CN107787249A - 制备吸着剂的方法 - Google Patents

制备吸着剂的方法 Download PDF

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CN107787249A
CN107787249A CN201680032432.8A CN201680032432A CN107787249A CN 107787249 A CN107787249 A CN 107787249A CN 201680032432 A CN201680032432 A CN 201680032432A CN 107787249 A CN107787249 A CN 107787249A
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sorbent
copper
calcining
copper sulfide
particulate
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CN107787249B (zh
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M·J·伊万斯
M·D·G·卢恩
M·G·帕特瑞治
C·J·杨
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Johnson Matthey PLC
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Abstract

描述了一种制备吸着剂的方法，该方法包括以下步骤：(i)将硫化铜材料微粒与经煅烧的、可再水合的氧化铝微粒混合在一起，(ii)使混合物成形，和(iii)将成形的混合物干燥，以形成经干燥的吸着剂。

Description

制备吸着剂的方法
本发明涉及制备吸着剂的方法，特别是制备包含硫化铜的吸着剂的方法。
含有硫化铜的吸着剂可以用来从流体料流中除去重金属。在流体料流如烃或其他气体和液体料流中少量存在重金属如汞。烃料流中还可能少量存在砷和锑。除了它的毒性之外，汞还可能造成铝热交换器和其他工艺设备的失灵。所以，需要有效地从流体料流中除去这些金属，优选在工艺流程中尽可能早地除去。
吸着剂中常规地形成硫化铜，或者通过含有可硫化的铜化合物的吸着剂前体与流体料流中存在的硫化氢(H2S)反应来原位形成，或者通过同样用硫化氢来预硫化吸着剂前体。对于氧化铜，该反应描述如下：
CuO+H2S→CuS+H2O
类似地，当使用碱式碳酸铜材料时，形成CO2和H2O。
WO2009/101429公开了一种制造吸收剂的方法，其包括以下步骤：(i)形成组合物，该组成物包含能够形成硫化铜的铜化合物微粒，载体材料微粒，和一种或多种粘结剂，(ii)使该组合物成形以形成吸收剂前体，(iii)干燥该吸收剂前体材料，和(iv)硫化该前体以形成该吸收剂。用来硫化吸收剂前体的硫化剂可以是一种或多种硫化合物，如硫化氢、硫化羰、硫醇和多硫化物或者这些的混合物。优选硫化氢。
据信铜化合物的转化是必须的，以提供具有适合的物理性质和对重金属的有效容量的吸着剂。但是，使用这些硫化剂的硫化方法如果不加仔细控制，会导致不均匀的产品和受损的物理性质。并且，硫化氢是有毒的气体，对于大规模硫化需要控制措施。所以，需要寻找替代方法，其本质上更安全、更简单，并且提供改进的产品均匀性。
还需要改进产品的物理性质，尤其是压碎强度，目前这依赖于使用一种或多种粘结剂。
已经发现，将载体材料微粒和粘结剂的组合用经煅烧的、可再水合的氧化铝微粒替换，改进了吸着剂性质。
所以，本发明提供一种制备吸着剂的方法，该方法包括以下步骤：
(i)将硫化铜材料微粒与经煅烧的、可再水合的氧化铝微粒混合在一起，
(ii)使混合物成形，和
(iii)将成形的混合物干燥，以形成经干燥的吸着剂。
本发明进一步提供一种能够通过该方法获得的吸着剂，和该吸着剂在从含重金属的流体料流中除去重金属如汞、砷、硒、镉和锑中的用途。
“吸着剂”包括吸收剂和吸附剂。
“经煅烧的、可再水合的氧化铝”是指经煅烧的无定形或结晶差的过渡氧化铝包括ρ-、χ-和假γ-氧化铝中的一种或多种。这样的氧化铝能够再水合，并且能够在反应性形式中保留大量水。经煅烧的、可再水合的氧化铝可商购，例如以“CP alumina powders”获自BASF AG。它们可以通过将三水铝矿(Al(OH)3)研磨到1-20μm粒度，再在短的接触时间内闪速煅烧来制备，如美国专利2,915,365中所述。除了三水铝矿之外，无定形氢氧化铝和其他天然存在的矿物晶体氢氧化物如三羟铝石和新三水氧化铝，或一氧化氢氧化物如勃姆石(AlOOH)和水铝石也可以用作经煅烧的、可再水合的氧化铝的来源。
用来制备吸着剂的硫化铜微粒可以是商业来源，或者可以通过多种方法来制备。适合的方法包括用单质硫焙烧铜或铜化合物，溶剂热(solvothermal)过程，水热过程(例如微波辐射)，电沉积技术，从溶液沉淀硫化铜，使用硫化氢来硫化铜化合物，电子辐射，或者通过机械化学过程，在该过程中在使单质铜与单质硫反应的条件下将粉末状铜金属与单质硫混合，以形成一种或多种铜硫化物。这样的方法描述在Materials Research Bulletin，第30卷，第12期，1495-1504页，1995中。
可以使用的铜硫化物包括硫化铜(II)、CuS(铜蓝)和/或亚化学计量的铜硫化物，例如式Cu2-xS，其中x是0-1，如Cu9S5(蓝辉铜矿)。可以使用一种或多种铜硫化物。优选CuS高的铜硫化物，并且硫化铜微粒的总S:Cu原子比优选≥0.8，更优选≥0.9，最优选≥0.95。令人期望地，吸着剂中基本上全部的经硫化的铜是硫化铜(II)，CuS的形式。硫化铜微粒可以是粉末形式，优选平均粒度即D50为5-100μm的粉末。
经干燥的吸着剂可以包含5-75wt％，优选10-75wt％，更优选15-55wt％，尤其15-50wt％的硫化铜(用CuS来表示)。
经煅烧的、可再水合的氧化铝微粒优选是无定形或结晶差的过渡氧化铝包括ρ-氧化铝、χ-氧化铝和假γ-氧化铝中的一种或多种。优选经煅烧的、可再水合的氧化铝微粒由ρ-氧化铝、χ-氧化铝和假γ-氧化铝中的一种或多种，尤其是ρ-氧化铝组成。经煅烧的、可再水合的氧化铝微粒令人期望地是粉末形式，更优选是D50粒度为1-100μm，优选1-20μm，尤其1-10μm的粉末。通过氮气吸附测定，经煅烧的、可再水合的氧化铝微粒的BET表面积可以是200-400m2/g，优选250-300m2/g。
经干燥的吸着剂可以包含25-95wt％，优选25-90wt％的经煅烧的、可再水合的氧化铝微粒。
已经发现，不需要其他添加剂，所以制备吸着剂的方法中的第一步骤可以包括形成由硫化铜微粒和经煅烧的、可再水合的氧化铝微粒组成的混合物。
可以包含一种或多种粘土粘结剂和/或水泥粘结剂，但这些不是必须的。
在一个优选的实施方案中，不包含粘结剂，在这种情况中吸着剂可以被认为是“无粘结剂的”。
在一个优选的实施方案中，吸着剂主要由硫化铜和经煅烧的、可再水合的氧化铝微粒组成。
将包含硫化铜和经煅烧的、可再水合的氧化铝微粒的混合物成形和干燥，来形成吸着剂。成形可以通过压丸、挤出或造粒。因此，可以通过在适当尺寸的模子中，模制通常含有例如石墨或硬脂酸镁的材料作为模制助剂的粉末组合物，来形成吸着剂丸粒，例如常规压片操作中那样。替代地，可以通过迫使适合的组合物和经常少量水和/或上述的模制助剂经过模头，然后将从模头形成的材料切成短长度，来形成吸着剂挤出物。例如，可以使用用于将动物饲料压丸的类型的压丸机来制造挤出物，其中将要压丸的混合物装入旋转穿孔圆筒，混合物被该圆筒内的棒或辊强制通过该圆筒的孔眼：用定位的刮刀从旋转圆筒的表面切下得到的挤出混合物，以提供所需长度的挤出丸粒。替代地，可以通过将粉末组合物与不足以形成浆料的少量液体如水混合，然后使该组合物在造粒机中附聚成大致球形的颗粒，来形成附聚物形式的吸着剂颗粒。液体的添加量将根据组分的孔隙率和可湿性而不同，但是可以是0.1-0.5ml/g载体混合物。可以使用含水或不含水液体，但是优选水。使液体使用量最小化有利地减少了吸着剂的干燥时间，并且可以减小不期望的铜硫化物的形成。类似地，在非氧化性气氛如不含氧气的氮气下将混合物造粒，减少了硫酸盐的潜在形成。适合的造粒机设备可商购。液体可以方便地通过喷雾来添加。
丸粒、挤出物或颗粒优选具有1-25mm的长度和宽度，并且长宽比(最长尺寸除以最短尺寸)≤4。
不同的成形方法对表面积、孔隙率和成形制品内的孔结构有影响，这经常又对吸着特性和堆密度有显著影响。所以，模制丸粒形式的吸着剂的床可以展现相对宽的吸附前端，而粒化的附聚物的床可以具有窄得多的吸附前端：这能够更加接近理论吸附容量。另一方面，附聚物通常具有比压片的组合物更低的堆密度。此外，鉴于存在硫化铜，优选涉及少量水的方法，以避免可能形成不期望的硫酸盐。因此，优选的是制造附聚物形式的成形单元，所以优选的成形方法包括在造粒机中将硫化铜和经煅烧的、可再水合的氧化铝的混合物造粒。优选直径为1-15mm的颗粒。已经发现，将混合物造粒中水的使用量对得到的颗粒的强度有影响。造粒中水的使用量可以是0.25ml/g粉末至0.6ml/g硫化铜和经煅烧的、可再水合的氧化铝的混合物。这高于典型地需要<0.2ml/g混合物的现有技术的粒化产品，源自于经煅烧的、可再水合的氧化铝的不寻常的性质。
成形的吸收剂可以经老化以在干燥前增强它的强度。含有经煅烧的、可再水合的氧化铝的吸着剂的老化适宜地在20-90℃，优选40-90℃进行。在吸着剂中仅使用经煅烧的、可再水合的氧化铝的好处是，与现有技术材料相比，可以显著地减少或消除老化步骤。所以，可以对含有经煅烧的、可再水合的氧化铝的颗粒进行老化0.5-8小时，优选0.5-6小时，更优选0.5-2小时，然后干燥。在非氧化性气氛如干燥氮气下老化减少了硫酸盐形成的可能性。
将成形的吸着剂干燥。可以使用常规的干燥温度。可以使用至多120℃的干燥温度。干燥时间可以是0.25-16小时。在非氧化性气氛如干燥氮气下干燥减小了硫酸盐形成的可能性。
吸着剂可以用来处理含有重金属的液态和气态流体料流，特别是含有汞和/或砷的流体料流。在一个实施方案中，流体料流是烃料流。烃料流可以是炼厂烃料流，如石脑油(例如含有具有5或更多个碳原子，和至多204℃的最终常压沸点的烃)，中间馏分或常压瓦斯油(例如具有177℃-343℃的常压沸点)，真空瓦斯油(例如常压沸点343-566℃)，或渣油(常压沸点高于566℃)，或者由这样的原料通过例如催化重整生产的烃料流。炼厂烃料流还包含载体料流，如FCC工艺中使用的“循环油”和溶剂萃取中使用的烃。烃料流还可以是原油料流，特别是当原油相对轻质，或是由例如焦油或煤提取生产的合成原油料流。可以使用本发明的方法处理气态烃，例如天然气或炼制的链烷烃或烯烃。特别地可以用吸着剂处理海上原油和海上天然气料流。还可以处理污染的燃料如汽油或柴油。替代地，烃可以是冷凝物，如液化天然气(NGL)或液化石油气(LPG)，或者气体如煤床甲烷、堆土废气或生物气。优选气态烃如天然气和相关的气体。
可以处理的非烃流体料流包括二氧化碳，其可以用于增强的采油过程或用于碳捕集和储存，用于咖啡脱咖啡因的溶剂，香料和香氛提取，煤的溶剂萃取等。用于清洗过程或干燥过程中的例如醇(包括二醇)和醚的流体(例如三乙二醇、单乙二醇、RectisolTM、PurisolTM和甲醇)可以通过本发明的方法进行处理。也可以从用于酸气去除单元中使用的胺料流中除去汞。任选地在进一步加工如氢化或酯交换之后，可以处理天然的油和脂肪如植物油和鱼油，以例如形成生物柴油。
可以处理的其他流体料流包括来自脱水单元的再生气体如分子筛废气，或者来自二醇干燥剂的再生的气体。
当流体料流含有水，优选以0.02-1vol％的低水平时，吸着剂是有用的。可以短期容许至多5vol％的较高水平。在长时间暴露于水后，可以简单地通过干燥气体，优选干燥惰性气体如氮气吹扫，来再生吸着剂。
优选重金属的吸着低于150℃，优选在或低于120℃的温度进行，因为在这样的温度重金属吸收的总体能力得到增强。可以使用低至4℃的温度。优选的温度范围是10-60℃。穿过吸着剂的气时空速可以是通常采用的范围。
此外，本发明可以用来处理含有一种或多种还原剂如氢和/或一氧化碳，尤其是氢的液态和气态流体料流。在一个实施方案中，流体料流是含有溶解的氢和一氧化碳的液态烃料流。在另一实施方案中，流体料流是含有氢气和/或一氧化碳的气态料流，即还原性气流。可以受益于该方法的气流包括来自常规蒸汽重整过程和/或部分氧化过程的合成气料流，和来自煤气化器的合成气料流，例如作为IGCC工艺的一部分，在气体清洗和热回收(冷却)步骤之后和酸性变换阶段之前。可以受益于本发明的其他料流包括炼厂排出料流，炼厂裂化器料流，高炉气体，还原性气体，特别是富氢气流，富乙烯料流，和从加氢处理过程如加氢脱硫或加氢脱氮进料或回收的液态或气态烃料流，例如石脑油。
在使用中，吸着剂可以置于吸着容器中，使含有重金属的流体料流经过它。令人期望地，根据已知方法，吸着剂置于容器中作为一个或多个的固定床。可以采用多于一个床，这些床在组成上可以相同或不同。
参考以下实施例进一步描述本发明。
实施例1.制备吸着剂
制备如下的硫化铜粉末和经煅烧的、可再水合的氧化铝粉末的混合物：
组分 来源 wt％
硫化铜(99％) Eurolub 67
经煅烧的、可再水合的氧化铝 CP-5，BASF 33
经煅烧的、可再水合的氧化铝粉末的性质如下：
物理性质
将粉末预混合以确保是均匀的混合物。然后通过使混合物在转盘中结粒来形成颗粒，同时将水(约0.33ml/g混合物)作为细雾喷到混合物上。发现在干燥前，水是成形附聚物的质量的约25wt％。这显著高于典型地仅包含约15wt％水的现有技术的粒化吸着剂的水含量。造粒之后，将材料在45℃老化。老化之后，将材料在流化床干燥机中在105℃干燥，以生成吸着剂。
测定吸着剂的物理性质，如下所示，与根据WO2009/101429中所述方法，使用碱式碳酸铜、水泥和粘土粘结剂以及三水合氧化铝(ATH)载体材料制备的硫化铜吸着剂进行比较。
振实堆密度(TBD)通过以下来测量：将约500ml吸着剂颗粒倒入500ml塑料量筒中，轻敲它直到达到恒定体积。通过用吸着剂质量除以振实体积来计算TBD。
筒翻滚损失(DrTL)通过以下来测量：根据ASTM方法D4058-96，使100g吸着剂以60rpm用30分钟旋转总计1800圈。DrTL记录为原始质量的百分比。
平均压碎强度(MCS)通过以下来测量：使用工程系统C53机器压碎每种吸着剂的25个颗粒，来基于正态分布计算平均压碎强度。
与使用混合的粘结剂和三水合氧化铝生产的现有技术材料相比，使用经煅烧的、可再水合的氧化铝提供了坚固得多的产品。与混合的粘结剂产品相比，在经煅烧的、可再水合的氧化铝产品中，强度发展的速率也明显更快，在1小时老化之后获得超过5倍的强度。

Claims (16)

1.制备吸着剂的方法，该方法包括以下步骤：
(i)将硫化铜材料微粒与经煅烧的、可再水合的氧化铝微粒混合在一起，
(ii)使混合物成形，和
(iii)将成形的混合物干燥，以形成经干燥的吸着剂。
2.根据权利要求1所述的方法，其中该经煅烧的、可再水合的氧化铝包含经煅烧的无定形氧化铝或过渡氧化铝，过渡氧化铝选自ρ-氧化铝、χ-氧化铝和假γ-氧化铝中的一种或多种。
3.根据权利要求1或2所述的方法，其中该硫化铜材料微粒通过以下来制造：用单质硫焙烧铜或铜化合物，从溶液沉淀硫化铜，使用硫化氢来硫化铜化合物，或者机械化学过程，在该过程中在使单质铜与单质硫反应的条件下将粉末状铜金属与单质硫混合，以形成一种或多种铜硫化物。
4.根据权利要求1-3中任一项所述的方法，其中该硫化铜包括选自以下的一种或多种铜硫化物：硫化铜(II)，CuS，和/或亚化学计量的式Cu2-xS的铜硫化物，其中x是0-1。
5.根据权利要求1-4中任一项所述的方法，其中该硫化铜微粒具有≥0.8，优选≥0.9，更优选≥0.95的总S:Cu原子比。
6.根据权利要求1-5中任一项所述的方法，其中该硫化铜材料微粒是平均粒度D50为5-100μm的粉末形式。
7.根据权利要求1-6中任一项所述的方法，其中该经干燥的吸着剂的硫化铜含量是5-75wt％(用CuS来表示)，优选10-75wt％，更优选15-55wt％，尤其15-50wt％。
8.根据权利要求1-7中任一项所述的方法，其中该经煅烧的、可再水合的氧化铝微粒是D50粒度为1-100μm，优选1-20μm，尤其1-10μm的粉末。
9.根据权利要求1-8中任一项所述的方法，其中通过氮气吸附测定的经煅烧的、可再水合的氧化铝的BET表面积是200-400m2/g，优选250-300m2/g。
10.根据权利要求1-9中任一项所述的方法，其中该经干燥的吸着剂主要由该硫化铜微粒和该经煅烧的、可再水合的氧化铝微粒组成。
11.根据权利要求1-10中任一项所述的方法，其中成形步骤包括在造粒机中将该混合物造粒，以生成颗粒形式的吸着剂。
12.根据权利要求11所述的方法，其中造粒在非氧化性气氛下进行。
13.根据权利要求11或12所述的方法，其中将颗粒老化0.5-8小时，优选0.5-6小时，更优选0.5-2小时，然后干燥。
14.根据权利要求1-13中任一项所述的方法，其中在非氧化性气氛下在至多120℃的温度干燥该吸着剂。
15.能够通过根据权利要求1-14中任一项所述的方法获得的吸着剂。
16.从含重金属的流体料流中除去一种或多种重金属的方法，该方法使该流体料流与根据权利要求15所述的吸着剂，或者根据权利要求1-14中任一项所述的方法制备的吸着剂接触。
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