CN106103636B - 变应原降低化组合物、包含其的喷雾剂和表面加工剂、变应原降低化方法、经变应原降低化的纤维结构体和建筑用内装材 - Google Patents
变应原降低化组合物、包含其的喷雾剂和表面加工剂、变应原降低化方法、经变应原降低化的纤维结构体和建筑用内装材 Download PDFInfo
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- CN106103636B CN106103636B CN201580014806.9A CN201580014806A CN106103636B CN 106103636 B CN106103636 B CN 106103636B CN 201580014806 A CN201580014806 A CN 201580014806A CN 106103636 B CN106103636 B CN 106103636B
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- LEYFXTUKPKKWMP-UHFFFAOYSA-K trichloroytterbium;hexahydrate Chemical compound O.O.O.O.O.O.Cl[Yb](Cl)Cl LEYFXTUKPKKWMP-UHFFFAOYSA-K 0.000 description 1
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- A61L9/00—Disinfection, sterilisation or deodorisation of air
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
- A61L2/18—Liquid substances or solutions comprising solids or dissolved gases
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Abstract
本发明提供能够使螨或杉花粉等变应原降低化、并且使变应原降低化对象物着色的情况少的变应原降低化组合物、使用了其的喷雾剂和表面加工剂、变应原降低化方法、经变应原降低化的纤维结构体和建筑用内装材。变应原降低化组合物含有选自由锌盐及铜盐组成的组中的一种以上的化合物(A)、和选自稀土类盐中的一种以上的化合物(B)。喷雾剂或表面加工剂含有上述中的任一变应原降低化组合物、和水或水溶性溶剂。变应原降低化方法是将上述的变应原降低化组合物在存在变应原的环境中进行处理的方法。纤维结构体是上述变应原降低化组合物经加工而得到的纤维结构体,建筑用内装材是上述的变应原降低化组合物经加工而得到的建筑用内装材。
Description
技术领域
本发明涉及使螨或花粉等变应原降低化的变应原降低化组合物和变应原降低化方法、或者用于对无纺布、纤维或纤维制品、建筑用内装材等赋予使变应原降低化的功能的变应原降低化组合物和变应原降低化方法。
背景技术
哮喘或特应性皮炎、过敏性鼻炎等过敏性疾病是让许多人苦恼的疾病,特别是近年来有增加的倾向。成为这些过敏性疾病的原因的是环境中存在的各种变应原,它们中栖居在屋内的螨或宠物的毛、花粉、霉作为代表性的吸入性变应原被众所周知。特别是栖息在房屋内的尘性螨即表皮螨类作为变应原的产生源成为大问题。关于表皮螨类,在草席、绒毯、寝具、窗帘等房屋内的纤维制品、或者在屋外的电车、汽车等移动车辆的座椅面料等也成为生长繁殖的温床。
表皮螨类中,美洲尘螨(Dermatophagoides farinae)和欧洲尘螨(Dermatophagoides pteronyssinus)为代表性品种,这些螨的尸体或粪便成为强的变应原物质。此外以初春飞散的杉(Cryptomeria japonica)的花粉为首,多种植物的花粉也成为变应原,特别是成为使过敏性鼻炎发病的原因。飞散的花粉不仅有初春的杉花粉,还有扁柏、艾蒿、猪草、鸭茅等许多种类,一年到头为某种花粉飞散的状态,认为在任何时期均有因花粉而引起过敏的危险性。
为了除去这样的螨或花粉等变应原,有使用空气调节器或空气净化器而将空气通过过滤器的方法,但能够除去的仅仅是在空气中飞舞的变应原,变成在过滤器中收集变应原物质的结果,在更换过滤器时有变应原再飞散的危险性。此外,口罩被用于防止吸入杉等的花粉,但附着在口罩上的花粉由于并非变应原消失,所以有通过再飞散而吸收的危险性。电吸尘器作为除去变应原的方法是有效的,但抽吸的垃圾中包含的大量的变应原仅仅被储藏在集尘袋中,认为在集尘袋的废弃时有变应原再飞散的危险性。
关于用于降低或者除去变应原物质的过敏性的药剂,自古以来已知有鞣酸,提出了应用鞣酸等多酚类化合物的方法。例如,公开了使用鞣酸作为变应原的失活化剂的方法(专利文献1)、使用茶提取物、羟磷灰石、表儿茶素、表没食子儿茶素、表儿茶素没食子酸酯、表没食子儿茶素没食子酸酯、没食子酸及没食子酸与碳原子数为1到4的醇的酯作为变应原的失活化剂的方法(专利文献2)。
作为利用了锌化合物的变应原降低化组合物,氧化锌、氯化锌、硫酸锌、硝酸锌等锌的无机氯化合物、或醋酸锌等水溶性锌化合物作为变应原的降低化成分、除去剂、中和组合物或不活化剂被提出(专利文献3~7)。此外,还提出了利用稀土类盐的变应原降低化组合物(专利文献8)。
现有技术文献
专利文献
专利文献1:日本特开昭61-44821号公报
专利文献2:日本特开平6-279273号公报
专利文献3:日本特开2006-239393号公报
专利文献4:日本特开2007-39620号公报
专利文献5:日本特开2003-96670号公报
专利文献6:日本特开2004-189606号公报
专利文献7:日本特表2004-510841号公报
专利文献8:日本特开2001-322937号公报
发明内容
发明所要解决的课题
然而,专利文献1中记载的那样的鞣酸虽然由于是安全性高的天然物,具有优异的变应原降低化效果,所以是优秀的制剂,但是存在呈色为褐色,进而因经时地进行着色而用途受到限制的问题。
锌化合物没有鞣酸那样的因着色而导致的用途的限制的问题。但是,氧化锌那样的非水溶性盐将变应原降低化的效果不充分,氯化锌、硫酸锌、硝酸锌、醋酸锌那样的水溶性锌化合物由于毒性高,相当于有害物质,此外在添加到树脂乳液等乳化分散物中的情况下引起聚集,所以作为变应原降低化组合物实用化存在问题。
专利文献8中记载的利用了稀土类盐的变应原降低化组合物关于使变应原降低化的效力也不一定能够令人满意。
因此,本发明的目的是提供使螨或杉花粉等变应原降低化、进而能够对无纺布、纤维或纤维制品赋予使变应原降低化的功能、并且使变应原降低化对象物着色的情况少的变应原降低化组合物、使用了其的喷雾剂和表面加工剂、变应原降低化方法。
用于解决课题的方案
本发明人为了解决这样的课题而进行了深入研究,结果出乎意料地发现,含有锌盐或铜盐和稀土类盐这两种化合物的组合物表现出飞跃地高的使变应原降低化的协同效果,该组合物能够将螨或杉花粉等变应原降低化,从而完成本发明。
即,根据本发明的变应原降低化组合物含有选自由锌盐及铜盐组成的组中的一种以上的化合物(A)、和选自稀土类盐中的一种以上的化合物(B)。在根据本发明的变应原降低化组合物中,锌盐优选为羟基酸锌,羟基酸锌更优选为葡萄糖酸锌。此外,在根据本发明的变应原降低化组合物中,铜盐优选为羟基酸铜,羟基酸铜更优选为葡萄糖酸铜。进而,在根据本发明的变应原降低化组合物中,稀土类盐优选为选自由镧盐、铈盐、铒盐、及镱盐组成的组中的一种以上的化合物,稀土类盐更优选为镧盐或铈盐。
此外,在根据本发明的变应原降低化组合物中,(A)选自由锌盐及铜盐组成的组中的一种以上的化合物与(B)选自稀土类盐中的一种以上的化合物的混合比率以重量比计为优选为1∶9~9∶1。
此外,在根据本发明的变应原降低化组合物中,优选含有总计0.5~70重量%的(A)选自由锌盐及铜盐组成的组中的一种以上的化合物和(B)选自稀土类盐中的一种以上的化合物。
此外,根据本发明的喷雾剂或表面加工剂含有上述中的任一变应原降低化组合物和水或水溶性溶剂。
此外,根据本发明的变应原降低化方法是将上述中的任一变应原降低化组合物在存在变应原的环境中进行处理的方法。根据本发明的变应原降低化方法优选使变应原降低化对象空间内、或变应原降低化对象物的表面存在上述中的任一变应原降低化组合物。在根据本发明的变应原降低化方法中,变应原降低化组合物优选通过将上述的喷雾剂喷雾到变应原降低化对象空间内而存在于变应原降低化对象空间内。此外,在根据本发明的变应原降低化方法中,变应原降低化组合物优选通过使上述的表面加工剂存在于变应原降低化对象物的表面而存在于变应原降低化对象物的表面。
此外,根据本发明的纤维结构体是上述中的任一变应原降低化组合物经加工而得到的纤维结构体。此外,根据本发明的建筑用内装材是上述中的任一变应原降低化组合物经加工而得到的建筑用内装材。
发明效果
通过这样操作,能够提供使螨或杉花粉等变应原降低化、进而能够对无纺布、纤维或纤维制品赋予使变应原降低化的功能、并且使变应原降低化对象物着色的情况少的变应原降低化组合物、使用了其的喷雾剂和表面加工剂、变应原降低化方法。
具体实施方式
本发明中使用的锌盐只要是水溶性的锌盐,则任意化合物均可以使用,可例示出硫酸锌、氯化锌等无机锌盐、醋酸锌、丙酸锌等有机酸锌盐,但从安全性的方面出发,优选羟基酸的锌盐。羟基酸是具有一个或者两个以上羟基的羧酸,作为具体的例子,可列举出甘醇酸、甘油酸、葡萄糖酸、葡糖醛酸、乳酸、丙醇二酸、2-羟基丁酸、3-羟基丁酸、苹果酸、酒石酸、柠苹酸、柠檬酸、异柠檬酸、亮氨酸、甲羟戊酸、泛解酸、蓖麻醇酸、莽草酸等,它们中优选葡萄糖酸、柠檬酸、乳酸,进一步更优选葡萄糖酸。例如,葡萄糖酸锌的急性经口毒性在大鼠中为超过5000mg/kg的值,安全性非常高,作为母乳替代食品、此外作为以预防或治疗锌缺乏症为目的的保健功能食品被利用。
本发明中使用的铜盐只要是水溶性的铜盐,则任意的化合物均可以使用,可例示出硫酸铜、氯化铜等无机铜盐、醋酸铜、丙酸铜等有机酸铜盐,但从安全性的方面出发,优选羟基酸的铜盐。作为羟基酸铜,可列举出例如葡萄糖酸铜,作为铜的增补品或保健功能食品被利用。
本发明中使用的稀土类盐可列举出钪盐、钇盐、镧盐、铈盐、镨盐、钕盐、钐盐、铕盐、钆盐、铽盐、镝盐、钬盐、铒盐、铥盐、镱盐、镥盐,特别优选镧盐、铈盐、铒盐、镱盐,更优选镧盐、铈盐。这些稀土类盐可以使用作为一般的试剂或工业用原料而市售的物质。
作为盐,具有任意的抗衡离子的盐均可以使用,可例示出氯化物盐、硫酸盐、硝酸盐、溴化物盐、碘化物盐、碳酸盐、磷酸盐、有机酸盐、氢氧化物等。作为有机酸盐,可列举出一价或二价的羧酸或羟基酸的盐,具体而言,作为羟基酸,可例示出乳酸、葡萄糖酸、酒石酸、柠檬酸、苹果酸,作为一价或二价的羧酸,可例示出醋酸、丙酸、丙二酸、琥珀酸、戊二酸、己二酸、壬二酸等。它们中,优选氯化物盐、羟基酸盐,进一步更优选氯化物盐、葡萄糖酸盐、乳酸盐。
羟基酸稀土类盐可以使用作为一般的试剂或工业用原料而市售的物质,此外,也可以由羟基酸和通用的无机的稀土类盐或稀土类氧化物制备。关于用于制备的这些羟基酸,可以使用一般作为试剂或工业用原料而市售的物质。为了制备,可列举出使稀土类的氧化物与羟基酸的水溶液直接反应的方法。此外,可以通过使碱金属的氢氧化物与氯化物等无机稀土类盐的水溶液反应而预先制备稀土类盐的氢氧化物,进一步使羟基酸与氢氧化物反应而制备稀土类的羟基酸。作为碱金属的氢氧化物,可列举出例如氢氧化钠、氢氧化钾、氢氧化锂等,优选氢氧化钠。
本发明的变应原降低化组合物作为对象的变应原中,可列举出来自欧洲尘螨(Dermatophagoides pteronyssinus)的粪便的变应原(Der p1)及来自虫体的变应原(Derp2)、来自美洲尘螨(Dermatophagoides farinae)的粪便的变应原(Der f1)及来自虫体的变应原(Der f2)。此外,作为来源于植物的变应原,以来自杉(Cryptomeria japonica)的花粉的变应原(Cry j1)为首,可列举出扁柏、猪草、艾蒿、鸭茅、黄花茅等变应原。除此以外,还可列举出来自狗的毛或头皮的变应原(Can f1、Can f2)、来自猫的毛或头皮的变应原(Feld1)、来自蟑螂的变应原(Bra g1、Bra g2)、来自霉的变应原(Alt a1)、来自天然胶乳的变应原等。它们中,来自螨的变应原及来自杉花粉的变应原作为需要降低化的变应原特别受到重视。通过使用本发明的组合物、及将本发明的组合物加工而得到的无纺布、纤维或纤维制品、建筑用内装材等,能够将上述列举的各种变应原降低化,能够实质性地消除多种变应原。
本发明的变应原降低化组合物通过存在于作为存在变应原的环境的变应原降低化对象物的表面,能够将变应原降低化对象物的变应原降低。作为变应原降低化对象物,例如有无纺布、纤维、纤维制品、建筑用内装材。另外,它们是变应原降低化对象物的例示,变应原降低化对象物并不限定于这些。无纺布、纤维、纤维制品为纤维结构体的一个例子。
在变应原降低化对象物为无纺布、纤维或纤维制品那样的纤维结构体的情况下,通过浸渍、涂布、喷雾等方法使变应原降低化组合物存在于变应原降低化对象物的表面。作为纤维或纤维制品,可列举出衣服、地毯、沙发、壁纸、窗帘等室内装饰类、被罩、被套、被棉絮、床单、枕套、垫子等寝具类、汽车座椅、汽车脚垫等汽车部件类、缝制玩具等,作为无纺布,可列举出扫除用湿巾、口罩、过滤器材料、电吸尘器的集尘袋等。
能够使用本发明的变应原降低化组合物进行处理的无纺布或纤维有各种,例如可列举出尼龙、棉、聚酯、羊毛等,也可以是使用了两种以上这些纤维的复合纤维。此外还可以对使用了聚乙烯或聚丙烯的无纺布进行使用。本发明的变应原降低化组合物向无纺布、纤维或纤维制品的加工或处理方法没有特别限定,可以进行浸渍处理、喷雾处理、吸尽加工等。
此外,在变应原降低化对象物为建筑用内装材的情况下,通过利用作为含有变应原降低化组合物的表面加工剂的一个例子的涂敷剂、涂料等进行建筑用内装材的表面加工,使建筑用内装材的表面存在变应原降低化组合物。作为建筑用内装材,可列举出使用了氯乙烯等树脂的壁纸、天花板材料、胶合板等木质材料、地板材料等。
在对这些建筑用内装材进行本发明的变应原降低化组合物的处理的情况下,优选通过表面加工来进行。特别是通过使用在水溶性或水性的表面加工剂或涂敷剂中添加了本发明的变应原降低化组合物的表面加工剂,能够有效地进行表面加工。此外,对于涂料,优选向水性的涂料中进行添加。
水性的表面加工剂可以使用一般作为工业用制品市售的物质。这样的表面加工剂没有特别限制,可列举出淀粉、酶改性淀粉等各种改性淀粉、聚乙烯基醇、聚丙烯酰胺、羧甲基纤维素等水溶性高分子,此外可列举出丙烯酸系树脂乳液、醋酸乙烯酯系树脂乳液、丙烯酸-苯乙烯系树脂乳液、丙烯酸-醋酸乙烯酯系树脂乳液、氯乙烯系树脂乳液、氯乙烯-丙烯酸系树脂乳液、氨基甲酸酯系树脂乳液等水性的树脂乳液。与在本发明的变应原降低化壁纸中使用水溶性高分子相比,优选使用可以期待固化皮膜的耐水性的水性的树脂乳液。所谓“为水性”表示表面加工剂中含有的高分子溶解于水中、或非水溶性的高分子以树脂乳液的形式分散于水或极性溶剂中,这样的水性的表面加工剂能够以任意的比率与水全盘均匀地进行混合。
例如,可列举出作为丙烯酸系树脂乳液的VONCOAT(注册商标、DIC株式会社制)、作为氯乙烯系树脂乳液、或氯乙烯与丙烯酸酯或醋酸乙烯酯等的共聚树脂乳液的Vinyblan(注册商标、日信化学工业株式会社制)、作为氨基甲酸酯系乳液的SUPERFLEX(注册商标、第一工业制药株式会社制)、ADEKA BONTIGHTER(注册商标)HUX(株式会社ADEKA制)等。
在以上列举的各种用途中进行本发明的变应原降低化组合物的加工时,可以将变应原降低化组合物制成适于加工的制剂,以使能够容易地进行处理。作为这样的制剂,可列举出溶解于水或水溶性溶剂中的水溶性剂、对非水溶性剂提高了溶解性的油剂或乳剂、此外保持于适当的载体上的粉剂、粒剂等。它们中,优选溶解于水或水溶性溶剂中的水溶性剂。
此外在将本发明的变应原降低化组合物作为喷雾剂适用时,以水作为基础的液剂是适合的,以有效成分的总计计在0.01~20%、优选在0.1%~5.0%、进一步优选在0.1~2%的范围内含有锌盐或铜盐和稀土类盐。此外,为了提高喷雾时的干燥性,也可以添加挥发性的有机溶剂。作为这样的有机溶剂,没有特别限制,但作为安全性没有问题的挥发性高的溶剂,可列举出乙醇。进而,喷雾剂中,作为其他的成分,也可以添加香料、除臭成分、抗菌成分等。
此外,在将本发明的变应原降低化组合物作为表面加工剂适用时,以有效成分的总计计可以在0.5~70%、优选在1%~50%、进一步优选在2~30%的范围内含有锌盐或铜盐和稀土类盐。锌盐或铜盐与稀土类盐的混合比率以重量比计优选为1∶9~9∶1。
上述的喷雾剂可以相对于作为存在变应原的环境的室内等居住空间、车或电车等交通工具内的空间适用,能够降低在空间内通过附着或者浮游而存在的螨或花粉等各种变应原。室内等居住空间或交通工具内的空间是变应原降低化对象空间的一个例子。
在进行制剂的方面,为了提高稳定性等目的,可以添加表面活性剂。表面活性剂没有特别限定,可列举出非离子性表面活性剂、阴离子性表面活性剂、阳离子性表面活性剂、两性表面活性剂。非离子性表面活性剂的种类没有特别限定,例如可列举出聚氧乙烯烷基苯基醚、聚氧乙烯苯乙烯基苯基醚、聚氧乙烯烷基醚、聚氧乙烯烯基醚、山梨糖醇酐脂肪酸酯、聚氧乙烯山梨糖醇酐脂肪酸酯等。阴离子性表面活性剂中可列举出烷基苯磺酸酯、聚氧乙烯烷基苯基醚硫酸酯、二烷基磺基琥珀酸酯等。阳离子性表面活性剂中可列举出脂肪族胺盐及其季铵盐等,两离子性表面活性剂中可列举出甜菜碱型表面活性剂、氨基羧酸盐等。此外,这些非离子性表面活性剂、阴离子性表面活性剂、阳离子性表面活性剂及两离子性表面活性剂可以单独使用一种,也可以将两种以上并用。
在本发明的变应原降低化组合物中,还可以在不损害物性的范围内,进一步添加公知的变应原降低化成分。作为变应原降低化成分,可列举出二羟基苯甲酸或2,4,6-三羟基苯甲酸等羟基苯甲酸系化合物或其盐、对羟基聚苯乙烯或聚苯乙烯磺酸盐等聚苯乙烯系化合物、柿漆等天然提取物、钙盐或锶盐等无机盐系化合物。
本发明的变应原降低化组合物以除去屋内尘性螨的变应原为目的而使用时,通过与杀螨剂同时并用,还能够使其变应原降低化效果进一步持续。使用的杀螨剂只要是相对于屋内尘性螨具有致死效果或驱除效果的物质,则没有特别限定,例如可以使用苄基醇、苯甲酸苄基酯、水杨酸苯酯、肉桂醛、海索油、胡萝卜籽油等,此外可以使用天然除虫菊酯、苯醚菊酯、氯菊酯等拟除虫菊酯系化合物、杀螟松、马拉硫磷、倍硫磷、二嗪农等有机磷系化合物、三氯杀螨醇、杀螨酯、噻螨酮、吡螨胺、哒螨灵、磺胺螨酯等。
本发明的变应原降低化组合物有时会担心霉或者菌的增殖。因此可以同时并用防霉剂或抗菌剂。防霉剂或抗菌剂的种类只要是具有防霉或抗菌效果的物质,则没有特别限定,例如可以使用5-氯-N-甲基异噻唑啉酮、二硫氰酸亚甲基酯、2-溴-2-硝基丙烷-1,3-二醇、戊二醛、碘丙炔基丁基氨基甲酸酯、吡啶硫醇-N-氧化物的锌盐、1,2-苯并异噻唑啉酮、1,2-二溴-2,4-二氰基丁烷、葡萄糖酸氯己定、2-异丙基-5-甲基苯酚、3-甲基-4-异丙基苯酚、邻苯基苯酚、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯、对氯间二甲苯酚、对氯间甲酚、聚赖氨酸、苯扎氯铵、二癸基二甲基氯化铵、N-正丁基苯并异噻唑啉酮、N-辛基异噻唑啉酮、2-(4-噻唑基)苯并咪唑、2-苯并咪唑基氨基甲酸甲酯、四氯间苯二甲腈、对甲苯基二碘甲基砜、对氯苯基-3-碘丙炔基缩甲醛、2,3,5,6-四氯-4-(甲基磺酰基)吡啶、脂肪酸甘油酯、扁柏油酚等。
在本发明的变应原降低化组合物的制剂化时,除了上述的表面活性剂、防螨剂、抗菌剂以外,根据需要还可以添加螯合剂、防锈剂、香料、防垢剂、消泡剂、抗静电剂、树脂粘合剂、增稠剂、柔软加工剂等。
作为本发明的变应原降低化组合物的使用形态,可列举出喷雾剂用途或加工剂用途。通过添加到环境中人有可能接触的组合物、例如柔软剂、除臭剂、防霉剂、除菌剂、杀虫剂、涂料、粘接剂等中,也能够使环境中的变应原降低化。通过将环境中人有可能接触的材料、例如木材、混凝土、金属、岩石、玻璃等建筑材料等、利用橡胶、纸、树脂、塑料的成型品等以本发明的变应原降低化组合物进行处理,也能够使环境中的变应原降低化。
实施例
通过实施例、试验例对本发明更详细地进行说明,但本发明不受它们的限定。另外,下述所示的%全部为重量%。
为了实施例及比较例的制备,作为原料,使用以下的试剂等。
氯化镧七水合物(和光纯药工业株式会社制)
氯化铈七水合物(和光纯药工业株式会社制)
氯化钐六水合物(和光纯药工业株式会社制)
氯化钆六水合物(和光纯药工业株式会社制)
氯化镝六水合物(和光纯药工业株式会社制)
氯化钬六水合物(和光纯药工业株式会社制)
氯化铒六水合物(和光纯药工业株式会社制)
氯化镱六水合物(和光纯药工业株式会社制)
硝酸镱四水合物(和光纯药工业株式会社制)
氧化镧(和光纯药工业株式会社制)
氧化钕(和光纯药工业株式会社制)
葡萄糖酸锌(Helshas Zn(注册商标)、扶桑化学工业株式会社制)
葡萄糖酸铜(和光纯药工业株式会社制)
氯化锌(和光纯药工业株式会社制)
硫酸铜五水合物(和光纯药工业株式会社制)
氯化钙二水合物(和光纯药工业株式会社制)
氯化锶六水合物(和光纯药工业株式会社制)
氯化铝六水合物(和光纯药工业株式会社制)
硝酸镓n水合物(n=7~9)(和光纯药工业株式会社制)
氯化铟四水合物(稀产金属株式会社制)
氯化钴六水合物(OUTKUMPU公司制)
氯化镍六水合物(和光纯药工业株式会社制)
碱性氯化锆(约45%)(Zircosol ZC-2(注册商标)、第一稀元素化学工业株式会社制)
90%乳酸(株式会社武藏野化学研究所制)
苹果酸(DL-苹果酸:和光纯药工业株式会社制)
50%葡萄糖酸水溶液(和光纯药工业株式会社制)
鞣酸(富士化学工业株式会社制)
乳酸镧水溶液的制备
在安装有球型冷凝管的100mL容量的三角烧瓶中,将90%乳酸溶液4.5g与离子交换水69.0g混合,进一步添加氧化镧1.2g。在热水浴中加温至75℃并继续搅拌3小时,使氧化镧溶解。放冷,得到含有约4%的乳酸镧的水溶液。
乳酸钕水溶液的制备
在安装有球型冷凝管的100mL容量的三角烧瓶中,将90%乳酸10.4g与离子交换水29.4g混合,进一步添加氧化钕4.2g。在热水浴中加温至75℃并搅拌1小时后,添加硫酸1滴。进一步继续搅拌1小时,使氧化钕溶解。冷却后取出,使用离子交换水将总量稀释至120g,得到含有约4%的乳酸钕的紫色的水溶液。
葡萄糖酸钕水溶液的制备
在安装有球型冷凝管的500mL容量的三角烧瓶中,将50%葡萄糖酸水溶液20.5g与离子交换水300g混合,进一步添加氧化钕2.2g。在热水浴中加温至75℃并搅拌1小时后,添加硫酸1滴。进一步继续搅拌3小时,使用离子交换水将总量稀释至480g,使氧化钕溶解。放冷,得到含有约2%的葡萄糖酸钕的紫色的溶液(比较例24)。
苹果酸镧水溶液的制备
在安装有球型冷凝管的300mL容量的三角烧瓶中,将苹果酸3.1g与离子交换水200g混合,进一步添加氧化镧1.2g。在热水浴中加温至75℃并搅拌2小时后,添加硫酸1滴。进一步搅拌3小时,使氧化镧溶解。放冷,得到含有约2%的苹果酸镧的水溶液(比较例39)。
苹果酸钕水溶液的制备
在安装有球型冷凝管的300mL容量的三角烧瓶中,将苹果酸3.1g与离子交换水200g混合,进一步添加氧化钕1.2g。在热水浴中加温至75℃并搅拌2小时后,添加硫酸1滴。进一步搅拌3小时,使氧化钕溶解。放冷,得到含有约2%的苹果酸钕的紫色的水溶液(比较例40)。
以表1~3中所示的配方制备实施例1~24,以表4~9中所示的配方制备比较例1~46。
[表1]
[表2]
[表3]
[表4]
[表5]
[表6]
[表7]
[表8]
[表9]
[试验例1]
由变应原降低化组合物带来的螨变应原的降低化效果的测定
相对于含有螨变应原Der f2的以蛋白质量计约为900ng/1mL{磷酸缓冲液(pH7.2)}的变应原液,分别使25μL的实施例1~24、比较例1~46反应。对这些试样,通过Derf2酶免疫测定法(ELISA)的夹心法进行螨变应原降低化效果的测定。首先,将以磷酸缓冲液(pH7.4)稀释至2μg/mL的抗Der f2单克隆抗体15E11添加到F16MAXISORP NUNC-IMMUNOMODULE板(NUNC公司制)中,每1孔各添加100μL,在4℃下敏化3天以上。敏化后,将溶液舍弃,每1孔各添加200μL阻断试剂{1重量%牛血清白蛋白+磷酸缓冲液(pH7.2)},在37℃反应60分钟。反应后,利用磷酸缓冲液(pH7.2)将板进行洗涤。
接着,每1孔各滴加100μL的使螨变应原与上述组合物反应而得到的提取液,在37℃反应60分钟。反应后,利用磷酸缓冲液(pH7.2)将板进行洗涤。将过氧化物酶标记的抗Derf2单克隆抗体以磷酸缓冲液{pH7.2、含有1重量%牛血清白蛋白及0.05重量%聚氧乙烯(20)山梨糖醇酐单月桂酸酯}溶解成200μg/mL,每1孔各添加100uL的将其以磷酸缓冲液(pH7.2、含有1重量%牛血清白蛋白及0.05重量%聚氧乙烯(20)山梨糖醇酐单月桂酸酯)稀释1200倍的溶液。在37℃反应60分钟后,用磷酸缓冲液(pH7.2)将板进行洗涤。每1孔各添加100μL的在0.1mol/L磷酸缓冲液(pH6.2)6.5mL中加入邻苯二胺二盐酸盐(13mg Tablet、和光纯药工业株式会社制)一片和30%双氧水6.5μL而得到的溶液,在37℃反应3分钟。之后,立即各加入50μL的1mol/LH2SO4而使反应停止,用微孔板用分光光度计(Tecan Japan Co.,Ltd.制)测定吸光度(OD490nm)。将结果示于表10~12中。
[表10]
[表11]
[表12]
[试验例2]
由变应原降低化组合物带来的杉花粉变应原的降低化效果的测定
相对于作为杉花粉变应原Cry j1的约12.5ng/1mL{磷酸缓冲液(pH7.2)}的变应原液,分别使25μL的实施例1、7、8、10、11、12、14、15、16、18、19、24、比较例1、7、8、10、11、12、22、23、43、44、45、46反应。对这些试样,利用Cry j1酶免疫测定法(ELISA)的夹心法进行杉花粉变应原降低化效果的测定。首先,将以磷酸缓冲液(pH7.4、含有0.1重量%NaN3)稀释成2μg/mL的Cry j1单克隆抗体013添加到F16MAXISORP NUNC-IMMUNO MODULE板(NUNC公司制)中,每1孔各添加100μL,在4℃下敏化1天以上。敏化后,将溶液舍弃,每1孔各添加200μL的阻断试剂{1重量%牛血清白蛋白+磷酸缓冲液(pH7.2、含有0.1重量%NaN3)},在37℃反应60分钟。反应后,利用磷酸缓冲液{pH7.2、含有0.1重量%聚氧乙烯(20)山梨糖醇酐单月桂酸酯}将板进行洗涤。
接着,每1孔各滴加100μL的杉花粉变应原反应液试样,在37℃反应60分钟。反应后,利用磷酸缓冲液{pH7.2、含有0.1重量%聚氧乙烯(20)山梨糖醇酐单月桂酸酯}将板进行洗涤。将过氧化物酶标记的Cry j1单克隆抗体053用蒸馏水溶解成200μg/mL,每1孔各添加100μL将其以磷酸缓冲液{pH7.2、含有1重量%牛血清白蛋白及0.1重量%聚氧乙烯(20)山梨糖醇酐单月桂酸酯}稀释1200倍的溶液。在37℃反应60分钟后,用磷酸缓冲液{pH7.2、含有0.1重量%聚氧乙烯(20)山梨糖醇酐单月桂酸酯}将板进行洗涤。每1孔各添加100μL的在0.1mol/L磷酸缓冲液(pH6.2)13mL中加入邻苯二胺二盐酸盐(SIGMA CHEMICAL CO.制:26mg片)和30%双氧水13μL而得到的溶液,在37℃反应5分钟。之后,立即各加入50μL的2mol/LH2SO4而使反应停止,用微孔板用分光光度计(Tecan Japan Co.,Ltd.制)测定吸光度(OD490mn)。将结果示于表13中。
[表13]
[试验例3]
将2%葡萄糖酸锌水溶液(比较例10)与2%氯化镧七水合物水溶液(比较例1)如表14中所示的那样以1∶9、3∶7、7∶3、9∶1的比率混合,分别作为实施例25~28。另外,还记载了以5:5的比率混合而得到的溶液(实施例1)。对于这些实施例,通过与试验例1同样的方法测定螨变应原Der f2的降低化效果。将结果示于表14中。
[表14]
[试验例4]
将2%葡萄糖酸锌水溶液(比较例10)与2%氯化镱六水合物水溶液(比较例8)如表15中所示的那样以1∶9、3∶7、7∶3、9∶1的比率混合,分别作为实施例29~32。另外,还记载了以5∶5的比率混合而得到的溶液(实施例8)。对于这些实施例,通过与试验例1同样的方法测定螨变应原Der f2的降低化效果。将结果示于表15中。
[表15]
向氯乙烯壁纸的表面加工剂的加工
[实施例33]
将葡萄糖酸锌4g、氯化镧七水合物4g、丙二醇3.5g溶解到离子交换水中,将总量设定为100g。
[比较例47]
将葡萄糖酸锌8g、丙二醇3.5g溶解到离子交换水中,将总量设定为100g。
[比较例48]
将氯化镧七水合物8g、丙二醇3.5g溶解到离子交换水中,将总量设定为100g。
氯乙烯片材的制备
作为氯乙烯壁纸表面层,将平均聚合度为700的氯乙烯粉末(PQB83、Shin Dai-ichi Vinyl Corporation制)100g、增塑剂邻苯二甲酸二异壬酯(DINP、田冈化学工业株式会社制)50g、作为稳定剂的ADK STAB(注册商标)FL100(株式会社ADEKA制)3g、异构烷烃(IPSolvent 2028、出光兴产株式会社制)7g使用搅拌机混合。作为基材层,在A4尺寸的PPC用纸上按照成为约200g/m2的方式涂布所制备的表面层液,在150℃下加热1分钟,得到氯乙烯壁纸。
[试验例5]
作为表面加工剂,使用氨基甲酸酯系树脂乳液(SUPERFLEX 500M(注册商标)、第一工业制药株式会社制),在其中分别添加12%的实施例33、比较例47、比较例48,均匀地混合。将该表面加工剂按照成为10g/m2的方式涂布到上述氯乙烯片材上,在室温下干燥而得到变应原降低化壁纸。
将这些变应原降低化壁纸的试样切取成直径为8cm的圆形,按照涂布有表面加工剂的一面变凹的方式将壁纸试样的边缘的部分约5mm折弯。在其上展开螨变应原水溶液(Der f2浓度为900ng/mL)1mL,从上面夹持按照经变应原降低化组合物加工的面变凸的方式将边缘的部分约5mm折弯的相同的试样,使加工面合在一起。为了防止变应原水溶液的挥发,将其放入带拉链的塑料袋内,在室温下保管1小时,使用移液管回收100μL的变应原水溶液,使用与[试验例1]同样的方法进行螨变应原量的测定。将结果示于表16中。
[表16]
[实施例34]
将葡萄糖酸锌0.8g、氯化镧七水合物0.4g、聚乙二醇(分子量20000)0.8g利用离子交换水溶解,将总量设定为100g而制成喷雾剂。
[比较例49]
将葡萄糖酸锌1.6g、聚乙二醇(分子量20000)0.8g利用离子交换水溶解,将总量设定为100g而制成喷雾剂。
[比较例50]
将氯化镧七水合物0.8、聚乙二醇(分子量20000)0.8g利用离子交换水溶解,将总量设定为100g而制成喷雾剂。
[试验例6]
利用喷雾剂的变应原降低化效果的测定
将实施例34、比较例49、比较例50分别加入触发器式喷雾容器中,将约20g喷雾到公司办公室的地毯0.5m2上。经过4小时后,在电吸尘器(日立制作所PV-H23:吸入功率为240W)的抽吸软管上安装微细尘捕集装置“集尘袋”(SC Environmental Science Co.,Ltd.制),从喷雾了实施例34或比较例49、50的部分和没有喷雾的部分(对照)各自0.5m2的面积抽吸、采集1分钟垃圾。将采集了垃圾的集尘袋放入带拉链的乙烯袋中,利用磷酸缓冲5mL提取螨变应原。将螨变应原量的提取液作为测定试样,利用Der f2酶免疫测定法(ELISA)的夹心法并使用与[试验例1]同样的方法进行螨变应原量的测定。将结果示于表17中。
[表17]
[试验例7]
相对于加工无纺布的变应原降低化效果的测定
在将实施例27、比较例1、10分别以离子交换水稀释成规定浓度的溶液50g中,将80g/m2的聚丙烯制无纺布(20cm×15cm)浸渍1分钟,以轧液率约200%进行处理后,在100℃下干燥15分钟。按照加工量以有效成分量计约成为0.15g/m2的方式制备稀释率。将这些变应原降低化无纺布的试样切取成5cm×5cm,放入带拉链的聚袋内,进一步添加螨变应原水溶液(含有Der f2、以蛋白质浓度计为900ng/mL)或杉花粉变应原水溶液(Cry j1浓度为12.5ng/mL)1mL。在室温下保管1小时,使用移液管回收100μL的变应原水溶液,使用与[试验例1]或[试验例2]同样的方法进行螨变应原量或杉花粉变应原量的测定。将结果示于表18及表19中。
[表18]
[表19]
[试验例8]
利用铁的着色性试验
分别采集2mL的实施例1、14、18、比较例45到10mL容量的玻璃制样品瓶中,进一步放入1根铁钉(长度为38mm)。经时地观察外观。将结果示于表20中。含有鞣酸的比较例45在与铁钉接触后立即着色为紫色,但实施例1、14、18的外观没有见到着色。
[表20]
试样 | 初期外观 | 1小时后 | 1天后 | 3天后 |
实施例1 | 透明 | 透明 | 透明 | 透明 |
实施例14 | 透明 | 透明 | 透明 | 透明 |
实施例18 | 淡蓝色 | 淡蓝色 | 透明 | 透明 |
比较例45 | 淡褐色 | 紫色 | 浓紫色 | 浓紫色 |
使用本发明的变应原降低化组合物,能够提供能够对室内的地板、地毯、沙发、壁纸、窗帘等室内装饰类、被罩、被套、被棉絮、床单、枕套、垫子等寝具类、汽车座椅、汽车脚垫等汽车部件类、缝制玩具等进行喷雾的制剂,此外通过对无纺布、纤维或纤维制品、建筑用内装材等进行加工,能够提供具有使螨或杉花粉等变应原降低化的功能的过滤器材料、口罩等的无纺布、纤维或纤维制品、地板材料、天花板材料、壁纸等建筑用内装材。此外能够解决以往使用鞣酸时无法避免的着色、经时的变色、相对于铁的腐蚀之类的问题。
产业上的可利用性
通过使用本发明的含有锌盐或铜盐和稀土类盐的变应原降低化组合物,能够提供能够使螨或花粉等变应原降低化、此外在不引起着色的情况下用于对无纺布、纤维或纤维制品那样的纤维结构体赋予使变应原降低化的功能的变应原降低化组合物、及能够将变应原降低化的无纺布、纤维或纤维制品、壁纸、地板材料、天花板材料等建筑用内装材。
Claims (10)
1.一种变应原降低化方法,其将变应原降低化组合物在存在变应原的环境中进行处理,
所述变应原降低化组合物含有(A)选自锌盐中的一种以上的化合物和(B)选自稀土类盐中的一种以上的化合物,
所述变应原降低化组合物为水溶液,
所述变应原降低化组合物是用于使螨变应原或杉花粉变应原降低化的变应原降低化组合物,
所述锌盐为羟基酸锌。
2.一种变应原降低化方法,其使变应原降低化组合物存在于变应原降低化对象空间内,
所述变应原降低化组合物含有(A)选自锌盐中的一种以上的化合物和(B)选自稀土类盐中的一种以上的化合物,
所述变应原降低化组合物为水溶液,
所述变应原降低化组合物是用于使螨变应原或杉花粉变应原降低化的变应原降低化组合物,
所述锌盐为羟基酸锌。
3.一种变应原降低化方法,其将喷雾剂喷雾到变应原降低化对象空间内,
所述喷雾剂含有变应原降低化组合物、和水或水溶性溶剂,
所述变应原降低化组合物含有(A)选自锌盐中的一种以上的化合物和(B)选自稀土类盐中的一种以上的化合物,
所述变应原降低化组合物为水溶液,
所述变应原降低化组合物是用于使螨变应原或杉花粉变应原降低化的变应原降低化组合物,
所述锌盐为羟基酸锌。
4.一种变应原降低化方法,其使变应原降低化组合物存在于变应原降低化对象物的表面,
所述变应原降低化组合物含有(A)选自锌盐中的一种以上的化合物和(B)选自稀土类盐中的一种以上的化合物,
所述变应原降低化组合物为水溶液,
所述变应原降低化组合物是用于使螨变应原或杉花粉变应原降低化的变应原降低化组合物,
所述锌盐为羟基酸锌。
5.一种变应原降低化方法,其使表面加工剂存在于变应原降低化对象物的表面,
所述表面加工剂含有变应原降低化组合物、和水或水溶性溶剂,
所述变应原降低化组合物含有(A)选自锌盐中的一种以上的化合物和(B)选自稀土类盐中的一种以上的化合物,
所述变应原降低化组合物为水溶液,
所述变应原降低化组合物是用于使螨变应原或杉花粉变应原降低化的变应原降低化组合物,
所述锌盐为羟基酸锌。
6.根据权利要求1~5中任一项所述的变应原降低化方法,其中,
所述羟基酸锌为葡萄糖酸锌。
7.根据权利要求1~5中任一项所述的变应原降低化方法,其中,
所述稀土类盐为选自由镧盐、铈盐、钆盐、铒盐及镱盐组成的组中的一种以上的化合物。
8.根据权利要求7所述的变应原降低化方法,其中,
所述稀土类盐为镧盐或铈盐。
9.根据权利要求1~5中任一项所述的变应原降低化方法,其中,
所述(A)选自锌盐中的一种以上的化合物与所述(B)选自稀土类盐中的一种以上的化合物的混合比率以重量比计为1:9~9:1。
10.根据权利要求1~5中任一项所述的变应原降低化方法,其中,
所述变应原降低化组合物总计含有0.5重量%~70重量%的所述(A)选自锌盐中的一种以上的化合物和所述(B)选自稀土类盐中的一种以上的化合物。
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