CN102046269A - 包含金属硫化物的流通式吸着剂 - Google Patents

包含金属硫化物的流通式吸着剂 Download PDF

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Publication number
CN102046269A
CN102046269A CN2009801209384A CN200980120938A CN102046269A CN 102046269 A CN102046269 A CN 102046269A CN 2009801209384 A CN2009801209384 A CN 2009801209384A CN 200980120938 A CN200980120938 A CN 200980120938A CN 102046269 A CN102046269 A CN 102046269A
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China
Prior art keywords
sorbent
flow type
type sorbent
mixture
metal sulfide
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CN2009801209384A
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K·P·加德卡里
刘安波
J·F·麦齐
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Corning Inc
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Corning Inc
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Publication of CN102046269A publication Critical patent/CN102046269A/zh
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Abstract

本发明提供一种流通式吸着剂，该吸着剂包含至少30重量％的金属硫化物和粘结剂。该吸着剂可用于例如除去流体流中的污染物，例如汞。

Description

包含金属硫化物的流通式吸着剂
相关申请交叉参考
本申请要求于2008年5月30日提交的美国申请第12/129,798号的优先权，其内容通过参考结合于此。
发明领域
本发明涉及某些包含金属硫化物的流通式吸着剂。该吸着剂可用于例如除去流体流中的污染物，例如汞。
背景技术
有害污染物排放已经成为日益受到关注的环境问题，因为它们威胁人类健康。例如，燃煤发电厂和医疗废弃物焚烧是与人类活动相关的排放到大气中的汞的主要来源。
据估计，每年从美国燃煤发电厂排放的汞有48吨。美国能源部能量信息管理局的一份年度能量展望报告(DOE-Energy Information Administration annual energy outlook)提出，随着燃煤发电容量的增加，用于发电的煤耗将从2002年的9亿7600万吨增加到2025年的14亿7700万吨。但是，对燃煤发电厂还没有严格地执行汞排放控制法规。主要原因在于缺乏能以合理成本操作的有效控制技术，特别是对于元素汞的控制。
目前用于控制元素汞以及氧化的汞的技术是活性炭注入(ACI)。ACI方法涉及将活性炭粉末注入到废气流中，使用织物过滤器或静电沉淀器来收集带有吸着的汞的活性炭粉末。ACI技术通常需要高C∶Hg比来实现所需的汞去除水平(＞90％)，这导致吸着材料占据很大一部分成本。高C∶Hg比表明ACI没有充分利用碳粉末的汞吸着能力。
活性炭填充床可实现高汞去除水平，更有效地利用吸着材料。但是，典型的粉末或颗粒填充床具有极高的压降，这将明显降低能效。此外，这些固定床通常是一种中断型技术，因为它们需要根据材料的吸着能力频繁地更换吸着材料。
US 2007/0261557所揭示的活性炭蜂窝体可以用来以高去除水平除去污染物，例如有毒的金属。本发明人已经发现了用于流通式吸着剂如蜂窝体的新材料，见下文所述。
实施方式详述
本发明的一个实施方式是一种流通式吸着剂，其包含：
至少30重量％的金属硫化物；和
粘结剂。
示例性的流通式吸着剂包括例如任何包含通道、多孔网或任何其它通路的结构，该结构允许流体流流过该吸着剂。例如，流通式吸着剂可以为整体型结构，或者是按一定形式排列的互连结构，流体流可以通过这样的结构。流通式吸着剂可以是包含入口端、出口端以及从所述入口端延伸到所述出口端的多条孔道的蜂窝体吸着剂，所述孔道由交叉的多孔孔道壁限定。蜂窝体吸着剂可任选地包含一个或多个选择性堵塞的蜂窝体孔道端，以提供能使流体流和孔道壁之间更紧密地接触的壁流通式结构。
流通式吸着剂包含至少30重量％的金属硫化物。例如，流通式吸着剂可包含至少35重量％、至少40重量％、至少45重量％、至少50重量％、至少55重量％、至少60重量％、至少65重量％、至少70重量％、至少75重量％或至少80重量％的金属硫化物。金属硫化物的重量百分数是以吸着剂体的总重量为基准计算的，可使用任何合适的分析技术如质谱来测定。
示例性的金属硫化物包括锰、铜、钯、钼或钨的硫化物，以及它们的组合。但是，金属硫化物中的金属元素不限于这些例子。例如，金属硫化物中的金属元素可选自碱金属、碱土金属、过渡金属、稀土金属(包括镧系金属)和其它金属，例如铝、镓、铟、锡、铅、铊和铋。金属硫化物的重量百分数包括吸着剂中所有金属硫化物的重量百分数。
粘结剂可以是无机粘结剂、有机粘结剂或无机粘结剂和有机粘结剂的组合。粘结剂通过与金属硫化物或其它粘结剂材料熔合以及/或者通过形成金属硫化物分散在其中的基质而为吸着剂提供机械完整性。
示例性的无机粘结剂包括氧化物、硫酸盐、碳酸盐和磷酸盐，例如金属或半金属如硅和锗的氧化物、硫酸盐、碳酸盐和磷酸盐。例如，滑石、粘土(例如膨润土粘土)和巴黎石膏可用作无机粘结剂。在一些实施方式中，流通式吸着剂包含最多达70重量％、60重量％、50重量％、40重量％、30重量％、20重量％或10重量％的无机粘结剂，例如氧化物、硫酸盐或碳酸盐或它们的组合。
本发明的流通式粘结剂可包含有机粘结剂。在本发明中，术语“有机粘结剂”不仅包括有机化合物，而且如果这类化合物已经因为暴露于碳化或煅烧条件(例如高温)而被碳化或者煅烧，则该术语还包括这类化合物的碳残余物。因此，当称一具体材料为“有机粘结剂”时，包括该材料以及该材料的碳化或煅烧残余物。在一些实施方式中，流通式吸着剂包含最多达70重量％、60重量％、50重量％、40重量％、30重量％、20重量％或10重量％的有机粘结剂，或者最多达70重量％、60重量％、50重量％、40重量％、30重量％、20重量％或10重量％的有机粘结剂和无机粘结剂的组合。
示例性的有机粘结剂包括纤维素化合物。纤维素化合物包括纤维素醚，例如甲基纤维素、乙基羟基乙基纤维素、羟丁基纤维素、羟丁基甲基纤维素、羟乙基纤维素、羟甲基纤维素、羟丙基纤维素、羟丙基甲基纤维素、羟乙基甲基纤维素、羧甲基纤维素钠和它们的混合物。甲基纤维素粘结剂的一个例子是陶氏化学公司(Dow Chemical Company)出售的METHOCEL A。羟丙基甲基纤维素粘结剂的例子包括也是由陶氏化学公司出售的METHOCEL E，F，J，K。同样由陶氏化学公司出售的METHCEL 310系列的粘结剂也可用于本发明中。METHOCEL A4M是可与RAM挤出机配套使用的粘结剂的例子。METHOCEL F240C是可与双螺杆挤出机配套使用的粘结剂的例子。
示例性的有机粘结剂还包括有机树脂。有机树脂包括热固性树脂和热塑性树脂(例如聚偏二氯乙烯，聚氯乙烯、聚乙烯醇等)。可使用合成的聚合物材料，例如酚醛树脂或糠醇基树脂，如呋喃树脂。合适的酚醛树脂的例子是可熔酚醛树脂，例如普力芬(plyophen)树脂。一种合适的呋喃液体树脂的例子是美国印第安纳州QO化学品公司的Furcab-LP(Furcab-LP，QO Chemicals Inc.，IN，U.S.A.)。示例性的固体树脂是固体酚醛树脂或酚醛清漆树脂。在本发明的流通式吸着剂中，任何有机树脂粘结剂可以是未固化的、固化的或者碳化的。
除了金属硫化物和粘结剂外，流通式吸着剂可包含任何其它合适的材料。例如，除了金属硫化物中存在的硫外，吸着剂可包含硫。该额外的硫可包括任何氧化态的硫，包括元素硫(0)、硫酸盐(+6)和亚硫酸盐(+4)。因此，术语“硫”包括元素硫或者以化合物或化学组成部分存在的硫。
可通过任何合适的技术制备流通式吸着剂。在一个实施方式中，可通过一种方法制备吸着剂，该方法包括：
提供一种混合物，该混合物包含：
金属硫化物，或者1)金属氧化物或金属硫化物与2)额外硫源的组合，和
无机粘结剂；
使该混合物成形为流通式结构的形状，例如通过挤出实现该操作；和
干燥该成形的结构，还任选地进行额外的烧制处理。
金属硫化物和无机粘结剂可以是上文所述的任何金属硫化物或无机粘结剂。在金属氧化物作为与额外硫源的混合物提供的实施方式中，这两种物质在暴露于高温(例如烧制温度)时可能反应形成金属硫化物。金属氧化物中示例性的金属包括上述可形成金属硫化物的任何金属。未反应的金属氧化物可仍然作为无机粘结剂。
额外的硫源可以是元素态或氧化态形式的任何硫源。该硫源包括硫粉、含硫粉末状树脂、硫化物、硫酸盐和其它含硫化合物，以及其中任何两种或更多种的混合物或组合。示例性的含硫化合物包括硫化氢和/或其盐、二硫化碳、二氧化硫、噻吩、三氧化硫、卤化硫、硫酸酯、亚硫酸、硫磺酸、二甲基硫蒽(sulfatol)、氨基磺酸、液体三氧化硫(sulfan)、硫烷、硫酸和其盐、亚硫酸盐、磺酸、二苯砜和它们的混合物。
成形的结构可以进行干燥，例如在75-200℃的环境中干燥。还可以对成形的结构进行烧制，通过烧结和/或形成金属硫化物分散在其中的基质来增强该结构的机械完整性，例如无机粘结剂与金属硫化物或其它粘结剂材料的粘附性。烧制条件也可以煅烧或碳化该结构中存在的任何有机粘结剂，例如纤维素化合物。
示例性的烧制条件包括在受控的气体环境中，以例如0.5-2℃/分钟的加热速率在900℃-1500℃烧制0.5-10小时。在另一个实施方式中，烧制过程可以在空气或者氮气和氧气的混合物中，在1100-1300℃进行20-45小时。在另一个实施方式中，可以将结构例如在600℃或更高的温度加热，以煅烧任何有机粘结剂，然后在更高的温度进行烧制，实现无机粘结剂材料的烧结。
制备流通式吸着剂的另一种技术包括具有以下步骤的方法：
提供一种混合物，该混合物包含：
金属硫化物，
任选的额外的硫源，和
可固化的有机粘结剂，例如有机树脂；
使该混合物成形为流通式结构的形状，例如通过挤出实现该操作；和
干燥该成形的结构，还任选地固化该成形的结构。
金属硫化物、额外的硫源和可固化的有机粘结剂的特征在前文中已经进行了描述。固化可以例如在空气中、在大气压下进行，通常将结构在70℃-200℃的温度加热约0.5-5.0小时。在一些实施方式中，将结构分阶段从低温加热到更高的温度，例如从70℃，到90℃，到125℃，到150℃，每个温度保持一段时间。另外，也可通过在室温下加入固化添加剂(例如酸添加剂)来实现固化。
上述任一方法中的混合物还可任选地包含成形助剂。示例性的成形助剂包括肥皂，脂肪酸如油酸、亚油酸，硬脂酸钠等，聚氧乙烯硬脂酸酯等，以及它们的组合。可用于改善该批料的挤出和固化特性的其他添加剂是磷酸和油。示例性的油包括分子量约为250-1000，包含石蜡族和/或芳族和/或脂环族化合物的石油。一些有用的油是3M公司(3M Co.)的三合一油，或者是新泽西州韦恩市的RC公司(Reckitt and Coleman Inc.，Wayne，N.J.)的三合一家用润滑油。其他有用的油可包括基于聚(α-烯烃)、酯、聚亚烷基二醇、聚丁烯、硅酮、聚苯基醚、CTFE油和其他市售油的合成油。也可使用植物油，例如葵花籽油、芝麻油、花生油、豆油等。
流通式吸着剂可用于吸着流体中的任何污染物。例如，流体可通过流通式吸着剂，例如上文讨论的蜂窝体整体型吸着剂。流体的形式可以为气体或液体。气体或液体还可包含其它相，例如在气体或液体流中的固体微粒，或者在气体流中的液滴。气体流的例子包括燃煤废气(例如来自烟煤和亚烟煤类或褐煤)，以及在煤的气化过程中产生的合成气流。
术语“吸着”、“吸着性”和“吸着的”指吸附、吸收或其它以物理、化学或物理和化学方式在吸着剂上捕集污染物的过程。
待吸着的污染物包括例如在流体流中等于或小于3重量％的污染物，例如等于或小于2重量％，或者等于或小于1重量％。污染物还可包括例如在流体流中等于或小于10,000微克/米3的污染物。污染物的例子包括金属，包括毒性金属。术语“金属”和本文对具体金属或其它污染物的任何指称包括金属或其它污染物的元素形式以及氧化态。因此，金属或其它名称的污染物的吸着包括吸着元素形式的金属或其它污染物，以及吸着包含该金属或其它污染物的任何有机或无机化合物或组合物。
可被吸着的金属的例子包括镉、汞、铬、铅、钡、铍，以及包含这些元素的化合物或组合物。在一个实施方式中，金属是元素形式(Hgo)或氧化态形式(Hg+或Hg2+)的汞。氧化的汞的例子包括HgO和卤化汞，例如Hg2Cl2和HgCl2。其它示例性的金属污染物包括镍、钴、钒、锌、铜、锰、锑、银和铊，以及包含它们的有机或无机化合物或组合物。其它污染物包括元素态和任何氧化态形式的砷和硒，包括包含砷或硒的有机或无机化合物或组合物。
污染物可以是能吸着在流通式吸着剂上的任何相。因此，例如，污染物可以作为在气体流体流中的液体存在，或者作为在液体流体流中的液体存在。或者，污染物可以作为在气体流体流或液体流体流中的气相污染物存在。在一个实施方式中，污染物是煤燃烧产生的废气或合成气流中的汞蒸汽。
下面参照以下非限制性实施例进一步描述本发明。
实施例1
将二氧化锰(61.5重量％)、滑石(21.5重量％)、硫(9.1重量％)、甲基纤维素(6.9重量％)和作为润滑剂的硬脂酸钠(1重量％)与水混合，研磨，得到可挤出的批料。将该批料通过壁厚度为17密耳的100cpsi模具挤出。得到品质极佳的挤出件。然后将该挤出样品在1)空气和2)氮气中，在900-1000℃烧制，得到品质良好的蜂窝体。
实施例2
将硫化锰(61.5重量％)、滑石(23重量％)、甲基纤维素粘结剂(7重量％)和硬脂酸钠(1重量％)与水在研磨机中混合，形成可挤出的糊料。然后，将该糊料通过100cpsi模具挤出，得到含有无机粘结剂和有机粘结剂的硫化锰蜂窝体结构。与实施例1一样，得到极佳的挤出结构。
实施例3
重复实施例2的实验，但是用硫化铜代替硫化锰，得到良好的挤出结构。
实施例4
重复实施例1的实验，不同的是加入酚醛树脂粘合剂代替滑石。挤出后，对蜂窝体进行干燥和固化，而不是进行烧制。
应当理解，虽然就某些说明性实施方式详细描述了本发明，但是应该认为本发明不限于这些具体实施方式，在不背离所附权利要求书所限定的本发明精神和范围的前提下，可以对列举的实施方式进行各种可能的修改。

Claims (20)

1.一种流通式吸着剂，其包含：
至少30重量％的金属硫化物；和
粘结剂。
2.如权利要求1所述的流通式吸着剂，其特征在于，所述金属硫化物是锰、铜、钯、钼或钨的硫化物。
3.如权利要求1所述的流通式吸着剂，其特征在于，所述粘结剂是无机粘结剂。
4.如权利要求3所述的流通式吸着剂，其特征在于，所述无机粘结剂包括氧化物、硫酸盐、碳酸盐或磷酸盐。
5.如权利要求4所述的流通式吸着剂，其特征在于，所述无机粘结剂包括金属的氧化物、硫酸盐、碳酸盐或磷酸盐。
6.如权利要求5所述的流通式吸着剂，其特征在于，所述无机粘结剂包括滑石或粘土。
7.如权利要求1所述的流通式吸着剂，其特征在于，所述粘结剂是有机粘结剂。
8.如权利要求7所述的流通式吸着剂，其特征在于，所述有机粘结剂包括纤维素化合物或有机树脂。
9.如权利要求8所述的流通式吸着剂，其特征在于，所述有机粘结剂包括甲基纤维素或固化的酚醛树脂。
10.如权利要求1所述的流通式吸着剂，其特征在于，所述吸着剂包含无机粘结剂和有机粘结剂。
11.如权利要求1所述的流通式吸着剂，其特征在于，除了金属硫化物中存在的硫外，所述吸着剂还包含硫。
12.如权利要求11所述的流通式吸着剂，其特征在于，所述吸着剂包含元素硫。
13.如权利要求1所述的流通式吸着剂，其特征在于，所述吸着剂的形式为整体型。
14.如权利要求1所述的流通式吸着剂，其特征在于，所述吸着剂的形式为蜂窝体。
15.一种制备如权利要求1所述的流通式吸着剂的方法，该方法包括：
提供一种混合物，该混合物包含：
金属硫化物，或者1)金属氧化物或金属硫化物与2)额外的硫源的组合，和
无机粘结剂；
使所述混合物成形为流通式结构的形状；和
干燥该成形的结构，还任选地烧制该成形的结构。
16.如权利要求15所述的方法，其特征在于，所述混合物包含元素硫作为额外的硫源。
17.如权利要求15所述的方法，其特征在于，该方法包括通过挤出使所述混合物成形为流通式结构的形状。
18.一种制备如权利要求1所述的流通式吸着剂的方法，该方法包括：
提供一种混合物，该混合物包含：
金属硫化物，
任选的额外的硫源，和
可固化的有机粘结剂；
使所述混合物成形为流通式结构的形状；和
干燥该成形的结构，还任选地固化该成形的结构。
19.如权利要求18所述的方法，其特征在于，所述混合物包含元素硫作为额外的硫源。
20.如权利要求18所述的方法，其特征在于，该方法包括通过挤出使所述混合物成形为流通式结构的形状。
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