3.68mmol·g-1. In all cases, the experimental data agreed with the predicated breakthrough model. The regression analysis values of the data were0.99or higher under various conditions.
CTP-30exihibited an excellent regenerabtion performance. The TPD results indicated that CTP-30had two desorption peaks at313K and358K, respectively. And vacuum and temperature swing adsorption (VTSA) was used to regenerate CO2. The results implied that the regeneration can be operated at relatively low temperature (353K) and the efficiency was95%or higher.The initial desorption rate of CTP-30(5kPa,373K) was quicker than that in other conditions (0.71mmol·min-1) and the adsorbent could be completely regenerated in15min. According to the results, a two-bed device using CTP-30was conceptually designed to remove CO2in space station, alternating between adsorption and desorption process. The operation unite time was about30min.The bed volumn was about0.06mJ, the blowing rate was0.3m3·h-1and the consumption energy was22.9kWh·kg-1CO2. The device can support up to10astronauts working inside the space station simultaneously, and can keep the CO2concentration around0.3%. The results also have some practical value to the CO2capture in flue gas application.
以多孔材料SBA-16、NTs为载体,四乙烯五胺(TEPA)、三乙烯四胺(TETA)为氨基改性剂,采用浸渍法合成新型CO2吸附剂。研究结果表明,吸附剂通过浸渍改性后均保持了原有主孔道结构。吸附剂的比表面积、孔容以及孔径随着TETA或TEPA浸渍量的增加而减小。改性后SBA-16和CNTs吸附剂的CO2吸附量随着TETA或TEPA浸渍量的升高而增加,并存在最佳浸渍量,均为30wt%左右。改性后SBA-16和CNTs吸附剂的C02吸附量随着吸附温度(288-308K)的升高而增大,在308K时,样品CTP-30和CTT-30表现出较高的吸附容量,分别为3.37mmol·g-1和2.65mmol·g-1。经过5次的吸附脱附循环再生,改性后SBA-16和CNTs吸附剂均表现出较为稳定的吸附性能。
固定床动态吸附实验表明,在实际密闭空间温度范围内(283-313K),随着温度的升高,样品CTP-30的CO2动态吸附量从2.52mmol·g-1升至3.56mmol·g-1,其吸附C02过程以化学吸附为主,在283～313K之间,CTP-30的化学吸附量qec占吸附量q的比例达到74%以上。CTP-30对CO2的吸附等温线(283～313K)属于Ⅰ型吸附等温线。利用Langmuir方程模拟实验所得结果,相关系数均大于0.99,其平均等量吸附热为32.68kJ·mol-1
气体中一定量水分的存在能提高CTP-30的CO2吸附量。在298K时,随着混合气体中水汽含量由0%升至2%,吸附量由2.97mmol·g-1增加到3.87mmol·g-1。但随着水汽含量继续增加到7%,吸附量逐渐下降,基本保持在2.67mmol·g-1。采用半吸附时间作为衡量手段,考察改性CNTs在密闭空间环境下对低浓度CO2的吸附动力学。在模拟密闭空间环境空气条件下,CTP-30吸附剂具有良好的吸附再生稳定性。经过20次的循环吸附脱附实验后,CO2的吸附容量有所下降,但吸附容量仍维持在3.68mmol·g-1以上。利用失活动力学模型对CTP-30在不同反应条件下的CO2吸附穿透曲线进行模拟分析。结果证明,模拟曲线与实验结果的相关系数R2均大于0.99。
CTP-30吸附剂具有良好的脱附再生性能。TPD实验结果发现CTP-30存在两个明显的强弱脱附峰,其脱附温度分别为313K和358K。采用真空加热耦合脱附技术后,CTP-30可以在较低温度下(353K)实现脱附,脱附效率达到95%以上。而在5kPa压力,373K温度的脱附条件下实验所得初始最高脱附速率明显高于其它条件下的脱附速率,达到了0.7mmol·min-1,且在15min内达到基本完全脱附。根据实验结果,设计空间站小型改性碳纳米管两床式CO2清除概念装置,要求吸附脱附过程同时交替进行,单位操作时间为30min。吸附床层总容积为0.06m3,装置的处理量为0.3m3·h-1,最低耗能约为22.9kWh·kg-1CO2,可支持空间站内10名宇航员同时工作,同时将密闭舱室CO2浓度控制在03%以下。本研究对烟气中CO2的捕集也有借鉴意义。
CO2would be harmful and needs to be removed in confined space, such as submarines and space capsules. A key function of environment control and life support system is the removal of metabolic CO2from the atmosphere in the living quarters. The system needs indicate that any future CO2sequestration technologies must be high efficiency, stable and secure, and then the device must be small, light, low energy consumption, durable and easy operation. In this paper, according to the advantages of adsorption method, we developed a series of solid amine adsorbents by impregnating TEPA and TETA into SBA-16and CNTs porous material support. This material removed CO2at a low concentration at ambient temperature, similar to cabin atmosphere conditions. The adsorption and desorption performance of the adsorbent was investigated at a fixed-bed column. The main conclusions are as follows:
The solid amine adsorbents for CO2removal were developed by SBA-16and CNTs impregnated with TEPA or TETA. After impregnation, the shapes, fundamental channels and pore structures of adsorbents were not changed. But the surface area and pore volumn decreased remarkably with the increasing amine loading amounts. And the CO2adsorption capacity was changed with a contrary tendency.The maximum amount of amine loading in the pore channel was about30wt.%. After modification, the CO2adsorption capacity improved with the temperature (288-308K). When the temperature reached308K, the maximum capacity was3.37and2.65mmol·g-1fo CTP-30and CTT-30, respectively. The adsorption performance of modified SBA-16and CNTs was relatively stable afer5adsorption/desorption cycles.
The CO2adsorption capacity of CTP-30was remarkably improved with the increasing temperature from2.52to3.56mmol·g-1with the increasing temperature from283to313K. And the adsorption of CO2on CTP-30was mainly chemisorption. The ratio of chemisorption capacity was no less than74%of total adsorption capacity. The shapes of the adsorption isotherms of for CTP-30corresponded to type I at various temperatures. The average isosteric heat of adsorption is32.68kJ·mol-1.
The adsorption capacity was also influenced by moisture.It increased significantly from2.97to2.88mmol·g-1as the water vapor increased from0to2%but began to decrease from3.88to2.67mmol·g-1as the water vapor further increased from2to7%. As a preliminary assessment of the adsorption kinetics of these materials under low CO2concentration, the adsorption half time was measured using the fixed-bed column. The CTP-30also exhibited a relatively stable CO2regeneration performance in adsorption capacity after20cycles, which remained around3.68mmol·g-1. In all cases, the experimental data agreed with the predicated breakthrough model. The regression analysis values of the data were0.99or higher under various conditions.
CTP-30exihibited an excellent regenerabtion performance. The TPD results indicated that CTP-30had two desorption peaks at313K and358K, respectively. And vacuum and temperature swing adsorption (VTSA) was used to regenerate CO2. The results implied that the regeneration can be operated at relatively low temperature (353K) and the efficiency was95%or higher.The initial desorption rate of CTP-30(5kPa,373K) was quicker than that in other conditions (0.71mmol·min-1) and the adsorbent could be completely regenerated in15min. According to the results, a two-bed device using CTP-30was conceptually designed to remove CO2in space station, alternating between adsorption and desorption process. The operation unite time was about30min.The bed volumn was about0.06mJ, the blowing rate was0.3m3·h-1and the consumption energy was22.9kWh·kg-1CO2. The device can support up to10astronauts working inside the space station simultaneously, and can keep the CO2concentration around0.3%. The results also have some practical value to the CO2capture in flue gas application.
引文
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