改性钙基吸收剂的CO_2吸收循环特性研究
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摘要
近年,工业生产过程中伴随着污染物的大量排放,其中温室气体(主要组分为C02)的排放被认为是造成全球气候变化异常的主要诱因,且30%以上的C02排放量来自于以化石燃料为原料的能源生产过程。因此,有效控制能源工业中C02的排放量已成为全球未来经济和环境可持续发展的必然选择。以钙基吸收剂固体颗粒作为C02载体,捕集燃烧化石燃料所产生的烟气中C02,形成的CaC03产物热解,释放高浓度C02气体,进一步液化后注入地质处置层或深海,被认为是可帮助实现电力生产过程中近零或零C02排放的污染控制方式,但其弊端是CO2吸收循环效率呈现衰减趋势,因此,若采用天然石灰石作为吸收剂,其消耗量较大。为全面解释钙基吸收剂CO2吸收循环过程的化学反应机理,并寻找改善其吸收效率衰竭特性的方式,本文主要研究内容为以流化床作为主要实验设备,气体吸附仪、扫描电镜及X荧光衍射光谱测量仪为实验辅助分析设备,探讨天然、合成及高温改性钙基吸收剂的C02吸收循环特性,以确定最适于进行长期煅烧／碳酸化循环的钙基吸收剂颗粒种类,探讨各种碳酸化反应参数、改性处理参数等对吸收剂样品的作用机理,且基于实验数据,建立晶粒重叠生长模型,模拟吸收剂颗粒的CO2吸收循环过程。
利用流化床反应器,以天然石灰石作为CO2载体,在不同反应参数(温度、压力及气氛)条件下进行煅烧／碳酸化循环,测量其C02吸收循环特性；并对天然吸收剂样品的颗粒结构特性变化进行测量。实验结果表明,随着碳酸化循环的深入,样品颗粒内小孔(dpre<200nm)容积的不断降低,导致其C02吸收能力呈现衰减趋势。
为改善天然钙基吸收剂的CO2循环吸收衰减特性,基于CaO水合反应,制备以A1203或MgO为主要杂质的合成钙基吸收剂,同样利用流化床实验及颗粒结构分析,探讨不同种类合成吸收剂的煅烧／碳酸化循环特性。以A1203为杂质的合成钙基吸收剂的CO2吸收循环特性较优,具体而言,样品具有较高的C02吸收能力；较高的碳酸化反应活性；稳定的CO2吸收循环特性；较低的损耗率。相较于天然石灰石样品,部分合成吸收剂颗粒显示出不同的CO2循环吸收特性,即随着碳酸化反应气氛中C02摩尔分数的增加,其C02吸收效率增加。
对钙基吸收剂进行高温改性处理,也被认为是一种改变吸收剂碳酸化循环特性的方式。在不同改性处理参数(温度、气氛)条件下,分别对天然石灰石及合成钙基吸收剂进行改性处理,获得的高温改性吸收剂样品,投入流化床反应器,测量其煅烧／碳酸化循环反应特性。高温改性合成吸收剂样品的C02吸收循环特性明显优于改性天然吸收剂样品,其C02吸收效率较高,且C02吸收循环效率基本保持稳定,特别是,部分高温改性合成钙基吸收剂样品的C02吸收能力产生了一定量的再生,原因可能是杂质的存在阻碍了样品的烧结。高温改性钙基吸收剂颗粒的孔隙结构分析数据表明,颗粒中小孔(dpore<200nm)容积的再生改善了其C02吸收能力。
建立重叠球形颗粒生长模型,模拟钙基吸收剂颗粒的煅烧／碳酸化循环过程。分别采用天然石灰石、合成钙基吸收剂及高温改性钙基吸收剂作为计算样本,设定天然石灰石颗粒的晶粒分布为均匀分布,合成吸收剂及改性吸收剂颗粒的晶粒分布为离散均匀分布,并分别基于各自样品的分形维数参数,对假定晶粒分布进行矫正,模拟结果与实验数据吻合良好。进一步对合成吸收剂及改性吸收剂颗粒的SEM电镜图像进行图像处理,所得到的颗粒表面晶粒分布数据与假定晶粒离散分布区间相似。
Recently, there have been a large amount of pollutants emissed to the atmosphere during the process of industry, and the change of climate was due to the emission of greenhouse gas (CO2),30%of which was developed by the generation of electricity from coal. Thus, there is a growing impetus in the world to control the emission of CO2produced during the process of coal firing in the foreseeable future. Ca-based sorbent is employed as the carrier of CO2, then by heating the CaCO3, CO2is released as a concentrated stream suitable for sequestration in the earth or injection to ocean, the above processes are workable to achieve zero, or near-zero emission of CO2in the power industry. But the adsorption activity with CO2based on CaO decreases markedly with the number of forward and reverse steps undergone in reaction, resulting in the large use of limestone, where natural Ca-based sorbents are being considered. Thus, this dissertation was focused on the characteristics of CO2chemical looping employed the natural, synthetic or thermal pretreated calcium-based sorbents as the carrier of CO2based on fluidized bed, the analysis of microstructure of sorbents based on gas adsorption, SEM and X-ray diffraction, the confirmation of sorbents with better CO2capturing capacity, and the influence of the carbonation parameters and the pretreatment parameters on the reaction activity of sorbents, the propulsion of the overlapping grain model to simulate the CO2chemical looping.
Based on fluidized bed system,4different kinds of limestone were employed as sorbents for capturing CO2, and the calcination/carbonation cycles were conducted in different reaction parameters, such as temperature, pressure and atmosphere, then the capacity and activity of CO2were recorded, in addition, the change of particle microstructure was tested. The results showed that the decreased of small pore(dpore<200nm) volume was responsible to de-activity of natural sorbents with the proceeding of CO2capturing cycle.
Improved, Ca-based synthetic sorbents have been prepared and tested, the purity was Al2O3or MgO. One of them, a mixed oxide consisting of CaO and Al2O3, met the criteria for an ideal sorbent for CO2, specifically, large uptake of CO2per unit mass of sorbent, reasonably high reactivity during carbonation, stable uptake of CO2after a large number of calcination/carbonation cycles, and good resistance to attrition. Moreover, comparing with limestone, some of synthetic sorbents were represented the increase of uptake with increasing the concentration of CO2during carbonation.
The thermal pretreatment of Ca-based sorbent under various conditions (temperature, atmosphere) was completed to modify its activity during long-term calcination/carbonation cycle. The pretreated synthetic sorbents were shown larger overall uptake during long-term CO2capturing cycles comparing with limestone. Noticeably, some of pretreated synthetic sorbents'activity were regenerated, as was related to the regeneration of small pore(dpore<200nm) volume.
The overlapping grain model was developed to formulate the process of calcination/carbonation based on Ca-based sorbent. In case of limestone, synthetic sorbent and thermal pretreated sorbent, the assumed grain diameter distributions were revised based on theirs fractal dimension respectively, the simulations were shown the good agreement with experimental results. Moreover, the surface morphology of synthetic sorbent and also thermal pretreated sorbent was found to be impressive agreement to the assumed morphology of sorbent.
利用流化床反应器,以天然石灰石作为CO2载体,在不同反应参数(温度、压力及气氛)条件下进行煅烧／碳酸化循环,测量其C02吸收循环特性；并对天然吸收剂样品的颗粒结构特性变化进行测量。实验结果表明,随着碳酸化循环的深入,样品颗粒内小孔(dpre<200nm)容积的不断降低,导致其C02吸收能力呈现衰减趋势。
为改善天然钙基吸收剂的CO2循环吸收衰减特性,基于CaO水合反应,制备以A1203或MgO为主要杂质的合成钙基吸收剂,同样利用流化床实验及颗粒结构分析,探讨不同种类合成吸收剂的煅烧／碳酸化循环特性。以A1203为杂质的合成钙基吸收剂的CO2吸收循环特性较优,具体而言,样品具有较高的C02吸收能力；较高的碳酸化反应活性；稳定的CO2吸收循环特性；较低的损耗率。相较于天然石灰石样品,部分合成吸收剂颗粒显示出不同的CO2循环吸收特性,即随着碳酸化反应气氛中C02摩尔分数的增加,其C02吸收效率增加。
对钙基吸收剂进行高温改性处理,也被认为是一种改变吸收剂碳酸化循环特性的方式。在不同改性处理参数(温度、气氛)条件下,分别对天然石灰石及合成钙基吸收剂进行改性处理,获得的高温改性吸收剂样品,投入流化床反应器,测量其煅烧／碳酸化循环反应特性。高温改性合成吸收剂样品的C02吸收循环特性明显优于改性天然吸收剂样品,其C02吸收效率较高,且C02吸收循环效率基本保持稳定,特别是,部分高温改性合成钙基吸收剂样品的C02吸收能力产生了一定量的再生,原因可能是杂质的存在阻碍了样品的烧结。高温改性钙基吸收剂颗粒的孔隙结构分析数据表明,颗粒中小孔(dpore<200nm)容积的再生改善了其C02吸收能力。
建立重叠球形颗粒生长模型,模拟钙基吸收剂颗粒的煅烧／碳酸化循环过程。分别采用天然石灰石、合成钙基吸收剂及高温改性钙基吸收剂作为计算样本,设定天然石灰石颗粒的晶粒分布为均匀分布,合成吸收剂及改性吸收剂颗粒的晶粒分布为离散均匀分布,并分别基于各自样品的分形维数参数,对假定晶粒分布进行矫正,模拟结果与实验数据吻合良好。进一步对合成吸收剂及改性吸收剂颗粒的SEM电镜图像进行图像处理,所得到的颗粒表面晶粒分布数据与假定晶粒离散分布区间相似。
Recently, there have been a large amount of pollutants emissed to the atmosphere during the process of industry, and the change of climate was due to the emission of greenhouse gas (CO2),30%of which was developed by the generation of electricity from coal. Thus, there is a growing impetus in the world to control the emission of CO2produced during the process of coal firing in the foreseeable future. Ca-based sorbent is employed as the carrier of CO2, then by heating the CaCO3, CO2is released as a concentrated stream suitable for sequestration in the earth or injection to ocean, the above processes are workable to achieve zero, or near-zero emission of CO2in the power industry. But the adsorption activity with CO2based on CaO decreases markedly with the number of forward and reverse steps undergone in reaction, resulting in the large use of limestone, where natural Ca-based sorbents are being considered. Thus, this dissertation was focused on the characteristics of CO2chemical looping employed the natural, synthetic or thermal pretreated calcium-based sorbents as the carrier of CO2based on fluidized bed, the analysis of microstructure of sorbents based on gas adsorption, SEM and X-ray diffraction, the confirmation of sorbents with better CO2capturing capacity, and the influence of the carbonation parameters and the pretreatment parameters on the reaction activity of sorbents, the propulsion of the overlapping grain model to simulate the CO2chemical looping.
Based on fluidized bed system,4different kinds of limestone were employed as sorbents for capturing CO2, and the calcination/carbonation cycles were conducted in different reaction parameters, such as temperature, pressure and atmosphere, then the capacity and activity of CO2were recorded, in addition, the change of particle microstructure was tested. The results showed that the decreased of small pore(dpore<200nm) volume was responsible to de-activity of natural sorbents with the proceeding of CO2capturing cycle.
Improved, Ca-based synthetic sorbents have been prepared and tested, the purity was Al2O3or MgO. One of them, a mixed oxide consisting of CaO and Al2O3, met the criteria for an ideal sorbent for CO2, specifically, large uptake of CO2per unit mass of sorbent, reasonably high reactivity during carbonation, stable uptake of CO2after a large number of calcination/carbonation cycles, and good resistance to attrition. Moreover, comparing with limestone, some of synthetic sorbents were represented the increase of uptake with increasing the concentration of CO2during carbonation.
The thermal pretreatment of Ca-based sorbent under various conditions (temperature, atmosphere) was completed to modify its activity during long-term calcination/carbonation cycle. The pretreated synthetic sorbents were shown larger overall uptake during long-term CO2capturing cycles comparing with limestone. Noticeably, some of pretreated synthetic sorbents'activity were regenerated, as was related to the regeneration of small pore(dpore<200nm) volume.
The overlapping grain model was developed to formulate the process of calcination/carbonation based on Ca-based sorbent. In case of limestone, synthetic sorbent and thermal pretreated sorbent, the assumed grain diameter distributions were revised based on theirs fractal dimension respectively, the simulations were shown the good agreement with experimental results. Moreover, the surface morphology of synthetic sorbent and also thermal pretreated sorbent was found to be impressive agreement to the assumed morphology of sorbent.
引文
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