分离CH_4/CO_2的吸附剂研究
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摘要
沼气的主要成分是甲烷(CH4,55%～65%),其次是二氧化碳(CO2,30%-40%),沼气的能量来源于CH4,而过多的CO2降低了沼气的能量密度,致使单位能量的运输和贮存成本增加,影响沼气的工业化发展,因此去除沼气中的CO2,降低CH4的储运成本是沼气工业化急待解决的问题。
与其他气体净化技术相比,吸附法因其污染小、设备简单、成本低等优点而备受关注。吸附法的核心问题是要拥有高性能的吸附剂。而目前,在分离CH4与CO2的研究领域,吸附系统的发展水平要远远超过吸附剂材料。本文研究的主要目的是找到适合从沼气中脱除CO2的吸附剂类型,并对沼气脱碳吸附剂的深入研究提供工作基础和研究思路,最终解决沼气脱碳技术的难题,为沼气的产业化运营提供技术参考。
分子筛类和碳基吸附剂是目前发展最成熟的商业化脱碳吸附剂,本文研究了分子筛类和碳基吸附剂分离CH4与CO2的性能、再生性能和对水蒸气的敏感性。此外,本文选用硅胶为载体,乙醇胺(MEA)和乙醇胺/N-甲基-二乙醇胺复合胺(MEA/MDEA)为改性剂合成新型同体胺吸附剂,并对合成吸附剂进行了深入研究。主要研究结论如下：
(1)常温(25℃)低压下(0.2MPa)下,在3A、4A、5A、10X、13X中,13X分子筛对CH4与CO2混合气分离效果最好,其次是5A分子筛。5A和13X分子筛经过一次使用后,性能都无法完全复原,吸附剂再生度分别为65%和7O%左右。吸附剂不能完全再生的原因是分子筛上吸附的部分CO2可以与吸附剂发生强相互作用,形成二齿或螯合状态的含碳物种,使吸附剂的活性位减少,红外光谱结果说明了这一原因。此外,分子筛对水蒸气非常敏感,水蒸气可以使吸附剂完全丧失分离CH4与CO2的能力,这一点对沼气脱碳技术是十分不利的。
(2)市售的碳分子筛对CH4与CO2混合气的分离效果要明显好于活性炭,但还不如13X分子筛,碳分子筛对CH4的吸附量较大,这意味着会降低原料气中CH4的回收率。然而在室温条件下,碳分子筛很容易完全再生。在水蒸气存在下,碳分子筛性能有所下降,但依然具有对CH4与CO2分离的能力,即碳分子筛对水蒸气不是十分敏感,这一性能远好于沸石分子筛。碳分子筛在分离CH4与CO2方面的优点与缺点都源于碳质材料极性较弱的性质。
(3)显微镜结果显示A型硅胶在改性过程中骨架破碎,FNG-Ⅱ型硅胶改性后骨架结果比较稳定。说明有机胺改性吸附剂的多孔载体需要筛选,这个领域有继续深入研究价值。热重、红外、低温N2吸脱附法的结果都说明浸渍法可以成功的将MEA修饰在硅胶表面,表面修饰了MEA后,吸附剂对CO2有一定的吸附能力。MEA负载率较低时,增加改性剂的负载率可以提高吸附剂对CO2的吸收能力。而当MEA在FNG-Ⅱ型硅胶上负载率增大到20%后,吸附剂对CO2的吸附能力会趋近饱和,原因是再进一步增加MEA的量,过多的MEA会大量填充吸附剂孔道,使得吸附剂的比表面及孔容大幅度下降。在室温条件下,无论是抽真空法还是惰气冲洗法都不能使MEA改性吸附剂再生。105℃以下吸附剂无法再生,在110℃和120℃时吸附剂再生效果较好,但再生后的吸附剂性能也会下降。150℃再生时,吸附剂的性能会明显下降。在水蒸气存在下,吸附剂能不受影响,可以保持原有的对CH4与CO2分离的能力,这一性能是MEA改性吸附剂的优势。
(4)本文初步研究复合胺MEA/MDEA改性硅胶吸附剂‘试验结果表明MDEA的加入对吸附剂的再生性能有所改善。
综上,分子筛对CH4与CO2有很好的分离效果,但是其骨架的化学结构导致其与C02、H20都有强的相互作用,这将增加沼气净化的再生耗能并对沼气脱水步骤要求苛刻。因此相比之下骨架结构是非极性的碳材料更有优势,但目前的碳材料对CH4和CO2的分离效果还不够理想,新型功能化的碳材料的研发可能会解决这个问题,但还需要相当长的一段时间。MEA改性FNG-Ⅱ型硅胶可以很好的分离CH4与CO2,对水的耐受性较强,但其再生性的缺点也是非常明显的。然而,MEA改性硅胶吸附剂只是众多有机胺改性吸附剂中的一种,由于可以作为改性剂的有机胺及多孔材料种类繁多,因此有很大的研究空间。此外,有机胺改性吸附剂的研究还可以从化学吸收工艺中取得经验,是比较有应用前景的一种吸附剂。
Biogas is mainly composed of methane (CH4,55%-65%) and carbon dioxide (CO2,30%-40%). The energy source of biogas is from CH4, and CO2significantly reduces its energy content, which result in high cost for transportation and storage of the gas. Therefore, it is critical to develop effective methods for the sequestration of CO2from biogas.
Adsorption is considered very promising compared with other technologies, because of its intrinsic eco-compatibility and low cost. It is of great importance to develop an efficient CO2adsorbent with a high CO2adsorption capacity, a high selectivity, and good regeneration property. In this paper, the main aim was to find an excellent adsorbent to separate CO2and CH4, which will be benefit for large-scale biogas purification.
Three families of adsorbents have been studied. They are molecular sieves, carbon-based adsorbents and amino-functionalized silicas. The separation/regeneration performance of the adsorbents has been compared, and their sensitivity to moisture has been researched. The main research conclusions are as follows:
(1) Selective adsorption of CO2from its mixture with CH4on several commercial molecular sieves has been studied at ambient temperature(25℃) and low pressure (0.2MPa). The behaviors of the molecular sieves have been compared by using three basic parameters:selectivity, adsorption capacity and regenerability. The results indicate3A and4A molecular sieves have low CO2adsorption capacity. However5A and13X molecular sieves show high efficiency in dynamic separation of CH4and CO2when the adsorbents were used for the first time. The separation coefficient between CH4and CO2on13X molecular sieve is higher than5A, which prove13X molecular sieve show better performance in separating CO2from its mixture with CH4. But5A and13X molecular sieve could not be regenerated completely and the adsorption/regeneration performance became stable from their second use. The reason why separation performance of5A and13X molecular sieves decrease is explained by FTIR spectroscopy that the partial poisoning of the molecular sieves happened. That is to say, the regenerability of the two molecular sieves need improve. In addition, molecular sieves are sensitive to water vapor, vapor can make adsorbent completely lose the ability of separation of CH4and CO2, which is very disadvantageous to biogas purification technology.
(2) The removal of CO2from a CH4/CO2mixture on commercial carbon-based adsorbents has been researched. And the performance in separating CO2from its mixture with CH4on carbon-based adsorbents was compared with13X molecular sieve. The results indicate carbon molecular sieve can separate the mixture well but its selectivity is lower than13X molecular sieve. However carbon molecular sieve can be well regenerated and are not very sensitive to water vapor, which are much better than13X molecular sieve. All the properties of carbon-based adsorbent are mainly governed by its texture. In order to improve the adsorption selectivity of carbon molecular sieve for CH4and CO2, the new preparation process should be urgently researched, which may be benefit for large-scale biogas purification.
(3) amino-functionalized silicas were synthesized using MEA and silicas. The adsorbents were characterized by N2adsorption isotherm, thermogravimetry and FTIR, which show that MEA have been successfully modified in the FNG-Ⅱ silica pores. And the performance of adsorbents was researched by adsorption and desorption experiments. The results indicate MEA-functionalized silicas could separation CO2and CH4well in its first or second use, but the performance deducted afterwards. The MEA-functionalized silicas can not regeneration under105℃. When MEA loading is low, the performance improves with MEA loading. However, the performance would not improve when MEA more than20%, because the pores would be occupied so much that the specific surface would decrease in a large number. The most noteworthy is that MEA functionalized silicas can not be affected by vapor.
(4) A preliminary study on MEA/MDEA modified silica, the results showed that the addition of MDEA could improve the regeneration performance of adsorbents.
In conclusion, molecular sieves can separate CH4and CO2well, but their skeleton chemical structures make them strong interact with CO2and they are too sensitive to vapor. Carbon-based materials have some advantages on regeneration but they also have low recovery rate of CH4. Development of new functional carbon materials may solve this problem, but this also need quite a long time. MEA modified silica can separate CH4and CO2well and has strong tolerance to water, but the disadvantage of the regeneration is very obvious. Too much work should be done to improve the regeneration of amino-functionalized absorbents, and it will be an attractive research field.
与其他气体净化技术相比,吸附法因其污染小、设备简单、成本低等优点而备受关注。吸附法的核心问题是要拥有高性能的吸附剂。而目前,在分离CH4与CO2的研究领域,吸附系统的发展水平要远远超过吸附剂材料。本文研究的主要目的是找到适合从沼气中脱除CO2的吸附剂类型,并对沼气脱碳吸附剂的深入研究提供工作基础和研究思路,最终解决沼气脱碳技术的难题,为沼气的产业化运营提供技术参考。
分子筛类和碳基吸附剂是目前发展最成熟的商业化脱碳吸附剂,本文研究了分子筛类和碳基吸附剂分离CH4与CO2的性能、再生性能和对水蒸气的敏感性。此外,本文选用硅胶为载体,乙醇胺(MEA)和乙醇胺/N-甲基-二乙醇胺复合胺(MEA/MDEA)为改性剂合成新型同体胺吸附剂,并对合成吸附剂进行了深入研究。主要研究结论如下：
(1)常温(25℃)低压下(0.2MPa)下,在3A、4A、5A、10X、13X中,13X分子筛对CH4与CO2混合气分离效果最好,其次是5A分子筛。5A和13X分子筛经过一次使用后,性能都无法完全复原,吸附剂再生度分别为65%和7O%左右。吸附剂不能完全再生的原因是分子筛上吸附的部分CO2可以与吸附剂发生强相互作用,形成二齿或螯合状态的含碳物种,使吸附剂的活性位减少,红外光谱结果说明了这一原因。此外,分子筛对水蒸气非常敏感,水蒸气可以使吸附剂完全丧失分离CH4与CO2的能力,这一点对沼气脱碳技术是十分不利的。
(2)市售的碳分子筛对CH4与CO2混合气的分离效果要明显好于活性炭,但还不如13X分子筛,碳分子筛对CH4的吸附量较大,这意味着会降低原料气中CH4的回收率。然而在室温条件下,碳分子筛很容易完全再生。在水蒸气存在下,碳分子筛性能有所下降,但依然具有对CH4与CO2分离的能力,即碳分子筛对水蒸气不是十分敏感,这一性能远好于沸石分子筛。碳分子筛在分离CH4与CO2方面的优点与缺点都源于碳质材料极性较弱的性质。
(3)显微镜结果显示A型硅胶在改性过程中骨架破碎,FNG-Ⅱ型硅胶改性后骨架结果比较稳定。说明有机胺改性吸附剂的多孔载体需要筛选,这个领域有继续深入研究价值。热重、红外、低温N2吸脱附法的结果都说明浸渍法可以成功的将MEA修饰在硅胶表面,表面修饰了MEA后,吸附剂对CO2有一定的吸附能力。MEA负载率较低时,增加改性剂的负载率可以提高吸附剂对CO2的吸收能力。而当MEA在FNG-Ⅱ型硅胶上负载率增大到20%后,吸附剂对CO2的吸附能力会趋近饱和,原因是再进一步增加MEA的量,过多的MEA会大量填充吸附剂孔道,使得吸附剂的比表面及孔容大幅度下降。在室温条件下,无论是抽真空法还是惰气冲洗法都不能使MEA改性吸附剂再生。105℃以下吸附剂无法再生,在110℃和120℃时吸附剂再生效果较好,但再生后的吸附剂性能也会下降。150℃再生时,吸附剂的性能会明显下降。在水蒸气存在下,吸附剂能不受影响,可以保持原有的对CH4与CO2分离的能力,这一性能是MEA改性吸附剂的优势。
(4)本文初步研究复合胺MEA/MDEA改性硅胶吸附剂‘试验结果表明MDEA的加入对吸附剂的再生性能有所改善。
综上,分子筛对CH4与CO2有很好的分离效果,但是其骨架的化学结构导致其与C02、H20都有强的相互作用,这将增加沼气净化的再生耗能并对沼气脱水步骤要求苛刻。因此相比之下骨架结构是非极性的碳材料更有优势,但目前的碳材料对CH4和CO2的分离效果还不够理想,新型功能化的碳材料的研发可能会解决这个问题,但还需要相当长的一段时间。MEA改性FNG-Ⅱ型硅胶可以很好的分离CH4与CO2,对水的耐受性较强,但其再生性的缺点也是非常明显的。然而,MEA改性硅胶吸附剂只是众多有机胺改性吸附剂中的一种,由于可以作为改性剂的有机胺及多孔材料种类繁多,因此有很大的研究空间。此外,有机胺改性吸附剂的研究还可以从化学吸收工艺中取得经验,是比较有应用前景的一种吸附剂。
Biogas is mainly composed of methane (CH4,55%-65%) and carbon dioxide (CO2,30%-40%). The energy source of biogas is from CH4, and CO2significantly reduces its energy content, which result in high cost for transportation and storage of the gas. Therefore, it is critical to develop effective methods for the sequestration of CO2from biogas.
Adsorption is considered very promising compared with other technologies, because of its intrinsic eco-compatibility and low cost. It is of great importance to develop an efficient CO2adsorbent with a high CO2adsorption capacity, a high selectivity, and good regeneration property. In this paper, the main aim was to find an excellent adsorbent to separate CO2and CH4, which will be benefit for large-scale biogas purification.
Three families of adsorbents have been studied. They are molecular sieves, carbon-based adsorbents and amino-functionalized silicas. The separation/regeneration performance of the adsorbents has been compared, and their sensitivity to moisture has been researched. The main research conclusions are as follows:
(1) Selective adsorption of CO2from its mixture with CH4on several commercial molecular sieves has been studied at ambient temperature(25℃) and low pressure (0.2MPa). The behaviors of the molecular sieves have been compared by using three basic parameters:selectivity, adsorption capacity and regenerability. The results indicate3A and4A molecular sieves have low CO2adsorption capacity. However5A and13X molecular sieves show high efficiency in dynamic separation of CH4and CO2when the adsorbents were used for the first time. The separation coefficient between CH4and CO2on13X molecular sieve is higher than5A, which prove13X molecular sieve show better performance in separating CO2from its mixture with CH4. But5A and13X molecular sieve could not be regenerated completely and the adsorption/regeneration performance became stable from their second use. The reason why separation performance of5A and13X molecular sieves decrease is explained by FTIR spectroscopy that the partial poisoning of the molecular sieves happened. That is to say, the regenerability of the two molecular sieves need improve. In addition, molecular sieves are sensitive to water vapor, vapor can make adsorbent completely lose the ability of separation of CH4and CO2, which is very disadvantageous to biogas purification technology.
(2) The removal of CO2from a CH4/CO2mixture on commercial carbon-based adsorbents has been researched. And the performance in separating CO2from its mixture with CH4on carbon-based adsorbents was compared with13X molecular sieve. The results indicate carbon molecular sieve can separate the mixture well but its selectivity is lower than13X molecular sieve. However carbon molecular sieve can be well regenerated and are not very sensitive to water vapor, which are much better than13X molecular sieve. All the properties of carbon-based adsorbent are mainly governed by its texture. In order to improve the adsorption selectivity of carbon molecular sieve for CH4and CO2, the new preparation process should be urgently researched, which may be benefit for large-scale biogas purification.
(3) amino-functionalized silicas were synthesized using MEA and silicas. The adsorbents were characterized by N2adsorption isotherm, thermogravimetry and FTIR, which show that MEA have been successfully modified in the FNG-Ⅱ silica pores. And the performance of adsorbents was researched by adsorption and desorption experiments. The results indicate MEA-functionalized silicas could separation CO2and CH4well in its first or second use, but the performance deducted afterwards. The MEA-functionalized silicas can not regeneration under105℃. When MEA loading is low, the performance improves with MEA loading. However, the performance would not improve when MEA more than20%, because the pores would be occupied so much that the specific surface would decrease in a large number. The most noteworthy is that MEA functionalized silicas can not be affected by vapor.
(4) A preliminary study on MEA/MDEA modified silica, the results showed that the addition of MDEA could improve the regeneration performance of adsorbents.
In conclusion, molecular sieves can separate CH4and CO2well, but their skeleton chemical structures make them strong interact with CO2and they are too sensitive to vapor. Carbon-based materials have some advantages on regeneration but they also have low recovery rate of CH4. Development of new functional carbon materials may solve this problem, but this also need quite a long time. MEA modified silica can separate CH4and CO2well and has strong tolerance to water, but the disadvantage of the regeneration is very obvious. Too much work should be done to improve the regeneration of amino-functionalized absorbents, and it will be an attractive research field.
引文
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