CN1040020C - 漂白或消毒组合物和方法 - Google Patents

漂白或消毒组合物和方法 Download PDF

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CN1040020C
CN1040020C CN92114898A CN92114898A CN1040020C CN 1040020 C CN1040020 C CN 1040020C CN 92114898 A CN92114898 A CN 92114898A CN 92114898 A CN92114898 A CN 92114898A CN 1040020 C CN1040020 C CN 1040020C
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F·E·哈迪
A·D·威利
S·夏拉
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Abstract

本发明涉及在漂白或消毒操作中作为过酸先质体的酰化柠檬酸酯。本发明包括这些酰化柠檬酸酯的使用、含酰化柠檬酸酯的粒状或液体组合物。描述了活化组合物以及活化漂白组合物。

Description

漂白或消毒组合物和方法
本发明涉及在漂白或消毒操作中使用某种酰化柠檬酸酯作为过酸的先质体。
漂白操作中使用过氧化氢或能产生过氧化氢的混合物，下文称为过氧化物漂白剂，在现有技术中已有广泛的描述。这种过氧化物漂白剂优于含氯漂白剂，因为他们是温和漂白剂。这一优点在纤维洗涤操作过程中尤其重要，因为过氧化物漂白剂不损害纤维颜色并不致使白色纤维变黄。过氧化物漂白剂的主要缺陷是在低温时比含氯漂白剂的活性低，而低温是在现代洗涤操作或处理硬表面时经常遇到的。因此，过氧化物漂白  活化剂得以发展并在现有技术中被广泛论述。这些活化剂可以是过渡金属或过酸先质体。过酸先质体同过氧化氢反应产生过酸。过酸是“活化的”漂白种类，它在低温时是有效的。
这类产生过酸的体系在非洗涤应用方面也很重要，因为过酸除漂白作用外，还有消毒作用。这种作用在厨房和浴室表面，尤其是抽水马桶中特别有效。
过氧化物类漂白剂优于氯漂白剂也是由于其环境相容性，并且不断需要发展更加与环境相容的产品。特别需要发展环境相容性过酸先质体。
另外，含有过氧化物漂白剂和活化剂的产品在漂白操作中需要使该混合物的自稳定性和其在水中尽可能快的反应能力间达到平衡。这两个特性在某种程度上是相矛盾的。这个问题在水为介质的液体组合物中尤为尖锐，但在干产品中也存在同  样的问题，如果干产品放在潮湿的环境中，由于产品受潮失去一些活性，产品的自稳定性成为问题。
EP241137提出了使用一种在酸性水介质中不溶，但在碱性介质中可溶的固体过酸先质体。这一体系据说具有储存稳定性，但这里提出的所有活化剂含有苯环，因此，特别不能与环境相容。
EP210674提出了由对苯磺酸碳酸酯作为过氧化氢活化剂。所有这些组合物都含有苯基，因此不具有环境相容性。
EP396287描述了在漂白过程中使用过氧化氢和过酸先质体来控制pH，开始时升高洗涤pH，然后降低以增进漂白效率。该文件包括了该领域中详尽无遗的过酸先质体系列。
业已发现按本发明的酰化柠檬酸酯能满足上面描述的所有目的。按照本发明的酰化柠檬酸酯由于能够完全分解为柠檬酸和醇，因而是完全与环境相容的，与现有技术中的活化剂相比，它们在温和的酸性介质甚至在含过氧化物的液体组合物中都特别地具有储存稳定性。
按照本发明，一些酰化柠檬酸酯还提供了其它益处，那就是它们表现出引人关注的增效作用，这一益处在洗涤应用方面特别有用。
这样，按照本发明，酰化柠檬酸酯允许很大的灵活性，因此它们可用于任何产品，粉状或液体，有或没有过氧化物漂白剂的场合。
本发明包括含有过酸先质体的用于漂白或消毒操作的组合物。其特征在于过酸先质体是具有下列分子式的酰化柠檬酸酯：
其中R选自C1-9的烷基或链烯基，取代或非取代苯基，烷基苯基或链烯基苯基，R′，R″，和R选自H，C1-18的烷基，链烯基，取代或非取代苯基、烷基苯基或链烯基苯基，附加条件为R′，R″和R不全是H；也可是所述活化剂的混合物。
本发明包括含有所述的酰化柠檬酸酯的粒状或液体状活化组合物，含有所述的酰化柠檬酸酯和过氧化氢或能产生过氧化氢的化合物组成的活性漂白剂组合物，以及使用所述的酰化柠檬酸酯作为过氧化氢活化剂。在一个优选的实施例中，按照本发明的酰化柠檬酸酯是以在含有过氧化氢的酸性水溶液中配制而成。1)酰化柠檬酸酯
本发明提出的用作过酸先质体的酰化柠檬酸酯具有如下的分子式：
在漂白或消毒操作中，按照本发明的酰化柠檬酸酯将同过氧化氢反应产生过酸和柠檬酸酯。过酸的产生依赖于R基的选择，R一般选自C1-9烷基或链烯基，取代或非取代苯基，烷基苯基或链烯基苯基。优选的取代苯基为磺基苯基。优选的R是甲基或庚基，最优选为甲基。在这种情况下，酰化柠檬酸酯产生过乙酸，其效率是众所周知的。R′，R″和R选自H，C1-18烷基或链烯基、取代或非取代苯基，烷基苯基或链烯基苯基。按照本发明过酸先质体的稳定性和效率是很重要的。因此在一个给定分子中R′，R″和R不能都是H。优选R′，R″和R由H或C1-4烷基或链烯中选择。最优选R′，R″和R是甲基或乙基。虽然不属优选，但也可以使用仅部分酯化的酰化柠檬酸酯，这就是R′，R″或R或它们的混合体为H，唯一的先决条件是在一给定的分子中，不是所有的三个R′，R″和R都是H。在仅仅R′，R″或R中的一个是H的情况下，也就是酰化柠檬酸酯是一个二酯，优选为“中心”二酯，即优选R″不是H。在R′、R″和R中有两个是氢的情况下，即酰化柠檬酸酯是单酯，优选为对称单酯，即中心单酯，也就是优选R″不是H。当使用单酯的时候，优选的酯链是很长的，即接近18个碳原子。因此，柠檬酸酯作为沉淀助洗剂。
按照本发明，也可以使用所述活化剂的混合物。
按照本发明，最优选的化合物是乙酰柠檬酸三乙酯和辛酰柠檬酸三甲酯、最好是前者。
按照本发明的一些化合物可以是商购的，如这里优选的乙酰柠檬酸三乙酯。其它化合物可以按本领域技术人员熟知的方法合成。辛酰柠檬酸三甲酯作为一个例子在下文描述。2)含酰化柠檬酸酯的粒状组合物
按照本发明的酰化柠檬酸酯以粒状组合物的方式被使用。由于本发明的一些化合物如酰化柠檬酸三乙酯是液体的，因此必须将这些液体组合物吸收在固体载体上，如多孔硅酸盐，滑石，淀粉或交联聚合物吸收剂或使其形成胶囊，例如在EP242135中描述的如酵母一类的微生物，或者将它们包括在固体状态的复合物中，例如同环糊精形成的复合物，用于粒状组合物。这种把液体加入粒状产品的方法在现有技术中已被广泛描述在这里不作进一步描述。
这种粒状产品可以配制成无任何产生过氧化氢的化合物的活化组合物，用于同含过氧化氢或能产生过氧化氢化合物的第二组份相混合。另外，按照本发明的含酰化柠檬酸酯的粒状产品，也可以配制成含有产生过氧化氢的化合物。这类能产生过氧化氢的化合物已在现有技术中被广泛描述，包括各种盐及过硼酸，过碳酸盐形式等等。
按本发明的粒状组合物也可以配制成传统组合物或“所谓”具有较高的堆积密度的“浓缩”或“压紧”组合物，其堆积密度至少600g/l。因此，按照本发明的粒状组合物，如果有，将含有全部组合物重量的2％到60％的可产生过氧化氢的化合物，优选10％-40％。产生过氧化氢化合物的用量按预知的给定组合物的确切使用而调整。按照本发明完全配制的洗涤剂组合物将倾向于含较少量的所述化合物，而作为漂白助剂所配制的组合物可以含有较多量的可产生过氧化氢的化合物，同样地，按本发明的粒状组合物可含有全部组合物重量0.5％至60％的本发明酰化柠檬酸酯组合物或它们的混合物，优选为全部组合物重量的5％-30％。这里，酰化柠檬酸酯的最佳量也将按所配制的组合物的使用目的而调整。这种组合物的例子将在下文提供。
这种粒状产品也可能含有填料材料，例如硫酸钠或硫酸钾，氯化物或碳酸盐。按照产品的使用目的，产品中可以含有外加配料。例如，在洗涤用洗涤剂系列中，希望在产品中含有如表面活性剂、缓冲剂，去污剂、污物悬浮剂和酶等配料，所有这些都已在现有技术中广为描述。虽然本发明的酰化柠檬酸酯提供了增效作用，但也希望含有助洗剂，荧光增白剂和其它在本领域公知的配料。2)含酰化柠檬酸酯的液体组合物
在本发明优选的实施例中，本发明的酰化柠檬酸酯用于液体水介质组合物。在这种情况下，液体组合物也可配制成不含过氧化氢，活化组合物，或含有过氧化氢的活化的漂白组合物。在这两种情况下，按本发明的酰化柠檬酸酯由于表现出优越的水解稳定性而特别有用。对于最优的稳定性，液体组合物必须在温和的酸性范围内配制和缓冲，即pH1至6，优选3至5。组合物适当的缓冲作用可由氧化稳定的有机或无机酸提供；适宜的酸的例子是己二酸、酒石酸、戊二酸、磷酸、琥珀酸和柠檬酸。最优选是柠檬酸。这种液体组合物具有显著的储存稳定性，因此极少出现尖活，以及有效氧极少损失。当用于洗涤操作时，主要由于稀释使洗涤剂介质的pH升高，***能有效地反应产生过酸。本发明的组合物也用于含有洗涤剂组合物的洗涤水溶液，洗涤剂本身能提供碱性。因此能获得有效的洗涤漂白效果。在非洗涤应用时，产生少量过酸，因此消毒作用的获得此漂白作用更重要。所以按照本发明的含水液体组合物可以用于洗涤时的漂白，也可以用于硬表面消毒。
按照本发明，含水液体组合物含全部组合物重量的0.5％至50％的本发明酰化柠檬酸酯，或其混合物，优选2％-20％。
按照本发明活化的含水液体漂白组合物含有全部组合物重量的0.5％至30％的过氧化氢，优选2％至20％。调整最佳酰化柠檬酸酯和过氧化氢的量以及酰化柠檬酸酯和过氧化氢的比率以便获得预期的漂白性能。
由于本发明的一些酰化柠檬酸酯在水中溶解性差，在组合物中可以含有溶剂体系，以期提高酰化柠檬酸酯在组合物中的溶解性。典型的这种溶解体系含有醇。
按照本发明的含水液体组合物可进一步含有过氧化氢稳定剂、例如锡酸盐、焦磷酸盐，络合剂如EDTA和WTA，自由基捕捉剂如BHT等等。
正如在上面描述  的干性组合物，按本发明的含水液体体组合物也可含有传统的配料，这取决于该组份的使用目的。这些传统的配料包括表面活性剂，酶，助洗剂，去污剂、染料、遮光剂、香料及其它少量成分。表面活性剂特别的益处是它们能促使本发明的某些难溶于水的酰化柠檬酸酯溶解，如酰化柠檬酸三乙酯。
实施例
下面的实施例用来阐述本发明；它们不意味着限制本发明的范围。实施例1：辛酰化柠檬酸三甲酯的合成
柠檬酸三甲酯(11.81g；0.05mole)溶解在50℃干燥吡啶(4.35g；0.055mole)和甲苯(50ml)的混合物中，辛酰氯(8.95g；0.055mol)同另外甲苯(10ml)混合，在搅拌下滴加并将产生悬浮液维持在65℃过夜。过滤后，用酸(5％HCl)和水洗涤液体，干燥(Na2SO4)并蒸发至干，产生所需的(NMR光谱)淡黄色的油状酯(12.05g，产率67％)。NMR信号响应如下
1H信号(由TMS内标)：(a)0.88，t；(b)1.31，m，(c)2.35，t ；(d)3.17，S；(e)3.61，S；(f)3.65，S
TLC色谱法(Merck G60平板，氯仿为溶剂，二氯荧光黄显色)确定酯为单点，RF0.43。
这个物质(0.2％)的水解作用，在40℃，在含四水合过硼酸钠(0.3％)和磷酸乙二胺四甲酯(40ppm)的标准重型洗涤剂产品溶液(1％；Ariel  Ultra R)中，用同硫代硫酸盐滴定来测定，在30分钟内，得到55％(理论产率)的过辛酸。实施例2：粒状洗涤剂组合物
酰化柠檬酸三乙酯(ATC)按EP242135(AD2Limited)描述的方法在酵母细肿胶囊化至填充53％(重量)。产生的可自由流动的固体胶囊加入下面的粒状洗涤剂组合物中：配料                           重量％线型烷基苯磺酸盐               7.9脂肪醇硫酸盐                   2.1Dobanol 45/E7                       2.8丙烯酸/马来酸共聚物                 3.5沸石                                21.6柠檬酸酯/柠檬酸                     10.5硅酸钠                              1.0螯合剂                              0.7泡沫抑制剂                          1.7—水合过硼酸钠                      11.3酰化柠檬酸三乙酯胶囊                19.8(＝10.5ATC)蛋白酶                              1.2香料                                0.3其它                                15.6
这种洗涤剂组合物的全水解作用，用硫代硫酸盐滴定的方法测定，在少于15分钟给出过乙酸的理论产率。实施例3：碱性粒状漂白增效剂
胶囊化的酰化柠檬酸三乙酯(ATC)(如上所述)加入到下面的粒状漂白增效剂组合物中：配料                                 量％线型烷基苯磺酸盐                     18.6柠檬酸酯                             24.9螯合剂                               1.7碳酸盐                               7.8ATC胶囊                              47
在加入到含—水合过硼酸盐的典型粒状洗涤剂的1％溶液中过乙酸的理论产率，通过用硫代硫酸盐滴定，在少于15分钟得到。实施例4：酸性粒状漂白增效剂
胶囊化的酰化柠檬酸三乙酯(如上所述)加入下列粒状漂白增效剂组合物中：
配料                       重量％
LAS                        18.6
柠檬酸                     24.9
螯合剂                     1.7
碳酸盐                     7.8
ATC胶囊                    47
在加入到含一水合过硼酸盐的典型粒状洗涤剂的1％溶液中过乙酸的理论产量，用硫代硫酸盐通过滴定的方法测量，在小于15分内得到结果。实施例5：粒状漂白 添加剂
胶囊化的酰化柠檬酸三乙酯(如上所述)加入到下列粒状漂白添加剂组合物中：
配料                       重量％
过碳酸盐                   30
ATC胶囊                    40
线型烷基苯磺酸盐           10.5
柠檬酸酯                   14.1
碳酸盐                     4.4
螯合剂                    1.0
在加入到不含漂白剂的粒状洗涤剂的1％溶剂中过乙酸的理论产量，用硫代硫酸钠滴定，小于15分钟内得到的结果。
实施例6-10：液体组合物
          6     7     8    9    10过氧化氢      6.0   6.0   6.0  6.0  5.0烷基硫酸钠    8.0   8.0   8.0  8.0  -HLAS          8.0   8.0   6.0  -    7.0ATC           2.0   4.0   4.0  3.5  4.0柠檬酸        1.0   1.0   1.0  0.5  1.0异丙醇        -     7.0   6.0  -    -己醇          -     5.0   5.0  -    -NaOH          pH4   pH4   pH4  pH4  pH4水和微量成分               加至100％
检验了组合物6，7，8的稳定性。有效氧和活化剂活性都是用新的组合物，并在50℃下该组合物储存两周后测试的。其结果用损失％表示。有效氧是通过高锰酸仪滴定的方法测量，滴定终点由pt电极的电位计确定。相对AVO由下面的表达式确定：
％AVO损失＝100*(AVO(新)-AVO(老化)/AVO(新)。活化剂的活性通过滴定(用NaOH，滴定终点由混合玻璃电极的电位计确定)全部新产物和老化产物的酸性来测定。假定酸度的增加完全是由于活化剂的分解。因此产生酸的摩尔数与活化剂分解的摩尔数相等。相对活化剂损失通过下面表达式确定：％活化剂损失＝100*(酸摩尔数(老化)-酸摩尔数(新)/ATC摩尔数
           稳定性数据
     50℃两周后相对AVO损失(％)    50℃两周后相对活化剂损失(％)
6    7.8                          15.0
7    5.4                          10.0
8    8.7                          7.5
这些结果表明，根据有效氧和根据活化剂稳定性两个方面，这些组合物都是稳定的，即使在恶劣的储存条件下。
       性能数据
于40℃和60℃下，在耐洗牢度试验仪测试中，DASHR粉末顶部，比较了上面提到的组合物1及不含ATC的同样组合物的洗涤漂白性能。结果是：(结果以Psu表示)
温  度      40℃    60℃
咖  啡      1.0s    0.8
  茶        2.4s    1.3s
  酒        0.6     0.3
可可粉      0.8     0.4
这些结果表明对要漂白的污迹如茶迹具有明显的漂白效果，特别是在低温如40℃时传统漂白体系通常是低效时更明显。

Claims (15)

1.一种漂白或消毒组合物，包括
a)0.5％-60％(重量)通式如下的过酸先质体或其混合物：
Figure C9211489800021
其中R选自C1-9烷基，C2-9链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；R′选自氢，C1-18烷基，C2-18链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；R″选自氢，C1-18烷基，C2-18链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；R选自氢，C1-18烷基，C2-18链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；条件是R′，R″和R不全是氢；
b)2％-60％(重量)的选自过氧化氢或产生过氧化氢的化合物的过氧化氢源；
c)平衡量的选自表面活性剂，缓冲剂，污垢解脱剂，污垢悬浮剂，酶，增效助剂，染料，香料，遮光剂，过氧化氢稳定剂和荧光增白剂的一种或多种常规洗涤剂组分。
2.权利要求1的组合物，其中R为甲基或庚基。
3.权利要求1的组合物，其中R′、R″和R选自H或C1-4烷基或C2-4链烯基。
4.权利要求3的组合物，其中R′、R″和R选自H和甲基。
5.权利要求3的组合物，其中R′、R″和R选自H和乙基。
6.权利要求1的组合物，其中过酸先质体选自乙酰柠檬酸三乙酯，辛酰柠檬酸三甲酯及其混合物。
7.权利要求1的组合物，其中全部组合物重量的0.5％-30％为过氧化氢。
8.权利要求4的组合物，其中全部组合物重量的0.5％-30％为过氧化氢。
9.权利要求5的组合物，其中全部组合物重量的0.5％-30％为过氧化氢。
10.权利要求6的组合物，其中全部组合物重量的0.5％-30％为过氧化氢。
11.一种漂白或消毒织物的方法，该方法包括使需要漂白或消毒的织物与一种水溶液接触的步骤，该水溶液含有：
a)0.5％-60％(重量)通式如下的过酸先质体或其混合物：
其中R选自C1-9烷基，C2-9链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；R′选自氢，C1-18烷基，C2-18链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；R″自氢，C1-18烷基，C2-18链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；R选自氢，C1-18烷基，C2-18链烯基，苯基，磺基苯基，烷基苯基，链烯基苯基及其混合物；条件是R′，R″和R不全是氢；
b)2％-60％(重量)的选自过氧化氢，产生过氧化氢的化合物和其混合物的过氧化氢源；
c)平衡量的选自表面活性剂，缓冲剂，污垢解脱剂，污垢悬浮剂，酶，增效助剂，染料，香料，遮光剂，过氧化氢稳定剂和荧光增白剂的一种或多种常规洗涤剂组分。
12.权利要求11的方法，其中R是甲基或庚基。
13.权利要求11的方法，其中R′、R″和R选自H，C1-4烷基和C2-4链烯基。
14.权利要求11的方法，其中R′、R″和R独立地选自H，甲基和乙基。
15.权利要求11的方法，其中所说的过酸先质体选自乙酰柠檬酸三乙酯，辛酰柠檬酸三甲酯及其混合物。
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WO1993012067A1 (en) 1993-06-24
TR26792A (tr) 1994-08-08
EP0624154A4 (en) 1995-05-03
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MA22733A1 (fr) 1993-07-01
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