CN1330822C - 用于改善表面的涂层组合物 - Google Patents
用于改善表面的涂层组合物 Download PDFInfo
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- CN1330822C CN1330822C CNB028043170A CN02804317A CN1330822C CN 1330822 C CN1330822 C CN 1330822C CN B028043170 A CNB028043170 A CN B028043170A CN 02804317 A CN02804317 A CN 02804317A CN 1330822 C CN1330822 C CN 1330822C
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Abstract
本专利公开了包括纳米微粒系统的涂层组合物、使用方法及制品,这种纳米微粒系统用来给所有类型的柔软表面(在有些情况下给硬表面)赋予表面改善性质。在一些实施方案中,人们通过利用纳米微粒在适当的载体介质中扩散发明了对被改善的表面有多种使用益处的涂层组合物、使用方法及制品。这些表面改善可以产生持久的或半持久的多种使用益处,在一些实施方案中,与未使用这样的纳米微粒系统改善的表面相比,可包括至少下列改善表面特性之一:易清洗、可湿性、液体过水性、舒适性、耐污染、污迹清除、恶臭控制、表面摩擦改善、减少柔软表面的磨损和色彩增强。
Description
相关申请交叉参考
此申请要求美国临时专利申请提交日期的优先权,其提交日期为2001年1月30日,序列号为60/265,013。
发明领域
本发明涉及涂层组合物、产品使用方法及制品,其包括纳米微粒系统或使用同样系统将表面改善应用于所有类型的软表面,在某些情况下可以是硬表面。
发明背景
无机微粒(例如粘土、硅酸盐和氧化铝)已经广泛应用于辅助清洁剂和洗涤剂化合物的合成,以带来某种形式的抗静电和/或织品软化的益处。
现有技术采用的一种方法公开了使用无机微粒的抗静电益处。描述这些用途的专利包括美国专利3,594,212和3,862,058。
织品软化益处在现有技术中已广泛公开。描述这些用途的专利包括:美国专利3,886,075;美国专利4,806,253;美国专利4,885,101;美国专利5,004,556;美国专利5,019,292;美国专利5,209,857和美国专利5,721,205。
众所周知,无机微粒可以用于某些类型的纺织品例如地毯的清洗、清洁和除臭。例如,请参阅实施例美国专利3,716,488(Stevens J& Co);3,736,259(Colgate Pomalive);4,035,148(P&G);4,090,974(FMC);4,566,980(Creative Products);4,581,385和4,873,000(Sterling Drug)。在实际当中,用于这些清洁组合物中的粘土粒径介于10至60μm(10,000至60,000纳米)之间。
其它专利和专利出版物包括:3,936,537(P&G 1976);3,954,632(P&G 1976);3,962,100(P&G 1976);3,989,631(P&G 1976);4,178,254(P&G 1979);4,844,824(P&G 1989);5,209,857(Lever1993);JP 6172657(Nippon Shirika 1994);EP753567(P&G 1997);WO01/32820(Henkel 2001);WO 01/44425(Lever 2001);WO01/44561(Lever 2001)和WO 01/83662(Henkel 2001)。
显而易见,需要能改善包含各种不同的天然、人造、和/或合成纤维的布料和织物材料特性的方法。某些类型纤维,例如合成聚酯或尼龙的疏水性质,或者由于材料(例如棉花)的老化所导致的织物疏水改性,引起了许多软表面性能问题,这些问题包括:清除疏水性污迹(清洗)时更加困难,来自清洗液的更大的亲和污物力(洁白/再沉淀/抗污性),身体污迹(恶臭)更久的保持力,改变颜色(颜色控制)时更困难和织品传输水分的能力更差(可湿性和舒适性)。同时,为了更好地适应消费者的需要,需要使改善的表面益处维持永久或半永久。
发明概述
本发明涉及组合物、产品使用方法及制品,其包括纳米微粒系统或者把表面改善应用于所有类型的软表面,在一些情况下可以是硬表面。在一些实施方案中,这些益处可以维持永久或半永久。这些多重用途的益处可能包括下列性质中的一项或多项:改善的表面易清洗性、可湿性、过水性、舒适性、抗污染性、污迹清除、恶臭控制、表面摩擦改善、磨损破坏减少和与未用此类纳米微粒系统改善的表面有关的色彩增强特性。这里列举了许多本发明的非限制性实施方案。所有的实施方案,即使它们仅被描述为本发明的实施方案,也被认为是非限制性的(也就是说,这些实施方案以外还可能有其它实施方案),除非它们在本发明中被清楚地描述为限制性的。
本发明的一个非限制方案提供了一种软表面涂层组合物,其包括:(a)有效数量的纳米微粒;(b)任选的一种表面活性剂;(c)任选的和所述纳米微粒有关的一种或多种带电功能化分子,它们表现出来的性质选自亲水性、疏水性和混合性质;(d)任选的一种或多种辅助成分;和(e)一种适当的载体介质。
另一个非限制方案提供了一种使用涂层组合物改善软表面的方法,这种方法包含以下步骤:(a)把涂层组合物应用于软表面,和(b)让涂层组合物干燥后在软表面上形成涂层;和(c)如果需要,任意重复(a)和(b)中的任何步骤。
另一个非限制方案提供了一种包括涂抹器,例如喷涂器、浸渍容器、软管喷涂分配器附件、织物和/或海绵的制品,其中涂抹器包括:(a)如本发明所述的涂层组合物,其中涂层组合物的物理形态可以是液体、浓缩液、凝胶体、粉末、片剂、粒状体和其混合形态;和(b)任选的一种去离子水源;(c)任选的一种自来水源,和(d)任选的一套与该涂抹器有关的使用说明,其中包括把所述涂抹器中的涂层组合物分散到软表面上以改善该表面的说明。
应用改善软表面的表面涂层一定不可留下易察觉的残渣(例如,可见的或有气味的),否则将不会被客户所接受。纳米颗粒涂层相对于其它表面改善剂(例如,成膜聚合物)的优点在于它能够在表面上提供基本上不可见的膜。适当的纳米微粒涂层组合物可以提供一种透明的涂层,或者也可以选择适当的涂层组合物以提供一种纺织品表面上的独特的色彩增强。色彩增强为已经褪色的或穿旧的衣物提供颜色恢复和/或防止衣物掉色。可供选择地,纳米微粒可以和释放剂(例如亲水表面聚合体)结合使用以促进纳米微粒沉积并且提高表面改善的耐久性。
使用本发明中有益的化学剂材料(即纳米微粒系统)处理过的基质在不同的实施方案中可以在以下方面表现出更大的改进:易清洁性、可湿性、过水性(水分/液体通过该些基质传输)、舒适性、抗污染性、污迹清除、恶臭控制、表面磨损改善、磨损破坏减少和与那些没有用上述利益剂材料处理的基质相比所得到的色彩增强特性。
这些和其它实施方案、目的、特征和优点通过阅读后文中的详细描述、实施例和附加的权利要求书将会变得非常清楚。
除非另有说明,本发明的所有百分数、比率和比例均以纯产品重量计算。
附图简述
虽然说明书结尾的权利要求书已明确指出并清楚地声明了对构成本发明的主题进行保护,但相信结合以下描述与附图可以更好地理解本发明,其中:
图1是柔软表面的示意性侧视图,若干层纳米微粒在表面上形成涂层,并且部分纳米微粒涂层上带有污迹。
图2是与图1类似的示意性侧视图,仅仅显示如何通过除去纳米微粒顶层来清除沉积在涂层上的污迹。
图3也是与图1和2类似的示意性侧视图,显示进行移除过程中的进一步骤。
发明详述
定义
本说明中所用的术语“涂层”包括覆盖全部表面或部分表面的涂层(例如,连续涂层,包括在表面上形成薄膜的连续涂层),和仅仅覆盖部分表面的涂层,例如那些干燥后在表面的被覆盖区域留下间隙的涂层(例如,不连续涂层)。后一种涂层包括但不限于覆盖区域和未覆盖区域的交错区域,和那些纳米微粒间存在空隙的表面上的纳米微粒分布。在一些实施方案中,涂层优选地在已经涂过的表面上形成至少一层基本均匀的纳米微粒。但是,本说明中被描述为施用于表面的涂层,应知道涂层可以不覆盖整个表面,也可以覆盖整个表面。例如,即使涂层仅仅用于改善表面的一部分,它也被认为是应用于这个表面的。
光敏性纳米微粒是指那些需要用紫外光或可见光激活涂层使之具有亲水性的纳米微粒,如下列专利所描述的:日本专利1181339 A2;日本专利11172239 A2;日本专利10297436 A2;日本专利10046759 A2;日本专利09056549 A2;日本专利00128672 A2;日本专利00096800 A2;日本专利11300303 A2;日本专利10237431 A2;日本专利10212809 A2;日本专利09230107 A2和日本专利09228072 A2。获得上述激活效应所需要的紫外光或可见光的强度一般和太阳光的强度相当。
软表面
本说明中涉及的软表面包括任何已知的软表面,包括但不限于织物、衣物、纺织品和薄膜。在某些实施方案中,软表面可能包括一种或多种纤维。纤维被定义为一种来自动物、植物、矿物或合成来源的精微毛细结构体。可商购获得的纤维的粒径范围为小于约0.001mm(约0.00004in)至大于约0.2mm(约0.008in),并呈几种不同的形式:短纤维(一般是用作原料的纤维或切碎的纤维)、连续的单根纤维(细丝或单丝)、分开的成束的连续细丝(丝束)和搓成束的连续细丝(纱线)。纤维根据其产地、化学结构或同时考虑上述两方面进行分类。它们可以编成绳和索,制成毡(也称为无纺布或非纺织布),编织或针织织物,或者,如果是高强度纤维,则可用作混合物,也就是,用两种或更多不同的材料制成的产品中的加固成分。
软表面可以包括天然的(天然纤维)、人造的(合成或人造)纤维,或其组合物。天然纤维的实施例包括但不限于动物纤维,例如羊毛、丝绸、皮毛和毛发;植物纤维,例如纤维素、棉花、亚麻、亚麻制品和苎麻;和某些天然存在的矿物纤维。合成纤维可来自天然纤维或其它途径。来自天然纤维的合成纤维的实施例包括但不限于人造丝和溶胞,它们都来自纤维素(一种天然多糖纤维)。非来自天然纤维的合成纤维可从其它天然资源或矿物资源中得到。来自天然资源的合成纤维的实施例包括但不限于多糖,例如淀粉。来自矿物的纤维实施例包括但不限于例如聚丙烯纤维和聚乙烯纤维等聚烯烃纤维,它们来自石油和硅酸盐(例如玻璃与石棉)纤维。如果可能,合成纤维一般通过流体处理工艺(例如,挤压、汲取或旋转诸如树脂或溶液等流体)加工形成。合成纤维也可通过固体尺寸缩小处理工艺(例如,机械切碎或切割诸如独块制品、薄膜或织品等较大物体)加工形成。
不考虑其来源,当今许多合成纤维都得自有机聚合材料,并由长链有机高分子组成。聚合高分子包括多个一种或多种类型的重复单元。重复单元来自单体,这些单体经过化学反应形成重复单元链或束。聚烯烃高分子链通过加成聚合反应形成。大多数其它高分子链是通过缩聚反应形成的。单个的链可任选具有支链,也可以没有。单个的高分子链通常具有不同程度的从结晶区到非晶体区之间的形态。纤维中的高分子可以是热塑性的或热固性的。在一定压力下,热塑性纤维可以在达到分解温度之前通过加热至高分子链的流动温度进行软化。典型地,和高分子链交联的热固性纤维可以加热软化,但不可能在到达分解温度前软化至流动温度。
许多合成纤维由一种或多种树脂制成,其中树脂中的高分子链是预先形成的。树脂可以任选地包含一种或多种添加剂。添加剂的实施例包括但不限于表面活性剂、染色剂、溶剂和交联剂例如自由基引发剂。树脂可以是热塑性的或热固性的。由交联前可流动的热固性树脂所形成的纤维可以在纤维成形产生热固性的期间或其后进行交联。普通合成纤维树脂包括但不限于尼龙(聚酰胺)、丙烯酸(聚丙烯腈)、芳纶(芳族聚酰胺)、聚烯烃(聚乙烯和聚丙烯)、聚酯、丁二烯-苯乙烯嵌段共聚物、天然橡胶、胶乳和弹性纤维(聚氨酯)。热塑性树脂可以由产家分级、再处理或综合处理。如果相邻的重复单元的立体专一性不同,则必须谨慎选择树脂的立体专一性,以得到所需的满足最终用途的纤维性能。也要谨慎选择树脂的分子量分布,以得到所需的满足最终用途的纤维的中间性能。在一个非限制性实施例中,高分子量定型聚合的聚丙烯树脂是聚丙烯纤维的共同选择,因为合成纤维结构有许多在不同的中间和最终用途中被需要的性能。间规立构和无规立构聚丙烯可以产生不同的中间和最终性能。
包括多种重复单元的合成纤维可以通过分子水平上的重复单元的组合而得到,这种组合可以在每个高分子链(共聚物)内进行,也可在高分子链(均聚混合物)之间进行,或者以两种方式联合进行(共聚物混合物);重复单元的组合也可在较大尺度水平的纳米相、微相或宏相中进行(例如多组分纤维)。多组分纤维的每一组分都可以包括均聚物、共聚物或二者的混合物。双组分纤维是多组分纤维的常见形式。在共聚物中,两种或多种类型的重复单元可以随机排列,或两种类型交互嵌段排列。不同类型的重复单元嵌段可以在它们各自的终点互相连接(嵌段共聚物),或在至少一个嵌段的终点连接(接枝共聚物)。
无纺材料是典型地用纤维制成的一类网状格式的织物。无纺布描述在由ButlerI、BatraSK等人于1999年编写的非纺织织品手册(Nonwovens Fabrics Handbook)(非纺织织品行业协会)和由VaughnEA编写的非纺织的织品样品和技术参考数目(非纺织织品工业协会)中。
无纺布可以通过直接挤压加工形成,在加工过程中,纤维和网在大约同一时间点形成,或者预制纤维可以在较晚的时间点置入网中。直接挤压加工实施例包括但不限于纺粘法、熔吹法、溶剂旋转法、电镀旋转法和这些方法的组合来典型成层。“成层”加工的实施例包括湿法成层和干法成层。干法成层加工实施例包括但不限于气法成层、梳理和这两种方法的组合。上述方法的联合使用产生的无纺布通常称为混合材料或复合材料。联合使用方法的实施例包括但不限于纺粘-熔吹-纺粘法(SMS)、纺粘-梳理法(SC)、纺粘-气法成层法(SA)、熔吹-气法成层法(MA)和上述方法在层中典型的联合使用。包括直接挤压的组合可以在和直接挤压大约同时间进行(例如,SA和MA的旋转形与联合形),也可在稍后的时间内进行。在上述实施例中,一个或多个单独层可以通过各个加工处理过程形成。例如,SMS可以指一个三层“sms”网、一个五层“ssmms”网,或者任何适当的变体,在本说明中小写字体表示单个层,大写字母指出相似、相邻层的编制。
无纺布的纤维典型地在一些重叠连接的区域与一种或多种相邻纤维相连。这包括在每一层内连接的纤维及多于一层时层与层之间连接的纤维。纤维可以通过机械缠结、化学联结或这两种方法的组合进行连接。
机械缠结法包括所述的使用媒介物的方法、不使用媒介物的方法和两者的组合。不受理论的约束,媒介物在分子水平上部分地扩散到与它连接的纤维表面上(例如,物理吸附和范德华力作用),或者它在媒介物刚性增加(或“固化”)之前在纳米相、微观相或宏观相水平流进表面不规则部分或弯曲部分周围,或二种方式同时进行。媒介物可以以下列的形式使用:溶剂,溶剂能够软化纤维表面并使之流动;流体,能够流动然后固化,例如粘合剂;固体,例如热塑性粘合剂纤维;微粒,至少其中的一部分在加热或加压下能够流动然后重新固化。一种非限制性的热塑纤维粘合剂是双组分纤维,例如由熔点较低的聚乙烯外壳包围的聚丙烯核。一种非限制性的微粒粘合剂是胶乳粘合剂。加热或加压粘结可以导致作为媒介物的热塑性纤维或微粒粘合剂流动,但不会导致无纺布纤维必然以非纺织纤维、粘合剂和非纺织品方法为所述流动设计的相同程度流动(例如,通过选择低熔点的媒介或减少的热质媒介物)。线圈缠结是使用媒介物的机械缠结法的另一实施例,在加工过程中,细丝在高速织布机中粘结在纤维周围以连接纤维和纤维层。不使用媒介物的机械缠结法包括使一部分纤维(例如,纤维表面的一部分)扩散或流动的方法,和不涉及流动的方法。那些不包含媒介物但却包含流动的机械缠结法的实施例包括但不限于特定的热粘结和气压粘结方法。不受理论的约束,在上述热粘结和气压粘结方法中,一部分纤维表面(单组分或多组分纤维),在分子水平上扩散到与其连接的纤维表面上(例如,物理吸附和范德华力作用),或者在媒介物刚性增加(或“固化”)之前在纳米相、微观相或宏观相水平上流进表面不规则部分或弯曲部分周围,或者两种方式同时进行。热粘结可以通过以下方法实现:传导(例如热压光)、对流(例如热空气通过)、辐射热传输或者综合使用多种方法。那些不包含媒介物或纤维表面扩散或流动的机械缠结法的实施例包括但不限于针式穿孔法和典型的水缠结法。在针式穿孔法和水缠结法中,纤维自身的某些部分受移动的针或喷水口施加到纤维的机械力作用,环绕着附近纤维的表面弯曲部分发生弯曲或者移动。不受理论的约束,沿纤维间弯曲的路径间的摩擦提供了足够的力来维持其后的缠结。
化学粘结法包括那些使用媒介物的方法、不使用媒介物的方法和综合方法。典型地,除了采用化学键的方式外,化学粘结法和某些机械缠结方法相似。化学键包括从共价键(高强度)到氢键(低强度)之间范围内的各种键。不受理论的约束,某些化学粘结(或者化学吸附)与某些机械缠结(或者物理吸附)之间的界线有时很难分辨,并且当获得了所需的最终用途性能时,这些相对于最终用途的应用来说并不重要。
纤维和无纺布在形成后可能需要附加处理。对于无纺布来说,附加处理通常在纤维互相粘结后(后处理)进行。附加处理的实施例包括但不限于机械应力、化学添加剂或二者的组合。机械应力施加的方向可以是加工方向(MD)、垂直加工方向(CD)、垂直平面方向(z方向)或其组合。机械应力方法在本领域众所周知,它包括但不限于通过不同的技术达到的MD拉伸、CD拉伸、和z-方向的穿孔或切割,其中许多技术可以在不同的时间应用于部分或全部织物。机械后处理的实施例包括但不限于活化、环轧、同一化、拉伸、切割、切片和冲孔。
化学添加剂方法在本领域众所周知。化学添加剂可以通过不同的技术应用于单根纤维的一部分或全部周围,也可应用于织物的一面或两面,其中的许多技术可以在不同的时间段把化学添加剂应用于纤维或织物的一部分,或者应用于所有纤维或整个织物。化学添加剂可以采用固相、液相、气相添加,也可作为高能表面处理例如辐射、辐射氧化或等离子处理的结果添加。高能表面处理也可以用于促进纤维表面上或其附近材料的化学变化。一个非限制性固相技术的实施例是喷洒,在喷洒过程中气体(空气)在下降的宏观微粒间起分散剂的作用。另一个非限制性固相技术的实施例是起分散剂作用并且运载宏观微粒的空气流。在空气流的实施例中,空气是载体介质。液相技术的实施例包括但不限于喷射、浸渍、通过一个或多个滚筒(例如单面给液辊)传输,和传输印刷(例如旋转连续式印刷、照相凹版印刷和多功能图形印刷)。一个液相添加剂的实施例是把疏水性纤维表面变为亲水性的表面活性剂。典型的高能表面处理包括但不限于电晕放电处理、等离子处理、紫外辐射处理、离子束处理、电子束处理和某些包括脉冲激光的激光处理。某些高能表面处理产生的纤维表面或附近的添加剂或化学变化包括但不限于表面附近空气中的氧气中生成臭氧、在表面产生自由原子团或电子或其它基团或带电物质、表面侯选高分子的交联。典型地,作为交联侯选分子的高分子已经把相关功能添加到分子链中,例如双键或包含羟基的支链。
与大多数高能表面处理相关的共同局限性是耐用性问题,特别是对于热塑性表面。通过不同的高能表面处理传输到热塑性表面的部分或全部电荷会随着时间慢慢消失,半衰期有时从数天到数周不等。不受任何特定理论的约束,对这种现象的一种解释是空气中的氧气导致了部分或全部电荷之间的排斥。由于大多数热塑性聚合体的表面具有流动性,部分或全部电荷可旋转进入聚合物相内部,然后远离或无法接近与表面接触的电荷。
与纤维的高能表面处理相关的共同局限性典型地超出了相同材料的薄膜的局限性,特别是但不限于非穿孔薄膜。不受任何特殊理论的约束,关键的区别是表面几何形态。虽然薄膜在纳米水平上具有三维的表面外形,但与纤维相比较,就高能表面处理目的而言,薄膜可以在更大尺度上被视为近似二维的结构(长度与宽度决定仅在边缘处需考虑的厚度)。纤维,包括纤维织品的三维几何形状,使其厚度尺寸比薄膜的厚度尺寸更需要加以考虑。与许多薄膜相比,大多数纤维产生了组成表面区域的多个边界。此外,多数织品拥有与假想平面不相邻的纤维表面,该假想平面可以通过穿过织品任一侧最外层纤维的表面来绘制。事实上,上述非相邻纤维表面的一部分经常被视为隐蔽带。与多数纤维织品相关的局限性,是获得高能表面处理或任何通过高能表面处理产生并且部分或全部渗透到隐蔽带的电荷。所述局限性有时称为屏蔽。相反,由与纤维织品相同的材料组成的普通薄膜,例如非穿孔薄膜,如果它具有与纤维织品差不多的表面区域和纳米级外形,则具有较少的隐蔽带。当在高能表面处理中用足够多的剂量时,上述薄膜受剂量作用的表面区域将比上述纤维织品大。典型地,平均而言,薄膜表面的平均电荷密度将比织品纤维表面大。随着电荷的消失,纤维织品的局限性将继续存在。纤维织品具有更大的耗散电荷的表面区域,这些电荷开始主要位于朝外的纤维表面上。一个非限制性实施例是把定型聚合的聚丙烯树脂薄膜(约1米长×1米宽×150微米厚)和定型聚合的聚丙烯纺粘的无纺布比较,后者在通过无纺布任一边的最外层纤维所在表面绘制的假想平面间测量的厚度为约150微米,并且纤维表面区域与上述薄膜的表面区域大约相等的情况下,所述纺粘无纺布将具有更多的隐蔽带。
无纺布典型的特点是长度大于宽度、宽度大于厚度。无纺布或本身构成最终用户产品或者构成中间产品,这些中间产品可以随后转化为其他中间产品,并最终转化为最终用户产品。在转化为最终产品前被作为中间产品储存时,无纺布一般缠绕成卷形(连续长片)或包装成束状。
无纺布通常与组成复合织物的其它无纺布或薄膜相连。这些织物可以按照前面描述的方式进行粘结,粘结后的产品通常称为层压布。非限制性层压布的实施例是一次性的吸收性产品底片(例如尿布底片),其中无纺布与薄膜相连(例如多微孔薄膜)。层压布中不同的层宽度各不相同,以产生复杂的织物。未被切割成单个片段(特别是成品片段)的吸收性产品织物,是层压织物尤其是复杂织物的一个示例。
在制造过程中可确定的性能有:声学和热学性能、抗拉伸和抗破裂强度、空间稳定性、硬度、弹性、悬垂性、柔软度、流体传输或斥水性、抗磨损性、静电充电和其它在生产过程中特定条件下对于中间和最终产品很重要的织物特性。模制纤维产品为设计工程师在设计声学绝缘器时提供了更大的自由,它具有不同的厚度、密度和匹配外形的表面一致性,由此改善配合、修整和安装的容易程度。模制纤维产品的重量、密度和外形制造范围都很大。
纳米微粒系统
纳米微粒系统可以包括原料、组合物、设备、装置、步骤、方法、条件等,它们服务于共同的目的:改善表面(例如软表面,或者某些情况下硬表面)从而带来所需益处。这些益处可以经受表面的多重使用,许多益处包括但不限于下列一种或多种:改善的表面清洁、可湿性、过水性、舒适性、抗污染性、污迹清除、恶臭控制、表面摩擦改善、磨损破坏减小和与未用纳米微粒系统改善的表面相比得到的色彩增强特性。
可以使用的纳米微粒可以包括最大尺寸(例如直径)小于或小于等于约750nm(纳米)的微粒。本说明中有用的微粒还可包括任何最大尺寸小于或小于等于任一小于750nm的数值的且变化量为5nm的微粒,某些情况下甚至包括更大尺寸的微粒。本说明引入和包含的,即在此处明确说明的是微粒尺寸的全部变化范围为0nm至750nm。应知道,视情况而定,此说明全文给出的每一限制将包括每一个较低或较高的限制,如本说明已经明确说明的这些较低或较高的限制。此说明给出的每一范围都包括位于较大范围中的每一较小范围,如本说明中已经明确说明的此类较窄范围。这些微粒在技术上是非常重要的,因为它们可以用于形成结构、涂层和设备,这些结构、涂层和设备都因为其微粒组分非常小的尺寸而具有新的有用特性。从经济角度来说,可以生产尺寸为约2nm至约750nm范围的纳米微粒。纳米微粒的非限制性实施例中的微粒尺寸分布范围为约2nm至小于约750nm,或者是为约2nm至小于约200nm,或者为约2nm至小于约150nm。应知道,微粒尺寸的某些范围可能有助于提供某些益处,而其它范围的尺寸可能会提供其它益处(例如,色彩增强需要与其它特性不同的微粒尺寸范围)。不同类型微粒的平均尺寸可能随着微粒尺寸分布而不同。例如,一种层状合成硅酸盐可以具有约25纳米的平均微粒尺寸,同时它的微粒尺寸分布一般在约10nm至约40nm之间。应知道,本说明中描述的微粒尺寸是对散布在含水介质中的微粒而言的,平均微粒尺寸是以微粒数分布的平均值为基础的。非限制性的纳米微粒实施例可以包括结晶体或非晶体微粒,微粒尺寸为约2nm至约750nm。勃姆石氧化铝的平均微粒尺寸分布为2nm至750nm。纳米管可以包括长达1厘米的结构,其中微粒尺寸为约2nm至约50nm。
涂层组合物可以包括:纳米微粒;任选表面活性剂;任选与纳米微粒表面有关的一定数量的一种或多种功能化表面分子,这些分子可以具有亲水性、疏水性或混合性质;任选的一种或多种附加成分;一种适当的载体介质;并可在表面形成透明涂层。
有机纳米微粒在药理学领域应用广泛,而无机纳米微粒则广泛应用于消费者领域。无机纳米微粒一般以氧化物、硅酸盐、碳酸盐和氢氧化物形式存在。一些层状粘土矿物和无机金属氧化物都可能是纳米微粒。适合在本发明中使用的层状粘土矿物包括以下地质学类矿物:蒙脱石、高岭土、伊利石、绿泥石、凹凸棒石和混合层粘土。属于这些类型的具体粘土的典型实施例有蒙脱土、高岭土、伊利石、绿泥石、凹凸棒石和混合层粘土。举例来说,蒙脱土包括蒙脱石、膨润土、叶蜡石、锂蒙脱石、滑石、锌蒙脱石、绿脱石、云母、贝得石、铬高岭石和蛭石。高岭土包括高岭石、地开石、珍珠陶土、叶蛇纹石、蠕陶土、多水高岭石、indellite和温石棉。伊利石包括水白云母、白云母、钠云母、金云母和黑云母。绿泥石包括绿泥间蛭石、抗火蛭石、片桂铝石、铝绿泥石、叶绿泥石和斜绿泥石。凹凸棒石包括海泡石和polygorskyte。混合层粘土包括钠板石和蛭石黑云母。这些分状粘土矿物的变体和同形代替提供了独特的应用。
层状粘土矿物质可以是天然的也可以是合成的。一个涂层组合物的非限制性实施方案的实施例使用合成和天然的锂蒙脱石、蒙脱石和膨润土。另一实施方案使用可商购获得的锂蒙脱石粘土,可商购获得的锂蒙脱石的典型来源是来自美国Southern Clay Products,Inc.的LAPONITEsTM;来自美国R.T.Vanderbilt的Veegum Pro和Veegum F;来自美国Baroid Division,National Read Comp.的Barasyms、Macaloids和Propaloids。
天然粘土-天然粘土矿物典型地以层状硅酸盐矿物的形式存在,很少以非结晶矿物的形式存在。层状硅酸盐矿物具有排列成二维网络结构的SiO4四面体薄片。2∶1型层状硅酸盐矿化物具有几个或几十个硅酸盐薄片构成的层压结构,其中的硅酸盐薄片具有三层结构,镁八面体薄片或铝八面体薄片夹在两层硅四面体薄片之间。在一些实施方案中,希望涂层组合物包括多个纳米微粒,其中纳米微粒包括除2∶1型层状硅酸盐以外的不同类型(第一组)纳米微粒。应知道,这组纳米微粒涉及此种类型的纳米微粒,即它们可能以任何方式分布在整个涂层组合物中,而不需要聚集在一起。另外,即使在这些方案中涂层组合物可能包含至少一些(可能是非功能性数量)包括2∶1型层状硅酸盐(它可能包括第二组纳米微粒)的纳米微粒。
可延展分层硅酸盐薄片带有负电荷,由于碱金属阳离子和/或碱土金属阳离子的存在,负电荷可以被中和。蒙脱石或可延展云母可以分散在水中形成具有触变性质的溶胶。此外,用不同的阳离子有机或无机化合物进行反应,可以生成复杂的多种蒙脱石变体。例如,此种有机化合物的例子-亲有机质粘土,就是通过交换阳离子引入二甲乙醇铵离子(一种四元铵离子)的,这种粘土已经进行工业生产,并用作涂层胶凝剂。
人造粘土-通过合适的工艺控制,合成纳米级粉末(即人造粘土)的生产工艺的确可以生产初级的纳米级微粒。然而,这些微粒通常不以离散微粒的形式存在,而是主要以凝聚团的形式存在,这是初级微粒固结的结果。这些凝聚团直径可能高达几千纳米,这就导致与微粒纳米级大小相关的所需性质不能体现出来。这些微粒可以散开,例如,通过EP-A637,616所描述的研磨,或者通过散布在合适的载体介质中如水或水/酒精和其混合物。
以下纳米级粉末的生产是普遍的,例如层状含水硅酸盐、层状含水硅酸铝、氟代硅酸盐、云母-蒙脱石、水滑石、锂镁硅酸盐和锂镁氟代硅酸盐。锂镁硅酸盐替代变体的一个例子是用氟取代部分羟基。也可用铝代替部分锂和镁。事实上,锂镁硅酸盐可以从由镁、铝、锂、铁、铬、锌和其混合物中任选一种进行同形代替。
人造锂蒙脱石第一次合成于十九世纪六十年代早期,今天Southern Clay Products,Inc.是用LAPONITETM商标进行商售。市场上有许多LAPONITETM的等级或变体以及同形代替物。商用锂蒙脱石的实施例有:LAPONITE BTM、LAPONITE STM、LAPONITE XLSTM、LAPONITE RDTM、LAPONITE XLGTM)和LAPONITE RDSTM。本发明的一个实施方案使用具有以下特征的LAPONITE XLSTM:分析(干燥质)SiO2 59.8%,MgO 27.2%,Na2O 4.4%,Li2O 0.8%,结构H2O 7.8%,另外焦磷酸四钠盐(6%);比重2.53;堆密度1.0。
人造锂蒙脱石例如LAPONITE RDTM不含氟。氟同形取代氢氧基将会产生名为钠镁锂氟代硅酸盐的人造粘土。这些以LAPONITETM和LAPONIT ESTM出售的钠镁锂氟代硅酸盐可包含约10%重量百分比的氟离子。应知道,本说明所描述的有用的氟离子含量包括从0至10之间的任意整数或小数百分比,或者更大。LAPONITE BTM,一种钠镁锂氟代硅酸盐,具有扁平圆盘式外形,平均粒径由氟离子的含量决定,此直径可以是约25至100纳米范围内的任何值(或更窄范围内的值)。例如,在一个非限制性的实施方案中,LAPONITE BTM的直径可以在约25至40纳米之间,其厚度为约1纳米。另外一种称为LAPONITE STM的变体包含约6%的焦磷酸四钠作为添加剂。
微粒最大直径与最小直径的比率称为微粒的纵横比。在某些情况下,纳米微粒的纵横比对于形成有所需性质的薄膜非常重要。LAPONITEBTM的单个微粒的平均纵横比为约20至40,LAPONITE RDTM的单个微粒的平均纵横比为约10至15。在一些实施方案中,在使用纳米尺寸的粘土材料形成薄膜时需要较大的纵横比。散布在合适载体介质(如水)中的微粒纵横比也是非常重要的。对于分散媒体中的微粒,可以认为几个微粒聚集时纵横比低于单个微粒的纵横比。分散体的纵横比可以通过TEM(透射电镜)测量。LAPONITE BTM在分散体中基本上以单个粘土微粒或两个粘土微粒堆积的形式出现。LAPONITE RDTM基本上以两个或多个粘土微粒堆积的形式出现。这样,如果发生单个微粒聚集的情况,散布在载体介质中的微粒纵横比将受影响。在某些非限制性实施方案中,如果至少一些(最好是多个)单个(非聚集的)板状和盘形纳米微粒具有至少大于等于0.5纳米的直径和大于等于约15的纵横比是可取的。LAPONITE BTM的纵横比是约20至40,LAPONITE RDTM的纵横比小于15。同杆状微粒相比,板状和盘形微粒要求有较大的纵横比。纳米尺寸粘土的纵横比明显小于天然粘土的纵横比,后者的纵横比典型地大于250纳米。
杆状微粒,例如小的勃姆石氧化铝(例如Disperal P2TM),在维持充分成膜特性的同时,其纵横比低于盘形或板状微粒的纵横比。在某些非限制性实施方案中,如果至少一些(最好是多个)单个(非聚集的)杆状纳米微粒具有至少大于等于0.5纳米的直径和大于等于约3的纵横比是可取的。
球状纳米微粒的纵横比一般小于等于约5。氧化铝、纳米胶乳、氧化钛和一些勃姆石氧化铝是低纵横比纳米微粒的非限制实施例。本实施方案在此处优选的纳米微粒,其纵横比小于等于约250nm。在其它的非限制性实施方案中,纳米微粒的纵横比小于约10是可取的。
LAPONITETM,锂镁硅酸盐的分子式如下:
[MgwLixSi8O20OH4-yFy]z-
其中w等于3至6,x等于0至3,y等于0至4,z=12-2w-x,全部晶格负电荷可以由电性相反的离子中和;电性相反的离子选自:Na+、K+、NH4 +、Cs+、Li+、Mg++、Ca++、Ba++、N(CH3)4 +或它们的混合离子。(如果LAPONITETM使用阳离子有机化合物“中和”,则“反离子”就是任何阳离子有机基团(R)。)
根据具体应用,使用LAPONITETM的变体和同形替代物可以在对本发明的涂层组合物的所需特性进行工程设计时提供更大的灵活性。LAPONITETM的单个板状粒子表面带负电,并且在与水交界的表面上浓度较高。根据本实施方案,当水或水/表面活性剂或水/酒精/表面活性剂等合适的载体介质应用于基片时,软表面改善后可能具有亲水性,也可能表现出令人惊奇的性质,并且显著提高表面清洁、可湿性、过水性、舒适性、恶臭控制、表面摩擦改善、减少磨损破坏和色彩增强等特性。另外,LAPONITETM改善后的表面也可表现出污迹清除(抗污染性、清除污迹)等特性,因为纳米涂层的顶层可以通过适度的机械作用或化学方法剥离。
无机金属氧化物-无机金属氧化物一般有两类纳米微粒:光敏性和非光敏性。光敏性金属氧化物纳米微粒的普通实施例包括氧化锌和氧化钛。光敏性金属氧化物纳米微粒需要来自可见光(例如,氧化锌)或紫外光(TiO2)的光敏化作用。氧化锌涂层一般用作抗微生物试剂或抗污染剂。应知道,光敏纳米微粒可以应用在涂层组合物中,即使它们没有光敏化,也能提供益处。
应用于组合物的无机金属氧化物可以是天然的或人工合成的二氧化硅或氧化铝纳米微粒。在许多天然矿产中可以发现铝,例如高岭石和铝矾土。天然的氧化铝矿产可以通过霍尔(Hall)工艺或贝尔(Bayer)工艺生产所需要的氧化铝。商业上可用的各种形态的氧化铝来自Condea,Inc厂家的三水铝矿、一水硬铝石和勃姆石。
勃姆石氧化铝([Al(O)(OH)]n)是一种水分散性的无机金属氧化物,它可以精制成具有不同的颗粒尺寸或尺寸范围,包括平均微粒径为约2nm至小于等于约750nm的微粒。例如,North American Sasol,Inc生产的平均粒径为约25nm、商标名为Disperal P2TM、平均粒径为约140nm、商标名为Dispal14N4-25的勃姆石氧化铝纳米微粒。
非光敏性金属氧化物纳米微粒不需要使用紫外光或可见光来产生所需效果。非光敏性金属氧化物纳米微粒的实施例包括但不限于无水硅酸、氧化锆、氧化铝、氧化镁、和勃姆石氧化铝纳米微粒以及混合氧化物纳米微粒,包括但不限于蒙脱石、滑石粉和水滑石。
无机金属氧化物纳米微粒与层状粘土相比具有额外的益处,即无需胶凝就可制作无机金属氧化物的浓缩溶胶,这对于应用涂层组合物前进行稀释特别有利。另外,无机金属氧化物纳米微粒可以给软水提供耐受性,这些软水用于制作纳米微粒分散体、稀释纳米微粒分散组合物,和表面包含软水离子的纳米微粒组合物的应用。
纳米胶乳-“胶乳”是一种由球状不溶于水的聚合物微粒构成的胶体分散系。本发明所使用的“纳米胶乳”是一种粒径小于或等于约750nm的胶乳。纳米胶乳可以通过乳液聚合作用形成。在“乳液聚合作用”过程中,使用表面活性剂把胶乳单体分散在水中形成稳定的乳液,然后所述乳液发生聚合作用,这个过程中产生的粒径为约2至约600nm。
带电的功能化分子
本发明使用的术语“功能化”涉及改变表面的特性。被功能化的表面可能是具有纳米微粒涂层的软表面(或基质),或者是纳米微粒本身。功能化分子为软表面和纳米微粒提供改进的特性,或者稳定或增强纳米微粒在表面上的吸附。
软表面(或基质)的亲水性改善可以通过两步来完成,首先把纳米微粒(例如LAPONITETM)用作底部涂层或顶部涂层,然后使用功能化带电分子处理带负电的表面。如果需要,可以添加额外的纳米微粒和功能化带电分子涂层,例如,使用超过两步的方法提供相同的交替层。
带电功能化表面分子包含至少两种不同类型的功能化表面分子。带电功能化表面分子选自下列物质:聚合物、共聚物、表面活性剂和其混合物。功能化表面分子也可以选自含有下列多价离子的无机盐:Ca+2、Mg+2、Ba+2、Al+3、Fe+2、Fe+3、Cu+2和其混合离子,并使用一种合适的阴离子来中和电荷。
LAPONITETM和乙氧基化或季铵化的低聚胺的顺序分层导致了被处理表面接触角的减小及延展性/可湿性的增加。此外,如果带电功能化分子含有亲脂性组分,则经过LAPONITETM处理的表面的疏水性就改变了。纳米粘土和带电功能化分子联合使用为调整软表面的亲水性/亲脂性性质提供了一种新的方法。
同样地,亲水性改善也可以通过两步来实现,首先把氧化铝用作底部涂层或顶部涂层,然后使用功能化带电分子处理带正电的表面。特别是氧化铝和亲水性阴离子聚合物的顺序分层导致了被处理表面延展性/可湿性的提高。此外,如果带电功能化分子含有亲脂性组分,则经过氧化铝处理的表面的疏水性就改变了。无机金属氧化物和带电功能化分子联合使用为调整软表面的亲水性/亲脂性提供了一种新方法。
I.组合物
本发明的涂层组合物可以呈任何形态,例如液体(含水的或不含水的)、粒状体、糊状物、粉末、喷雾、泡沫、片状、凝胶体等等。粒状组分可以是“压缩”形式的,而液体混合物也可以是“浓缩”形式的。在一个非限制性实施方案中,涂层组合物可以是液体。而在其它非限制性实施方案中,涂层组合物可以是液体清洁剂。
涂层组合物可以应用于所有类型的软表面,包括但不限于纺织纤维、非纺织纤维、皮革、塑料、人造薄膜和其混合物。应知道,在某些实施方案中,涂层组合物可以应用于硬表面并提供益处。
在一些实施方案中,涂层组合物可以包括:(a)多个纳米微粒,可以是有效数量的纳米微粒;(b)任选的一种或多种附属成分;和(c)一种合适的载体介质。也应知道,根据实施方案,用在本说明中所描述的各种涂层组合物中的纳米微粒可以是光敏性的、非光敏性的或混合性能。在这些或其它实施方案中,涂层组合物还可以包括如下一种或多种组分:表面活性剂;一种或多种带电功能化分子,这些分子具有亲水性、疏水性或其混合性能,这些性能与至少一些所述纳米微粒相关;或者同时包括二者。
此外,上述有效数量的纳米微粒被包含在组合物中,这些组合物用于对需要处理的软表面进行涂层。本发明使用的“有效数量的纳米微粒”涉及使用特定组合物提供所需软表面涂层益处的所必需的纳米微粒数量。这些有效数量很容易由本领域的普通技术确定,它由许多因素决定,例如被使用的特定纳米微粒、软表面涂层应用、软表面涂层化合物的具体成分、所需混合物是液体的还是干燥的(例如,粒状、粉末),等等。
有效数量的纳米微粒(例如天然粘土、人造粘土或无机金属氧化物)可能需要至少改善目标表面的约0.5%才能实现所需益处。
在一个非限制性实施方案中,如下制备涂层组合物:把干的纳米微粒粉末分散到去离子水中以形成1%至5%的浓缩混合物。在另一实施方案中,如下制备涂层组合物:用去离子水稀释纳米微粒凝胶以形成1%至5%的浓缩混合物。在另一非限制性实施方案中,如下制备涂层组合物:用去离子水稀释10%的浓缩勃姆石氧化铝(例如Disperal p2TM或来自North American Sasol,Inc.的Disperal14N4-25)涂层组合物以形成1至5%的浓缩混合物。在另一非限制性实施方案中,如下制备涂层组合物:用去离子水稀释1%的浓缩钠镁锂氟代硅酸盐(例如来自Southern Clay Products,Inc.的LAPONITE BTM)涂层组合物以形成0.1%的浓缩混合物。在另一非限制性实施方案中,如下制备涂层组合物:用去离子水稀释1%的浓缩锂镁钠硅酸盐(例如来自KoboProducts,Inc.的Lucentite SWNTM或LAPONITE RDTM)以形成0.1%的浓缩混合物。在另一非限制性实施方案中,如下制备涂层组合物:把干的纳米微粒粉末分散到去离子水中以形成0.1%的浓缩混合物。所有这些混合物都可在清洗过程中添加涂层组合物而应用到到表面上,并通过喷涂、浸渍、涂刷、擦拭或其它方式以得到涂层,特别是覆盖表面至少约0.5%(或更大)的透明涂层,包括但不限于至少约5%、至少约10%、至少约30%、至少约50%、至少约80%和至少约100%。
如果采取喷涂方式,涂层组合物的粘度应该可以使自身能通过喷涂设备的喷嘴。这些粘度众所周知,引入本发明中用作参考。混合物可以具有这样的粘性:当它处于“静止”状态时,它可以有较高的静止粘度,并且可以剪切稀释以便喷涂。
向纳米微粒表面提供亲水和/或疏水性质的有效数量带电功能化表面分子,定义为改善从约1%到约100%的纳米微粒表面,或者定义占涂层组合物的重量约0.01%至约5%。
下面进一步详细讨论使用了纳米微粒的各种涂层组合物的几个实施例。涂层组合物也可以包含占涂层组合物重量的约0.01%至约99.99%的附属材料。
本发明使用的“涂层组合物”包括手工和机械应用的组合物,这些组合物包括附加组合物和适合于应用于软表面浸湿和/或预处理的组合物。本发明的涂层组合物和/或使用产品的方法和/或制品适用于如下用途,包括制造业用途、商业和工业用途和/或家庭用途。
本发明的涂层组合物也可用作固体或液体形式的清洁剂附加产品。这种附加产品用来补充或提高用于清洁软表面的常规清洁剂组合物的性能,并且可以在清洁过程中的任何阶段添加,但在漂洗时添加更有效。通过密度可以最好地反映本发明涂层组合物的“紧密”程度,而以组合物的形式,则是通过无机填充盐的数量来反映这种程度的;无机填充盐是粉末状涂层组合物的常规成分。在常规涂层组合物中,填充盐占很大分量,典型地为占总组合物重量的17%至35%。在压缩混合物中,填充盐的分量不超过总组合物重量的15%、也可以不超过10%、也可以不超过5%。无机填充盐包括但不限于硫酸盐和氯化物的碱金属盐和碱土金属盐。优选的填充盐是硫酸钠。
根据本发明,含水液体涂层组合物也可以是“浓缩形式”的,在这种情况下,浓缩液体涂层组合物与常规液体清洁剂组合物相比,将包含较少量的水。典型地,浓缩液体涂层组合物的含水量可以小于涂层组合物重量的40%、也可小于30%、也可小于20%。
本发明包含液体涂层组合物或者含水液体涂层组合物。液体涂层组合物也可包含本说明描述的纳米微粒之外一种合适的载体介质。载体介质可以占涂层组合物重量的任意合适的比例,包括但不限于约10%至约99%,也可为约30%至约95%。合适载体介质包括能够形成纳米微粒的稳定分散体的介质。介质的实施例包括但不限于水、去离子水、甲醇、酒精、乙醇、丙酮和乙二醇及其混合物。
涂层组合物可以包含一种或多种附属材料或任选成分。不同的任选成分描述如下。如果附属材料与涂层组合物的其它成分不能共存,则可以使用适当的方法,把不能共存的附属材料与其它成分分离(不互相接触)直到适当的时候再结合两种成分。适当的方法可以是本领域任何已知方法,例如凝胶帽、密封、压片、物理分离等等。
涂层组合物也可以用作自动洗衣机的液态清洁剂附加用品。涂层组合物如果是液体,则可以是任意适当形式,包括但不限于各向同性液体、含水凝胶、多相液体组合物和/或有色液体组合物。涂层组合物也可以用作粉末、微粒、片剂或胶囊形式的清洁剂附加用品。这种附加用品可以补充或提高常规清洁剂组合物的性能,并且可以在清洗过程中的任何阶段添加,包括但不限于洗涤或漂洗阶段。
合适载体介质
合适的载体介质包括液体、固体和气体。一种合适的载体介质是水,可以是蒸馏水、去离子水或自来水。水的优点在于它的低价格、可用性、安全性和相容性。尽管含水载体介质比干燥无水介质更常用,但本发明也可以是干燥粉末、微粒或片剂或胶囊复杂形式。
任选地,除水之外或代替水,载体包括低分子量的有机溶剂。优选的溶剂是易溶于水的物质,例如乙醇、甲醇、丙醇、异丙醇和类似物质及其混合物。低分子量醇可以减小分散体的表面张力以提高软表面的可湿性。当软表面具有疏水性时,这特别有用。低分子量醇也有助于快速干燥处理表面。任选的水溶性低分子量溶剂可以以任何合适的用量水平使用。几个非限制性例子,以总组合物的重量计算,包括以下水平:高达约50%或更高;约0.1%至约25%;约2%至约15%;约5%至约10%。在涂层组合物中使用高水平用量溶剂时,需要考虑的因素有纳米微粒的气味、易燃性、分散性与环境的影响。
带电功能化分子的种类
聚合物种类和实施例
在本发明的组合物中,聚合物是任选的成分。必要时,组合物可以完全不含聚合物。
如果在本发明的非限制性方面使用聚合物,则聚合物作为两(或更多)步骤方法的一部分。在此类方法中,纳米微粒组合物可以应用于软表面以在表面上形成一层纳米微粒。在此纳米微粒层形成和干燥后,包含所需聚合物的组合物可以应用于纳米微粒层以进一步改善纳米微粒涂层表面。不受任何特殊理论的约束,当通过此方式应用聚合物组合物时,据信纳米微粒层把聚合物固定在软表面上。这种方法与单独使用纳米微粒相比,可以提供各种性质的纳米微粒涂层表面。在把聚合物应用于纳米微粒然后再把聚合物涂层纳米微粒应用于软表面时,使用这种两步骤方法是有优势的。一个优势是,两步骤方法通过纳米微粒首层的一致性为表面提供的涂层比通过在软表面上沉积聚合物纳米微粒形成涂层更加连续。另一优势是,与未改善的表面相比,通过提高聚合物层与纳米微粒涂层表面的相互作用,可以增加聚合物层的耐用性。
可以使用这样的聚合物和共聚物,其中至少一个链段或一个基团有助于固定或提高对纳米微粒表面的吸附功能。这些聚合物也可以包含至少一个有助于向吸附在纳米微粒上的聚合体提供附加特性链段或基团。附加特性的非限制性实施例包括亲水性或疏水性。注意,在一些情况下,固定的链段也会有助于提供附加特性。
固定的链段或基团的实施例包括聚胺、季铵化聚胺、氨基、季铵化氨基及其相应的胺氧化物;两性离子聚合体;多羧酸盐;聚醚;多羟基聚合物;缩聚磷酸盐和多磷酸盐;和聚合螯合物。
亲水性链段或基团的实施例包括:乙氧基化聚胺或烷氧基化聚胺;聚胺;多羧酸聚胺;水溶性聚醚;水溶性多羟基基团或聚合物,包括糖类和多糖;水溶性羧酸盐和多羧酸盐;水溶性阴离子基团,例如羧酸盐、磺酸盐、硫酸盐、磷酸盐、膦酸盐及其聚合物;水溶胺、季胺盐、胺氧化物及其聚合物;水溶性两性离子基及其聚合物;水溶性酰胺和聚酰胺;水溶性乙烯咪唑与乙烯吡咯烷酮的聚合物和共聚物。
疏水性链段或基团的实施例包括烃基、烯基、芳基和聚合脂肪族烃或聚合芳香族烃;碳氟化合物和包含碳氟化合物的聚合体;聚硅氧烷;疏水性聚醚,例如聚氧化苯乙烯、聚环氧丙烷、聚环氧丁烷、聚氧化四氢呋喃和聚十二烷基缩水甘油醚;和疏水性聚酯,例如聚已内酯和聚3-羟羧酸。
亲水性表面聚合物
亲水表面聚合物的实施例包括但不限于乙氧基化聚胺或烷氧基化聚胺;多羟基羧酸聚胺;多羟基羧酸盐包括但不限于聚丙烯酸酯;聚醚;多羟基材料;缩聚磷酸盐和膦酸盐。
疏水性表面聚合物
烷基聚胺包括但不限于使用脂肪烷基化试剂(例如,十二烷基溴化物、十八烷基溴化物、油烯基氯化物、十二烷缩水甘油醚和苯甲基氯化物及其混合物)进行烷基化的聚乙烯亚胺;使用脂肪酰化剂(例如甲基十二烷基羧酸盐和油酰氯)进行酰基化的聚乙烯亚胺;聚硅氧烷,包括但不限于带有悬垂氨丙基或氨基乙氨基丙基的二甲基聚硅氧烷;氟化聚合物包括但不限于包含烷基被全氟化或高度氟化的(甲基)丙烯酸酯作为单体的聚合体。
非聚合材料
也可以使用这样的分子,其中至少一个链段或基团具有帮助固定或提高纳米微粒表面吸附的功能。这些分子也可以包含至少这样的一个链段或基团,它们有助于向吸附在纳米微粒上的分子提供附加特性。附加特性的非限制性实施例可包括亲水性或疏水性。注意,在一些情况下,固定链段也可以有助于提供附加特性。
可以用作亲水性链段的固定链段或基团的实施例包括氨基、季铵化氨基及其相应的氧化胺基团;两性离子基团;羧酸基。
疏水性链段或基团的实施例包括烷基、芳基、烷芳基、硅氧烷、聚硅氧烷、氟代醚和带有阳离子、两性离子、半极性、非电离或阴离子首基的氟代烷基表面活性剂。
非聚合的表面改善材料的实施例
可以使用的脂肪胺和季胺包括:二牛油二甲基铵氯化物;辛基癸基三甲基铵溴化物;二油基胺;和卞基十四烷基二甲基铵氯化物。
基于碳氟化合物的表面活性剂的实施例包括:短列氨基酸,3-[[(十七氟代辛基)磺酰基]氨基]-丙基-N,N,N-三甲基胺碘化物(9CI)
短列氨基酸,3-[(8-氯代-2,2,3,3,4,4,5,5,6,6,7,7,8,8-十四氟代-辛酰基)氨基]-丙基-N,N,N-三甲基胺甲基硫酸化物(9CI)
基于聚硅氧烷的表面活性剂包括:短列氨基酸,3-[1-甲基-1-[(三甲基硅烷基)氧]硅烷基]-丙基-N,N,N-三甲基胺溴化物(9CI)
脂肪族两性离子表面活性剂包括:长列氨基酸,N-(2-羟基-3-磺丙烷基)-N,N-二甲基-十二烷基内盐(9CI)
其中包括脂肪族胺氧化物,例如己基癸基二甲基胺氧化物。脂肪族阴离子表面活性剂包括:油基硫酸钠;油酸钾;十二烷基苯磺酸盐;十四烷基硫酸钠和2-己基癸基丁二酸二钠。
表面活性剂
在本发明的一些实施方案中,表面活性剂是一种任选成分。在涂层组合物中,表面活性剂作为润湿剂促进了纳米微粒在软表面上的分散,这是特别有用的。当涂层组合物用于处理疏水性软表面时,或者当为了提高涂层组合物的喷涂特性并且让其(包括纳米微粒)分布更均匀而使用喷涂器施用涂层组合物时,表面活性剂皆可包含在其中。涂层组合物的分散也能让它更快干燥,这样被处理材料就可以更快地投入使用。对于浓缩组合物来说,表面活性剂可以促进许多附属成分的分散,例如抗菌活性剂和芳香剂。
合适的表面活性剂选自阴离子表面活性剂、阳离子表面活性剂、非离子表面活性剂、酸碱兼性表面活性剂、两性表面活性剂、两性离子表面活性剂及其混合物。合适的非离子、阴离子、阳离子、两性、两性离子和半极性非离子表面活性剂的例子公布在美国专利5,707,950和5,576,282中。非离子表面活性剂的特征是其HLB(亲水性-亲脂性平衡)为5至20或者为6至15。
在涂层组合物中使用表面活性剂时,可添加有效的数量以促进涂层组合物的应用和/或提供一种或多种本发明中所述的益处。典型地,表面活性剂可以占混合物重量的约0.01%至约60%或更大,或此范围内的任何数量(包括但不限于约0.01%至约20%和约0.01%至约10%)。
表面活性剂,包括其它非离子表面活性剂在本发明中使用,其重量百分率典型地为约1%到约50%的非限制实施例包括:常规的C11-C18烷基苯磺酸盐(“LAS”)和直链、支链和不规则C10-C20烷基硫酸盐(“AS”),C10-C18二级(2,3)烷基硫酸盐,其化学式为CH3(CH2)x(CHOSO3 -M+)CH3和CH3(CH2)y(CHOSO3 -M+)CH2CH3,其中x和(y+1)是至少为约7的整数,也可以至少为9,并且M是一种水溶性阳离子,特别是不饱和硫酸钠,例如油基硫酸盐、C10-C18烷基烷氧基硫酸盐(“AExS”;特别是EO1-7乙氧基硫酸盐)、C10-C18烷基烷氧基羧酸盐(特别是EO1-5乙氧基羧酸盐)、C10-18甘油醚、C10-C18烷基多糖苷和它们相应硫酸化多糖苷,和C12-C18a-磺化脂肪酸酯。如果需要,常规非离子和酸碱兼性表面活性剂,例如C12-C18烷基乙氧基化合物(“AE”),包含所谓的窄峰烷基乙氧基化物和C6-C12烷基苯酚烷氧基化物(特别是乙氧基化物和混合乙氧基/丙氧基化物)、C12-C18内铵盐、和磺酸化内铵盐(“硫酸化内铵盐”)、C10-C18胺氧化物和类似物质,也可包含在整个组合物中。也可用C10-C18N-烷基多羟基脂肪酸酰胺。典型的实施例包括C12-C18N-甲基葡萄糖酸酰胺。请参阅WO9,206,154。其它用糖制成的表面活性剂包括N-烷氧基多羟基脂肪酸酰胺,例如C10-C18N-(3-甲氧基丙基)葡萄糖酸酰胺。低起泡可以使用N-丙烷基通过N-己基C12-C18葡萄糖酸酰胺。也可使用C10-C20普通肥皂。如果需要高起泡,也可使用支链C10-C16肥皂。阴离子和非离子表面活性剂的混合物特别有用。其它常规的有用的表面活性剂列在标准文本中。
聚硅氧烷表面活性剂和/或聚硅氧烷是涂层组合物的另一有用成分,它可以溶解和/或散布聚硅氧烷润滑剂和/或包含聚硅氧烷的附属形状保持共聚物。它们可以单独使用和/或与上面本发明所描述的优选烷基乙氧基表面活性剂联合使用。聚硅氧烷表面活性剂的非限制性实施例是聚烯基氧化物聚硅氧烷,它拥有疏水性的二甲基聚硅氧烷和一条或多条亲水性聚烯基侧链,并且通式为:
R1-(CH3)2SiO-[(CH3)2SiO]a-[(CH3)(R1)SiO]b-Si(CH3)2-R1
其中a+b可从约1至约50中选择,每一R1可以相同或不同,并可从甲基和聚(乙烯基氧化物/丙烯基氧化物)共聚物基中选择,后者通式为:
-(CH2)nO(C2H4O)c(C3H6O)dR2
其中n为3或4;c(对于所有的多烯基氧侧基)为1至约100,或者为约6至约100;d为0至约14;或者为0;c+d为约5至约150或者约9至约10,每一R2可以相同或不同,它可以是氢、1至4个碳原子的烷基、乙酰基、或者氢和甲基。每个多烯基氧化物聚硅氧烷有至少一个R1基,即一个聚(乙烯基氧化物/丙烷基氧化物)共聚物基。来自Dow Corning的聚硅氧烷超级润湿剂,即聚硅氧烷乙二醇共聚物(例如Q2-5211和Q2-5212)是可用的。
涂层组合物,如果用于自动洗涤阶段,可以和常规清洁剂一起使用,也可实际在漂洗或预干燥阶段用于漂洗。涂层组合物可以包含一个纳米微粒系统和任意的表面活性剂或表面活性剂系统,其中表面活性剂可以是非离子和/或阴离子和/或阳离子和/或酸碱兼性和/或两性离子和/或半极性非离子表面活性剂。
表面活性剂也可和涂层组合物中的纳米微粒系统、合适的载体介质和任意附属成分匹配。
任选成分
涂层混合物可以包含其它任选的成分,包括但不限于碱性源、抗菌防腐剂、抗氧化剂、抗静电剂、漂白剂、漂白活化剂、漂白催化剂、蓝色漂白剂、助洗剂、介质、螯合剂、氨基羧酸盐螯合剂、着色剂、颜色成斑剂、调节剂、可水解助表面活性剂、染料、染色转移剂、分散剂、酶、非活性酶、酶稳定化系统、填充盐、荧光剂、杀真菌剂、昆虫和蛀虫防护剂、杀菌剂、水溶助物、金属盐、光敏性无机金属氧化物、光敏性纳米微粒、有机溶剂、气味控制材料、光亮剂、污迹清除聚合物、香料、光敏剂、聚合物、防腐剂、加工助剂、颜料和pH值调节剂(描述在美国专利5,705,464;5,710,115;5,698,504;5,695,679;5,686,014;5,576,282;5,646,101中)、增溶剂、抑泡剂、表面活性剂、水溶性重碳酸盐、润湿剂、紫外吸收剂、沸石及其混合物。这些任选的成分的含量以任意所需用量水平使用。
II.使用方法
概要
本发明的涂层组合物可以用来改善软表面,方法是把涂层组合物涂抹于表面并让其干燥,也可根据需要重复涂抹和其它任意的干燥方法。涂层组合物涂抹后的干燥是一种优选但可选择的方法。在本发明所描述的一些实施方案,包括但不限于涂抹多于一个涂层中,并不必须在应用过程中干燥涂层。
本发明所描述的术语“干燥”和“正在干燥”是指一种状态或过程,在此状态或过程中,液体涂层组合物比涂抹时含有更少的水分或液体。这些术语也可包含任意下列的状态:涂层组合物所涂抹的表面部分干燥;涂层在测试方法章节指定的实验室条件下处于平衡状态;在涂层中没有多余的水分,水的量是涂层在40℃/100%相对湿度下的吸水极限;涂层“完全干燥”,尽管这种干燥程度除指定外并不要求。
涂层组合物可以使用任何合适的方式涂抹于表面。当涂层组合物要涂抹的表面至少部分浸入涂层组合物液体(浸渍过程)时,或者没有浸入涂层混合物的表面(非浸渍过程)时,涂层组合物可以涂抹于表面。使用的具体方法包括但不限于(1)直接或间接地把涂层组合物应用于表面;(2)在清洗表面过程中把涂层组合物应用于表面;和(3)在漂洗表面过程中把涂层组合物应用于表面。另外,涂层组合物可以在另外类型的表面处理过程(如漂白、交联包含软表面的材料)中涂抹于表面。
通过使用多种多样的涂抹方法和设备可以实现涂层组合物的分配,这些设备包括但不限于喷涂设备、浸渍容器、印刷机、洗衣机、软管喷涂附件、滚筒、衬垫等等。在其它非限制性实施方案中,混合物可以使用喷涂管(或者其它合适的方式)进行涂抹,例如织品制造设备、衣物制造设备、专业干洗和/或洗烫设备。在其它非限制性实施方案中,混合物可以在密封空间由个人涂抹,例如橱柜或类似物体。本说明书所描述的涂层、涂层组合物、产品使用方法和制品可以应用于所有类型的操作和环境,包括但不限于制造(包括但不限于纺织品和/或衣物制造和生产后处理)、商业(包括但不限于干洗或洗烫操作)、工业、社会公共机构、农业和家庭环境。选择的涂抹方法和设备通常根据软表面涂层混合物的生产和涂抹方法而定。
任选的提高表面接受涂层组合物能力的方法
在任何本说明所描述方法的实施方案中,执行下一步骤是可取的:用某种合适的方式准备软表面从而提高表面接受涂层组合物的能力。例如,通过增加来更改或改变软表面的表面能量是可取的。这尤其适用于疏水性或临界亲水性纤维软表面。
疏水性或临界亲水性软表面包括但不限于诸如编织、纺织和非纺织品材料,这些材料由疏水性或临界亲水性结构成分组成。编织、纺织和非纺织材料的结构成分可以包括纱线、绳索、纤维、细丝或其它构件。部分或全部构件可为疏水性、临界亲水性或混合性能。疏水性构件其表面的全部或部分包含疏水性材料(例如一种多成分纤维,它以一种或多种材料为核心,这些材料部分或全部由疏水性外壳包围)。同样地,临界亲水性构件其表面的完全或部分包含临界亲水材料。如果构件表面同时包含疏水性材料和临界亲水性材料,那么认为它是疏水性的。疏水性物质通常是人造聚合体、共聚体、混合物或其组合。实施例包括但不限于聚烯烃(例如聚丙烯和聚乙烯)、某些聚酯(例如聚乙烯对苯二酸酯(PET))和某些聚酰胺。临界亲水性材料通常可以是人造聚合物、共聚物、混合物或其组合。实施例包括但不限于表现临界亲水性的聚酰胺和聚酯。具有临界亲水性的聚酯包括最近被命名为亲水性聚酯的聚酯类。一实施例是PET/支链聚乙烯乙二醇(支链PEG)共聚体,例如来自美国北卡罗来纳洲夏洛特Wellman,Inc.的T870、T289和T801级。另一个实施例是带有脂肪族重复单元而不是PET的部分或全部芳香族重复单元的聚合体。来自Cargill DowPolymers,LLC,Blair Nebraska的聚交酯(或聚交酯酸或PLA)聚合体包含脂肪族重复单元。
涂层表面接受涂层组合物的能力可以通过很多不同的方法提高。
本发明已讨论过,一种提高材料表面接受涂层组合物能力的方法是通过使用表面活性剂。表面活性剂减少了基于水的纳米微粒分散剂的表面张力,从而提高软表面的可湿性。润湿表面很重要,因为它允许分散剂携带纳米微粒穿过更大的表面区域,从而增加覆盖。
表面活性剂适用于多种应用,对于以上所述的一些疏水性或临界亲水性材料,当材料在使用中随后再次湿润时,涂层残留的表面活性剂可能特别难以解决,例如可传输流体的物品中,包括但不限于纺织品、吸收剂产品和一次性吸收产品,例如尿布和其它失禁和月经产品(例如女性衬垫,在使用过程中接触一种或更多种液体(例如尿、月经、汗和其它身体分泌物))。在使用过程中,液体喷出物把表面活性剂残余从软表面上冲洗进液体本身。即使液相中低含量的表面活性剂残渣也可减少液体表面张力。液相中减少的表面张力降低了表面沿纤维的芯吸张力(表面张力X接触角的余弦)。较低的芯吸张力减小了芯吸速率,还减小通过或沿着有孔织品的芯吸通量(单位时间内通过单位截面积的流量)。对于最终用户,减少的芯吸通量会导致较低的流体处理性能。
液相表面张力的减小也可增加它对疏水织品的润湿能力。一旦把原本具有疏水性的织品润湿,制品即可表现亲水性行为。疏水性表面不允许水等液体穿过或沿着纤维传送流体,这种流体是靠芯吸张力、重力、梯度压力或其它力来推动的。一个实施例是尿布的SMS紧固腿部的箍带,使用时纯尿液不能轻易通过。被残余表面活性剂污染的尿的减小的表面张力可以润湿并通过所述SMS织品。这会导致最终用户感觉到渗漏。
为了提高纳米微粒分散体润湿软表面的程度,另一方法是减小流体的表面张力从而增加软表面的表面能量。因而,在某些实施方案中,可以通过把某些高能表面处理应用于材料形成处理表面从而提高表面能量。高能表面处理包括但不限于电晕放电处理、等离子体处理、紫外辐射处理、离子束处理、电子束处理、某些包括脉冲激光的激光处理和其它照射技术,它们可使部分纤维的表面能增加。应小心避免对被处理材料产生不良影响。在某些情况下,需要对软表面的两面进行一些处理。另外,可以想象,这个任选的步骤可以是相对于把涂层组合物涂抹于软表面的独立的预处理步骤,这两种方法也可以结合使用。
增加表面能的高能表面处理是有用的,因为它们和纳米微粒一起可以为表面提供持久的亲水性质。依次,增加的表面能无需在分散剂中使用表面活性剂以就可增加软表面的可湿性。基于前述理由,不使用表面活性剂很有用。在一个非限制性示例中,电晕处理是在纤维热塑性表面进行瞬间充电。正如以前所讨论的,部分或全部放电超时,而且维持纤维热塑性表面上的部分或全部电荷是普通的限制。然而,已经发现,和纳米微粒相关的电晕处理可以在材料上持久充电,因而水可以一直吸附在材料上。纳米微粒与高能表面处理的联合使用,可以把此类处理的瞬间性质转化为时间更长的性质。在一个非限制性示例中,13克/平方米的疏水性SMS聚丙烯非纺织物的电晕处理(随后用纳米微粒分散体进行处理然后干燥),在多种损伤之后可以持久地表现出快速的过水性。不受理论的约束,电晕放电增加了纤维的表面能量。在电荷耗散前,没有表面活性剂的纳米微粒分散体与纤维表面进行接触。较高的表面能使得分散剂比没有电晕处理时能更好地润湿纤维表面。在润湿的表面上,纳米微粒结合部分或全部电荷,这些电荷在其它情况下是短暂的。这种关联可能采取范德华力作用或其它相互作用或化学键的形式。纳米微粒非常小,可以提供能经受多次浸湿的稳定关联。纳米微粒又足够大,可以抵制其从氧气中旋转进入聚合物,或大多数如先前讨论的那样耗散。纳米微粒需要通过高能表面处理达到无需表面活性剂的润湿性,并在烘干的表面上提供均匀的沉积;高能表面处理则要求纳米微粒用于持久带电的表面。
经过表面高能处理并且其上沉积了多个纳米微粒的材料可用于许多用途,包括但不限于用来在物品(例如包含疏水性或临界亲水性纤维的衣服)中或者在一次性吸收物品的一部分中传送液体。所述部分一次性吸收剂物品包括但不限于顶片、保存层、分散层、芯吸层、存储层、吸收核、吸收核外套和密封结构。
在某些实施方案中,用此类方法处理的材料,进行测试方法章节中的过水性试验时,在3次或更多次液体流出损伤之后,包括但不限于5次液体流出之后,10次液体流出之后,其液体过水时间小于或等于10秒、优选小于或等于约6秒、更优选小于或等于3秒。
无论是否经过高能表面处理,为了赋予材料亲水性,那些已经使用本发明所描述的涂层组合物进行处理的材料,在30秒时间的分散后,相对水具有导前的接触角,接触角小于等于或小于90°,或任何小于90的度数(包括但不限于45°)。
在另一个实施方案中,可以用其它方法来提高材料表面接受涂层组合物的能力。这些方法包括但不限于向材料提供压力梯度,包括但不限于通过使用压力滚筒、印染辊、压送辊、流体静压等等;在不使用表面活性剂的情况下,减小表面涂层组合物的表面张力,例如通过使用乙醇代替表面活性剂;通过使用“可降解的”或“可分裂的”表面活性剂;通过把组合物喷墨印刷在材料上,如下文所详细描述。
可分裂的表面活性剂是弱化学键分子材料,典型地在亲水性首基和疏水性尾基之间。此键可以容易地通过不同的化学处理断裂,产生不再具有表面活性的两个或更多个分子核素/片段。类似的化学处理包括但不限于酸、碱、氧化、热和紫外线。使用可分裂表面活性剂不需要诸如电晕放电和等离子体等高能预处理,也无需担心与纳米微粒组合物接触的液体介质的表面张力减小。最近的举例说明不同类型可分裂表面活性剂的论文包括Hellberg等人所著的2000年第1期第3卷的《表面活性剂和清洁剂》(Journal of Surfactants andDetergents)期刊。可分裂表面活性剂包括但不限于易于碱解的表面活性剂,包括季胺化乙醇胺酯、糖酯和单烷基碳酸盐;易于酸解的表面活性剂,包括烷基糖苷、1,3-二氧戊环和1,3-二氧六环表面活性剂、非环状乙缩醛表面活性剂和烷基原酸酯;易于光分裂的表面活性剂,包括含有烷基芳基酮磺酸盐和重氮磺酸盐表面活性剂。
本发明所指的表面也可是“基质”。不受任何特定理论或说明的限制,在一些实施方案中,本发明所参考的提高表面接受涂层组合物能力的处理等等可以被认为是表面的“底胶”。在一些实施方案中,纳米微粒涂层可被认为是包含活性材料(纳米微粒)的含水分散体。当涂层干燥后,表面上留下一层活性纳米微粒层。此外,不受任何特定理论或描述的限制,在一些实施方案中,底胶和纳米微粒是互相依存的。在一些实施方案中,分布在表面上的纳米微粒可以“锁定”底层涂料的性质,使这些性质比较持久,同时底层涂料更加有效地允许纳米微粒粘合在表面上。
(1)直接或间接应用
关于把涂层组合物直接或间接应用于软表面的方法有很多实施方案。本发明使用的术语“直接应用”是指一种把涂层组合物直接应用于软表面的方法。例如,直接应用可以包括但不限于把涂层组合物直接喷涂在软表面上。本发明使用的术语“间接应用”是指把涂层组合物应用于其它物品,再由这种物品把涂层组合物应用于软表面。例如,间接应用包括但不限于把涂层组合物应用于滚筒上,滚筒可将涂层组合物应用于软表面。
在一个非限制性实施方案中,本发明的有效量的液体涂层组合物还可以喷涂在软表面上和/或软表面物品上,包括但不限于衣服、挂帘、毛巾、家内装饰、毛毯、纸、书、皮革、天然和人造纤维等等。当涂层组合物喷涂于软表面上时,有效量的纳米微粒可以沉积在软表面上,而软表面会变湿或全部湿透。通过喷涂把涂层组合物应用于表面(例如软表面)有很多好处。如果需要,涂层混合物可以定位于要应用产品的物品的特定区域;或仅仅应用于物品的一侧(与沉浸过程相反);可以更加有效,因为更多的纳米微粒将固定在表面上,而不是在冲洗或漂洗过程中冲到排水沟。
也可通过沉浸容器中的浸渍和/或浸透过程加上可选的干燥步骤,把涂层组合物应用于诸如软表面等表面。在工业应用或消费者家中,可以通过大规模过程在软表面和/或成品上执行此应用过程。
本发明也包含使用浓缩液体或固体涂层组合物的方法,浓缩组合物经过稀释可以形成具有本发明上述“使用条件”给出的使用浓度的组合物。浓缩组合物包含较高用量水平的纳米微粒浓度,包括但不限于占浓缩混合物重量的约0.1%至约50%或约0.5%至约40%,也可为约1%至约30%。
使用浓缩组合物是为了提供较便宜的产品。根据涂层组合物的重量,浓缩产品可以使用1,000份或100份或10份载体介质加以稀释。
在另一非限制性实施方案中,可以将涂层混合物印刷到软表面上。要实现此目的,可使用任何合适的印刷技术,包括但不限于移动印刷,例如旋转、凹版、和橡皮凸版印刷和喷墨印刷。喷墨印刷有特别的好处,因为小滴的相对高惯性力能够把涂层混合物暂时沿着基质表面分布,以便提高涂层混合物润湿软表面的能力。低热质量的小滴使得载体介质快速蒸发,典型地是在约0秒至10秒内开始,优选地是在约0.1秒到1秒或更短的时间内开始。载体介质在小滴的表面张力可以从散布下列的影响中完全恢复前开始蒸发。纳米微粒保持在载体介质蒸发前分散体润湿表面的位置。所描述的纳米微粒分散体的喷墨打印在疏水性表面、临界亲水性表面、前进的接触角远远大于后退的接触角的表面上是有益的。
涂层组合物可以在相对低粘度分散体中生产(例如,必要时小于约10厘泊,优选小于约5厘泊),这样一来,涂层组合物将比分散体粘度较高时以更小的流动阻力通过喷墨嘴并穿过表面。不象普通分散体中的传统尺寸的微粒,纳米微粒非常小,不会在低粘度介质中沉淀,也不会阻塞喷墨打印机的喷嘴。可使用任何类型的喷墨打印技术,包括但不限于按需滴落墨水喷射印刷机上,例如带有振动加热元件的墨滴蒸发类型和带有机械泵和振动晶体的墨滴喷射类型。在其他实施方案中(如硬表面),墨水喷射印刷机可以经配置相对表面移动。(2)冲洗过程中的应用在其它非限制实施方案中,涂层组合物在冲洗过程中可以应用于诸如软表面等表面。清洗过程可包括但不限于商业或家庭冲洗过程。在这些实施方案中,涂层混合物可以在洗衣机中使用,也可以通过其它的方法应用。冲洗过程中可以用任何合适的方式添加涂层混合物,这些方式包括但不限于清洁剂或独立的小块、凝胶或液体。涂层混合物可以在冲洗液中提供任意的合适纳米微粒浓度,包括但不限于小于或等于约0.02%(或200ppm)和更小的浓度[包括但不限于0.01%(100ppm)]。如果多次冲洗(或漂洗)软表面,在一些实施方案中,表面上的纳米微粒很可能增加并积聚。(3)漂洗过程中的应用在其它非限制性实施方案中,提供了如下操作的方法:在漂洗操作时(例如在自动洗衣机的漂洗步骤中),使用液体涂层混合物或者浓缩液体涂层混合物处理如织物等的软表面。漂洗所用水中可以包含任意适当数量的纳米微粒,包括但不限于约0.0005%至约1%、或约0.0008%至约0.1%或约0.001%至约0.05%的纳米微粒。
另一个方法包括在漂洗周期结束干燥周期正要开始前,把本发明的涂层混合物从喷枪喷出进行软表面处理。优选按照使用说明进行处理,以保证客户知道可以获得何种益处、如何最好地获得益处。
附加用途/益处
如本发明所指出,涂层组合物可以提供给软表面增强的色彩(或颜色保护)等益处。可以提供色彩增强的软表面包括但不限于衣服、织品、纺织品、地毯、室内装饰和其它软表面。令人惊奇的是,已经发现把纳米微粒应用于此类物品可明显的恢复颜色。纳米微粒可以明显增强旧衣服和其它软表面的颜色,同时,还可防止织物褪色。纳米微粒也可对于紫外光引起的褪色提供保护。颜色增强通常表现为已经褪去的颜色明显加深。可以使用Hunter Miniscan XE仪器测量色彩增强,该仪器由美国Reston,VA的Hunter Associates Laboratory生产。
不受任何特定理论的限制,据信色彩增强原因在于到达软表面后从软表面反射回观察者的光的衰减。
色彩增强的水平取决于许多因素,包括但不限于微粒尺寸、微粒折射指数、沉淀在软表面上纳米微粒的数量、微粒形状、微粒在表面上的定位以及微粒对光的吸收性。
不受任何特殊理论的限制,据信色彩增强原因在于至少两种截然不同的由表面纳米微粒形成的结构。据信,这两种结构取决于纳米微粒的尺寸。至少在一些使用平均尺寸大于或等于约100纳米的纳米微粒的实施方案中,据信纳米微粒将在表面上分散。据信在这些方案中,沉淀在表面的相对较大的纳米微粒能够使光衰减,即使微粒覆盖率小于表面的约100%。在其它非限制性实施方案中,至少一些颜色区的至少一部分具有平均尺寸小于或等于100纳米的纳米微粒,这些纳米微粒沉积后覆盖大于或等于约25%的表面。
在许多实施方案中,需要纳米微粒的平均尺寸小于或等于约750纳米。在一些实施方案中,需要纳米微粒的折射指数大于或等于约1.3。在一些实施方案中,需要纳米微粒的折射指数小于或等于约5.5。纳米微粒的折射指数可以通过使用椭偏仪测量散装纳米微粒材料或散装纳米微粒材料制成的薄膜进行。
已经发现,在一些实施方案中,软表面颜色随着微粒尺寸的增加而加深。当然,不应使用在表面可见的大体积颗粒。包含不同材料的微粒将具有不同的色彩增强特性。例如,在使用勃姆石氧化铝增强色彩的方案中,需要纳米微粒平均尺寸为约140纳米。
能够提供色彩增强的纳米微粒不仅包括非光敏性纳米微粒,也包括钝化的光敏性纳米微粒。术语“钝化的光敏性纳米微粒”是指那些受光影响较小的光敏性纳米微粒。例如,钝化的光敏性纳米微粒可包含那些已经涂上一层抗反应屏障成分的光敏性纳米微粒。已经发现可增强色彩的纳米微粒包括但不限于勃姆石氧化铝、氧化铝、硅沸石(例如,ZSM-5)和纳米胶乳。已经发现可以避免褪色的纳米微粒包括但不限于涂有一层紫外吸收剂例如二氧化硅和氧化铝包覆的TiO2和ZnO的LAPONITE BTM。
可以使用任何合适方式把涂层组合物应用于软表面以提供保护颜色的功能。把涂层组合物应用于软表面而提供护色的合适的方式包括但不限于直接应用(包括但不限于喷涂、在冲洗过程的洗涤阶段中(也即“通过冲洗”)应用,在冲洗过程的漂洗阶段(也即“通过漂洗”)中应用)。直接应用和通过漂洗应用比较理想,因为它们可以把某些类型的纳米微粒更好的沉淀在软表面上。
在一些实施方案中,可以这样使用涂层组合物,使其干燥后,纳米微粒覆盖大于或等于约0.5%的软表面。沉积的百分比可以使用测试方法章节所描述的X-射线荧光(XRF)测试进行测量。
可以通过使用Hunter Miniscan XE设备的L、a和b(更小单位数值)测量色彩增强。在一些实施方案中,相对未处理的材料而言,纳米微粒可以使L、a和b值中的一个或多个值超过绝对值的约0.25。也可以使用Hunter Miniscan设备测量反射百分比。在一些实施方案中,相对于未处理样品而言,纳米微粒可以减少380纳米和700纳米之间的任何波长的反射比约1%。
在本发明所描述的任何实施方案中或者在其它实施方案中,纳米微粒涂层可以应用在这样的过程中:使用机械或化学方法,从处理过的表面的涂层上剥离至少一层纳米微粒以便去除表面的杂质(即污垢、点状残渣、食物等)。机械或化学方法并不排除对于该表面冲洗或任意正常使用(例如一件含有软表面的衣服的穿着)。不受理论的约束,据信图1至3描述了此方法的剥离薄膜过程。
在图1至3中,软表面对应参考数字20。个别纳米微粒对应参考数字22,由此形成的层对应参考数字24。沉积在纳米微粒上的污迹或污点对应参考数字26。在本发明的一个实施方案中,例如在洗烫应用中,有效数量的纳米涂层沉淀为不可见薄膜,防止污点凝结在软表面或织品20(图1)上。纳米微粒涂层可构成能够提供此益处的多重有效纳米微粒层24。在冲洗或剥离处理中,至少去除纳米微粒涂层的顶层24,同时清除其上的污点26(图2和3)。
III.制品
本发明也涉及在一个包装内包含本发明的涂层混合物的一种制品。可与所述涂层组合物同时提供使用说明,该说明是关于如何使用涂层组合物处理软表面使其得到改善,以获得至少一项本发明描述的所期望的结果。
在一个非限制性实施方案中,制品包括喷涂器中的混合物及使用说明,使用说明是关于如何正确地使用涂层混合物处理软表面,包括,例如喷涂组合物的方式和/或数量,以及应用涂层组合物的优选方法,下文有更详细的描述。重要的是,说明应尽可能简单明了,必要时可包括图片和图标。
喷涂器
要使涂层组合物分散到硬表面,可将涂层组合物置于喷涂器内。喷涂器可以是任何一种手动操作类型的,把涂层组合物应用于小块硬表面区和/或少量基片上,类似非人工操作,电动的喷涂器方便把涂层组合物应用于大块硬表面区和/或多个基片上。喷涂器包括但不限于下列任一种:浮质喷涂器、自压喷涂器、非浮质人工开动的泵喷涂器、人工开动触发喷涂器、触发喷涂器或指泵喷涂器、非人工操作的喷涂器(包括但不限于电动喷涂器、送气喷涂器、吸液喷涂器、静电喷涂器和喷雾喷涂器)。电动喷涂器可包括但不限于离心或正电置换设计。供应商如弗吉尼亚州的Solo,Newport News(例如,SoloSpraystarTM)可再充电喷涂器,列出在手动部件#:美国460 395,他们提供的喷涂器很易于使用。包括但不限于静电喷涂器的某些喷涂器,可以在应用于表面的过程中,将更少的肥皂泡或泡沫引进处理表面,从而在更广泛的情况下形成带有较少可见渣滓的合适涂层。这允许将更广范围的表面活性剂应用于涂层混合物。
优选的电动喷涂器利用一次性电池(例如可商购获得的碱电池)或可再充电电池组(例如可商购获得的镍镉电池组)的轻便直流电供电。电动喷涂器也可由大多数建筑物中的标准交流电源供电。释放喷嘴设计可以变化,以形成不同的喷涂性质(例如喷涂直径和微粒尺寸)。也可能有多重喷嘴表现出变化的喷涂性质。喷嘴可能包含也可能不包含允许改变喷涂性质的可调节喷嘴罩。
静电喷涂器通过高压电势把能量传送到含水的涂层组合物上。这种电能将把含水涂层组合物雾化并充电,以创造优良的雾状带电的微粒。带电微粒喷出喷涂器后,它们的同性电荷使它们互相排斥。这在微粒到达目标物体前产生两个影响。第一,它扩展了总喷雾。这在喷涂到达较远、较大区域时特别重要。第二,维持原始微粒尺寸。因为微粒互相排斥,它们不会聚集在一起象不带电微粒那样形成大的较重的微粒。这减少了重力的影响,增加了到达目标物体的带电微粒。在多个负电微粒接近目标物体时,它们把目标物体的电子向内推进,从而使得目标物体的所有外露表面暂时带正电。微粒与目标物体之间产生的吸引力超过了重力和惯性的影响。当微粒沉积在目标物体上时,目标物体上的该点电荷将被中和并且失去吸引力。因而,之后的自由微粒被最近的点吸引,并继续进行直到目标物体的整个表面被覆盖。因此,带电微粒改善了分布并减少了微粒的滴落。
可商购获得的静电喷涂器的非限制性实施例描述在下述美国专利中:5,222,664,Noakes,公布于1993年6月29日;4,962,885,Coffee,公布于1990年10月16日;2,695,002,Miller,公布于1954年11月;5,405,090,Greene,公布于1995年4月11日;4,752,034,Kuhn,公布于1988年6月21日;2,989,241,Badger,公布于1961年6月。供应商(例如Tae In Tech Co,South Korea和Spectrum,Houston,Texas)提供的静电喷涂器易于使用。
制品包括非人工操作喷涂器和盛有含水涂层组合物的单独的容器,后者在使用前添加到喷涂器和/或在填料/再次填料时拆下。单独的容器里可以盛有使用的组合物或浓缩组合物,浓缩组合物在使用前稀释,和/或与稀释喷涂器一起使用,例如使用如上所述的吸液喷涂器。
单独的容器具有与喷涂器其他部分配合的结构,以保证固体接头即使在运动或碰撞等之后或由没有经验的用户使用也不发生泄露。理想的喷涂器有安全的附件系统,该系统经设计允许用另一充满液体的容器置换原来的液体容器。例如,可以用填充容器替换流体储存器。如果喷涂器和容器都使用正确的装配和密封方法,就可以使填料(包括泄露)问题减少到最小的程度。在理想的状态下,喷涂器可以包括套,以保证正确的排列和/或允许使用替换容器上的较薄壁。从而将要循环和/或丢弃材料的数量减到最小。标准件密封或装配系统可以是螺纹封闭体(喷涂器),它可以替换填料螺纹容器上的现有封闭体。可以添加衬垫以提供附加的密封安全性并使泄露减到最小程度。喷涂器关闭时会使衬垫断裂。这些螺纹密闭系统可以依据行业标准制造。然而,比较理想的是使用具有非标准尺寸的螺纹密封系统,以保证通常可联合使用适当的喷涂器/瓶。这有助于阻止使用有毒流体,否则为预期目的使用喷涂器时可能会分出有毒流体。
另一可替换的密封系统可以以一个或多个联锁接线片和通道为基础。这些系统通常指“刺刀”系统。这些系统可以有不同的配置,从而更好地保证使用适当的替换流体。为了方便起见,锁定系统也可以为加料瓶提供“傻瓜”盖。这种“锁和钥匙”类型系统可以提供非常理想的安全性能。有许多不同的方法来设计这些锁和钥匙密封系统。
然而要小心防止系统增加填料和密封操作的难度。必要时,密封装置的锁和钥匙是一体的。但是,为了保证正确的充电和加料,可以将联锁零件和密封系统分开。例如,罩和容器可以设计为通用规格。这样只依靠容器的独特设计,即可为正确的充电/填料提供必要的保证。
本发明也涉及包含将涂层组合物喷涂和/或喷到整个软表面或物品的产品使用方法,而且多余的涂层组合物不能释放到开放环境中,同时提供使用说明,以保证用户至少用有效数量的纳米微粒系统和/或涂层组合物,以达到所需的软表面多重益处。
带有使用说明的产品
本发明也包括有关本发明涂层组合物使用的说明,包装内还包括本发明中的涂层组合物的标准件或其他形式的与涂层组合物的销售或使用有关的广告资料。可以用最终产品制造商或供应商典型使用的任何方式包括该说明。示例包括用以下方式提供说明:在盛放涂层混合物的容器标签上;购买时贴在容器上或附随的薄片上;在广告、演示和/或其它与涂层混合物使用或购买有关的书面或口头使用说明中。
特别地,如果喷涂、浸透或摩擦方法是合适的,使用说明将包括有关涂层组合物使用的说明,例如:用于表面或物品涂层的组合物的建议使用数量;应用于表面的混合物的建议数量。
涂层组合物可以包含在产品中。产品可以包含涂层组合物和使用说明,其中使用说明是关于:把需要处理的软表面与有效数量的涂层组合物接触,用产品洗烫软表面,给软表面带来一种或多种所需的益处。
下列实施例是对本发明的说明,而不是旨在限制或另外限定其范围。除非另有说明,本发明使用的所有的部分、百分数和比率均以百分重量表示。
虽然本发明的组合物和方法集中于软表面的家用性改善,它们也可用于软表面的工业改善,例如在纺织品工厂。
实施例
表1--实施例1至13
本发明中液体软表面涂层组合物配置如下(其中平衡物是水):
实施例# | 纳米微粒(Wt%) | 表面活性剂(Wt%) |
1 | LAPONITE BTM(0.1) | Neodol 91-6(0.075) |
2 | LAPONITE BTM(0.05) | Neodol 91-6(0.075) |
3 | LAPONITE BTM(0.05) | Silwet L-77(0.025) |
4 | LAPONITE RDTM(0.1) | Neodol 91-6(0.075) |
5 | LAPONITE RDTM(0.05) | Neodol 91-6(0.075) |
6 | LAPONITE RDTM(0.05) | Silwet L-77(0.025) |
7 | LAPONITE RDTM(0.1) | --- |
8 | LAPONITE BTM (0.1) | --- |
9 | Disperal 14N4-25(1%) | --- |
7 | LAPONITE RDTM(1) | --- |
8 | LAPONITE BTM(1) | --- |
10 | Disperal 14N4-25(1%) | --- |
11 | Disperal 14N4-25(1%) | Neodol 91-6(0.075) |
12 | Disperal 14N4-25(4%) | Neodol 91-6(0.075) |
13 | 1%ZSM5 |
1.LAPONITE BTM是Southern Clay Product s,Inc.提供的钠镁锂氟代硅酸盐。
2.LAPONITE RDTM是Southern Clay Products,Inc.提供的钠镁锂硅酸盐。
3.ZSM5是粒径从70至约400nm的纳米沸石。
表2-示例14至15
按照本发明,液体涂层组合物配制如下:
配方14 | 配方15 | |
LAPONITETMC13-15 EO7乙氧基化表面活性剂C12-14胺氧化物表面活性剂HLAS柠檬酸C12-18脂肪酸二乙烯三胺环戊烷磷酸羟基乙烷二亚甲基磷酸乙氧基化聚乙烯亚胺硼酸CaCl2丙二醇乙醇一乙醇胺NaOH蛋白酶淀粉酶纤维素酶纳米微粒系统水 | (Wt%)0.520560.40.452.6520.02181至pH8.50.770.060.161.0至100份 | (Wt%)1.020150.0220至pH8.50.060.162.5至100份 |
1.LAPONIT ETM()是Southern Clay Products,Inc.提供的锂镁硅酸盐。
表3--示例16至19
衣物漂洗附加组合物
按照本发明,液体涂层组合物配制如下:
成分Wt% | 16 | 17 | 18 | 19 |
TEADi-esterquatl乙醇(来自活性软化剂)己二醇(来自活性软化剂)己二醇TMPDNeodol91-82Tergitol 15S93CaCl2MgCl2DTPA4氯化铵TPED5香料LAPONITE RDTM去离子水 | 302.52.76--4.5----1.5--0.1--2.50.15余量 | 302.52.76--4.5----1.50.20.1--2.50.25余量 | 453.74.0--10--2.60.75------0.22.50.5余量 | 453.74.010----2.60.75------0.22.50.15余量 |
1 LAPONITE RDTM是Southern Clay Products,Inc.提供的钠镁锂硅酸盐。
2 二(酰基乙氧基)(2-羟乙基)甲基铵甲基硫酸盐,其中,酰基源自部分氢化的低芥酸菜子脂肪酸。
3 乙氧基化烷基乙醇,其商标为Shell。
4 乙氧基化烷基乙醇,其商标为Union Carbide。
5 二乙烯三胺五醋酸
6 四-(2-羟丙基)乙二胺
表4--示例20至21
按照本发明,粒状涂层组合物配制如下:
示例20 | 示例21 | |
纳米微粒LAPONITE RDTMLucentite SWNTM助洗剂沸石碳酸钠(总量)SKS6硅酸盐(2R) | 0.25021.5333.124.500.12 | 00.2521.5333.124.500.12 |
聚合体丙烯酸/顺丁烯二酸共聚物CMC | 2.430.15 | 2.430.15 |
表面活性剂LAS阳离子表面活性剂漂白剂PB4TAEDHEDP(60%)MgSO4EDDS酶Savinase(13KNPU)Termamyl(130KNU/g)Carezyme(1000s CEVU/g)泡沫抑制剂硅酮泡沫抑制剂美化剂/其它STS脂肪酸盐硫酸钠 | 9.951.999.01.630.210.410.180.450.140.191.171.00.7522.24 | 9.951.999.01.630.210.410.180.450.140.191.171.00.7522.24 |
1.LAPONITE RD(上)是Southern Clay Products,Inc.提供的钠镁锂硅酸盐。
2.Lucentite SWMTM是Kobo Products,Inc.提供的锂镁纳硅酸盐。
暴露于“实验室用放电处理器”(型号BD-20AC,由美国的Electro-Technic Products Inc.制造)的SMS聚丙烯无纺布(13克/平方米)的过水性结果,与本发明中的涂层组合物的过水性结果见表5。
表5.过水时间
样本 | 过水时间(秒) | ||
第一次 | 第二次 | 第三次 | |
0.2%的Laponite RD(Southern Clay Products) | 2.51.6 | 2.82.3 | 2.82.4 |
0.1%的Disperal P2(Condea) |
表6.使用纳米微粒产生的色彩增强效果
样本 | 绿色#41 | 栗色#47 | 黑色聚酯 | ||||||
ΔL | Δa | Δb | ΔL | Δa | Δb | ΔL | Δa | Δb | |
Disperal P2a | -1.4 | -1.4 | 0.2 | -1.0 | 0.4 | 0.9 | -0.4 | 0.0 | 0.2 |
Dispal 14N4-25a | -1.9 | -2.1 | 0.2 | -2.8 | 4.0 | 0.2 | -2.0 | 0.0 | 0.6 |
Dispal 11N7-12a | -1.0 | -1.3 | -0.4 | -1.7 | 2.8 | -0.6 | -2.2 | 0.0 | 0.2 |
Nanotek氧化铝b | -1.8 | -1.6 | 0.1 | -3.0 | 3.1 | -0.2 | -1.5 | 0.1 | 0.1 |
ZRYS4c | -1.4 | -1.7 | 0.4 | -1.4 | 1.6 | 0.7 | -0.6 | -0.1 | 0.2 |
AL20c | -2.0 | -3.2 | 0.3 | -1.0 | 2.0 | 0.3 | -0.6 | -0.1 | 0.2 |
ZSM5 | -1.7 | -0.3 | 0.4 | -1.3 | 1.3 | 0.6 | -1.7 | -0.1 | 0.7 |
Laponite BTMd | -0.6 | -1.2 | -0.3 | -1.7 | 2.0 | 0.2 | -0.6 | -0.2 | 0.3 |
aSasol North America Inc.
bNanophase Technologies Corporation
cNyacol Nanotechnologies,Inc.
dSouthern Clay Products
表7.棉织品的紫外光诱导颜色变化(Hunter MiniscanΔE1)
处理 | 粉红色 | 紫色 | 白色 |
A.未处理 | 1.3 | 2.4 | 7.8 |
B.TiO2(Altair,300nm) | 1.1 | 2.8 | 5.9 |
C.ZnO(纳米相、>250nm) | 1.6 | 1.6 | 9.7 |
D.氧化铝(Sasol,140nm) | 1.1 | 2.5 | 8.6 |
E.Laponite B(SCP,25nm) | 1.0 | 1.8 | 7.2 |
值为粗体的样品明显比未处理织品褪色少。
1ΔE是普通的最小估算结果(ΔE=[(ΔL)2+(Δa)2+(Δb)2]1/2)
表8.通过漂洗的勃姆石氧化铝沉积物。
一个循环代表在以下条件下冲洗一次:使用美国俄亥俄州辛辛那提的宝洁公司(The Procter&Gamble Company)提供的液态TIDE洗涤剂,溶液浓度为6gpg(克/加仑),水硬度(Ca∶Mg=3∶1),在漂洗阶段加入100ppm的勃姆石氧化铝,ULTRA DOWNY织物柔软剂同样由宝洁公司提供。织物上沉积的勃姆石氧化铝的数量是针对来自美国OH45237辛辛那提7616 Reinhold Drive的Empirical ManufacturingCompany,Inc.(或EMC)的白色棉织物CW-11并通过XRF方法测量的。颜色测量以染成绿色的棉(CW-11)织物为基础(染料:CAS#128-58-5),织物由Empirical Manufacturing Company提供。Δ“L”、“b”和“a”值代表未处理织品与处理织品之间的变化
(Δ值=处理过的值-未处理过的值),负值越大表示色彩增强越明显。
1个循环 | 5个循环 | |
沉积量(mg勃姆石/g织物) | 2.3 | 2.9 |
ΔL | -0.5 | 0.0 |
Δa | -0.1 | -0.5 |
Δb | 0.0 | 0.2 |
测试方法
除非另外说明,否则,所有检测试验皆在标准实验室条件(湿度50%,温度73(23℃))下进行。
接触角
使用由美国First Ten Angstroms公司制造的“FTA200动态接触角分析仪”测量动态接触角。在样品基质上滴一滴试验溶液。当液滴在基质表面铺开后,就开始进行数字视频记录,FTA200软件把液体与基质的接触角作为时间的函数进行测量。
液体过水性测试
使用由澳大利亚Lenzing AG公司制造的Lister型过水性检测设备测量液体过水时间。试验程序基于标准的EDANA(欧洲一次性用品和无纺布协会)方法150.3-96,把试验样品放在由十层滤纸(AhlstromGrade 632,来自Empirical Manufacturing Co.,Inc.,或者替代物)组成的吸水垫上。在典型的实验中,每分钟三次把5ml的试验液体(0.9%盐溶液)连续喷到非纺织品样品上,并且在不更换吸水垫的情况下记录每次的过水时间。
色彩增强测试
获得织物样品组。标准织品组包括:绿色棉织物(染料:CAS#128-58-5)、栗色棉织物(染料:CAS#27165-25-9)、粉红色棉织物(染料:CAS#128-58-5)、紫色棉织物(长袖T恤衫:Old Navy,11711Princeton Rd.,Springdale,OH45246,SKU#165578600028)、黑色聚酯(Ponte双面针织聚酯织品,Jo-Ann Fabric&Crafts,10214ColerainAve.,Bevis,OH 45251,SKU#864-595),和PW19(来自Empirical Manufacturing Co)。绿色、栗色和粉红棉织物是按照1996年10月第12期《the Society of Dyers and Colourists》杂志的287至293页列出的相关程序,并使用指定染料进行染色的。喷涂纳米微粒时使用Solo喷雾器和1%的活性水溶液,溶液要求如下:含1%的纳米微粒,其余部分是水和/或其它成分;中性,用NaOH或HCl将其pH值调到6附近。以织物的总重量计算,每克织物上附着的微粒量应为10毫克。使用Hunter Miniscan XE设备(C/2°,其中C是光源类型,2°是观测角)测量晾干的样品的颜色变化。Hunter Miniscan XE设备按照制造商提供的操作手册进行校准和操作。
褪色保护测试
将包含0.5%的纳米微粒的含水分散剂直接喷涂到织物上,加载容量为5mg活性剂(纳米微粒)/g织物。用风吹干织物。然后,按照AATCC(American Association of Textile Colorists and Chemists)测试方法16E,使用加拿大R.B.Atlas Inc.(9 Canso Road Toronto,Ontario M9W 4L9)提供的“Weather-Ometer”设备让织品经受10小时的紫外线照射之后,根据制造商提供的手册,用Hunter Miniscan XE设备(C/2°)测量出L、a和b的值。这样就能计算出ΔE值。经处理的基质的ΔE值小于未处理基质的ΔE值,证明了经处理的基质具有褪色保护效应。
X-射线荧光分析
X-射线荧光(XRF)是估定样品内部或表面成分浓度的非破坏性和非侵害性技术。使用美国Phillips Analytical 12 Michigan Dr.Natick,MA01760提供的Phillips Analytical PW2404 Sequential“4000W”X-射线分光计系统(序列号DY735)进行分析。XRF分析的仪器设置和规格见下面的表9。
测量程序:
1)在试验基质上用移液管滴上已知浓度的标准液,作仪器响应与分析物浓度之间的校正曲线。在测量执行前允许样品慢慢干燥。
2)化验样品时,首先将样品正面向下放进取样杯,然后把取样杯放进分光计,再初始化数据采集序列。如果是人造锂蒙脱石涂层,则测量Mg和Si的元素线,而氧化铝涂层则使用Al的元素线。
3)样品的浓度决定于样品的校正曲线。
表9.X射线荧光测试的一般条件
样品空间环境 | 真空 |
检测器类型 | 测角计 |
化验的元素线 | 被测量成分的Kal |
样品旋转器 | 打开 |
试管类型 | 铑 |
所有公开的专利、专利申请(和任何在本专利中公布的专利,及任何相应的已公开的国外专利申请)和本说明全文提及的出版物皆引入本文以供参考。然而,很明显,并未承认本文所引述的任何文档讲授或透露了本发明的相关内容。
至此已描述了主体发明的具体实施方案,该领域的专家应很清楚,在不违背本发明的精神实质与范围的情况下,可以对主体发明进行各种更改和修正。在附加的权利要求中,意欲涵盖本发明范围内的所有类似改进。
Claims (13)
1.使材料亲水的方法,所述方法的特征在于其包括以下步骤:
(a)提供一种包括疏水性或临界亲水性成分的材料;
(b)对所述材料进行高能表面处理以形成处理过的材料;和
(c)将一种涂层组合物应用于所述处理过的材料,所述涂层组合物包括适当的载体介质和所述载体介质中的多个纳米微粒,所述纳米微粒包括第一组纳米微粒,所述涂层组合物的特征在于所述第一组纳米微粒包括至少一种不是2∶1型层状硅酸盐的纳米微粒材料。
2.如权利要求1所述的方法,其中所述材料包括一种织物。
3.如权利要求2所述的方法,其中所述的织物是疏水性结构成分的无纺材料。
4.如权利要求1或2所述的方法,其中应用在步骤(b)中的高能表面处理包括选自下列的处理:电晕放电处理、等离子体处理、紫外辐射、离子束处理,和电子束处理。
5.如权利要求1或2所述的方法,其中所述的多个纳米微粒是以涂层组合物的形式,该组合物还含有表面活性剂。
6.如权利要求1所述的方法,其中所述纳米微粒是非光敏性的。
7.如权利要求1或6所述的方法,其中所述纳米微粒包括一种或多种下述材料:勃姆石氧化铝、硅沸石、胶乳、氧化铝和氧化锆。
8.如权利要求1所述的方法,其中所述纳米微粒是光敏性的。
9.如权利要求8所述的方法,其中所述纳米微粒包括至少下述材料之一:TiO2和氧化锌。
10.如权利要求1或6所述的方法,所述涂层组合物还包括至少一些包括2∶1型层状硅酸盐的纳米微粒。
11.如权利要求1或6所述的涂层组合物,还含有表面活性剂。
12.如权利要求11所述的方法,其中所述的表面活性剂是非离子型表面活性剂。
13.如权利要求1所述的方法,所述涂层组合物还包括一种或多种带电的功能化分子,所述功能化分子表现出亲水性、疏水性或其混合性能,所述性能与至少一些所述纳米微粒相关。
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- 2002-01-30 US US10/060,694 patent/US6863933B2/en not_active Expired - Fee Related
- 2002-01-30 AR ARP020100321A patent/AR032424A1/es not_active Application Discontinuation
- 2002-01-30 US US10/060,582 patent/US6645569B2/en not_active Expired - Fee Related
- 2002-01-30 CN CNB028043170A patent/CN1330822C/zh not_active Expired - Fee Related
- 2002-01-30 CA CA002433059A patent/CA2433059C/en not_active Expired - Fee Related
- 2002-01-30 BR BR0206737-4A patent/BR0206737A/pt not_active Application Discontinuation
- 2002-01-30 MX MXPA03006774A patent/MXPA03006774A/es active IP Right Grant
- 2002-01-30 AU AU2002253882A patent/AU2002253882A1/en not_active Abandoned
- 2002-01-30 WO PCT/US2002/002606 patent/WO2002064877A2/en active Application Filing
- 2002-01-30 JP JP2002564179A patent/JP2004518795A/ja active Pending
- 2002-01-30 US US10/060,708 patent/US7112621B2/en not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
AR032424A1 (es) | 2003-11-05 |
EP1356152A2 (en) | 2003-10-29 |
AU2002253882A1 (en) | 2002-08-28 |
US20040052957A1 (en) | 2004-03-18 |
JP2004518795A (ja) | 2004-06-24 |
WO2002064877A8 (en) | 2004-02-12 |
BR0206737A (pt) | 2004-02-03 |
US20020150678A1 (en) | 2002-10-17 |
US7112621B2 (en) | 2006-09-26 |
CA2433059C (en) | 2009-05-12 |
US20020192366A1 (en) | 2002-12-19 |
US20020160159A1 (en) | 2002-10-31 |
US6863933B2 (en) | 2005-03-08 |
MXPA03006774A (es) | 2003-10-24 |
US6645569B2 (en) | 2003-11-11 |
CA2433059A1 (en) | 2002-08-22 |
US6872444B2 (en) | 2005-03-29 |
WO2002064877A2 (en) | 2002-08-22 |
CN1575362A (zh) | 2005-02-02 |
WO2002064877A3 (en) | 2003-01-09 |
US20020151634A1 (en) | 2002-10-17 |
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