CN101500704A - 用于从包括空气的气体混合物中分离二氧化碳的纳米结构负载的固体再生的多元胺和多元胺多元醇吸收剂 - Google Patents

用于从包括空气的气体混合物中分离二氧化碳的纳米结构负载的固体再生的多元胺和多元胺多元醇吸收剂 Download PDF

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CN101500704A
CN101500704A CNA2007800297961A CN200780029796A CN101500704A CN 101500704 A CN101500704 A CN 101500704A CN A2007800297961 A CNA2007800297961 A CN A2007800297961A CN 200780029796 A CN200780029796 A CN 200780029796A CN 101500704 A CN101500704 A CN 101500704A
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sorbent
amine
carbon dioxide
nano
enough
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CN101500704B (zh
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G·A·奥拉
A·戈珀特
S·梅思
G·K·S·普拉卡什
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University of Southern California USC
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Abstract

本发明涉及包括沉积在纳米结构化的载体例如纳米二氧化硅上的胺或者胺/多元醇组合物的再生的负载型胺吸着剂。该吸着剂提供了结构整体性以及高选择性和提高的从包括空气的气体混合物中有效地俘获二氧化碳的能力。该吸着剂是再生的，并且可以通过多个吸收－解吸循环操作而使用。

Description

用于从包括空气的气体混合物中分离二氧化碳的纳米结构负载的固体再生的多元胺和多元胺多元醇吸收剂
发明领域
本发明涉及用于从包括空气的气体混合物中俘获和分离二氧化碳的纳米结构负载的(例如热解二氧化硅、氧化铝等固体)再生的多元胺-多元醇吸收剂。
发明背景
气候变化和全球变暖被认为是现今最紧迫和严重的环境问题之一。现在通常认为全球变暖的主要原因是所谓的温室气体向大气中的释放。主要的温室气体是二氧化碳(CO2)，其主要由化石燃料例如煤、石油和天然气的燃烧而释放。这些化石燃料一起供应世界上约80％的能量需求。由于化石燃料仍然相对廉价并且容易使用，并且由于还没有令人满意的替代物以所需的巨大规模能够替代它们，因此预期化石燃料将长期保持作为我们的主要能源。
削减CO2排放和它们对全球气候的影响的一种方式是从其来源例如来自化石燃料燃烧的发电厂和其他工业工厂的排放物、伴随天然气天然形成的CO2和空气中有效并且经济地俘获CO2。一旦被俘获，CO2可被隔绝在地质岩系中或在海之下，或者可被用作原料以合成燃料和合成烃。
目前，通过基于物理和化学工艺的技术例如通过液体溶液体系吸收、吸附在固体体系上、深冷分离和经隔膜渗透来实现从气流中分离和除去CO2。
在各种CO2分离技术中，基于胺溶液的CO2吸收/解吸体系是最适用于从高体积气流中俘获CO2的其中一种。这类体系中常用的溶剂是烷醇胺例如单乙醇胺(MEA)、二乙醇胺(DEA)、二异丙醇胺(DIPA)和甲基二乙醇胺(MDEA)的水溶液。某些位阻胺例如2-氨基-2-甲基-1-丙醇(AMP)由于它们高的CO2载荷能力(loading capacity)而因此也可被用作吸收剂。在这些当中，MEA由于其高CO2吸收率而被最广泛地使用，其使得能够使用较短的吸收塔。然而，MEA体系呈现出主要的缺点，包括再生溶剂所需要的大量热以及由腐蚀和化学降解造成的操作问题。为了防止过度的腐蚀，通常在胺水溶液中仅使用10～30wt％的MEA，剩余的是水。由于必须将其中70～90％是水的整个溶液加热以使MEA体系再生，因此在所述再生过程期间浪费了大量的能量。其他烷醇胺体系也呈现出缺点。例如，仲胺和受阻胺(例如DEA、DIPA、AMP)提供了比MEA更适度的CO2吸收率，并且也容易遭受腐蚀和化学降解。MDEA被已知仅在缓慢的速率下吸收CO2。通过将若干烷醇胺共混形成的配制物是令人感兴趣的，因为它们可以将各种化合物的有利特性组合同时部分抑制它们的不利特性。已经开发了许多共混的烷醇胺溶液，并且最常见的共混物是含有MEA或DEA的MDEA-基溶液。然而，共混的烷醇胺溶液并没有消除胺溶液-基体系的缺点。
也可以通过吸附在固体吸着剂(sorbent)上来俘获CO2。通常使用固体作为用于分离CO2的物理吸附剂(adsorbent)。该方法基于多孔固体可逆地吸附混合物中的某些组分的能力。所述固体可以具有大的孔径分布，正如硅胶、氧化铝和活性炭中那样，或者由晶体结构控制的孔径，例如沸石。在低温比如室温下，沸石基吸附剂具有高的CO2吸收能力(例如在25℃下在纯CO2中，对于沸石13X而言为160mgCO2/g，对于沸石4A而言为135mgCO2/g)。然而，这些吸附剂的吸附能力随着升高的温度而迅速降低。另外，由于气体仅仅被物理地吸附在所述吸附剂上，因此从气体混合物中实际分离单个气体的作用低。
为了获得CO2吸附的更高选择性，可以将提供化学吸收的化合物施加在所述固体吸附剂上。出于该目的，可以将胺或多元胺沉积或接枝在固体载体上。然而，化学结合(接枝)在固体例如二氧化硅和氧化铝-二氧化硅表面上的胺和多元胺表现出小于80mgCO2/g吸收剂并且在大多数情况下小于50～60mgCO2/g吸收剂的有限的吸收能力。例如，Leal等的美国专利No.5,087,597披露了一种在室温下使用具有120～240m2/g的表面积、用在其结构中含有一个或多个氨基部分的聚烷氧基硅烷改性的硅胶化学吸收CO2的方法。该材料被披露为能够吸收15～23mg干CO2/g吸收剂。Gray等的美国专利No.6,547,854披露了一种通过将所述胺引到被氧化的固体表面上而制备富含胺的吸着剂的方法。使用于He中10％CO2的气体混合物，所报导的吸收在这些固体上的CO2最大量为7.7mg/g吸收剂。可从所述数据中明显看出，由于它们的低胺覆盖量，因此可被吸收在各种固体载体上的接枝氨基上的CO2量仍然相对低。
一种更有前途的路径涉及用胺或多元胺浸渍固体载体。例如，S.Satyapal等的论文，J.Energy and Fuels 15：250(2001)描述了在高表面积的聚甲基丙烯酸甲酯聚合物载体上的聚乙烯亚胺(PEI)/聚乙二醇(PEG)的开发。该固体目前被用于航天飞机中以从机舱气氛中除去CO2并且将其释放到太空中。在50℃和0.02a tm.CO2下，其能力为约40mgCO2/g吸收剂。该材料和其改性物被披露在Bi rbara等的美国专利Nos.6,364,938；5,876,488；5,492,683和5,376,614中。描述于这些专利中的优选载体具有聚合物性质，其中丙烯酸酯树脂例如
Figure A200780029796D00071
被描述为具有特别合适的特性。美国专利Nos.5,376,614；5,492,683和5,876,488还披露了其他可能的载体，包括氧化铝、沸石和碳分子筛。然而，根据美国专利Nos.5,492,683和5,376,614，存在于所述吸着剂上的胺量有限，为1wt％～25wt％。
Zinnen等的美国专利No.4,810,266披露了一种通过用胺醇处理碳分子筛而生成CO2吸着剂的方法。该专利披露了单乙醇胺(MEA)基的材料不稳定并且于较高温度下在再生步骤期间会释放MEA。国际公开No.WO2004/054708披露了基于中孔二氧化硅载体的吸收剂。用于CO2吸收的活性组分是被化学连接或物理吸附在所述中孔二氧化硅表面上的胺或其混合物。在该公开物中描述的大多数吸收剂上的吸收作用低于70mgCO2/g。最好的结果是通过使用被物理吸附在载体上的二乙醇胺(DEA)获得的(约130mgCO2/g)。然而，由于在解吸条件下DEA的挥发性，因此该吸收剂的有效性通常随着增加的CO2吸收-解吸循环的数目而降低(在仅为60℃的适度再生温度下在5个周期之后约为16.8％)。Sirwardane等的美国专利No.6,908,497披露了一种通过用胺和/或醚处理具有0.72～26mg2/g的低表面积的粘土基材而制备吸着剂的方法。
醇、聚乙二醇和其他的氧化化合物(oxygenated compounds)也已被用于除去酸气(主要是CO2和H2S)数十年。例如，在商业工艺中使用得自Union Carbide(现在是Dow Chemicals)的SELEXOL
Figure A200780029796D0008105948QIETU
和得自BASF的SEPASOLV MPE
Figure A200780029796D0008105948QIETU
。在一些工艺例如二醇-胺工艺中，氧化化合物与胺组合作为混合的物理或化学吸着剂也已被用于除去酸气达许多年(参见Kohl，A.L.和Nielsen，R.B.，GAS PURIFICATION 5th ed.(GulfPublishing Co.))。McElroy的美国专利No.4,044,100阐述了使用二异丙醇胺和聚乙二醇二烷基醚的混合物用于从气流中除去气体，包括CO2。J.Yeh等，Energy and Fuels 15，pp.274-78(2001)还研究了使用乙二醇以改进从胺中吸收和解吸CO2。尽管该文献主要涉及在液相中使用胺和氧化化合物，但还探索了使用氧化化合物以提高在固相中气体吸着剂的特性。S.Satyapal等，Energy and Fuels 15：250(2001)提及了在聚合物载体上将聚乙二醇与聚乙烯亚胺组合使用以从航天飞机的密闭气氛中除去CO2。X.Xu等，Microporous and MesoporousMaterials 62：29(2003)表明引入中孔MCM-41/聚乙烯亚胺吸着剂中的聚乙二醇提高了测试材料的CO2吸收和解吸特性。还披露了由沉积在中孔MCM-41上的PEI组成的固体吸收剂的制备和性能(参见X.Xu等，Energy and Fules 16：1463(2002))。Birbara等的美国专利Nos.5,376,614和5,492,683使用多元醇以提高所述吸收剂的吸收和解吸质量。
用于俘获二氧化碳的另一种新材料是金属有机骨架化合物。被已知为MOF-177的优选化合物(J.Am.Chem.Soc.，2005,127，17998)在30巴的相对高压下具有140wt％的室温二氧化碳容量。
正如这些披露内容所示，需要一种用于俘获CO2的有效、经济、容易获得并且再生的、在环境温度以及升高的温度下提供高的除去能力的改进的吸着剂。另外，需要一种解决现有技术的腐蚀和蒸发问题的有效的吸收体系。
发明概述
本发明提供了包含沉积在纳米结构化载体上的胺或胺/多元醇组合物的负载型胺吸着剂，该吸着剂提供了结构整体性和提高的CO2吸收能力。
用于所述胺和胺/多元醇组合物的载体由纳米结构化的固体组成。该纳米结构化的载体可以具有小于约100nm的初级粒径，并且可以是纳米二氧化硅、热解或沉淀氧化物、硅酸钙、碳纳米管、或其混合物。胺可以是伯、仲或叔胺或者烷醇胺、芳胺、混合胺或其组合。在一个实例中，胺以所述吸着剂的约25～75wt％的量存在。多元醇可以选自例如甘油、乙二醇的低聚物、聚乙二醇、聚环氧乙烷、和其醚、改性物和混合物，并且可以所述着收剂的至多约25wt％的量提供。
根据一个实施方案，所述吸着剂是再生的。可以通过施加热量、降低的压力、真空、气体清洗(gaspurge)、贫吹扫气(lean sweep gas)或它们的组合使吸着剂解吸和再生。
本发明还涉及所述吸着剂的制备和所述吸着剂用于从气体源中俘获和分离二氧化碳的特殊用途。二氧化碳可以被释放并且用于制备甲醇。该方法包括在足以产生中间化合物的条件下还原二氧化碳和水，或者还原二氧化碳，随后用氢气将中间化合物催化加氢以形成甲醇。
在一个实施方案中，通过中间化合物例如甲酸甲酯的催化加氢而制备甲醇，其中用于所述加氢的氢气通过将从空气中获得的水电解而获得。在另一个实施方案中，通过以下方式制备甲醇：在足以产生一氧化碳的条件下还原二氧化碳，在足以得到甲酸甲酯的条件下使所述一氧化碳与甲醇反应，和在足以产生甲醇的条件下将所述甲酸甲酯催化加氢。
根据本发明制备的甲醇可被进一步加工成任何所希望的衍生物或改性化合物。例如，可以将甲醇脱水以制得二甲醚，其也可以在足以形成化合物例如乙烯和丙烯的条件下被进一步处理。乙烯和丙烯可被转化成高级烯烃、合成烃、芳族物质或相关的制品，并且因此可用作化学品的原料或用作运输燃料。
在另一个实施方案中，甲醇可被进一步用于单细胞蛋白质的微生物学制备。
优选实施方案的详述
本发明涉及用于吸收CO2的再生的负载型吸着剂。
该吸着剂包含在纳米结构化载体例如纳米二氧化硅载体上的胺用于吸收和解吸CO2。CO2可从任何所希望的来源(包括工业废物、化石燃料燃烧的发电厂的燃料气)以及天然来源中被吸收。根据本发明的纳米结构化载体为所述胺提供结构整体性以及提供用于固-气接触的高表面积。也可以将多元醇加入所述负载型胺吸着剂中以提高其CO2吸收能力和CO2吸收速率。
已经出乎意料地发现某些纳米级颗粒载体特别是二氧化硅纳米颗粒(纳米二氧化硅)具有作为胺、多元胺、聚合胺、和其改性物用载体对于吸收CO2而言的特别品质。根据本发明的具有纳米级载体的吸着剂提供了优于现有技术的吸着剂(例如具有聚合物载体的吸着剂)的显著优点，包括在环境温度和升高的温度下高的CO2选择性和除去能力。因此，本发明的吸着剂允许在多种条件和温度下从多种气体混合物中选择地俘获和分离CO2。本发明的吸着剂还容易在环境至中等温度下再生和循环，这使得能够进行多个吸收-解吸循环而无活性损失或者活性损失最少。该吸着剂还解决了现有技术吸收剂的腐蚀和蒸发问题。另外，不像可以含有仅1wt％～25wt％量的胺的现有技术吸着剂那样，根据本发明的基于纳米颗粒的胺吸着剂可以含有显著更高量的胺，例如约25wt％～75wt％。
因此，本发明的吸着剂体系对于从工业流出气体例如来自化石燃料燃烧的发电和其他工业工厂的那些、以及其他气流、特别是含有显著CO2浓度的天然气中分离CO2而言是实用的。重要地，该着收剂可用于从大气空气中分离CO2。
根据本发明的吸着剂被建议通过以下机理吸收CO2。当与含CO2的气流接触时，所述负载型胺通过形成氨基甲酸盐络合物而化学地吸收CO2。
Figure A200780029796D00111
                                        氨基甲酸盐
在水的存在下，氨基甲酸盐进一步反应以形成碳酸氢盐并释放出所述胺，所述胺可以进一步与CO2反应，由此提高总的CO2吸收能力。
                                                碳酸氢盐
根据本发明的一个实施方案，被吸收的CO2可以容易地被解吸并且所述负载型胺可以被再生。CO2的解吸和吸着剂的再生可以通过将吸着剂适度加热、施加降低的压力或真空、气体清洗和/或二氧化碳贫瘠的吹扫气来实现，这样从吸着剂中释放出CO2。容易的再生使得所述吸着剂能够容易地进行重复的吸收-解吸循环。
有利地，众多类型的胺和醚基化合物可用于本发明的纳米结构化的载体上。
可用于本发明中的胺包括伯、仲和叔烷基-和烷醇胺、芳胺、混合胺及其组合。伯胺和仲胺对于CO2吸收而言最有用。因此，所述胺吸收剂应该优选含有足够量的伯氨基和仲氨基组分。所述氨基组分也应该具有低的挥发性以避免或最小化胺的损失，胺的损失将污染所述气流并且降低该吸收体系随着时间的有效性。氨基组分的实例包括，但不限于单乙醇胺(MEA)、二乙醇胺(DEA)、甲基二乙醇胺、2-(2-氨基乙基氨基)-乙醇、二异丙醇胺、2-氨基-2-甲基-1，3-丙二醇、三乙醇胺、四亚乙基五胺、五亚乙基六胺、聚乙烯亚胺等，包括多种聚合的胺化合物和它们的混合物。聚乙烯亚胺由于它们的仲氨基和伯氨基官能团比例高和它们的挥发性低而因此是优选的。聚乙烯亚胺还提供了有利于将所述吸收剂中的氨基官能团的量最大化的高氮/碳比。具有大于600的分子量的聚乙烯亚胺是尤其优选的。所述吸着剂中的胺含量可以为所述吸着剂的总重量的约25％～约75％。
为了增强负载型胺吸着剂的CO2吸收和解吸特性，可以将多元醇以所述吸着剂的总重量的至多25％的量引入吸着剂组成中。多元醇的加入改善了吸着剂的吸收和解吸，并且降低了胺的粘度，使得CO2即使在较低温度(<50℃)下也能较好地接近吸着剂的活性氨基位点。用于本发明中的多元醇应该不对胺呈反应性，并且应该具有低挥发性以避免或最小化气体损失，所述气体胺的损失将污染气流并且降低吸收体系随着时间的有效性。用于本发明吸着剂中的多元醇的实例包括，但不限于甘油、乙二醇的低聚物、聚乙二醇、聚环氧乙烷、乙二醇低聚物的醚类、聚乙二醇的醚类、聚环氧乙烷的醚类、环醚的低聚物或聚合物例如聚四氢呋喃、和其改性物和混合物。优选的多元醇具有低于10,000的分子量。更优选地，多元醇具有低于1,000的分子量。
根据本发明的载体是初级粒径小于1,000nm、优选小于约100nm的材料。优选的载体是纳米二氧化硅，尤其是所谓的热解二氧化硅和沉淀二氧化硅。热解二氧化硅通常具有5～50nm的初级粒径和50～500m2/g的比表面积。热解二氧化硅通常通过带硅的卤化物例如四氯化硅(SiCl4)的气相水解而制备。可商购获得的热解二氧化硅的实例包括得自Degussa的
Figure A200780029796D00121
得自Cabot的
Figure A200780029796D00122
和得自Tokuyama的
Figure A200780029796D00123
沉淀二氧化硅通过在搅拌下碱性硅酸盐(例如硅酸钠)与无机酸(例如硫酸)反应而由水溶液形成。通过该方法形成的初级颗粒通常尺寸为3～50nm。这些初级颗粒可以随后聚集形成更大的微米尺寸颗粒。沉淀二氧化硅的比表面积通常为50～500m2/g。可商购获得的沉淀二氧化硅的实例包括得自PPG Industries的
Figure A200780029796D00124
以及得自Tokuyama的
Figure A200780029796D00125
和
Figure A200780029796D00126
热解二氧化硅和沉淀二氧化硅具有轻质、松软状白色粉末的外观。它们的小粒径使得它们能够吸收和保留足够量的胺同时保持自由流动粉末特性而无结块。热解二氧化硅和沉淀二氧化硅的另一个优点是它们的无毒性。该无毒性使得它们能够用于食品加工中，例如作为粉状食品例如代乳品中的防结块添加剂，和用于化妆品中，例如牙膏中的研磨材料。热解和沉淀二氧化硅通常是亲水的，但可以将它们的表面处理以制得疏水性的二氧化硅。亲水性和疏水性的二氧化硅以及其他改性的二氧化硅均适合用作根据本发明的纳米结构化的胺载体。
适用于本发明的胺吸着剂中的其他纳米结构化的材料包括热解或沉淀氧化物，例如热解氧化铝、热解氧化锆和热解氧化钛、沉淀氧化铝、沉淀氧化钛、沉淀氧化锆、硅酸钙、碳纳米管、和其混合物。
该负载型胺吸着剂可以通过浸渍或通过另外的常规技术制备。例如，当采用浸渍时，将所述纳米结构化的载体材料混合或分散在合适的溶剂中并且通过搅拌保持作为悬浮液。通过将所述胺完全溶于所述溶剂中而制备单独的胺溶液。然后在搅拌下将所述纳米结构化的载体和所述胺溶液合并。优选地，将所述胺溶液滴加到所述载体的悬浮液中以确保胺在载体表面上的优良分散。然后除去所述溶剂以形成负载型胺吸着剂。所得的胺吸着剂可以就这样使用或者可被粉碎和筛分以获得均匀的粉末。
可以加入多元醇以增强负载型胺吸着剂的吸收/解吸特性。当使用多元醇时，可以将多元醇与所述胺溶液一起混合并且加入所述载体的悬浮液中。也可以将多元醇单独溶于所述溶剂中并且与所述载体的悬浮液合并。在该情况下，优选首先将该多元醇溶液加入所述载体的悬浮液中，和然后除去所述溶剂而获得负载型多元醇物质。然后将得到的固体分散在所述溶剂中并在搅拌下加入所述胺在所述溶剂中的溶液。最后除去溶剂以形成负载型胺/多元醇吸着剂。所述吸着剂可以就这样使用或者可被粉碎和筛分以获得均匀的粉末。
可以使用能够溶解但不与所述胺和所述多元醇反应的任何溶剂。该溶剂应该优选容易地通过温和加热和/或真空从所述吸着剂中被分离。优选的溶剂包括但不限于醇，所述醇可以溶解胺和多元醇和可以容易地从吸着剂中被除去。例如可以使用甲醇、乙醇和异丙醇、和它们的各种混合物。
用于制备根据本发明的胺负载型吸着剂的方法廉价并且容易进行，更制得了优于通过以前已知的方法制备的吸着剂的吸着剂。
有利地，本发明获得了宽范围的CO2吸收能力用于多种天然和工业气源。吸收可以在多种条件下例如在0～100℃的温度范围内，和以任何合适的方式例如在规则流动体系中或者在固定、移动或流化的吸收床中进行。所述吸着剂俘获CO2的能力可以通过热重分析(TGA)测量吸收作用或者通过在静态条件下测量CO2吸收作用来说明。
一旦大量的胺例如约70～90％与CO2复合，则可以再生所述吸着剂。本文中使用的术语“再生”或“再生的”被理解为是指通过使被吸收的气体从所述吸着剂中释放或解吸，所述吸着剂可被重新使用。通过用实现所述释放的任何方法例如加热、降低的压力、真空、气体清洗和其组合来处理所述吸着剂而释放被吸收的气体。因此，通过多个吸收-解吸循环，根据本发明的被再生的吸着剂可以重复使用。在一个实例中，即使在重复的吸收-解吸循环之后，所述吸着剂也保持了其吸收效率。优选地，对于许多吸收-解吸循环而言，所述吸着剂保持其吸收效率。便利的是使用平行的吸收床，其使得吸收和解吸/再生能够连续进行。
例如对于CO2吸着剂而言，所述再生是吸热的，因此通过使吸着剂经受升高的温度(例如通过在约25℃～约120℃的温度下加热吸着剂)、降低的压力(例如通过变压吸附PSA)、气体清洗、真空、贫吹扫气或它们的任意组合而释放被吸收的CO2。再生处理使得与吸着剂的胺复合的基本上大部分的CO2被释放。CO2然后可以任何所希望的方式储存或使用，并且不含CO2(再生)的吸着剂被重新用于另外的CO2吸收-解吸循环中。
CO2的用途和反应包括上面提及的那些并且进一步披露于2006年8月10日提交的共同悬而未决的美国专利申请No.60/837,273中，该申请的整个内容通过引用并入本文。
根据本发明的吸着剂是热稳定的并且在吸收操作的温度和/或压力范围内不会释放负载型胺。另外，由于其在可容易地在所述过程中保持的温度范围内能够再生和有效地操作，因此除了用于CO2俘获和分离的高选择性和能力之外，该吸着剂对于提供高效率和长寿命而言是成本有效的。由于其灵活性和通用性，因此该吸着剂也可有利地用于处理来自多种来源的大量的含CO2的气体。
实施例
以下实施例仅仅是说明性的并且不应被解释为限制本发明的范围。
实施例I.负载型胺吸着剂的制备
该实施例说明了由50wt％聚乙烯亚胺和50wt％具有7nm平均初级粒径和390m2/g+/-40m2/g比表面积的热解二氧化硅组成的负载型胺吸着剂的制备。
将聚乙烯亚胺(25,000的分子量Mw)4g溶于25mL甲醇中。然后在搅拌下将该溶液滴加到悬浮在100mL甲醇中的4g热解二氧化硅中以确保聚乙烯亚胺在载体上良好分散。将该混合物再搅拌1小时，并且然后通过在50℃下在真空下在旋转蒸发器(rotovap)上加热随后过夜真空(<1mmHg)而将所述溶剂从该混合物中除去。得到的负载型胺吸着剂是白色固体，然后将其粉碎和筛分而制得均匀的粉末。
实施例II.负载型胺/多元醇吸着剂的制备
该实施例说明了由45wt％聚乙烯亚胺、10wt％聚乙二醇和45wt％具有7nm平均初级粒径、390m2/g+/-40m2/g比表面积的热解二氧化硅组成的负载型胺/多元醇吸着剂的制备。
将聚乙二醇(400的分子量Mw)2g溶于25mL甲醇中。然后在搅拌下将该溶液滴加到悬浮在200mL甲醇中的9g热解二氧化硅中以确保聚乙二醇在载体上良好分散。然后将该混合物再搅拌1小时。然后通过在50℃下在真空下在旋转蒸发器上加热随后过夜真空(<1mmHg)而将所述溶剂从该混合物中除去。得到的多元醇/载体是白色粉末，其被粉碎和筛分。
将5.5g得到的多元醇/载体与50mL甲醇混合。向该混合物中滴加溶于50mL甲醇中的4.5g聚乙烯亚胺(25,000的分子量Mw)以确保聚乙烯亚胺在多元醇/载体上良好分散。然后在有力搅拌下将该溶液再混合1小时。然后通过在50℃下在真空下在旋转蒸发器上加热随后过夜真空(<1mmHg)而将所述溶剂从该混合物中除去。得到的负载型胺/多元醇吸着剂是白色粉末，其被粉碎和筛分而制得均匀的粉末。
实施例III.负载型胺/多元醇吸着剂的制备
使用描述于实施例II的相同步骤制备由47.5wt％聚乙烯亚胺(25,000的分子量Mw)、10wt％聚乙二醇(400的分子量Mw)和42.5wt％具有7nm平均初级粒径的热解二氧化硅组成的吸着剂。得到的多元醇/胺负载型吸着剂是白色固体，其被磨碎和筛分而制得均匀的粉末。该粉末具有优良的流动特性。
实施例IV.使用静态***测量CO2吸收能力
使用由与气体输送和真空***相连的玻璃管组成的设备获得CO2吸收数据。使含CO2的气体通过预先称量量的根据本发明制备的吸收剂。监控吸收剂的重量增加直到饱和，即直到没有进一步的重量增加。由重量增加确定CO2吸收率。通过在80～110℃下在真空(<1mmHg)下将样品加热1小时而实现CO2的解吸。通过监控重量减少来确定解吸能力。
用一些吸收剂得到的吸收测量值概述于表1中。
表1.在静态条件下的CO2吸收能力测量值
 
吸收剂(重量比例) 吸收温度(℃) CO2吸收率(mgCO2/g吸收剂)
纳米结构化的热解二氧化硅负载的
热解二氧化硅/PEI(LMW)(50/50)热解二氧化硅/PEI(LMW)(50/50)疏水性热解二氧化硅/PEI(HMW)(50/50)热解二氧化硅/PEI(HMW)/PEG(45/45/10)热解二氧化硅/PEI(HMW)/PEG(42.5/47.5/10)热解二氧化硅/五亚乙基六胺(50/50)热解二氧化硅/四亚乙基五胺(50/50) 70858527278585 144146133142148181197
纳米结构化的沉淀二氧化硅负载的
沉淀二氧化硅/PEI(LMW)(50/50)沉淀二氧化硅/PEI(LMW)(50/50)沉淀二氧化硅/PEI(HMW)(50/50)沉淀二氧化硅/PEI(HMW)(50/50)沉淀二氧化硅/PEI(线型)(50/50)沉淀二氧化硅/五亚乙基六胺(50/50)沉淀二氧化硅/四亚乙基五胺(50/50) 70855070707070 144149110130178185195
PEI(HMW)：分子量Mw约25,000的聚乙烯亚胺
PEI(LMW)：分子量Mw约800的聚乙烯亚胺
PEG：Mn约400的聚乙二醇
实施例V.使用热重分析仪测量CO2吸收能力
使用热重分析仪(Shimadzu TCA-50)获得CO2吸收数据。将粉末状吸收剂(5～20mg)装入铂坩锅中并且放在仪器天平上。然后在所希望的温度下，通常为90～110℃下在氮气流下将所述固体吸收剂预处理1小时。随后将样品冷却至所希望的吸收温度并且将气流转换成CO2或者CO2与其他气体(例如N2、O2、天然气等)以不同比例的混合物。随着时间记录样品质量的变化以确定CO2吸收能力。对于根据实施例III制备的吸收剂(47.5wt％PEI、10wt％PEG和42.5wt％热解二氧化硅)，用该方法获得的吸收测量值的实例概述于表2中。
表2.由47.5％PEI、10％PEG和42.5％纳米结构化的热解二氧化硅1组成的吸收剂使用热重分析仪在50℃下的CO2吸收能力测量值
 
气体组成 CO2吸收率(mgCO2/g吸收剂)
100％CO2 140
在N2中的10％CO2 92
在空气(80％N2，20％O2)中的370ppmCO2(0.0370％) 27
1PEI：分子量Mw约25,000的聚乙烯亚胺
PEG：Mn约400的聚乙二醇
实施例VI.重复的吸收-解吸循环
使实施例III的固体吸着剂进行多个吸收和解吸循环，并且使用描述于实施例IV中的静态试验条件测量吸收-解吸循环(在室温下用纯的二氧化碳吸收3分钟，在110℃下解吸10分钟)。在10个吸收-解吸循环之后，吸收剂的CO2吸收能力保持不变(参见表3)。数据表明根据本发明的吸着剂能够进行多个重复的吸收-解吸循环而不出现降低的吸收能力，并且可以良好地历经10个吸收-解吸循环使用。
表3.重复的CO2吸收-解吸循环
 
循环 1 2 3 4 5 6 7 8 9 10
吸收能力(mgCO2/g吸收剂) 105 106 114 113 112 115 116 118 117 117

Claims (27)

1.一种用于从气体混合物中吸收二氧化碳的固体吸着剂，其包含胺和纳米结构化的固体载体。
2.根据权利要求1的吸着剂，其中所述纳米结构化的固体载体具有小于约100nm的初级粒径。
3.根据权利要求1的吸着剂，其中所述纳米结构化的载体是纳米二氧化硅、二氧化硅-氧化铝等、热解或沉淀氧化物、硅酸钙、碳纳米管、或其混合物。
4.根据权利要求1的吸着剂，其中所述胺是伯、仲或叔胺或烷醇胺、芳胺、或者其混合物或组合。
5.根据权利要求1的吸着剂，其中所述胺是单乙醇胺(MEA)、二乙醇胺(DEA)、甲基二乙醇胺、2-(2-氨基乙基氨基)-乙醇、二异丙醇胺、2-氨基-2-甲基-1，3-丙二醇、三乙醇胺、四亚乙基五胺、五亚乙基六胺或聚乙烯亚胺。
6.根据权利要求5的吸着剂，其中所述胺是分子量大于600的线型或支化聚乙烯亚胺。
7.根据权利要求1的吸着剂，其中所述胺以所述吸着剂的约25～75wt％的量存在。
8.根据权利要求1的吸着剂，其进一步包含用量为所述吸着剂的至多约25wt％的多元醇。
9.根据权利要求8的吸着剂，其中所述多元醇选自甘油、乙二醇的低聚物、聚乙二醇、聚环氧乙烷、和其醚、改性物和混合物。
10.根据权利要求1的吸着剂，其中所述纳米结构化的载体是纳米二氧化硅，所述胺是用量为所述吸着剂的约25～75wt％的聚乙烯亚胺，和所述吸着剂进一步包含用量为所述吸着剂的至多25wt％的聚乙二醇。
11.根据权利要求1的吸着剂，其当被处理用于再生时能够释放被吸收的二氧化碳。
12.根据权利要求11的吸着剂，其中用足够的热量、降低的压力、真空、气体清洗或它们的组合处理所述吸着剂以释放显著量或全部的被吸收的二氧化碳。
13.一种制备权利要求1的吸着剂的方法，其包括将所述纳米结构化的载体分散在溶剂中以形成悬浮液；将所述胺溶解在所述溶剂中以形成胺溶液；将所述悬浮液和所述胺溶液合并；和除去所述溶剂以形成吸着剂。
14.根据权利要求13的方法，其进一步包括在将所述胺溶液和所述悬浮液合并之前将多元醇加入所述胺溶液或所述悬浮液中。
15.根据权利要求13的方法，其进一步包括将多元醇加入所述悬浮液中；在加入多元醇之后将所述悬浮液干燥以形成负载型多元醇；将所述负载型多元醇分散在所述溶剂中；和在除去所述溶剂以形成吸着剂之前将所述被分散的负载型多元醇和所述胺溶液合并。
16.一种用吸着剂从气体混合物中连续俘获和分离二氧化碳的方法，其包括将根据权利要求1的吸着剂暴露于所述气体混合物以通过该吸着剂进行二氧化碳的吸收，和处理包含被吸收或俘获的二氧化碳的吸着剂以释放所述二氧化碳。
17.根据权利要求16的方法，其中所述吸着剂被提供在固定、移动或流化床中和所述气体与床接触足够的时间以将所述二氧化碳俘获在所述吸着剂中。
18.根据权利要求16的方法，其中用足够的热量、降低的压力、真空、气体清洗或它们的组合处理所述吸着剂以释放被吸收的二氧化碳。
19.根据权利要求18的方法，其中当至多90％的所述胺与二氧化碳复合时处理所述吸着剂。
20.根据权利要求16的方法，其进一步包括将被释放的二氧化碳反应以形成有用的制品。
21.根据权利要求20的方法，其中通过以下方式使用二氧化碳制备甲醇：(a)将二氧化碳在水中电化学还原或(b)在足以产生中间化合物的条件下还原二氧化碳和在足以形成甲醇的条件下用氢气将所述中间化合物催化加氢。
22.根据权利要求21的方法，其中所述中间化合物是甲酸甲酯。
23.根据权利要求20的方法，其进一步包括在足以产生一氧化碳的条件下还原二氧化碳，在足以得到甲酸甲酯的条件下使所述一氧化碳与甲醇反应，和在足以产生甲醇的条件下将所述甲酸甲酯催化加氢。
24.根据权利要求20的方法，其进一步包括在足以产生二甲醚的条件下将所述甲醇脱水。
25.根据权利要求24的方法，其进一步包括在足以形成乙烯和/或丙烯的条件下在酸性-碱性或沸石催化剂的存在下加热所述二甲醚。
26.根据权利要求25的方法，其进一步包括在足以产生高级烯烃、合成烃、芳族物质或由其制得的制品的条件下转化所述乙烯和/或丙烯，从而用作化学品的原料或用作运输燃料。
27.根据权利要求25的方法，其进一步包括在足以形成乙醇或丙醇的条件下将所述乙烯或丙烯水合。
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