介孔二氧化硅改性及其吸附CO_2研究
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摘要
全球气候变化是人类迄今面临的最重大环境问题，也是21世纪人类面临的最复杂挑战之一。化石燃料燃烧排放的大量CO_2是造成全球气候变化的主要原因，对全球变暖的贡献率已超过了60％。采用新型的多孔固体吸附剂对烟气中CO_2进行分离和捕集有可能是一种高选择性，低能耗的方法，已引起人们的广泛关注。然而，目前所开发的针对该体系的吸附剂均对吸附脱附条件比较敏感，尚有许多不足之处，制约了该吸附法的实际应用。本文正是基于上述背景采用氨基修饰及多种有机胺浸渍等方法来研制新型吸附剂，对提高该类CO_2吸附剂的相关性能做了有益的探索。主要研究结论如下：
对焙烧去除模板剂后的样品进行水化能使改性后的SBA-16的吸附容量和吸附速率增加。这是由于焙烧过程中SBA-16的一部分表面硅羟基发生缩合脱水，失去活性，而水化过程会使得Si-O-Si键重新生成硅羟基。SBA-16的颗粒粒径越小，经过表面修饰后的改性SBA-16的平衡吸附容量越大。分子筛的颗粒粒径越小，氨基活性基团更容易进入孔道内，因此嫁接量也较多。颗粒粒径在0．124-0．15mm之间的SBA-16(经过水化的样品)经过改性后具有最大的吸附容量，约为0．727 mmol g~(-1)(60℃)，是SBA-16载体吸附量的18．1倍，说明材料经过改性后，表面修饰的氨基与CO_2产生了一定的化学作用，从而导致吸附容量大大增加。经过氨基改性后的SBA-16的吸附焓可以高达70 kJ mol~(-1)左右，而物理吸附焓仅为40 kJ mol~(-1)左右，这也表明氨基与CO_2分子之间存在化学反应。同时，研究发现改性后样品的吸附容量与嫁接氨基量几乎成线性关系，即Y=0．3855X-0．4397，Y代表吸附容量(mmol g~(-1))，而X代表氨基浓度(mmol-N g~(-1))。
在传统的以沸石分子筛作为吸附剂的变温吸附中，烟气中水蒸气的存在与CO_2产生竞争吸附，因此需要对烟道气进行除湿，而除湿过程消耗的能量约占总耗能的30％。在变温吸附中，高温条件虽有利于脱附，但可能会使介孔分子筛表面嫁接的氨基基团分解。同时，高温和高湿度条件有可能会破坏介孔分子筛的结构。因此，本文首次研究了有机改性后介孔二氧化硅分子筛SBA-16的水热稳定性和热稳定性，以及硅烷化程度对于改性SBA-16疏水性能的影响。结果表明，氨基嫁接改性后的SBA-16比载体SBA-16表现出更强的疏水性能，而在烟道气中水分几乎是饱和的，所以这有利用于降低吸附剂再生时的能耗。在He或空气氛围中经过氨基改性的SBA-16的热稳定温度均能达到200℃，这有利用于吸附剂的快速再生。经多次循环吸附脱附试验后吸附剂的性能没发生明显劣化。根据~(29)Si MAS NMR和N_2物理吸附脱附分析结果，经过16 h水热处理后的改性SBA-16仍然表现出强的水热稳定性，改性后介孔SBA-16的水热稳定性取决于其硅烷化程度的大小。这些性质对于介孔吸附材料在高湿高温条件下吸附分离CO_2具有重要意义。
本文也通过浸渍方法在MCM-41原粉上负载了三种不同有机胺(DETA、TETA、AMP)制备CO_2吸附材料。采用低角度XRD、TGA／DTG、N_2物理吸附法、FTIR来表征负载胺在载体内的分散及负载情况。表征结果表明各种胺已经成功负载到载体上，并且材料在100℃下再生能够保持稳定。本文中吸附材料的制备过程不仅可以节约去除模板剂所需要的能量或者萃取溶剂，而且由于其不需要采用甲苯溶剂，所以避免了甲苯对环境的污染。采用动态吸附柱法对改性材料的CO_2的吸附性能进行了研究。研究结果表明，采用TETA浸渍的吸附材料由于具有最大的N含量，其对CO_2具有最大的吸附容量(2．22 mmol g~(-1))。采用失活模型对吸附柱法CO_2的吸附穿透曲线进行数学模拟，发现失活模型能较好地模拟这一过程。对烟气中杂质的影响也做了初步的探索，实验表明浓度为550 mgm~(-3)的SO_2对CO_2吸附材料性能并无显著影响。但由于SO_2会与胺基材料产生不可逆吸附反应，在将来可能的工业应用中吸附CO_2的单元宜设在脱硫装置以后，以尽量减小SO_2对吸附材料的影响。
The global climate change is the most critical environmental problem and is alsoone of the most complicated challenges facing to the whole mankind. CO_2 emissionfrom fossil fuels combustion contributes to more than 60% of the global climatechange, which has been the main reason that results in the global climate change.Therefore, the novel porous solids to capture CO_2 from flue gas have attractedparticular interest due to its high selectivity and low energy penalty. However, thepresent adsorbents are sensitive to the adsorption/desorption conditions and there stillexit some disadvanges. In this paper, three methods such as grafting, coating andimpregnation were used to prepare the novel adsorbents and to promote the CO_2capture capacity, regeneration, hydrophobicity and thermo stability of the adsorbents.
The samples of Hydrolyzed-N exhibited superior equilibrium adsorption capacityas well as adsorption rate to those of the samples of Calcined-N, mainly due to theincrease of silanol group concentration on the surface of the adsorbents by hydrolysis.The samples with finer particle size outperformed the samples with coarse particlesize in the equilibrium adsorption capacity. Fine particle size allowed goodaccessibility for the grafting agent. Hence more grafting agents were anchored.Measurements of the enthalpies of adsorption highlighted that the CO_2 adsorption onthe AEAPS functionalized SBA-16 was a strong interaction, indicating that theinteraction between the amine group and CO_2 isa chemisorption. The maximumamount of carbon dioxide adsorbed at 60℃was 0.727 mmol g~(-1) for the AEAPSfunctionalized SBA-16 (hydrolyzed SBA-16 as support) of the particle size range at0.124-0.15 mm., which is 18.1 times that of the SBA-16 support, suggesting thatadsorption of CO_2 on the AEAPS functionalized SBA-16 is mostly a chemisorption.The adsorption enthalpy is much higher than 40 kJ mol~(-1), about 70 kJ mol~(-1), whichalso suggests it is a chemisorption. The relationship between adsorption capacity andamine content is Y=0.3855X-0.4397 where Y is adsorption capacity (mmol g~(-1)) and Xis amine content (mmol-N g~(-1)).
In the traditional temperature swing adsorption using zeolites as adsorbents, about 30 % of the total energy is consumed to dehumidify flue gas before adsorption,owing to the competitive adsorption between water vapor and CO_2. High regenerationtemperature may promote desorption of CO_2, however, it may decompose the graftingamino groups. At the same time, high temperature and high humidity of flue gas afterFGD may cause the destruction of the mesoporous silica. Therefore, for the first time,thermal stability, hydrothermal stability and hydrophobicity of the SBA-16 supportsand the modified SBA-16 by silylation were investigated.
The amino-functionalized SBA-16 prepared by silylating various amine contentson the mesoporous silica SBA-16 exhibited super hydrophobicity to the SBA-16support. The amino-groups silylated on SBA-16 can be thermally stable up to 200℃whether in He or in air, which is advantageous to the regeneration of the adsorbents.The adsorption capacity remains stable during multiple adsorption/desorptions. Afterhydrothermal treatment for 16 h, the amino-functionalized SBA-16 still displaysstructure stability against boiling water. Hydrothermal stability of theamino-functionalized SBA-16 is related to the extent of silylation, namelyamino-groups contents, which are covalently bonded on the support.
The CO_2 adsorbents were also prepared through impregnating on theas-synthesized MCM-41 by three types of amines. The synthesis way not only savesthe energy or extractor to remove the template but also is environmentally friendlydue to the absence of the potential pollutants such as toluene. The sample impregnatedby TETA showed the highest adsorption capacity, about 2.22 mmol g~(-1) at 60℃due toits highest amino-groups content among the three samples. The CO_2 adsorptionbehavior was also investigated with the deactivation model, which showed excellentprediction of the breakthrough curves. No obvious effect of SO_2 with theconcentration of 550 mg m~(-3) on the adsorbent was found. However, CO_2 capture unitshould be placed after FGD unit to minimize the effect of SO_2 in the potentialcommercial applications, due to the irreversible adsorption of SO_2 on the impregnatedadsorbents.
对焙烧去除模板剂后的样品进行水化能使改性后的SBA-16的吸附容量和吸附速率增加。这是由于焙烧过程中SBA-16的一部分表面硅羟基发生缩合脱水，失去活性，而水化过程会使得Si-O-Si键重新生成硅羟基。SBA-16的颗粒粒径越小，经过表面修饰后的改性SBA-16的平衡吸附容量越大。分子筛的颗粒粒径越小，氨基活性基团更容易进入孔道内，因此嫁接量也较多。颗粒粒径在0．124-0．15mm之间的SBA-16(经过水化的样品)经过改性后具有最大的吸附容量，约为0．727 mmol g~(-1)(60℃)，是SBA-16载体吸附量的18．1倍，说明材料经过改性后，表面修饰的氨基与CO_2产生了一定的化学作用，从而导致吸附容量大大增加。经过氨基改性后的SBA-16的吸附焓可以高达70 kJ mol~(-1)左右，而物理吸附焓仅为40 kJ mol~(-1)左右，这也表明氨基与CO_2分子之间存在化学反应。同时，研究发现改性后样品的吸附容量与嫁接氨基量几乎成线性关系，即Y=0．3855X-0．4397，Y代表吸附容量(mmol g~(-1))，而X代表氨基浓度(mmol-N g~(-1))。
在传统的以沸石分子筛作为吸附剂的变温吸附中，烟气中水蒸气的存在与CO_2产生竞争吸附，因此需要对烟道气进行除湿，而除湿过程消耗的能量约占总耗能的30％。在变温吸附中，高温条件虽有利于脱附，但可能会使介孔分子筛表面嫁接的氨基基团分解。同时，高温和高湿度条件有可能会破坏介孔分子筛的结构。因此，本文首次研究了有机改性后介孔二氧化硅分子筛SBA-16的水热稳定性和热稳定性，以及硅烷化程度对于改性SBA-16疏水性能的影响。结果表明，氨基嫁接改性后的SBA-16比载体SBA-16表现出更强的疏水性能，而在烟道气中水分几乎是饱和的，所以这有利用于降低吸附剂再生时的能耗。在He或空气氛围中经过氨基改性的SBA-16的热稳定温度均能达到200℃，这有利用于吸附剂的快速再生。经多次循环吸附脱附试验后吸附剂的性能没发生明显劣化。根据~(29)Si MAS NMR和N_2物理吸附脱附分析结果，经过16 h水热处理后的改性SBA-16仍然表现出强的水热稳定性，改性后介孔SBA-16的水热稳定性取决于其硅烷化程度的大小。这些性质对于介孔吸附材料在高湿高温条件下吸附分离CO_2具有重要意义。
本文也通过浸渍方法在MCM-41原粉上负载了三种不同有机胺(DETA、TETA、AMP)制备CO_2吸附材料。采用低角度XRD、TGA／DTG、N_2物理吸附法、FTIR来表征负载胺在载体内的分散及负载情况。表征结果表明各种胺已经成功负载到载体上，并且材料在100℃下再生能够保持稳定。本文中吸附材料的制备过程不仅可以节约去除模板剂所需要的能量或者萃取溶剂，而且由于其不需要采用甲苯溶剂，所以避免了甲苯对环境的污染。采用动态吸附柱法对改性材料的CO_2的吸附性能进行了研究。研究结果表明，采用TETA浸渍的吸附材料由于具有最大的N含量，其对CO_2具有最大的吸附容量(2．22 mmol g~(-1))。采用失活模型对吸附柱法CO_2的吸附穿透曲线进行数学模拟，发现失活模型能较好地模拟这一过程。对烟气中杂质的影响也做了初步的探索，实验表明浓度为550 mgm~(-3)的SO_2对CO_2吸附材料性能并无显著影响。但由于SO_2会与胺基材料产生不可逆吸附反应，在将来可能的工业应用中吸附CO_2的单元宜设在脱硫装置以后，以尽量减小SO_2对吸附材料的影响。
The global climate change is the most critical environmental problem and is alsoone of the most complicated challenges facing to the whole mankind. CO_2 emissionfrom fossil fuels combustion contributes to more than 60% of the global climatechange, which has been the main reason that results in the global climate change.Therefore, the novel porous solids to capture CO_2 from flue gas have attractedparticular interest due to its high selectivity and low energy penalty. However, thepresent adsorbents are sensitive to the adsorption/desorption conditions and there stillexit some disadvanges. In this paper, three methods such as grafting, coating andimpregnation were used to prepare the novel adsorbents and to promote the CO_2capture capacity, regeneration, hydrophobicity and thermo stability of the adsorbents.
The samples of Hydrolyzed-N exhibited superior equilibrium adsorption capacityas well as adsorption rate to those of the samples of Calcined-N, mainly due to theincrease of silanol group concentration on the surface of the adsorbents by hydrolysis.The samples with finer particle size outperformed the samples with coarse particlesize in the equilibrium adsorption capacity. Fine particle size allowed goodaccessibility for the grafting agent. Hence more grafting agents were anchored.Measurements of the enthalpies of adsorption highlighted that the CO_2 adsorption onthe AEAPS functionalized SBA-16 was a strong interaction, indicating that theinteraction between the amine group and CO_2 isa chemisorption. The maximumamount of carbon dioxide adsorbed at 60℃was 0.727 mmol g~(-1) for the AEAPSfunctionalized SBA-16 (hydrolyzed SBA-16 as support) of the particle size range at0.124-0.15 mm., which is 18.1 times that of the SBA-16 support, suggesting thatadsorption of CO_2 on the AEAPS functionalized SBA-16 is mostly a chemisorption.The adsorption enthalpy is much higher than 40 kJ mol~(-1), about 70 kJ mol~(-1), whichalso suggests it is a chemisorption. The relationship between adsorption capacity andamine content is Y=0.3855X-0.4397 where Y is adsorption capacity (mmol g~(-1)) and Xis amine content (mmol-N g~(-1)).
In the traditional temperature swing adsorption using zeolites as adsorbents, about 30 % of the total energy is consumed to dehumidify flue gas before adsorption,owing to the competitive adsorption between water vapor and CO_2. High regenerationtemperature may promote desorption of CO_2, however, it may decompose the graftingamino groups. At the same time, high temperature and high humidity of flue gas afterFGD may cause the destruction of the mesoporous silica. Therefore, for the first time,thermal stability, hydrothermal stability and hydrophobicity of the SBA-16 supportsand the modified SBA-16 by silylation were investigated.
The amino-functionalized SBA-16 prepared by silylating various amine contentson the mesoporous silica SBA-16 exhibited super hydrophobicity to the SBA-16support. The amino-groups silylated on SBA-16 can be thermally stable up to 200℃whether in He or in air, which is advantageous to the regeneration of the adsorbents.The adsorption capacity remains stable during multiple adsorption/desorptions. Afterhydrothermal treatment for 16 h, the amino-functionalized SBA-16 still displaysstructure stability against boiling water. Hydrothermal stability of theamino-functionalized SBA-16 is related to the extent of silylation, namelyamino-groups contents, which are covalently bonded on the support.
The CO_2 adsorbents were also prepared through impregnating on theas-synthesized MCM-41 by three types of amines. The synthesis way not only savesthe energy or extractor to remove the template but also is environmentally friendlydue to the absence of the potential pollutants such as toluene. The sample impregnatedby TETA showed the highest adsorption capacity, about 2.22 mmol g~(-1) at 60℃due toits highest amino-groups content among the three samples. The CO_2 adsorptionbehavior was also investigated with the deactivation model, which showed excellentprediction of the breakthrough curves. No obvious effect of SO_2 with theconcentration of 550 mg m~(-3) on the adsorbent was found. However, CO_2 capture unitshould be placed after FGD unit to minimize the effect of SO_2 in the potentialcommercial applications, due to the irreversible adsorption of SO_2 on the impregnatedadsorbents.
引文
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