CN101918324B - 用于处理被污染的流体的聚集体组合物 - Google Patents
用于处理被污染的流体的聚集体组合物 Download PDFInfo
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- CN101918324B CN101918324B CN200880123682.8A CN200880123682A CN101918324B CN 101918324 B CN101918324 B CN 101918324B CN 200880123682 A CN200880123682 A CN 200880123682A CN 101918324 B CN101918324 B CN 101918324B
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Abstract
聚集体组合物以及该聚集体组合物的制造方法。所述聚集体组合物包含不溶性的含稀土化合物以及聚合物粘结剂。所述不溶性的含稀土化合物可包含铈、镧或镨中的一种或多种。合适的不溶性的含铈化合物可得自碳酸铈或铈盐。在特定的实施方案中,所述聚集体组合物基本上由一种或多种铈氧化物、所述聚合物粘结剂、以及任选的助流剂组成。所述组合物的制造方法包括:将所述不溶性的含稀土化合物与聚合物粘结剂混合以形成混合物;以及对该混合物进行机械、化学和/或热处理以使所述稀土化合物附着到该聚合物粘结剂上。所述聚集体组合物可用于各种流体处理应用,以去除流体中的一种或多种化学和生物污染物。
Description
技本领域
本发明大体上涉及流体处理领域,且主要涉及用于处理溶液和气体的组合物。更具体地,本发明涉及适用于对含一种或多种化学和生物污染物的水溶液和气体进行处理的聚集体组合物、及这样的聚集体组合物的制造方法。
背景技术
对水及其它水溶液进行净化和过滤对于许多应用是必须的,例如供应安全的可饮的饮用水、与各种工业过程有关的原料、工艺物流及副产物的处理、以及城市废水的处理和加工。用于对水溶液进行净化的已知方法包括反渗透、蒸馏、离子交换、化学吸附、凝结、絮凝、以及过滤或截留。这些净化实践的许多可为昂贵的、能量效率低的且需要重要的技术秘密和改进以大规模和小规模两者实施。因此,许多先进的流体净化技术在市政或工业应用之外具有有限的应用。
生物污染物例如细菌和真菌可通过超滤从水溶液中去除,但是,病毒通常太小,以致于过滤不是有效的净化手段。由于过滤仅是稍稍有效的,因而使用化学添加剂的处理趋于成为解决这样的污染物的存在的所选方法。化学添加剂的实例包括强氧化剂如氯、过氧化氢、臭氧或季胺盐、絮凝剂、以及沉淀剂。但是,使用化学添加剂要求对被处理的溶液的仔细的管理和监控,且需要专门的处理、运输和储存,这使得它们对于许多应用是更昂贵的且不太合乎需要的。因此,从水溶液中去除生物污染物的简化手段是期望的。
此外,由于近来恐怖主义的增多,世界各国政府已经变得越来越关注化学战剂、生物制剂、工业化学品及其它毒性物质的影响。由于各国储备用于工业应用和用作战剂两者的这样的物质,因而由于通过吸入、吸收和/或摄取的潜在暴露,这样的污染物表现出对武装部队和平民等的危险。因此,地下水及其它饮用水源被化学和生物污染物污染是军队和地方政府以及公共事业区域(utility district)的首要关注内容。
通常已知的化学战剂包括基于有机硫的化合物例如2,2′-二氯二乙硫醚(HD、芥子、芥子气、S芥子气或硫芥子气),它们被称为“糜烂性”或“疱肿性”毒剂且大剂量时可致死。其它化学战剂包括基于有机磷(“OP”)的化合物例如甲基硫代膦酸O-乙基S-(2-二异丙氨基)乙酯(VX)、甲基氟代膦酸2-丙酯(GB或沙林)和甲基氟代膦酸3,3′-二甲基-2-丁酯(GD或索曼),它们通常被称为“神经”毒剂,由于它们攻击中枢神经系统,且它们可在短时间内导致麻痹以及可能导致死亡。其它化学污染物包括一些工业化学品、杀虫剂和农药例如对硫磷、对氧磷和马拉硫磷,它们也可具有有害的影响。
用于对暴露于化学战剂的表面进行净化的方法和材料是本领域已知的。Yang等人的“Decontamination of Chemical Warfare Agents”,Chem Rev.Vol.92,第1729-1743页(1992)。这些方法和材料趋于通过与所述化学战剂化学反应和/或通过吸附所述化学战剂而起作用,但是这些方法和材料着重于对已暴露于所述战剂的运载工具、设备、人员、以及其它表面进行净化。由于这样的方法和材料对于处理溶液中的化学战剂是不适合的或不足够有效的,因此仍然需要用于从水溶液去除和/或解毒广谱化学污染物的简化手段,其中所述化学污染物包括但不限于神经毒剂、糜烂性毒剂、农药、杀虫剂以及其它有毒化学药剂。
此外,通过吸入暴露于化学和生物污染物也是还未得到充分解决的所关注的问题。用于控制空气质量的基本方法包括过滤、在固体吸附剂上的吸收、静电沉积、化学转化、以及用各种形式的辐射处理,所述辐射包括热、紫外光和微波。气体过滤方法趋于受过滤器的孔径大小的限制,且通常不能去除许多种生物和化学污染物。使用超小的孔径由于过滤器上的颗粒趋于堵塞,产生对于许多应用来说无法接受的跨越过滤器的过度的压力降。静电沉积通过如下工作:在粒子上强加电荷,然后将它们从气流中移出到带相反电荷的表面例如收集板上。该技术不适于高速气流、含有挥发性化学污染物的流体或其它难以带电的污染物。化学反应趋于仅对小体积的气体有效,且可需要气体的额外的加工或处理以去除残留的不合乎需要的和潜在有害的反应物和副产物。虽然加热对于从气体中去除许多种生物和化学污染物是有效的,但加热对于较高速度的气流趋于是无效的。紫外光可为有效的,但对于在较大的气体体积上执行是困难的,因为所述光趋于仅被气流中紧靠光源的部分中的那些污染物吸收。
气体在吸附剂上的吸附可为有效的,特别是当吸附剂与要从气体中去除的污染物特定匹配时。然而,当污染物的具体性质未知时或者当气流含有许多不同的污染物时,使用已知的吸附剂无法充分地使气体净化。因此,仍然需要能够对可存在于各种流体中的不同组的生物和化学污染物例如细菌、病毒、神经毒剂、糜烂性毒剂、农药、杀虫剂及其它有毒化学药剂进行去除、失活和/或解毒的组合物,所述流体包括水溶液和气体两者。
发明内容
在一个实施方案中,本发明提供用于对含有一种或多种污染物的流体进行处理的聚集体组合物。该聚集体组合物包含不溶性的含稀土化合物以及聚合物粘结剂。
该聚合物粘结剂可为所述组合物的低于约15重量%,在一些情况下所述组合物的低于约10重量%,且在还另外的情况下所述组合物的低于约8重量%。所述聚合物粘结剂可包含选自热固性聚合物、热塑性聚合物、弹性体聚合物、纤维素聚合物以及玻璃中的一种或多种聚合物。当该聚合物粘结剂包括乙烯-乙烯基共聚物时,所述不溶性的含稀土化合物基本上由无水的不溶性的含稀土化合物组成。
所述不溶性的含稀土化合物可包括任何不溶性的稀土化合物,但具体地说可包含铈、镧或镨中的一种或多种。在一些实施方案中,所述不溶性的含稀土化合物可包括得自碳酸铈的热分解或者草酸铈的分解的含铈化合物。在另外的实施方案中,所述不溶性的含稀土化合物可包括得自铈盐的沉淀的含铈化合物。在另外的实施方案中,所述不溶性的含稀土化合物包括铈氧化物。在更具体的实施方案中,所述聚集体组合物基本上由一种或多种铈氧化物、所述聚合物粘结剂、以及任选的助流剂组成。所述不溶性的含稀土化合物可包括附着于所述聚合物粘结剂外表面的颗粒。
所述聚集体组合物可包括平均表面积为至少约1m2/g,在一些情况下至少约5m2/g,且在还另外的情况下至少约25m2/g的聚集颗粒。所述聚集体组合物可包括平均聚集体尺寸为至少约1μm的聚集颗粒。所述聚集体组合物具有至少约50mg/g所述聚集体组合物的从水溶液中去除砷的吸附能力。在一些情况下,所述组合物从水溶液中去除砷的吸附能力至少为约60mg/g所述聚集体组合物,且在另外的情况下为至少约70mg/g。
在本发明的另一方面,提供用于处理含一种或多种污染物的流体的聚集体组合物的制造方法。该方法包括将不溶性的含稀土化合物与聚合物粘结剂进行混合以形成混合物的初始步骤。
对该混合物进行机械处理、化学处理和热处理的一种或多种,以使所述不溶性的含稀土化合物附着到所述聚合物粘结剂上。机械处理可包括压制、压缩、挤压、混合、挤出、以及向所述混合物施加振动或波。化学处理可包括化学转化以及使用粘合剂的一种或多种。热处理可包括将所述混合物加热至升高的温度并使所述混合物冷却以形成聚集体组合物。在一些实施方案中,所述升高的温度为低于所述聚合物粘结剂的熔点的温度,在该温度处所述聚合物粘结剂是有延展性的或发粘的且所述不溶性的含稀土化合物附着到所述聚合物粘结剂上。在其中所述不溶性的含稀土化合物包括颗粒的实施方案中,所述颗粒可附着到所述聚合物粘结剂的外表面上。
所述不溶性的含稀土化合物可包括附着于所述聚合物粘结剂外表面的颗粒。任选地,该方法可包括对经加热的聚合物粘结剂和不溶性的含稀土化合物的混合物进行压缩。
任选的步骤可包括降低所述聚集体组合物的尺寸。可通过对所述聚集体组合物进行切割、粉碎、研磨以及筛分的一种或多种来实现尺寸降低。
该聚合物粘结剂可为所述组合物的低于约15重量%,在一些情况下所述组合物的低于约10重量%,且在还另外的情况下所述组合物的低于约8重量%。所述聚合物粘结剂可包括选自热固性聚合物、热塑性聚合物、弹性体聚合物、纤维素聚合物和玻璃的一种或多种聚合物。当所述聚合物粘结剂包括乙烯-乙烯基共聚物时,所述不溶性的含稀土化合物基本上由无水的不溶性的含稀土化合物组成。
所述聚合物粘结剂可为固体。在一些实施方案中,所述聚合物粘结剂包括纤维、颗粒、纤维和或颗粒的聚集体、以及其混合物的一种或多种。所述不溶性的含稀土化合物可包括平均粒径大于约1nm的颗粒。所述不溶性的含稀土化合物可包括任何不溶性的稀土化合物,但具体地说可包含铈、镧或镨的一种或多种。在一些实施方案中,所述不溶性的含稀土化合物可包括得自碳酸铈的热分解的含铈化合物。在另外的实施方案中,所述不溶性的含稀土化合物可包括得自铈盐的沉淀的含铈化合物。在另外的实施方案中,所述不溶性的含稀土化合物包括铈氧化物。在更具体的实施方案中,所述聚集体组合物基本上由一种或多种铈氧化物、所述聚合物粘结剂、以及任选的助流剂组成。
具体实施方式
在下文中描述本发明的说明性实施方案。为了清楚起见,在本说明书中未描述实际实施方案的所有特征。当然,应当理解,在任何这样的实际实施方案的开发中,必须作出许多实施-具体决定以实现开发者的特定目的,例如服从与体系相关的和与商业相关的约束条件,其将随着不同实施而变化。此外,应当理解,这样的开发努力可为复杂且耗时的,但仍然是受益于本公开内容的本领域的普通技术人员所采取的常规工作。
应当知道,在此所述的聚集体组合物可用于对水溶液或气体中的一种或多种化学和生物污染物进行去除、失活和/或解毒。可用在此所述的组合物处理的溶液的实例其中包括:饮用水系统中的溶液;废水处理系统中的溶液;以及在各种工业过程的原料流、工艺物流或废液流中的溶液。此外,需要在开阔环境中例如在战场上、在封闭空间中例如在建筑物或类似的构筑物中、在运载工具如飞机、宇宙飞船、船舶或军用车辆内、以及任何可发现这样的污染物的地方,对含有这样的污染物的气体进行处理。所述组合物可用于从具有各种体积和流速特性的水溶液及气体中去除化学和生物污染物,且可用于各种固定应用、移动应用和便携式应用中。虽然本文的部分公开内容描述了从水中去除污染物,但这样的内容是说明性的且不看做是限制性的。
当如本文中使用的“...的一个(种)或多个(种)”和“...的至少一个(种)”用于几个要素或几类要素例如X、Y和Z或者X1-Xn、Y1-Yn和Z1-Zn的序言时,其意指选自X或Y或Z的单独的要素、选自同类的要素的组合(例如X1和X2)、以及选自两类或更多类的要素的组合(例如Y1和Zn)。
术语“除去”或“去除”包括对可存在于溶液或气体中的病原和其它微生物例如细菌、病毒、真菌和原生动物、以及化学污染物进行吸附、沉淀、转化和杀灭。术语“失活”、“解毒”和“抵消”包括从流体中去除生物或化学污染物或使其对人类或其它动物为非病原的或良性的,例如通过杀灭微生物或将化学药剂转化为无毒形式或种类。
术语“生物污染物”、“微生物”等包括细菌、真菌、原生动物、病毒、藻类以及可在水溶液中发现的其它生物体和病原物质。生物污染物的具体的非限定性实例可包括:细菌,例如大肠杆菌、粪链球菌、志贺氏菌属菌种、钩端螺旋体、嗜肺性军团病杆菌(Legimella pneumophila)、小肠结肠炎耶尔森氏菌、金黄色葡萄球菌、绿脓杆菌、土生克雷伯菌、炭疽杆菌、霍乱弧菌、和伤寒沙门氏菌;病毒,例如甲型肝炎、诺如病毒(noroviruse)、轮状病毒和肠道病毒;原生动物,例如痢疾内变形虫、贾第鞭毛虫、小球隐孢子虫等。生物污染物还可包括各种虽然通常是非病原的但有利地去除的物质例如真菌或藻类。这样的生物污染物如何存在于溶液或气体中的,通过天然存在还是通过有意或无意的污染,是本发明不限制的。
术语“化学污染物”或“化学药剂”包括已知的化学战剂和工业化学品和物质例如农药、杀虫剂和化肥。在一些实施方案中,所述化学污染物可包括有机硫药剂、有机磷药剂或它们的混合物中的一种或多种。这样的药剂的具体的非限定性实例包括:氟代膦酸o-烷基酯,例如沙林和索曼;氨基氰膦酸o-烷基酯,例如塔崩;烷基硫代膦酸o-烷基s-2-二烷基氨乙酯和相应的烷基化或质子化的盐,例如VX;芥子化合物,包括2-氯乙基氯甲基硫醚、双(2-氯乙基)硫醚、双(2-氯乙基硫基)甲烷、1,2-双(2-氯乙基硫基)乙烷、1,3-双(2-氯乙基硫基)-正丙烷、1,4-双(2-氯乙基硫基)-正丁烷、1,5-双(2-氯乙基硫基)-正戊烷、双(2-氯乙基硫基甲基)醚和双(2-氯乙基硫基乙基)醚;路易氏毒气,包括2-氯乙烯基二氯胂、双(2-氯乙烯基)氯胂、三(2-氯乙烯基)胂;双(2-氯乙基)乙胺和双(2-氯乙基)甲胺;蛤蚌毒素;蓖麻毒素;烷基膦酰二氟;亚膦酸烷基酯;氯沙林;氯索曼;胺吸磷;1,1,3,3,3,-五氟-2-(三氟甲基)-1-丙烯;二苯乙醇酸3-奎宁环基酯;甲基膦酰二氯;甲基膦酸二甲酯;二烷基氨基膦酰二卤;氨基磷酸烷基酯;二苯基羟基乙酸;喹核-3-醇;二烷基氨乙基-2-氯;二烷基氨基乙烷-2-醇;二烷基氨基乙烷-2-硫醇;硫二甘醇;频哪醇;碳酰氯;氯化氰;氰化氢;三氯硝基甲烷;磷酰氯;三氯化磷;五氯化磷;烷基磷酰氯;亚磷酸烷基酯;三氯化磷;五氯化磷;亚磷酸烷基酯;一氯化硫;二氯化硫;以及亚硫酰氯。
可有效地用本文所述组合物处理的工业化学品和物质的非限定性实例包括具有阴离子官能团的材料例如磷酸盐、硫酸盐和硝酸盐和具有电负性官能团的材料例如氯化物、氟化物、溴化物、醚和羰基化物。具体的非限定性实例可包括:乙醛、丙酮、丙烯醛、丙烯酰胺、丙烯酸、丙烯腈、艾氏剂/狄氏剂、氨、苯胺、砷、莠去津、钡、联苯胺、2,3-苯并呋喃、铍、1,1′-联苯、二(2-氯乙基)醚、二(氯甲基)醚、溴二氯甲烷、溴仿、溴甲烷、1,3-丁二烯、1-丁醇、2-丁酮、2-丁氧基乙醇、丁醛、二硫化碳、四氯化碳、硫化羰、氯丹、十氯酮和灭蚁灵、毒虫畏、氯化二苯并-对-二噁英(CDD)、氯、氯苯、氯化二苯并呋喃(CDF)、氯乙烷、氯仿、氯甲烷、氯苯酚、毒死蜱、钴、铜、杂酚油、甲酚、氰化物、环己烷、DDT、DDE、DDD、DEHP、邻苯二甲酸二(2-乙基己基)酯、二嗪农、二溴氯丙烷、1,2-二溴乙烷、1,4-二氯苯、3,3′-二氯联苯胺、1,1-二氯乙烷、1,2-二氯乙烷、1,1-二氯乙烯、1,2-二氯乙烯、1,2-二氯丙烷、1,3-二氯丙烯、敌敌畏、邻苯二甲酸二乙酯、甲基膦酸二异丙酯、邻苯二甲酸二正丁酯、乐果、1,3-二硝基苯、二硝基甲酚、二硝基苯酚、2,4-二硝基甲苯和2,6-二硝基甲苯、1,2-二苯肼、邻苯二甲酸二正辛基酯(DNOP)、1,4-二噁烷、二噁英、乙拌磷、硫丹、异狄氏剂、乙硫磷、乙苯、环氧乙烷、乙二醇、乙基对硫磷、倍硫磷、氟化物、甲醛、氟利昂113、七氯和环氧七氯、六氯苯、六氯丁二烯、六氯环己烷、六氯环戊二烯、六氯乙烷、六亚甲基二异氰酸酯、己烷、2-己酮、HMX(奥克托今)、液压流体、肼、硫化氢、碘、异佛尔酮、马拉硫磷、MBOCA、甲胺磷、甲醇、甲氧氯、2-甲氧基乙醇、甲基乙基酮、甲基异丁基酮、甲硫醇、甲基对硫磷、甲基叔丁基醚、甲基氯仿、二氯甲烷、亚甲基双苯胺、甲基丙烯酸甲酯、甲基-叔丁基醚、灭蚁灵和十氯酮、久效磷、N-亚硝基二甲胺、N-亚硝基二苯胺、N-亚硝基二正丙胺、萘、硝基苯、硝基苯酚、全氯乙烯、五氯苯酚、苯酚、磷胺、磷、多溴联苯(PBB)、多氯联苯(PCB)、多环芳烃(PAH)、丙二醇、邻苯二甲酸酐、除虫菊酯和拟除虫菊酯、吡啶、RDX(三次甲基三硝基胺)、硒、苯乙烯、二氧化硫、三氧化硫、硫酸、1,1,2,2-四氯乙烷、四氯乙烯、三硝基苯甲硝胺、铊、四氯化物、三氯苯、1,1,1-三氯乙烷、1,1,2-三氯乙烷、三氯乙烯(TCE)、1,2,3-三氯丙烷、1,2,4-三甲基苯、1,3,5-三硝基苯、2,4,6-三硝基甲苯(TNT)、乙酸乙烯酯和氯乙烯。
在本发明的一个实施方案中,提供用于对含有一种或多种化学和生物污染物的流体进行处理的聚集体组合物。该聚集体组合物包含不溶性的含稀土化合物以及聚合物粘结剂。
在本文中使用的“不溶性”是指在标准的温度和压力条件下不溶于水或至多微溶于水的物质。
所述组合物可包含低于或超过10.01重量%的不溶性的含稀土化合物。所述不溶性的含稀土化合物可占所述聚集体组合物的超过约11重量%、超过约12重量%或超过约15重量%。在一些情况下,较高的含稀土化合物浓度(concentration)可为需要的。取决于应用和组合物中其它组分的性质,所述组合物可含有至少约20重量%,在另外的情况下至少约50重量%,在还另外的情况下至少约75重量%,且在更另外的情况下超过95重量%的不溶性的含稀土化合物。
所述不溶性的含稀土化合物可包括稀土的一种或多种,所述稀土包括:镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥。在一些实施方案中,所述不溶性的含稀土化合物可包含铈、镧或镨中的一种或多种。不溶性的含稀土化合物是可商购的且可由本领域技术人员已知的任意来源或通过本领域技术人员已知的任意方法获得。所述聚集体组合物不必包含单独的含稀土化合物,而是可以包含两种或更多种不溶性的含稀土化合物。这样的化合物可包含相同或不同的稀土元素和可包含混合的化合价或氧化态。例如,当所述不溶性的含稀土化合物包括铈氧化物时,所述聚集体组合物可包含一种或多种铈氧化物例如CeO2(IV)和Ce2O3(III)。
在其中所述不溶性的含稀土化合物包括含铈化合物的实施方式中,所述含铈化合物可得自铈盐的沉淀。在另一实施方案中,不溶性的含铈化合物可得自碳酸铈或草酸铈。更具体地说,可通过在空气的存在下在炉中在约100℃~约350℃的温度下对碳酸铈或草酸铈进行热分解来制备高表面积的不溶性的含铈化合物。取决于含铈起始材料的组成和不溶性的含稀土化合物的所需物理性能,可改变温度和压力条件。所述反应可概括如下:
Ce2(CO3)3+1/2O2-→2CeO2+3CO2
可对产物进行酸处理和洗涤以去除残余的碳酸盐。用于产生具有各种特征的铈氧化物的热分解方法描述于美国专利No.5,897,675(比(特定的)表面积)、美国专利No.5,994,260(具有均匀层状结构的孔)、美国专利No.6,706,082(特定的粒径分布)、以及美国专利No.6,887,566(球形粒子)中,并将这样的描述在此引入作为参考。碳酸铈和含碳酸铈的材料是可商购的且可得自本领域技术人员已知的任意来源。
在其中不溶性的含稀土化合物包括铈氧化物的实施方案中,所述不溶性的含稀土化合物可包括铈氧化物例如CeO2。在具体的实施方案中,所述聚集体组合物可基本上由一种或多种铈氧化物、聚合物粘结剂、以及任选的助流剂组成。
所述不溶性的含稀土化合物可以微粒、晶体、微晶、粒子或其它颗粒的一种或多种的形式存在于聚集体组合物中,它们在本文中通称为“颗粒”。所述不溶性的含稀土化合物的颗粒可具有至少约0.5nm直到约1μm或更高的平均粒径。具体地说,这样的颗粒的平均粒径可为至少约0.5nm,大于约1nm,更特别地至少约5nm,还更特别地至少约10nm。在另外的实施方案中,所述颗粒的平均粒径可为至少约100nm,特别地至少约250nm,更特别地至少约500nm,且还更特别地至少约1μm。
为了促进所述不溶性的含稀土化合物与溶液或气体中的污染物之间的相互作用,所述聚集体组合物可包括平均表面积为至少约1m2/g的不溶性的含稀土化合物的聚集颗粒。取决于应用,较高的表面积可为需要的。具体地说,所述颗粒的表面积可为至少约5m2/g,在另外的情况下超过约10m2/g,且在更另外的情况下超过约25m2/g。当需要较高的表面积时,所述颗粒的表面积可超过约70m2/g,在另外的情况下超过约85m2/g,在还另外的情况下超过115m2/g,且在更另外的情况下超过约160m2/g。此外,预计具有较高表面积的颗粒是有效的。本领域技术人员将认识到,在其中溶液或气体流过所述组合物的应用中,所述组合物的表面积将影响具有聚集体组合物的流体的流体动力学。因此,可需要对由提高的表面积而得到的利益与可发生的不利情况例如压力降进行平衡。
在所述组合物中包括聚合物粘结剂以形成具有所需大小、结构、密度、孔隙率以及流体性能的聚集体。在一些实施方案中,所述聚合物粘结剂可包含纤维、颗粒、纤维和或颗粒的聚集体、以及其混合物的一种或多种。合适的聚合物粘结剂可包括在使用条件下粘结和/或支撑所述不溶性的含稀土化合物的任意聚合物材料。合适的聚合物粘结剂包括天然存在的聚合物和合成的聚合物两者、以及这样的聚合物的合成改性物。本领域技术人员将认识到,所述聚合物粘结剂材料的选择取决于如组合物的组分、这样的组分的性能、它们的粘结特性、最终组合物的特性、以及预期的使用方法的因数。
通常,在约50℃~约500℃、更具体在约75℃~约350℃、甚至更具体在约80℃~约200℃之间熔化的聚合物适用于对所述组合物的组分进行聚集。非限定性实例可包括:在约85℃~约180℃的范围内软化或熔化的聚烯烃;在约200℃~约300℃的范围内软化或熔化的聚酰胺;以及在约300℃~约400℃的范围内软化或熔化的氟化聚合物。所述聚合物粘结剂的熔点优选不超过所选的不溶性的含稀土化合物的烧结温度。
基于聚集体组合物的总重,这样的聚合物材料通常以约0重量%~约90重量%的量包括在所述组合物中。在一些实施方案中,所述聚合物粘结剂以低于所述组合物的约15重量%的量存在。更具体地说,所述聚合物粘结剂可为所述组合物的低于约10%,且在另外的实施方案中低于约8重量%。
取决于所述组合物的所需性能,聚合物粘结剂可包括一种或多种通常分为热固性、热塑性、弹性体、或其组合的聚合物;以及纤维素聚合物和玻璃。合适的热固性聚合物包括,但不限于:聚氨酯、有机硅、氟代有机硅、酚醛树脂、三聚氰胺树脂、三聚氰胺甲醛和脲甲醛。合适的热塑性材料可包括,但不限于:尼龙及其它聚酰胺;聚乙烯,包括LDPE、LLDPE、HDPE、以及与其它聚烯烃的聚乙烯共聚物;聚氯乙烯(增塑的和未增塑的);氟碳树脂,例如聚四氟乙烯;聚苯乙烯;聚丙烯;纤维素树脂,例如乙酸丁酸纤维素;丙烯酸类树脂,例如聚丙烯酸酯和聚甲基丙烯酸甲酯;热塑性共混物或接枝物,例如丙烯腈-丁二烯-苯乙烯或丙烯腈-苯乙烯;聚碳酸酯;聚乙酸乙烯酯;乙烯-乙酸乙烯酯;聚乙烯醇;聚氧化亚甲基;聚甲醛;聚缩醛;聚酯,例如聚对苯二甲酸乙二醇酯;聚醚醚酮;以及苯酚-甲醛树脂,例如甲阶酚醛树脂和线型酚醛清漆。合适的弹性体可包括,但不限于:天然橡胶和/或合成橡胶,如苯乙烯-丁二烯橡胶、氯丁橡胶、丁腈橡胶、丁基橡胶、有机硅、聚氨酯、烷基化的氯磺化聚乙烯、聚烯烃、氯磺化聚乙烯、全氟弹性体、聚氯丁二烯(氯丁橡胶)、乙烯-丙烯-二烯三元共聚物、氯化聚乙烯、氟化弹性体和ZALAKTM(Dupont-Dow弹性体)。在其中聚合物粘结剂包括乙烯乙烯基共聚物的具体实施方式中,所述不溶性的含稀土化合物基本上由无水的含稀土化合物组成。本领域技术人员将认识到:取决于交联度,以上所列的热塑性材料的一些也可为热固性材料,和取决于其机械性能,各自中的一些可为弹性体。以上所用的分类是为了便于理解,且不应认为是限定性的或控制性的。
纤维素聚合物可包括天然存在的纤维素例如棉、纸和木材、以及纤维素的化学改性物。在特定实施方案中,可将所述不溶性的含稀土化合物与纸纤维混合或者可直接引入纸浆中,以形成含有该不溶性的含稀土化合物的基于纸的过滤料。
聚合物粘结剂还可包括玻璃材料,例如玻璃纤维、玻璃珠和玻璃毡。可将玻璃固体物与不溶性的含稀土化合物的颗粒混合,并加热直至该固体物开始软化或变得发粘,使得该不溶性的含稀土化合物附着到玻璃上。类似地,在玻璃处于熔化态或部分熔化态时或借助于粘合剂,压纺或纺成的玻璃纤维可用不溶性的含稀土化合物的粒子包覆。或者,在制造期间,可使玻璃组成掺杂有不溶性的含稀土化合物。用于将不溶性的含稀土化合物沉积或附着到基底材料上的技术描述在美国专利No.7,252,694以及涉及玻璃抛光的其它文献中。例如,金属粘合剂的应用以及电沉积技术在美国专利No.6,319,108中被描述为在玻璃抛光领域中是有用的。在此将这样的技术的描述引入作为参考。
在一些应用中,水溶性的玻璃如美国专利No.5,330,770、6,143,318和6,881,766中所述的那些可为适当的聚合物粘结剂。在此将所提及的文献中的这样的玻璃的描述引入作为参考。在另外的应用中,还可使用通过流体吸收而溶胀的材料,该材料包括但不限于聚合物例如合成制得的聚丙烯酸和聚丙烯酰胺以及天然存在的有机聚合物例如纤维素衍生物。能生物降解的聚合物例如聚乙二醇、聚乳酸、聚乙烯醇、共聚丙交酯乙交酯等也可用作聚合物粘结剂。
当期望通过杀菌来使组合物再生时,所选的聚合物粘结剂应在杀菌条件下是稳定的,和应以另外的方式与所预期的杀菌方法相适应。适用于包括暴露于高温的杀菌方法的聚合物粘结剂的具体的非限定性实例包括硝酸纤维素、聚醚砜、尼龙、聚丙烯、聚四氟乙烯、以及混合纤维素酯。在根据已知的标准制备时,用这些粘结剂制备的组合物可用高压釜处理。由于对于有效率且有效果的再生可需要杀菌方法的组合,因而聚集体组合物应对于蒸汽杀菌或高压釜处理是稳定的以及对于通过与氧化或还原性的化学物质接触的化学杀菌是稳定的。在其中杀菌包括氧化或还原性化学物质的电化学产生的实施方案中,通过将所述组合物用作电极之一,可以获得产生所述物质必需的电势。例如,通过包含足够高含量的导电粒子例如粒状活性炭、炭黑或金属粒子,可使含有通常绝缘的聚合物粘结剂的组合物导电。或者,如果炭或其它粒子的所需含量不足够高至使绝缘性的聚合物导电,可在粘结剂材料中包括固有导电的聚合物。
适用于所述聚集体组合物中的任选组分可包括下列的一种或多种:可溶性的含稀土化合物、净化剂、杀生物剂、吸附剂、助流剂、非聚合物粘结剂和基底等。取决于所述组合物的预期效用和/或所需特性,所述聚集体组合物中可包含这样的任选组分。
任选的可溶性的含稀土化合物可具有不同的活性和作用。例如,已经认识到,一些可溶性的含稀土化合物具有抑菌作用或抗微生物作用。在“TheBacteriostatic Activity of Cerium,Lanthanum,and Thallium”,Burkes等,Journal of Bateriology,54:417-24(1947)中,氯化铈、硝酸铈、无水硫酸高铈、以及氯化镧被描述为具有这样的活性。类似地,在美国专利No.4,088,754中,描述了使用可溶性的铈盐例如硝酸铈、乙酸铈、硫酸铈、卤化铈和它们的衍生物、以及草酸铈用于燃烧处理,这样的描述在此引入作为参考。其它可溶性的含稀土化合物,无论本质上是有机的还是无机的,可赋予所述组合物其它期望的性能,且可任选地使用。
任选的净化剂可包括能够从各种表面上除去或解毒化学污染物的物质。可为适宜的净化剂的非限定性实例包括:过渡金属和碱金属,如美国专利No.5,922,926中所述的;多金属氧酸盐,如美国专利申请公开No.2005/0159307A1中所述的;氧化铝,如美国专利No.5,689,038和6,852903中所述的;季铵络合物,如美国专利No.5,859,064中所述的;沸石,如美国专利No.6,537,382中所述的;以及酶,如美国专利No.7,067,294中所述的。在此将在所提及的文献中的这些净化剂的描述引入作为参考。
对于将溶液或气体中的生物污染物作为目标,可任选地包含杀生物剂。适于用作杀生物剂的材料包括但不限于:碱金属、碱土金属、过渡金属、锕系元素、以及它们的衍生物和混合物。辅助(secondary)杀生物剂的具体的非限定性实例包括下列的元素或化合物:银、锌、铜、铁、镍、锰、钴、铬、钙、镁、锶、钡、硼、铝、镓、铊、硅、锗、锡、锑、砷、铅、铋、钪、钛、钒、钇、锆、铌、钼、锝、钌、铑、钯、镉、铟、铪、钽、钨、铼、锇、铱、铂、金、汞、铊、钍等。这样的杀生物剂的衍生物可包括乙酸盐、抗坏血酸盐、苯甲酸盐、碳酸盐、羧酸盐、柠檬酸盐、卤化物、氢氧化物、葡糖酸盐、乳酸盐、硝酸盐、氧化物、磷酸盐、丙酸盐、水杨酸盐、硅酸盐、硫酸盐、磺胺嘧啶、以及它们的组合。当所述聚集体组合物任选地包含含钛化合物例如氧化钛时,该含钛化合物与不溶性的含稀土化合物的重量比低于约2∶1。在所述聚集体组合物任选地包含含铝化合物时,该含铝化合物与不溶性的含稀土化合物的重量比低于约10∶1。在所述聚集体组合物的组分的一种或多种将被烧结时,所述组合物包含选自钇、钪和铕的不超过两种元素。在包含选自过渡金属、过渡金属氧化物和过渡金属盐的任选的杀生物剂的实施方案中,所述聚集体组合物包含低于约0.01重量%的银和铜的金属纳米颗粒的混合物。
可适于用作杀生物剂的其它物质包括:有机试剂,例如季铵盐,如美国专利No.6,780,332中所述;和有机硅化合物,如美国专利No.3,865,728所述。还可使用已知使生物污染物失活的其它有机物质及其衍生物。例如,多金属氧酸盐在美国专利No.6,723,349中被描述为在从流体中去除生物污染物方面是有效的。该专利提及M.T.的Heteropo1y and Isopoly Oxometalates,Springer Verlag,1983和Chemical Reviews,vol.98,No.1,第1-389页,1998作为描述有效的多金属氧酸盐的实例。在此将所提及的文献中的这些有机杀生物剂的描述引入作为参考。
所述聚集体组合物可任选地包含一种或多种助流剂。助流剂部分地用于改善流体在所述聚集体组合物上或者通过聚集体组合物的流体动力学、防止该聚集体组合物的组分的分离、防止细粒的沉降,且在一些情况下,使聚集体组合物保持在原位。合适的助流剂可包括有机材料和无机材料两者。无机助流剂可包括硫酸铁、氯化铁、硫酸亚铁、硫酸铝、铝酸钠、聚氯化铝、三氯化铝、二氧化硅、硅藻土等。有机助流剂可包括本领域已知的有机絮凝剂,例如聚丙烯酰胺(阳离子型、非离子型、及阴离子型),EPI-DMA(表氯醇-二甲胺)、DADMAC(聚二烯丙基二甲基-氯化铵)、双氰胺/甲醛聚合物、双氰胺/胺聚合物、天然瓜耳胶等。当存在助流剂时,可在聚集体组合物的形成过程中将助流剂与不溶性的含稀土化合物和聚合物粘结剂混合。或者,可将聚集体组合物的颗粒和助流剂的颗粒混合以得到物理混合物,所述助流剂均匀分散在整个混合物内。在另一可供选择的方法中,助流剂可布置于所述聚集体组合物的上游和下游的一个或多个不同的(distinct)层中。当存在助流剂时,通常以所述聚集体组合物的低于约20重量%,在一些情况下低于15重量%,在另外的情况下低于10重量%,且在还另外的情况下低于约8重量%的低浓度使用助流剂。
其它的任选组分可包括各种无机试剂,所述无机试剂包括:离子交换材料,例如合成离子交换树脂;活性炭;沸石(合成或天然存在的);矿物和粘土,例如膨润土、蒙脱石、高岭土、白云石、蒙脱土(montmorillinite)以及它们的衍生物;金属硅酸盐材料和矿物例如磷酸盐和氧化物类。具体地说,含有高浓度的磷酸钙、硅酸铝、铁氧化物和/或锰氧化物以及较低浓度的碳酸钙和硫酸钙的矿物组合物为适宜的。可通过许多方法对这些材料进行煅烧和加工,以获得不同组成的混合物。
该聚集体组合物的其它任选组分可包括添加剂,例如粒子表面改性添加剂、偶联剂、增塑剂、填料、膨胀剂、纤维、抗静电剂、引发剂、悬浮剂、光敏剂、润滑剂、润湿剂、表面活性剂、颜料、染料、UV稳定剂和悬浮剂。选择这些材料的量以提供所需的性能。
通过使流体与所述聚集体组合物接触,该组合物可用于对溶液或气体中的化学和生物污染物进行去除、失活或解毒。熟悉流体处理领域的技术人员应当理解,对于不同的应用可改变所述聚集体组合物的组分、外形尺寸和形状,且对这些变量中的改变可改变流速、背压以及组合物的用于处理一些污染物的活性。因此,取决于预期的使用方法,所述聚集体组合物的尺寸、形式和形状可显著改变。在其中使用聚集体组合物处理含砷水溶液的实施方案中,所述聚集体组合物可具有至少约50mg砷/克所述聚集体组合物的从溶液中去除砷的吸附能力。在一些情况下,该吸附能力为至少约60mg/g,且在另外的情况下至少约70mg/g。据信,该吸附能力部分取决于用于制备所述聚集体组合物的不溶性的含稀土化合物的表面积以及所得聚集体组合物的表面积。
可通过下列的一种或多种形成该聚集体组合物:混合;挤出;模塑;加热;煅烧;烧结;挤压;压制;使用粘合剂;和/或本领域中已知的其它技术。在其中期望所述聚集体组合物具有较高表面积的实施方案中,烧结是不太期望的。使用所述聚合物粘结剂使得能够产生用于处理溶液和气体的足够的尺寸、结构、和耐久性的聚集体组合物。所述聚合物粘结剂与不溶性的含稀土化合物的组合产生聚集体组合物,其具有用于对流体净化的提高的活性,而无需对处理的流体强加显著的(substantial)压力降。
所述聚集体组合物可包含能流动的颗粒、微粒、珠、小球、粉末、纤维或类似的形式。这样的颗粒的平均粒径可为至少约1μm、特别地至少约5μm、更特别地至少约10μm、且还更特别地至少约25μm。在另外的实施方案中,所述聚集体的平均粒径为至少约0.1mm、特别地至少约0.5mm、更特别地至少约1mm、还更特别地至少约2mm、且仍更特别地大于5.0mm。可对所述聚集体组合物进行粉碎、切割、切碎或研磨,然后筛分以获得所需粒径。这样的能流动的颗粒可用于固定或流化的床或反应器、搅拌反应器或罐中,分布在颗粒过滤器中,封装或封入在膜、网状物(mesh)、筛子、过滤物或其它流体渗透性结构体内,沉积在过滤器基底上,且可进一步成型为用于不同应用的所需形状例如片、膜、毡或整体料。
此外,所述聚集体组合物可引入过滤器基底中或涂覆到过滤器基底上。过滤器基底可包括本文所述的聚合物及非聚合物粘结剂材料、以及例如陶瓷、金属、碳等的材料。过滤器基底可由颗粒、纤维、片、膜、以及它们的组合制得。过滤器基底的结构取决于应用而改变,但可包括具有适于使用条件的所需形状和外形尺寸的任何流体渗透性结构体。非限定性实例包括网状物、筛子、膜、片、管、蜂窝状结构、整体料、以及包括圆筒形和环形的各种形状的块状体。
在另一实施方案中,本发明提供用于处理含有一种或多种污染物的流体的聚集体组合物的制造方法。该方法包括将不溶性的含稀土化合物与聚合物粘结剂混合以形成混合物的步骤。在上文中已经对所述不溶性的含稀土化合物和聚合物粘结剂材料进行了详细描述。在更具体的实施方案中,所述不溶性的含稀土化合物包括不溶性的含铈化合物的高表面积颗粒,更具体地经煅烧的碳酸铈的产物。可与所述不溶性的含稀土化合物混合的聚合物粘结剂的具体实例包括聚烯烃、乙酸纤维素、丙烯腈-丁二烯-苯乙烯、PTFE、纸纤维、玻璃纤维或玻璃珠、以及粘合剂聚合物。应当选择所述聚合物粘结剂以具有不超过所选的不溶性的含稀土化合物的烧结温度的熔点,因为所述不溶性的含稀土化合物的烧结可降低最终聚集体组合物的表面积。
本领域已知用于对颗粒和纤维进行混合的技术和设备可用于混合组分。使组分混合足以获得相对均匀的混合物的时间。此外,为了确保所述不溶性的含稀土化合物在整个聚集体组合物中更均匀的分布,在其中对混合物进行热处理的实施方案中,优选在加热前对组分进行彻底混合。
对混合物进行机械处理、化学处理和热处理的一种或多种,以使所述不溶性的含稀土化合物附着到所述聚合物粘结剂上。机械处理可包括压制、压缩、挤压、混合、挤出、以及使混合物经受振动或波。取决于聚集体组合物的所需性能,可在加热混合物之前、期间、或者之后,实施该混合物的压缩。可在压机、测试筒(test cylinder)、挤出机、或本领域已知用于将材料压缩或压制为所需形状或形式的其它设备中对混合物进行压缩。压力的大小以及施加这样的压力的持续时间取决于所选的组分、它们的粘结特性、以及聚集体组合物的预期用途。在一定范围内,施加较高的压力和/或施加压力较长的时间用于防止聚集体组合物在使用条件下降解或产生细屑。化学处理可包括化学转化以及使用化学粘合剂的一种或多种,例如本领域中已知的。例如,可使用交联剂以促进聚合物粘结剂的交联。热处理可包括将混合物加热至升高的温度以促进化学和/或物理转化。
在一个实施方案中,将混合物加热至低于所述聚合物粘结剂的熔点的温度,在该温度所述聚合物粘结剂软化且变得有延展性或触觉上发粘。应将混合物加热至足以确保所述不溶性的含稀土化合物附着于聚合物粘结剂上而不使该聚合物粘结剂完全熔化的温度。具体的温度取决于所选的聚合物粘结剂的组成。然后,可使该混合物冷却以形成聚集体组合物。
在一些实施方案中,所述聚合物粘结剂包含纤维、颗粒、纤维或颗粒的聚集体、以及其混合物的一种或多种,且当对混合物处理时,所述不溶性的含稀土化合物附着于所述聚合物粘结剂的外表面上。当所述不溶性的含稀土化合物为颗粒形式时,所述聚集体组合物产物可包含附着到所述聚合物粘结剂外表面上或包埋于所述聚合物粘结剂外表面中的不溶性的含稀土颗粒的基体。
任选的步骤可包括降低所述聚集体组合物的尺寸。可通过本领域已知的技术实现尺寸降低,包括切割、粉碎、研磨以及筛分所述聚集体组合物降至所需尺寸的一种或多种。
提供下列实施例以说明本发明的具体实施方案。本领域技术人员应当理解,下列实施例中所公开的方法仅代表本发明的示例性实施方案。但是,根据本发明的公开内容,本领域技术人员应当理解,不脱离本发明的精神和范围,可对所述特定实施方案进行许多改变并仍获得类似或相近的结果。
实施例1-粒状聚合物粘结剂
在该实施例中,由F(FN50100)(得自Equistar的低密度聚乙烯)制备聚集体。F为超细且球形的粉末,具有20微米平均粒径、23g/10分钟的熔体指数和92.0℃~114.5℃的熔化范围。铈氧化物(CeO2)得自HEFA Rare Earth Canada Company,Ltd.。
以不同组成(以重量计),由所述铈氧化物和聚合物制得物理混合物。称取各组分,并使用设定在≈160rpm下旋转的装有桨叶附件的实验室混合机混合约30分钟以获得均匀混合物。将内径为1.125英寸的Carver测试筒加热至从90℃到100℃变化的温度。将4克二氧化铈/聚合物混合物倒入到加温的模具中并加压至范围为3400磅/平方英寸~10000磅/平方英寸的压力。加压时间从5分钟到20分钟变化。在压制小球之后,将它们切割并在18×70筛上筛分以获得约500μm的颗粒。使用制造商的指定方法,在MicromeriticsFlowsorbII 2300单点BET仪上测定比表面积。
表1详细给出了参数组。
表1
温度(℃) | 压力(磅/平方英寸) | 时间(分钟) | 粘结剂% | SSA(m2/g) |
90 | 3400 | 5 | 2.5 | 107.74 |
90 | 10000 | 20 | 2.5 | 88.11 |
90 | 3400 | 20 | 10 | 79.01 |
95 | 6800 | 12.5 | 6.25 | 107.08 |
100 | 3400 | 5 | 10 | |
100 | 10000 | 5 | 2.5 | 102.45 |
100 | 3400 | 20 | 2.5 | 92.72 |
100 | 10000 | 20 | 10 | 38.67 |
实施例2-粒状聚合物粘结剂
在该实施例组中,由得自The Plastics Group of America的RPABS(丙烯腈-丁二烯-苯乙烯)三元共聚物形成聚集体。该热塑性树脂的熔体流动为4~8g/10分钟且维卡软化点为98.9℃。
对该ABS进行筛分以获得小于100微米的颗粒,然后,按照与实施例1相同的程序,使其与铈氧化物混合、压制并筛分。将测试筒的温度范围升高至105℃到110℃。其它所有参数均保持不变。然后,切割该4g小球并在18×70筛上筛分以获得500μm的平均粒径。如实施例1所述测定比表面积。
通过用10mg所制备的聚集体挑战500ml的400ppb砷溶液来测定砷能力。在NSF水中制备该溶液,并将pH调节至7.5。将500ml溶液和10mg材料均置于广口塑料瓶中,并翻滚24小时。在24小时之后,对该聚集体进行过滤并使用Agilent的7500CE型ICP-MS(感应耦合等离子体质谱仪)分析砷浓度。对于每种组合物,制备、测试和分析三个样品。所报告的As能力数据代表每种组合物的三个样品的平均值。
表2详细给出了参数组。
表2
温度(℃) | 压力(磅/平方英寸) | 时间(分钟) | 粘结剂% | SSA(m2/g) | As(V)能力(mg As/g材料) |
105 | 10000 | 5 | 10 | 91.68 | 1.33 |
107.5 | 6800 | 12.5 | 6.25 | 87.46 | 1.28 |
105 | 3400 | 5 | 2.5 | 115.54 | 4.38 |
105 | 10000 | 20 | 2.5 | 112.27 | |
110 | 3400 | 5 | 10 | 88.4 | 3.41 |
105 | 3400 | 20 | 10 | 114.86 | 2.95 |
110 | 10000 | 5 | 2.5 | 78.42 | 2.15 |
110 | 3400 | 20 | 2.5 | 89.48 | 4.11 |
110 | 10000 | 20 | 10 | 115.41 | 3.24 |
实施例3-具有硅藻土的粒状聚合物粘结剂
在该实施例中,对实施例2的参数组的改变仅在于加入硅藻土(DE)。DE的组成范围为1%~5%(以重量计),且其它所有参数和过程均保持不变。然后,切割该4g小球并在18×70筛上进行筛分以获得500μm的平均粒径。如前述实施例所述测定比表面积。
表3详细给出了参数组。
表3
温度(℃) | 压力(磅/平方英寸) | 粘结剂% | DE% | SSA(m2/g) |
110 | 3400 | 2.5 | 5 | 91 |
105 | 10000 | 2.5 | 5 | 75 |
105 | 3400 | 2.5 | 1 | 71 |
107.5 | 6800 | 6.25 | 3 | 72 |
110 | 3400 | 10 | 1 | 88 |
110 | 10000 | 2.5 | 1 | 73 |
105 | 10000 | 10 | 1 | 83 |
110 | 10000 | 10 | 5 | 64 |
105 | 3400 | 10 | 5 | 70 |
107.5 | 6800 | 6.25 | 3 | 83 |
实施例4
测试筒的温度在60℃到100℃之间改变,压制压力为3400磅/平方英寸~10000磅/平方英寸,且加压时间为0.5~5分钟。切割该4g小球并在18×70筛上进行筛分以获得500μm的平均粒径。如前述实施例所述测定比表面积。
表4列出了该具体实施例的参数矩阵(parameter matrix)。
表4
温度(℃) | 压力(磅/平方英寸) | 时间(分钟) | 粘结剂% | SSA(m2/g) |
80 | 6800 | 2.75 | 6 | 82.13 |
100 | 10000 | 5 | 10 | 84.02 |
60 | 10000 | 0.5 | 10 | |
60 | 3400 | 0.5 | 2 | |
100 | 3400 | 5 | 2 | 118.01 |
100 | 3400 | 0.5 | 10 | 87.28 |
80 | 6800 | 2.75 | 6 | 90.26 |
60 | 3400 | 5 | 10 | |
60 | 10000 | 5 | 2 | |
100 | 10000 | 0.5 | 2 |
实施例5-纤维状聚合物粘结剂
在该实施例中,使用得自Mini Fibers,Inc的ShortPolyethylenepulp制造聚集体。这些纤维是高密度的原纤化聚乙烯,具有125℃~136℃的熔化范围、0.1mm~0.6mm的长度和5μm的直径的热塑性材料。铈氧化物与前述实施例中所述的相同。
称取各组分,并使用设定在≈160rpm下旋转的装有叶片附件的实验室混合机混合约30分钟以获得均匀混合物。将内径为1.125英寸的Carver测试筒加热至从70℃到115℃变化的温度。将4克二氧化铈/聚合物混合物倒入到加温的模具中并加压至范围为3400磅/平方英寸~10000磅/平方英寸的压力。此时,加压时间也从30到120秒变化。切割该4g小球并在18×35筛上进行筛分以获得500μm的最小粒径。如实施例2所述测定比表面积和As能力。
表5详细给出了参数组。
表5
温度(℃) | 压力(磅/平方英寸) | 时间(秒) | 粘结剂% | SSA(m2/g) | As(III)能力(mg As/g材料) | As(V)能力(mg As/g材料) |
115 | 10000 | 120 | 7 | 81.8 | 6.22 | 1.26 |
115 | 3400 | 120 | 2 | 105.86 | 7.51 | 3.13 |
92.5 | 6800 | 75 | 4.5 | 74.91 | 5.72 | 1.62 |
70 | 10000 | 120 | 2 | 93.17 | 5.21 | 1.77 |
70 | 3400 | 120 | 7 | 90.19 | 7.41 | 2.07 |
115 | 10000 | 30 | 2 | 105.86 | 5.88 | 1.05 |
115 | 3400 | 30 | 7 | 144.81 | 5.43 | 1.07 |
70 | 10000 | 30 | 7 | 82.77 | 5.2 | 2.16 |
70 | 3400 | 30 | 2 | 102.85 | 5.72 | 2.82 |
92.5 | 6800 | 75 | 4.5 | 84.59 | 7.02 | 3.39 |
实施例6-具有硅藻土的纤维状聚合物粘结剂
除了加入硅藻土(DE)以外,使用与实施例5相同的材料和过程制备该实施例的聚集体。DE的组成范围为1%~5%(以重量计),粘结剂的组成范围为2%~5%(以重量计),且Carver测试筒的温度范围为70℃~115℃。压制压力和加压时间保持恒定为在6800磅/平方英寸下1分钟。切割该4g小球并在18×35筛上进行筛分以获得500μm的最小粒径。如实施例2所述测定比表面积和As能力。
表6详细给出了参数组。
表6
温度(℃) | 粘结剂% | DE% | SSA(m2/g) | As(III)能力(mg As/g材料) | As(V)能力(mg As/g材料) |
70 | 5 | 5 | 61.2 | 5.41 | 4.22 |
115 | 5 | 1 | 80.85 | 5.39 | 3.58 |
115 | 2 | 5 | 89.81 | 6.20 | 3.94 |
92.5 | 3.5 | 3 | 91.61 | 7.54 | 3.73 |
70 | 5 | 1 | 101.64 | 5.53 | 4.11 |
115 | 2 | 1 | 94.62 | 5.66 | 3.28 |
70 | 2 | 1 | 83.76 | 7.23 | 3.59 |
70 | 2 | 5 | 100.72 | 7.86 | 2.98 |
92.5 | 3.5 | 3 | 65.11 | 5.81 | 3.49 |
115 | 5 | 5 | 58.32 | 7.56 | 3.08 |
以上公开的具体实施方案仅为说明性的,因为本发明可以对于受益于本文中的教导的本领域技术人员来说显而易见的不同但等价的方式改进和实施。此外,除了权利要求书中所述的之外,没有限制用于在本文中所示的结构或设计的细节。因此,显然可改变或改进以上公开的具体实施方案,且认为所有这样的变化均在本发明的范围和精神内。因而,权利要求书阐述了本发明所要求保护的范围。
Claims (48)
1.用于处理含有一种或多种污染物的流体的聚集体组合物,该组合物包含:
占所述聚集体组合物的低于10重量%的聚合物粘结剂;
任选的可溶性的含稀土化合物;和
不溶性的含稀土化合物,其中所述不溶性的含稀土化合物占所述聚集体组合物的至少75重量%,其中所述不溶性的含稀土化合物包括一种或多种铈氧化物,其中所述一种或多种铈氧化物包括铈IV氧化物(CeO2),和其中所述聚集体组合物为能流动的颗粒或纤维的形式。
2.权利要求1的聚集体组合物,其中所述聚合物粘结剂为所述聚集体组合物的低于8重量%。
3.权利要求1的聚集体组合物,其中所述聚合物粘结剂包括选自如下的一种或多种聚合物:聚氨酯、有机硅、聚酰胺、聚烯烃、纤维素树脂、聚甲醛、聚酯、聚醚醚酮、天然橡胶、合成橡胶、三聚氰胺甲醛、脲甲醛、苯酚-甲醛树脂、增塑的聚氯乙烯、未增塑的聚氯乙烯、氟碳树脂、丙烯酸类树脂、聚乙烯醇、聚乙酸乙烯酯、乙烯-乙酸乙烯酯、和氯化聚乙烯。
4.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物以具有超过70m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
5.权利要求1的聚集体组合物,其中所述聚集体组合物具有60mg/g所述聚集体组合物的从水溶液中去除砷的吸附能力。
6.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物的颗粒具有至少0.5nm的平均粒径。
7.权利要求1的聚集体组合物,进一步包括一种或多种助流剂。
8.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物以具有超过115m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
9.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物的颗粒具有大于1nm的平均粒径。
10.权利要求7的聚集体组合物,其中所述助流剂选自:无机助流剂和有机助流剂。
11.权利要求1的聚集体组合物,其中所述能流动的颗粒或纤维的形式的聚集体组合物具有至少1μm的平均粒径。
12.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物以具有至少25m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
13.权利要求1的聚集体组合物,其中所述聚集体组合物具有选自至少50mg/g所述聚集体组合物的砷吸附能力的从水溶液中去除砷的吸附能力。
14.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物的颗粒具有至少100nm的平均粒径。
15.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物包括镧、铈、镨、钕、钷、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥的一种或多种。
16.权利要求1的聚集体组合物,其中所述聚集体组合物包括超过95重量%的所述不溶性的含稀土化合物。
17.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物以具有超过85m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
18.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物的颗粒具有至少10nm的平均粒径。
19.权利要求1的聚集体组合物,其中所述聚集体组合物包括两种或更多种不溶性的含稀土化合物,其中所述两种或更多种不溶性的含稀土化合物包括铈、镧和镨的一种或多种,和其中所述不溶性的含稀土化合物包含混合的化合价或氧化态。
20.权利要求1的聚集体组合物,其中所述可溶性的含稀土化合物选自硝酸铈、无水硫酸高铈、氯化镧、乙酸铈、硫酸铈、卤化铈和草酸铈,和其中所述不溶性的含稀土化合物以具有至少5m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
21.权利要求20的聚集体组合物,其中所述不溶性的含稀土化合物以具有至少25m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
22.权利要求20的聚集体组合物,其中所述不溶性的含稀土化合物的颗粒具有至少100nm的平均粒径。
23.权利要求1的聚集体组合物,进一步包括无机试剂和添加剂的一种或两者。
24.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物以具有超过10m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
25.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物的颗粒具有至少250nm的平均粒径。
26.权利要求1的聚集体组合物,其中所述粘结剂具有熔点,其中所述不溶性的含稀土化合物具有烧结温度,和其中所述聚合物的熔点不超过所述不溶性的含稀土化合物的烧结温度。
27.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物以具有至少1m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
28.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物的颗粒具有至少500nm的平均粒径。
29.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物包括附着于所述聚合物粘结剂外表面的颗粒。
30.权利要求1的聚集体组合物,其中当所述不溶性的含稀土化合物为颗粒形式时,所述聚集体组合物包括附着到所述聚合物粘结剂外表面上或包埋于所述聚合物粘结剂外表面中的不溶性的含稀土颗粒的基体。
31.权利要求1的聚集体组合物,通过包括如下的方法制造:
混合聚合物粘结剂和不溶性的含稀土化合物以形成混合物;和
对该混合物进行机械处理和热处理的一种或多种,以使所述不溶性的含稀土化合物附着到所述聚合物粘结剂上,
其中所述聚合物粘结剂占所述聚集体组合物的低于8重量%,
其中所述机械处理包括挤出,和
其中所述热处理包括将所述混合物加热至升高的温度和所述混合物冷却以形成聚集体组合物。
32.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物包含铈、镧和镨的一种或多种。
33.权利要求3的聚集体组合物,其中所述有机硅为氟代有机硅,其中所述聚酰胺为尼龙,其中所述聚烯烃为聚乙烯、与其它聚烯烃的聚乙烯共聚物、乙烯-丙烯-二烯三元共聚物、聚苯乙烯、聚丙烯的一种或多种,和其中所述纤维素树脂为乙酸丁酸纤维素,和其中所述聚酯为聚对苯二甲酸乙二醇酯或聚碳酸酯,其中所述合成橡胶为苯乙烯-丁二烯橡胶、氯丁橡胶、丁腈橡胶、丁基橡胶、聚氯丁二烯、氟化弹性体、氯磺化聚乙烯和烷基化的氯磺化聚乙烯的一种,和其中所述氟碳树脂为聚四氟乙烯。
34.权利要求33的聚集体组合物,其中所述聚乙烯为LDPE、LLDPE和HDPE的一种或多种,和其中所述氟化弹性体为全氟弹性体。
35.权利要求1的聚集体组合物,其中所述聚合物粘结剂包括酚醛树脂、热塑性共混物和热塑性接枝物的一种或多种。
36.权利要求1的聚集体组合物,其中所述聚集体组合物包括具有至少1μm的平均聚集体尺寸的聚集颗粒。
37.权利要求1的聚集体组合物,其中所述不溶性的含稀土化合物以具有超过160m2/g的平均表面积的微粒、晶体、微晶、粒子或颗粒的一种或多种的形式存在于所述聚集体组合物中。
38.权利要求1的聚集体组合物,其中所述聚集体组合物具有选自至少70mg/g所述聚集体组合物的砷吸附能力的从水溶液中去除砷的吸附能力。
39.权利要求23的聚集体组合物,其中所述无机试剂包括离子交换材料、活性炭、沸石、矿物或粘土,和其中所述添加剂选自偶联剂、增塑剂、填料、膨胀剂、纤维、抗静电剂、引发剂、光敏剂、润滑剂、表面活性剂、颜料、染料、UV稳定剂和悬浮剂。
40.权利要求39的聚集体组合物,其中所述离子交换材料包括合成离子交换树脂,其中所述沸石为合成或天然存在的沸石的一种,其中所述粘土为膨润土粘土、蒙脱石粘土、高岭土粘土、白云石粘土、和蒙脱土粘土的一种,其中所述矿物为磷酸盐或氧化物类矿物的一种,和其中所述表面活性剂为润湿剂。
41.权利要求23的聚集体组合物,其中所述无机试剂为硅酸铝,其中所述添加剂为粒子表面改性添加剂。
42.权利要求10的聚集体组合物,其中所述无机助流剂选自硫酸铁、氯化铁、硫酸亚铁、硫酸铝、铝酸钠、聚氯化铝、三氯化铝、二氧化硅和硅藻土。
43.权利要求10的聚集体组合物,其中所述有机助流剂选自阳离子型聚丙烯酰胺、非离子型聚丙烯酰胺、阴离子型聚丙烯酰胺、表氯醇-二甲胺、聚二烯丙基二甲基-氯化铵、双氰胺/甲醛聚合物、双氰胺/胺聚合物、和天然瓜耳胶。
44.权利要求31的聚集体组合物,其中所述聚集体组合物包括可溶性的含稀土化合物。
45.权利要求1的聚集体组合物,其中所述聚集体组合物包括可溶性的含稀土化合物。
46.权利要求1的聚集体组合物,其中所述能流动的颗粒为微粒或珠的一种。
47.权利要求46的聚集体组合物,其中所述微粒为小球或粉末的一种。
48.权利要求20的聚集体组合物,其中所述卤化铈包括氯化铈。
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- 2008-10-24 WO PCT/US2008/081079 patent/WO2009058676A1/en active Application Filing
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US20090111689A1 (en) | 2009-04-30 |
BRPI0816585A2 (pt) | 2015-09-08 |
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CA2703821A1 (en) | 2009-05-07 |
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EP2209743A4 (en) | 2012-02-29 |
US8349764B2 (en) | 2013-01-08 |
EP2209743A1 (en) | 2010-07-28 |
CL2009000853A1 (es) | 2010-12-24 |
JP2014111256A (ja) | 2014-06-19 |
EP2209743B1 (en) | 2019-07-03 |
JP2011502045A (ja) | 2011-01-20 |
BRPI0816585B1 (pt) | 2019-04-09 |
US8557730B2 (en) | 2013-10-15 |
MX2010004589A (es) | 2010-06-01 |
AR069155A1 (es) | 2009-12-30 |
ES2748278T3 (es) | 2020-03-16 |
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