CN111527048B - 含有角蛋白和六角板状氧化锌的粒状复合体 - Google Patents
含有角蛋白和六角板状氧化锌的粒状复合体 Download PDFInfo
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- CN111527048B CN111527048B CN201880077647.0A CN201880077647A CN111527048B CN 111527048 B CN111527048 B CN 111527048B CN 201880077647 A CN201880077647 A CN 201880077647A CN 111527048 B CN111527048 B CN 111527048B
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- keratin
- zinc oxide
- granular composite
- hexagonal
- oxide particles
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Abstract
提供一种能够制备反射近红外线并实现高光滑感和低粗糙感的外用组合物的材料。具体而言,提供一种包含角蛋白和六角板状氧化锌颗粒的粒状复合体。
Description
技术领域
本发明涉及包含角蛋白和六角板状氧化锌的粒状复合体、以及含有该粒状复合体的组合物等。
背景技术
太阳光被认为是肌肤老化的原因之一。太阳光由各种波长的光组成,除可见光以外,例如还包括紫外线、近红外线等。对于紫外线,由于其能量较大,因此正在开发一种减轻紫外线对肌肤造成的伤害的方法。另一方面,对于近红外线,由于其能量较小,因此对于对肌肤造成伤害的研究没有太大进展。但近年来发现,紫外线主要被皮肤表层吸收而不会到达深部,而近红外线从真皮到达肌肉层,甚至对深部产生影响。因此,为了减轻太阳光对肌肤的伤害,要求反射近红外线。
因此,正在研究将具有反射近红外线的能力的物质混配在外用组合物中。由于外用组合物适用于皮肤,因此在适用时获得肌肤的光滑度(高光滑感)、无粗糙(低粗糙感)也变得重要。因此,要求一种反射近红外线并实现高光滑感和低粗糙感的外用组合物。
此外,在工业上,各个领域中也期望着遮光能力高的材料,如果能够开发出可以有效屏蔽近红外线的材料,则认为其不限于上述外用组合物,也会应用于各个领域中,是有用的。
现有技术文献
专利文献
专利文献1:国际公开第2012/147886号
专利文献2:国际公开第2015/118777号
发明内容
发明要解决的问题
本发明的课题在于,开发一种能够提供反射近红外线并实现高光滑感和低粗糙感的外用组合物。
用于解决问题的方案
上述专利文献1中记载了特定的六角板状氧化锌,还记载了该六角板状氧化锌在某种程度上能够反射红外线(包括近红外线波长区域)。本发明人等发现,对于六角板状氧化锌经角蛋白处理而得到的粒状复合体,其反射近红外线的能力与六角板状氧化锌本身的能力基本相同或在其之上,而且该粒状复合体显示出较低的MIU(平均摩擦系数)和较低的MMD(摩擦系数的平均偏差),因此,混配有该粒状复合体的外用组合物可显示出优异的光滑度和低的粗糙感。
此外,对于六角板状氧化锌经角蛋白处理而得到的粒状复合体是否可以利用于外用组合物以外的用途也进行了研究,并发现,在六角板状氧化锌经特定的角蛋白处理而得到的粒状复合体与有机硅形成混合组合物时,可以起到特别优异的近红外线遮光效果。
本发明包括例如以下的项中记载的主题。
项1.
一种粒状复合体,其包含角蛋白和六角板状氧化锌颗粒。
项2.
根据项1所述的粒状复合体,其在六角板状氧化锌颗粒表面具备角蛋白。
项3.
根据项1或2所述的粒状复合体,其中,角蛋白为选自由天然角蛋白、水解角蛋白、阳离子化水解角蛋白和甲硅烷基化水解角蛋白组成的组中的至少1种。
项4.
根据项1~3中任一项所述的粒状复合体,其中,角蛋白含量为0.05~5质量%。
项5.
根据项1~4中任一项所述的粒状复合体,其一次粒径为0.1~5μm。
项6.
根据项1~5中任一项所述的粒状复合体,其中,
角蛋白为选自由源自羊毛的阳离子化水解角蛋白、源自羊毛的甲硅烷基化水解角蛋白和源自羽毛的水解角蛋白组成的组中的至少1种,且数均分子量为500~2000。
项7.
一种外用组合物,其包含权利要求1~6中任一项所述的粒状复合体。
项8.
根据项7所述的外用组合物,其为化妆品组合物、准药品组合物或医药品组合物。
项9.
一种组合物,其含有项6所述的粒状复合体和有机硅。
项10.
根据项9所述的组合物,其为有机硅薄膜。
发明的效果
本发明的包含角蛋白和六角板状氧化锌颗粒的粒状复合体与六角板状氧化锌颗粒本身相比,起到了进一步优异的光滑度和低粗糙感。进而,也能够起到与六角板状氧化锌本身基本相同或在其之上的近红外线反射效果。因此,特别能够优选用于对外用组合物的混配等。
此外,对于包含特定的角蛋白和六角板状氧化锌颗粒的粒状复合体,在与有机硅形成混合组合物时,能够起到特别优异的近红外线遮光效果。
附图说明
图1示出针对包含角蛋白和六角板状氧化锌颗粒的粒状复合体、以及六角板状氧化锌颗粒本身测定光谱反射率而得到的结果。
图2示出针对包含角蛋白和六角板状氧化锌颗粒的粒状复合体、以及六角板状氧化锌颗粒本身测定光谱反射率的结果。
图3示出将包含各种角蛋白和六角板状氧化锌颗粒的粒状复合体、以及六角板状氧化锌颗粒本身与有机硅橡胶混合而制备干燥涂膜,并测定该涂膜的屏蔽率而得到的结果。
图4示出将包含各种角蛋白和六角板状氧化锌颗粒的粒状复合体、以及六角板状氧化锌颗粒本身与有机硅橡胶混合而制备干燥涂膜,并测定该涂膜的屏蔽率而得到的结果。
图5示出将包含角蛋白和六角板状氧化锌颗粒的粒状复合体、以及六角板状氧化锌颗粒本身与有机硅橡胶混合而制备干燥涂膜,并测定该涂膜的屏蔽率而得到的结果。
具体实施方式
下面,对本发明的各实施方式进行详细说明。
本发明所包括的粒状复合体包含角蛋白和六角板状氧化锌颗粒。
作为角蛋白,没有特别限制,但可以使用作为化妆品材料(例如皮肤调理剂、毛发调理剂等)使用的公知的各种角蛋白。作为这样的角蛋白,例如可举出天然角蛋白、水解角蛋白、阳离子化水解角蛋白、甲硅烷基化水解角蛋白等。作为水解角蛋白,可举出用酸、碱或酶等将角蛋白蛋白质水解而得到的物质。此外,能够用改性剂等使水解角蛋白阳离子化或甲硅烷基化、或者使已预先改性的阳离子化角蛋白蛋白质或甲硅烷基化角蛋白蛋白质水解,从而制备阳离子化水解角蛋白、甲硅烷基化水解角蛋白。作为阳离子化水解角蛋白,例如可举出羟丙基三铵水解角蛋白、硬脂二铵羟丙基水解角蛋白、月桂二铵羟丙基水解角蛋白等。此外,作为甲硅烷基化水解角蛋白,例如可举出(二羟甲基甲硅烷基丙氧基)羟丙基水解角蛋白等。
作为角蛋白的平均分子量,没有特别限制,但例如优选100~50000左右。更优选200~40000左右。优选水解后平均分子量变小的角蛋白,例如优选300~5000左右、更优选400~3000左右、进一步优选500~2000左右。该平均分子量为数均分子量。此外,来自各化妆品材料制造商的市售品提供了数均分子量值,作为本发明中的角蛋白的平均分子量,可以优选使用该制造商提供的数均分子量值。
角蛋白的原料也没有特别限制,用作化妆品材料的公知的各种角蛋白例如由羊毛或羽毛而制备,在本发明中也可以优选使用由羊毛或羽毛制备的角蛋白。
需要说明的是,在与有机硅橡胶混合并使用粒状复合体时,该粒状复合体所含的角蛋白优选为源自羊毛的阳离子化水解角蛋白、源自羊毛的甲硅烷基化水解角蛋白、以及源自羽毛的水解角蛋白。此外,在这一情况下,角蛋白的平均分子量优选为500~2000。更优选600~1800、进一步优选700~1500。该平均分子量与上述同样,为数均分子量。
角蛋白可以单独使用1种或组合使用2种以上。
作为六角板状氧化锌颗粒,优选一次粒径为0.1~10μm的颗粒、更优选为0.1~5μm的颗粒、进一步优选为0.2~4μm的颗粒、更进一步优选为0.5~3μm的颗粒。若为这样的一次粒径,则具有高光滑度、低粗糙感,并且近红外线反射效果更加优异。
需要说明的是,六角板状氧化锌颗粒的一次粒径是如下得到的值:在利用扫描型电子显微镜(SEM)(例如JSM-6510A:日本电子社制造)拍摄到的照片的2000~50000倍的视野中,对100个颗粒测量对角线直径(六角板状面的3条对角线中的任意1条的对角线的长度)(μm),并由其累积分布的50%而求出的值。
此外,六角板状氧化锌颗粒优选长厚比为2.5以上。长厚比更优选为2.7以上、进一步优选为3.0以上。通过为长厚比为2.5以上的板状,从而具有来源于形状的更高的光滑度、低粗糙感、更高的近红外线反射效果。
需要说明的是,该长厚比是如下得到的值:在利用扫描型电子显微镜(SEM)(例如JSM-6510A:日本电子社制造)对六角板状氧化锌颗粒进行拍摄而得到的照片的2000~50000倍的视野中,针对六角板状表面朝向前面的颗粒测量其对角线直径(六角板状氧化锌颗粒的情况下为六角板状面的3条对角线中的任意1条的对角线的长度)(μm),将测量100个颗粒而得到的平均值设为L,并针对六角板状氧化锌颗粒的侧面朝向前面的颗粒(看起来呈长方形的颗粒)测量其厚度(μm)(长方形的较短一边的长度),将测量100个颗粒而得到的平均值设为T时,以这些值的比(L/T)的形式而求出的值。
六角板状氧化锌颗粒被例如国际公开第2012/147886号、2015/118777号等公开,可以通过例如这些文献中记载的方法来制造。更具体而言,例如可以通过包括使微粒氧化锌在锌盐水溶液中熟化的工序的制造方法而得到。下面,针对该制造方法进行详细阐述。
上述微粒氧化锌没有特别限定,但优选使用粒径为0.005μm以上且0.2μm以下的原料氧化锌。上述原料氧化锌的粒径相当于具有与通过BET法求出的比表面积相同的表面积的球的直径。即,粒径是由通过BET法进行测定并求出的比表面积:Sg和氧化锌的真比重:ρ,并通过下述计算式求得的值。在基于BET法的测定中,可以使用全自动BET比表面积测定装置(例如Macsorb Model HM-1200(Mountech公司制造))。
粒径(μm)=[6/(Sg×ρ)]
(Sg(m2/g):比表面积、ρ(g/cm3):颗粒的真比重)
需要说明的是,在该计算中,颗粒的真比重:ρ使用氧化锌的真比重的值即5.6。
上述原料氧化锌没有特别限定,可以使用通过公知的方法制造的氧化锌。作为市售的氧化锌,例如可以举出堺化学工业株式会社制造FINEX-75、FINEX-50、FINEX-30、SF-15、微细氧化锌等。
六角板状氧化锌颗粒可以通过使上述微粒氧化锌在锌盐水溶液中熟化而得到。即,可以通过将上述微粒氧化锌分散在锌盐水溶液中,以该状态进行加热并使其晶体生长而得到。
上述锌盐水溶液中的锌盐没有特别限定,例如可以举出乙酸锌、硝酸锌、硫酸锌、氯化锌、甲酸锌等锌盐化合物。在锌盐水溶液中,特别是使用乙酸锌水溶液的情况下,也能够适宜地获得本发明的特定的六角板状氧化锌颗粒。
此外,这些锌盐水溶液也可以通过将氧化锌、酸和水混合来对氧化锌进行酸水解而制备。在利用氧化锌、酸和水来制备锌盐水溶液时所使用的氧化锌的颗粒形状、粒径没有特别限定,但从尽量减少杂质的观点出发,氧化锌的Zn纯度优选为95%以上。此外,作为酸,例如可举出乙酸、硝酸、硫酸、盐酸、甲酸、柠檬酸、草酸、丙酸、丙二酸、乳酸、酒石酸、葡萄糖酸、琥珀酸等。特别是在使用乙酸时,能够适宜地获得本发明的特定的六角板状氧化锌颗粒。在这些锌盐水溶液之中,可以并用2种或2种以上来使用。
锌盐水溶液中的锌盐浓度优选大于0.1mol/l且为4.0mol/l以下,特别是在使用乙酸锌水溶液时,该水溶液中的乙酸锌浓度优选大于0.2mol/l且为2.0mol/l以下。
在不损害本发明的效果的范围内,上述锌盐水溶液也可以少量含有除锌盐、水以外的成分。例如也可以含有分散剂等。
在锌盐水溶液中添加微粒氧化锌并制成浆料时,优选微粒氧化锌的浓度相对于浆料总量为10~500g/l。
在上述熟化时,在不损害本发明的效果的范围内,也可以少量添加除微粒氧化锌、锌盐、水以外的成分。例如也可以添加分散剂等。
熟化优选在45~110℃进行。熟化时间可以举出0.5~24小时。可以通过熟化温度、熟化时间、原料氧化锌浓度、锌盐浓度等条件来实现粒径的调整,因此,对于这些条件,优选根据目标六角板状氧化锌颗粒进行适当设定。
对于如此得到的六角板状氧化锌颗粒,也可以根据需要进行过滤、水洗、干燥等后处理。
对于通过上述方法制造的六角板状氧化锌颗粒,也可以根据需要进行分级。作为该分级,例如可以举出利用筛的分级。作为利用筛的分级方法,例如可以举出湿式分级、干式分级。此外,也可以进行湿式粉碎、干式粉碎等处理。
上述制造方法可以不进行焙烧处理而得到六角板状氧化锌颗粒,但对通过上述方法得到的六角板状氧化锌颗粒实施焙烧处理也无妨。在焙烧时,可以举出利用公知的任意装置的方法,处理条件等也没有特别限定。
需要说明的是,作为六角板状氧化锌颗粒,也可以使用市售品。例如可以优选使用六角板状氧化锌XZ系列(堺化学工业株式会社制造),其中,可以更优选地使用XZ-1000F、XZ-2000F和XZ-3000F等。需要说明的是,该市售品的平均粒径目录值是利用激光衍射式粒度分布装置得到的测定值,因此与本发明的平均粒径值不同。
六角板状氧化锌颗粒可以单独使用1种或组合使用2种以上。
本发明的粒状复合体包含角蛋白和六角板状氧化锌颗粒,但优选在六角板状氧化锌颗粒表面具备角蛋白。特别优选角蛋白存在于六角板状氧化锌颗粒的板的表面。
作为使六角板状氧化锌颗粒表面具备角蛋白的方法(换言之,六角板状氧化锌颗粒表面的角蛋白处理方法),例如可举出具有将含有六角板状氧化锌颗粒和角蛋白的浆料干燥的工序的方法。更详细地,例如通过将六角板状氧化锌和水混合而制备浆料,一边搅拌该浆料一边以特定量(例如,以角蛋白的添加量相对于氧化锌和角蛋白总量为0.5~10质量%或1~8质量%左右的方式)添加角蛋白,并以特定时间(例如30~120分钟左右)进行熟化,根据需要进行过滤和水洗,进一步进行干燥(例如30~50℃下12~24小时左右),从而可以制备六角板状氧化锌颗粒表面具备角蛋白的粒状复合体。
本发明的粒状复合体的角蛋白含量优选为0.05~5质量%、更优选为0.8~4质量%、进一步优选为0.1~3质量%。通过以这种比例包含角蛋白,可以在光滑度、粗糙感、红外线反射性方面获得更加优异的效果。需要说明的是,该下限也可以为0.2、0.3、0.4或0.5质量%。此外,该上限也可以为2.5、2或1.5质量%。需要说明的是,该粒状复合体的角蛋白含量是以如下方式求得的值:在坩埚中加入粒状复合体及其原料的六角板状氧化锌颗粒分别各2g,在电炉中以500℃加热1小时,测定加热后的重量。然后,按照粒状复合体所含的角蛋白全部消失、并且作为原料的六角状氧化锌颗粒的减少率在任一情况下均相同,算出粒状复合体中的角蛋白含有率(质量%)。
需要说明的是,本发明的粒状复合体优选在表面具备角蛋白。此外,该粒状复合体可以仅由六角板状氧化锌颗粒和角蛋白组成,也可以在不损害本发明的效果的范围内包含除这些以外的成分。不过,优选角蛋白存在于复合体的部分或整个表面。此外,优选该粒状复合体本身为六角板状的形状。又例如,优选六角板状氧化锌颗粒和角蛋白形成层叠体。此外,优选角蛋白在六角板状氧化锌颗粒的板的表面被处理并固定化。虽然不希望进行限定性解释,但在复合体本身为六角板状的情况下,可认为当该复合体以面状铺展时,能够没有大的间隙地铺展成面。进而可认为,通过以该复合体的被角蛋白处理的表面为外表地铺展,从而在铺展面的外表形成角蛋白处理面,是优选的。
需要说明的是,在该粒状复合体中包含除六角板状氧化锌颗粒和角蛋白以外的成分的情况下,其优选存在于六角板状氧化锌颗粒和角蛋白之间。例如,在对利用其他成分进行表面处理而得到的六角板状氧化锌颗粒实施角蛋白处理并制备该粒状复合体时,在六角板状氧化锌颗粒和角蛋白之间存在其他成分(在六角板状氧化锌颗粒表面预先进行的表面处理中所使用的成分)。
需要说明的是,在本说明书中,六角板状氧化锌颗粒表面具备角蛋白的粒状复合体的概念是指,还包括在六角板状氧化锌颗粒和角蛋白之间包含其他成分的粒状复合体。换言之,六角板状氧化锌颗粒表面具备角蛋白的粒状复合体只要在粒状复合体的表面具备角蛋白,既可以与六角板状氧化锌颗粒表面相接触地具备角蛋白,也可以在角蛋白与六角板状氧化锌颗粒表面之间具备其他成分。
作为该可以预先在六角板状氧化锌颗粒表面实施的表面处理,没有特别限定,例如可以举出:利用选自由硅氧化物、硅氧化物的水合物、铝的氧化物和铝的氢氧化物组成的组中的至少1种化合物形成覆膜的表面处理;利用疏水性有机化合物的表面处理;利用硅烷偶联剂、钛偶联剂等偶联剂的表面处理等。也可以将这些中的2种以上的表面处理组合进行。
对于利用上述选自由硅氧化物、硅氧化物的水合物、铝的氧化物和铝的氢氧化物组成的组中的至少1种化合物形成覆膜,可以利用通过水解、加热分解等使Si源化合物和/或Al源化合物在粉体表面析出等方法来进行。作为上述Si源化合物和/或Al源化合物,可以使用四烷氧基硅烷或其水解缩合物、硅酸钠、硅酸钾、烷醇铝或其水解缩合物、偏铝酸钠等容易转变成SiO2、Al(OH)3、Al2O3的化合物等。
上述水解没有特别限定,可举出使用硫酸、盐酸、乙酸、硝酸等酸的方法。使用该水分散体的二氧化硅的处理方法中的中和方法可以为如下方法中的任一种:在含有六角板状氧化锌颗粒的分散体中加入酸,然后添加Si源化合物和/或Al源化合物的方法;在分散体中加入Si源化合物和/或Al源化合物,然后添加酸的方法;在分散体中同时添加Si源化合物和/或Al源化合物以及酸的方法。
作为利用上述疏水性有机化合物的处理,没有特别限定,但可举出例如硅油、烷基硅烷、烷基钛酸酯、烷基铝酸酯、聚烯烃、聚酯、金属皂、氨基酸、氨基酸盐等。其中,从化学稳定性来看,硅油是优选的。作为该硅油的具体例,可以举出利用二甲基聚硅氧烷(例如信越化学工业制造KF-96A-100cs、旭化成Wacker Silicon制造DM10)、甲基氢聚硅氧烷(例如信越化学工业制造KF-99P、Toray Dow Corning制造SH1107C)、聚二甲基硅氧烷/聚甲基硅氧烷共聚物(例如信越化学工业制造KF-9901)、甲基苯基硅酮(例如信越化学工业制造KF-50-100cs)、氨基改性硅酮(例如信越化学工业制造KF-8015、Toray Dow Corning制造JP-8500Conditioning Agent、旭化成Wacker Silicon制造ADM6060)、三乙氧基甲硅烷基乙基聚二甲基硅氧基乙基二甲聚硅氧烷(例如信越化学工业制造KF-9908)、三乙氧基甲硅烷基乙基聚二甲基硅氧基乙基己基二甲聚硅氧烷(例如信越化学工业制造KF-9909)的处理等。
作为上述利用硅烷偶联剂的处理,可以举出:乙烯基三(2-甲氧基乙氧基)硅烷、乙烯基三氯硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、2-(3,4环氧环己基)乙基三甲氧基硅烷、3-环氧丙氧基丙基三甲氧基硅烷、3-环氧丙氧基丙基甲基二乙氧基硅烷、3-环氧丙氧基丙基三乙氧基硅烷、对苯乙烯基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二乙氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、N-2(氨基乙基)3-氨基丙基甲基二甲氧基硅烷、N-2(氨基乙基)3-氨基丙基三甲氧基硅烷、N-2(氨基乙基)3-氨基丙基三乙氧基硅烷、3-氨基三乙氧基硅烷、3-三乙氧基甲硅烷基-N-(1,3-二甲基-亚丁基)丙胺、N-苯基-3-氨基丙基三甲氧基硅烷、N-(乙烯基苄基)-2-氨基乙基-3-氨基丙基三甲氧基硅烷盐酸盐、3-脲丙基三乙氧基硅烷、3-氯丙基三甲氧基硅烷、3-巯丙基甲基二甲氧基硅烷、3-巯丙基三甲氧基硅烷、双(三乙氧基甲硅烷基丙基)四硫化物、3-异氰酸酯基丙基三乙氧基硅烷、四甲氧基硅烷、四乙氧基硅烷、甲基三甲氧基硅烷、甲基三乙氧基硅烷、苯基三乙氧基硅烷、六甲基二硅氮烷、己基三甲氧基硅烷、癸基三甲氧基硅烷。
作为上述利用钛偶联剂的处理,可以举出钛酸四异丙酯、钛酸四正丁酯、钛酸丁酯二聚体、四(2-乙基己基)钛酸酯、钛酸四甲酯、乙酰丙酮钛、四(乙酰丙酮基)钛、(乙氧乙酰乙酰)合酞、辛二醇合酞、乳酸钛、三乙醇胺酞、多羟基硬脂酸钛。
在进行上述表面处理(在角蛋白处理前,预先在六角板状氧化锌颗粒表面实施的表面处理)的情况下,表面处理优选以相对于处理后的粉体总量为0.1~30重量%的比例进行。通过设为该范围内,从光滑性提高且耐湿性提高、在树脂中的分散性提高的观点来看是优选的。
作为本发明的粒状复合体的一次粒径,优选与上述六角板状氧化锌颗粒的一次粒径相等的粒径,其中,优选为0.1~5μm、更优选为0.2~4μm、进一步优选为0.5~3μm。若为这样的一次粒径,则具有更高的光滑度、低粗糙感,且近红外线反射效果更加优异。需要说明的是,该上限也可以为2.5μm、2μm、1.5μm或1μm。
需要说明的是,粒状复合体的一次粒径是如下得出的值:在利用扫描型电子显微镜(SEM)(例如JSM-6510A:日本电子社制造)拍摄到的照片的2000~50000倍的视野中,对100个颗粒测量对角线直径(特别是当粒状复合体为六角板状的形状时,为六角板状面的3条对角线中的任意1条对角线的长度)(μm),并由其累积分布的50%而求出的值。
此外,本发明的粒状复合体优选长厚比为2.5以上。长厚比更优选为2.7以上、进一步优选为3.0以上。通过为长厚比为2.5以上的板状,从而具有来源于形状的更高的光滑度、低粗糙感、更高的近红外线反射效果。
需要说明的是,当粒状复合体为六角板状的形状时,该长厚比是以如下得到的值:在利用扫描型电子显微镜(SEM)对六角板状粒状复合体进行拍摄而得到的照片的2000~50000倍的视野中,针对六角板状的粒状复合体的表面朝向前面的颗粒测量其对角线直径(六角板状面的3条对角线中的任意1条的对角线的长度)(μm),将测量100个颗粒而得到的平均值设为L,并针对六角板状的粒状复合体的侧面朝向前面的颗粒(看起来呈长方形的颗粒)测量其厚度(μm)(长方形的较短一边的长度),将测量100个颗粒而得到的平均值设为T时,以这些值的比(L/T)的形式而求出的值。
对于本发明的粒状复合体,在例如混配于外用组合物中等并使用时,能够产生优异的光滑度和低粗糙感。具体而言,本发明的粒状复合体(粉体)显示出小的MIU(平均摩擦系数)和小的MMD(摩擦系数的平均偏差)。MIU(平均摩擦系数)的值越小,则意味着光滑性越好、越容易滑动。此外,MMD(摩擦系数的平均偏差)的值越小,则意味着粗糙感越小。需要说明的是,此处的比较对象是作为粒状复合体的原料而使用的六角板状氧化锌颗粒本身。若更具体地阐述,也就是说,与作为该粒状复合体的原料而使用的六角板状氧化锌颗粒(粉体)相比,本发明的粒状复合体(粉体)显示出小的MIU(平均摩擦系数)和MMD(摩擦系数的平均偏差)。
例如,没有特别限制,但本发明的粒状复合体(粉体)例如优选MIU为1.15以下、更优选为1.1以下、进一步优选为1.05以下。此外,优选MMD为0.05以下。MMD为0.04以下或0.03以下则是更优选的。其中,优选同时满足这些MIU值和MMD值的复合体。
MIU值和MMD值是按照如下方式测定的值。即,使用摩擦感测试器(例如KES-SE摩擦感测试器(Kato Tech公司制造)),针对在双面胶带上展开的粒状复合体(粉体),在摩擦测定载荷25gf、表面测定试样移动速度1mm/秒、测定距离范围20mm的条件下测定MIU和MMD而得到的值。
本发明的粒状复合体也可以与其他成分混合,并混配于例如外用组合物(例如医药品、准药品和化妆品)、油墨、涂料、塑料等中。特别是,由于具有上述特性,因而可以得到光滑性好、粗糙也少的具有优异的粉体触感的外用组合物,从这点出发是优选的。其中,适宜混配于化妆品中使用。
作为上述化妆品没有特别限定,根据需要在这种粉体中混合化妆品原料,从而可以得到防晒剂等紫外线防御用化妆品;粉底等底妆化妆品;口红等彩妆化妆品;化妆水、乳霜等护肤化妆品;护理剂和定型剂等护发化妆品等。此外,本发明的六角板状氧化锌颗粒除了具有上述优异的粉体触感之外,还一并具有紫外线吸收能力,因此,在用于化妆品中时具有优异的性能。上述化妆品可以形成例如油性化妆品、水性化妆品、O/W型化妆品、W/O型化妆品等任意形态。
上述化妆品也可以合用在化妆品领域中能够使用的任意水性成分、油性成分。作为上述水性成分和油性成分没有特别限定,例如可以含有油成分、表面活性剂、保湿剂、高级醇、螯合剂、天然和合成高分子、水溶性和油溶性高分子、紫外线屏蔽剂、各种提取液、有机染料等色剂、防腐剂、抗氧化剂、色素、增稠剂、pH调整剂、香料、冷感剂、止汗剂、杀菌剂、皮肤活化剂、各种粉体等成分。
上述油剂没有特别限定,例如可例示出:天然动植物油脂(例如橄榄油、貂油、蓖麻油、棕榈油、牛脂、月见草油、椰子油、蓖麻油、可可油、澳洲坚果油等);蜡(例如荷荷巴油、蜂蜡、羊毛脂、巴西棕榈蜡、小烛树蜡等);高级醇(例如月桂醇、硬脂醇、鲸蜡醇、油醇等);高级脂肪酸(例如月桂酸、棕榈酸、硬脂酸、油酸、山嵛酸、羊毛脂脂肪酸等);高级脂肪族烃(例如液体石蜡、固体石蜡、角鲨烷、凡士林、纯地蜡、微晶蜡等);合成酯油(例如硬脂酸丁酯、月桂酸己酯、己二酸二异丙酯、癸二酸二异丙酯、肉豆蔻酸辛基十二烷基酯、肉豆蔻酸异丙酯、棕榈酸异丙酯、肉豆蔻酸异丙酯、异辛酸鲸蜡酯、二癸酸新戊二醇酯);硅酮衍生物(例如甲基硅酮、甲基苯基硅酮等硅油)等。此外,也可以混配油溶性的维生素、防腐剂、美白剂等。
作为上述表面活性剂,可以举出亲油性非离子表面活性剂、亲水性非离子表面活性剂等。作为上述亲油性非离子表面活性剂没有特别限定,例如可以举出:山梨糖醇酐单油酸酯、山梨糖醇酐单异硬脂酸酯、山梨糖醇酐单月桂酸酯、山梨糖醇酐单棕榈酸酯、山梨糖醇酐单硬脂酸酯、山梨糖醇酐倍半油酸酯、山梨糖醇酐三油酸酯、五-2-乙基己酸双甘油山梨糖醇酐、四-2-乙基己酸双甘油山梨糖醇酐等山梨聚糖脂肪酸酯类;单棉籽油脂肪酸甘油酯、单芥酸甘油酯、倍半油酸甘油酯、单硬脂酸甘油酯、α,α’-油酸焦谷氨酸甘油酯(α,α’-glyceryl oleate pyroglutamate)、单硬脂酸甘油苹果酸等甘油聚甘油脂肪酸类;单硬脂酸丙二醇酯等丙二醇脂肪酸酯类;氢化蓖麻油衍生物、烷基甘油醚等。
作为亲水性非离子表面活性剂没有特别限定,例如可以举出POE山梨糖醇酐单油酸酯、POE山梨糖醇酐单硬脂酸酯、POE山梨糖醇酐四油酸酯等POE山梨聚糖脂肪酸酯类;POE山梨糖醇单月桂酸酯、POE山梨糖醇单油酸酯、POE山梨糖醇五油酸酯、POE山梨糖醇单硬脂酸酯等POE山梨糖醇脂肪酸酯类;POE甘油单硬脂酸酯、POE甘油单异硬脂酸酯、POE甘油三异硬脂酸酯等POE甘油脂肪酸酯类;POE单油酸酯、POE二硬脂酸酯、POE二油酸酯、二硬脂酸乙二醇酯等POE脂肪酸酯类;POE月桂基醚、POE油烯基醚、POE硬脂基醚、POE二十二烷基醚、POE2-辛基十二烷基醚、POE胆甾烷醇醚等POE烷基醚类;POE辛基苯基醚、POE壬基苯基醚、POE二壬基苯基醚等POE烷基苯基醚类;普朗尼克等普朗尼克型类;POE/POP十六烷基醚、POE/POP2-癸基十四烷基醚、POE/POP单丁醚、POE/POP氢化羊毛脂、POE/POP甘油醚等POE/POP烷基醚类;特普(Tetronic)等四POE/四POP乙二胺缩合物类;POE蓖麻油、POE氢化蓖麻油、POE氢化蓖麻油单异硬脂酸酯、POE氢化蓖麻油三异硬脂酸酯、POE氢化蓖麻油单焦谷氨酸单异硬脂酸二酯、POE氢化蓖麻油马来酸酯等POE蓖麻油氢化蓖麻油衍生物;POE山梨糖醇蜂蜡等POE蜂蜡/羊毛脂衍生物;椰子油脂肪酸二乙醇酰胺、月桂酸单乙醇酰胺、脂肪酸异丙醇酰胺等烷醇酰胺;POE丙二醇脂肪酸酯、POE烷基胺、POE脂肪酰胺、蔗糖脂肪酸酯、POE壬基苯基甲醛缩合物、烷基乙氧基二甲基氧化胺、三油醇磷酸酯等。
作为其他表面活性剂,在稳定性和皮肤刺激性没有问题的范围内,例如也可以混配:脂肪酸皂、高级烷基硫酸酯盐、POE月桂基硫酸三乙醇胺、烷基醚硫酸酯盐等阴离子表面活性剂;烷基三甲基铵盐、烷基吡啶鎓盐、烷基季铵盐、烷基二甲基苄基铵盐、POE烷基胺、烷基胺盐、多胺脂肪酸衍生物等阳离子表面活性剂;以及咪唑啉系两性表面活性剂、甜菜碱系表面活性剂等两性表面活性剂。
作为保湿剂没有特别限定,例如可以举出:木糖醇、山梨糖醇、麦芽糖醇、硫酸软骨素、透明质酸、硫酸粘多糖、栝楼仁酸、缺端胶原、胆甾醇-12-羟基硬脂酸酯、乳酸钠、胆汁酸盐、dl-吡咯烷酮羧酸盐、短链可溶性胶原蛋白、二甘油(EO)PO加合物、刺梨提取物、蓍草提取物、草木犀提取物、1,3-丁二醇等
作为高级醇没有特别限定,例如可以举出:月桂醇、鲸蜡醇、硬脂醇、山嵛醇、肉豆蔻醇、油醇、十六十八醇等直链醇;单硬脂基甘油醚(鲨肝醇)、2-癸基十四烷醇、羊毛脂醇、胆固醇、植物甾醇、己基十二烷醇、异硬脂醇、辛基十二烷醇等支链醇等。
作为螯合剂没有特别限定,例如可以举出:1-羟基乙烷-1,1-二膦酸、1-羟基乙烷-1,1-二膦酸四钠盐、柠檬酸钠、聚磷酸钠、偏磷酸钠、葡萄糖酸、磷酸、柠檬酸、抗坏血酸、琥珀酸、依地酸等。
作为天然的水溶性高分子没有特别限定,例如可以举出:阿拉伯胶、黄蓍胶、半乳聚糖、瓜尔胶、角豆胶、刺梧桐胶、角叉菜胶、果胶、琼胶、榅桲籽(榅桲)、藻类胶(褐藻提取物)、淀粉(水稻、玉米、马铃薯、小麦)、甘草酸等植物系高分子;黄原胶、葡聚糖、琥珀酰葡聚糖、出芽短梗霉多糖等微生物系高分子;胶原蛋白、酪蛋白、白蛋白、明胶等动物系高分子。作为半合成的水溶性高分子没有特别限定,例如可以举出羧甲基淀粉、甲基羟基丙基淀粉等淀粉系高分子;甲基纤维素、硝基纤维素、乙基纤维素、甲基羟基丙基纤维素、羟基乙基纤维素、纤维素硫酸钠、羟基丙基纤维素、羧甲基纤维素钠(CMC)、结晶纤维素、纤维素粉末等纤维素系高分子;海藻酸钠、海藻酸丙二醇酯等海藻酸系高分子等。
作为合成的水溶性高分子没有特别限定,例如可以举出:聚乙烯醇、聚乙烯基甲醚、聚乙烯吡咯烷酮等乙烯基系高分子;聚乙二醇20,000、40,000、60,000等聚氧乙烯系高分子;聚氧乙烯聚氧丙烯共聚物共聚系高分子;聚丙烯酸钠、聚丙烯酸乙酯、聚丙烯酰胺等丙烯酸系高分子;聚甘油、聚亚乙基亚胺、阳离子聚合物、羧基乙烯基聚合物、烷基改性羧基乙烯基聚合物、(丙烯酸羟乙酯/丙烯酰二甲基牛磺酸Na)共聚物、(丙烯酸Na/丙烯酰二甲基牛磺酸Na)共聚物、(丙烯酰二甲基牛磺酸铵/乙烯基吡咯烷酮)共聚物、(丙烯酰二甲基牛磺酸铵/山嵛醇聚醚-25甲基丙烯酸酯)交联聚合物等。
作为无机的水溶性高分子没有特别限定,例如可以举出:膨润土、硅酸AlMg(veegum)、锂皂石、锂蒙脱石、无水硅酸等。
作为紫外线屏蔽剂没有特别限定,例如可以举出:对氨基苯甲酸(以下简称为PABA)、PABA单甘油酯、N,N-二丙氧基PABA乙酯、N,N-二乙氧基PABA乙酯、N,N-二甲基PABA乙酯、N,N-二甲基PABA丁酯等苯甲酸系紫外线屏蔽剂;N-乙酰基邻氨基苯甲酸高薄荷醇酯等邻氨基苯甲酸系紫外线屏蔽剂;水杨酸戊酯、水杨酸薄荷酯、水杨酸高薄荷酯、水杨酸辛酯、水杨酸苯酯、水杨酸苄酯、对-异丙醇水杨酸苯酯等水杨酸系紫外线屏蔽剂;肉桂酸辛酯、乙基-4-异丙基肉桂酸酯、甲基-2,5-二异丙基肉桂酸酯、乙基-2,4-二异丙基肉桂酸酯、甲基-2,4-二异丙基肉桂酸酯、丙基-对甲氧基肉桂酸酯、异丙基-对甲氧基肉桂酸酯、异戊基-对甲氧基肉桂酸酯、2-乙氧基乙基-对甲氧基肉桂酸酯、环己基-对甲氧基肉桂酸酯、乙基-α-氰基-β-苯基肉桂酸酯、2-乙基己基-α-氰基-β-苯基肉桂酸酯、甘油基单-2-乙基己酰基-二对甲氧基肉桂酸酯等肉桂酸系紫外线屏蔽剂;2,4-二羟基二苯甲酮、2,2’-二羟基-4-甲氧基二苯甲酮、2,2’-二羟基-4,4’-二甲氧基二苯甲酮、2,2’,4,4’-四羟基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-羟基-4-甲氧基-4’-甲基二苯甲酮、2-羟基-4-甲氧基二苯甲酮-5-磺酸盐、4-苯基二苯甲酮、2-乙基己基-4’-苯基-二苯甲酮-2-甲酸酯、2-羟基-4-正辛氧基二苯甲酮、4-羟基-3-羧基二苯甲酮等二苯甲酮系紫外线屏蔽剂;3-(4’-甲基亚苄基)-d,l-樟脑、3-亚苄基-d,l-樟脑、尿刊酸、尿刊酸乙酯、2-苯基-5-甲基苯并噁唑、2,2’-羟基-5-甲基苯基苯并三唑、2-(2’-羟基-5’-叔辛基苯基)苯并三唑、2-(2’-羟基-5’-甲基苯基)苯并三唑、二苯并吖嗪、二茴香酰基甲烷、4-甲氧基-4’-叔丁基二苯甲酰基甲烷、5-(3,3-二甲基-2-降冰片烯基)-3-戊烷-2-酮等。
作为其他试剂成分没有特别限定,例如可以举出:维他命A油、视黄醇、棕榈酸视黄醇酯、肌醇、盐酸吡多辛、烟酸苄酯、烟酰胺、Dl-α-生育酚烟酸酯、抗坏血酸磷酸镁、2-O-α-D-吡喃葡萄糖基-L-抗坏血酸、维他命D2(麦角钙化固醇)、dl-α-生育酚、dl-α-生育酚乙酸酯、泛酸、生物素等维他命类;雌二醇、乙炔基雌二醇等激素;精氨酸、天冬氨酸、胱氨酸、半胱氨酸、蛋氨酸、丝氨酸、亮氨酸、色氨酸等氨基酸;尿素囊、甘菊环等抗炎剂;熊果苷等美白剂;丹宁酸等收敛剂;L-薄荷醇、樟脑等清凉剂;硫磺、氯化溶菌酶、氯化吡哆醇等。
作为各种提取液没有特别限定,例如可以举出:鱼腥草提取物、黄檗提取物、草木犀提取物、短柄野芝麻提取物、甘草提取物、芍药根提取物、皂草提取物、丝瓜提取物、奎宁皮提取物、虎耳草提取物、苦参提取物、萍蓬草提取物、茴香提取物、樱草提取物、玫瑰提取物、地黄提取物、柠檬提取物、紫草根提取物、芦荟提取物、菖蒲根提取物、桉树提取物、巨木贼提取物、鼠尾草提取物、百里香提取物、茶提取物、海藻提取物、黄瓜提取物、丁香提取物、悬钩子提取物、香蜂花提取物、胡萝卜提取物、七叶树提取物、桃提取物、桃叶提取物、桑提取物、矢车菊提取物、金缕梅提取物、胸腺提取物、蚕丝提取液、甘草提取物等。
作为各种粉体,例如可以举出:红色氧化铁、黄色氧化铁、黑色氧化铁、云母钛、氧化铁包覆云母钛、氧化钛包覆玻璃薄片等光辉性着色颜料;云母、滑石、高岭土、绢云母、二氧化钛、二氧化硅等无机粉末;或者,聚乙烯粉末、尼龙粉末、交联的聚苯乙烯、纤维素粉末、有机硅粉末等有机粉末等。优选的是,为了提高官能特性、提高化妆持续性,利用有机硅类、氟化合物、金属皂、油剂、酰基谷氨酸盐等物质,采用公知的方法对粉末成分的一部分或全部进行疏水化处理并使用。此外,也可以混合不属于本发明的其他复合粉体并使用。
将本发明的粒状复合体用作油墨中的添加成分的情况下,可以举出:二氧化钛、氧化铁红、锑红、镉黄、钴蓝、普鲁士蓝、群青、碳黑、石墨等有色颜料;以及碳酸钙、高岭土、粘土、硫酸钡、氢氧化铝、滑石等体质颜料。此外,作为有机颜料,可以与可溶性偶氮颜料、不溶性偶氮颜料、偶氮色淀颜料、缩合偶氮颜料、酞菁铜颜料、缩合多环颜料等颜料成分;虫胶树脂、丙烯酸系树脂、苯乙烯-丙烯酸系树脂、苯乙烯-马来酸树脂、苯乙烯-丙烯酸-马来酸树脂、聚氨酯树脂、聚酯树脂、聚酰胺树脂等粘合剂树脂等粘合剂树脂;水混溶性有机溶剂等一并使用。
将本发明的粒状复合体用作涂料组合物中的添加成分的情况下,可以与丙烯酸系树脂、聚酯树脂、环氧树脂等涂膜形成树脂;着色颜料、体质颜料、光亮性颜料等各种颜料;固化催化剂、表面调节剂、消泡剂、颜料分散剂、增塑剂、成膜助剂、紫外线吸收剂、抗氧化剂等一并使用。此外,涂料中的树脂可以具有固化性,也可以不具有固化性。
本发明还包括含有上述本发明的粒状复合体的树脂组合物。对于这种树脂组合物,该粒状复合体作为散热性填料而发挥作用,从而具有优异的散热性。此外,由于在红外线(特别是近红外线)反射能力方面优异,因此也可以作为具有这些性能的树脂组合物来使用。
如上所述,本发明的六角板状氧化锌颗粒具有红外线(特别是近红外线)反射性能,因此也能够作为各种领域中的红外线(特别是近红外线)屏蔽材料来使用。
此外,对于本发明的包含角蛋白和六角板状氧化锌颗粒的粒状复合体,当角蛋白为特定的角蛋白的情况下,与有机硅(特别是有机硅橡胶)混合并用作有机硅组合物时,可以起到特别优异的近红外线遮光效果。作为该特定的角蛋白,例如可举出数均分子量为500~2000的、源自羊毛的阳离子化水解角蛋白、源自羊毛的甲硅烷基化水解角蛋白、或者源自羽毛的水解角蛋白。
有机硅组合物也可以包含除有机硅和粒状复合体以外的成分。作为这种成分,例如可举出固化剂。作为固化剂,例如可以使用作为有机硅橡胶固化剂而公知的物质。此外,有机硅组合物的形状也没有特别限制。例如可举出薄膜状。
需要说明的是,在本说明书中,“包含”也包括“实质上由……组成”和“由……组成”(The term"comprising"includes"consisting essentially of”and"consistingof.")。
实施例
下面,对本发明进行更详细地说明,但本发明不限定于下述实施例。
对氧化锌颗粒的各种角蛋白处理1
(实施例1):对XZ-1000F的阳离子化水解角蛋白处理(5质量%)
将粒径为0.66μm的六角板状氧化锌(XZ-1000F、堺化学工业株式会社制造)150g添加至750g水中,充分搅拌,从而得到氧化锌浓度为193g/L的水性浆料。接着,一边搅拌浆料,一边添加纯度15%的阳离子化水解角蛋白水溶液(硬脂二铵羟丙基水解角蛋白:promoisWK-SAQ、成和化成社制造)52.6g,以使得角蛋白的添加量相对于氧化锌95质量%为5质量%。直接熟化60分钟,然后进行过滤、水洗,40℃下干燥16小时,从而得到一次粒径为0.67μm的含有角蛋白和氧化锌颗粒的粒状复合体。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察所得粒状复合体的尺寸和形态。
(实施例2):对XZ-1000F的甲硅烷基化水解角蛋白处理(5质量%)
将粒径为0.66μm的六角板状氧化锌(XZ-1000F、堺化学工业株式会社制造)150g添加至750g水中,充分搅拌,从而得到氧化锌浓度为193g/L的水性浆料。接着,一边搅拌浆料,一边添加纯度25%的甲硅烷基化水解角蛋白水溶液((二羟甲基甲硅烷基丙氧基)羟丙基水解角蛋白:promois WK-HSIGF、成和化成社制造)31.6g,以使得角蛋白的添加量相对于氧化锌95质量%为5质量%。直接熟化60分钟,然后进行过滤、水洗,40℃下干燥16小时,从而得到一次粒径为0.64μm的含有角蛋白和氧化锌颗粒的粒状复合体。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察所得粒状复合体的尺寸和形态。
(实施例3):对XZ-1000F的水解角蛋白处理(5质量%)
将粒径为0.66μm的六角板状氧化锌(XZ-1000F、堺化学工业株式会社制造)150g添加至750g水中,充分搅拌,从而得到氧化锌浓度为193g/L的水性浆料。接着,一边搅拌浆料,一边添加水解角蛋白粉体(成和化成社制造)7.9g,以使得角蛋白的添加量相对于氧化锌95质量%为5质量%。直接熟化60分钟,然后进行过滤、水洗,40℃下干燥16小时,从而得到一次粒径为0.63μm的含有角蛋白和氧化锌颗粒的粒状复合体。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察所得粒状复合体的尺寸和形态。
(实施例4):对XZ-1000F的天然角蛋白处理(5质量%)
将粒径为0.66μm的六角板状氧化锌(XZ-1000F、堺化学工业株式会社制造)150g添加至750g水中,充分搅拌,从而得到氧化锌浓度为193g/L的水性浆料。接着,一边搅拌浆料,一边添加纯度5%的天然角蛋白水溶液(成和化成社制造)158.0g,以使得角蛋白的添加量相对于氧化锌95质量%为5质量%。直接熟化60分钟,然后进行过滤、水洗,40℃下干燥16小时,从而得到一次粒径为0.66μm的含有角蛋白和氧化锌颗粒的粒状复合体。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察所得粒状复合体的尺寸和形态。
(实施例5):对XZ-1000F的阳离子化水解角蛋白处理(1质量%)
将粒径为0.66μm的六角板状氧化锌(XZ-1000F、堺化学工业株式会社制造)150g添加至750g水中,充分搅拌,从而得到氧化锌浓度为193g/L的水性浆料。接着,一边搅拌浆料,一边添加纯度15%的阳离子化水解角蛋白水溶液(硬脂二铵羟丙基水解角蛋白:promoisWK-SAQ、成和化成社制造)10.1g,以使得角蛋白的添加量相对于氧化锌99质量%为1质量%。直接熟化60分钟,然后进行过滤、水洗,40℃下干燥16小时,从而得到一次粒径为0.70μm的含有角蛋白和氧化锌颗粒的粒状复合体。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察所得粒状复合体的尺寸和形态。
(实施例6):对XZ-1000F的阳离子化水解角蛋白处理(10质量%)
除了将角蛋白的添加量变更为角蛋白的添加量相对于氧化锌90质量%为10质量%以外,与实施例1和5同样地得到含有角蛋白和氧化锌颗粒的粒状复合体,并进行形态观察和物性评价。
(实施例7):对XZ-1000F的阳离子化水解角蛋白处理(20质量%)
除了将角蛋白的添加量变更为角蛋白的添加量相对于氧化锌80质量%为20质量%以外,与实施例1和5同样地得到含有角蛋白和氧化锌颗粒的粒状复合体,并进行形态观察和物性评价。
(实施例8):对XZ-3000F的阳离子化水解角蛋白处理(5质量%)
将粒径为2.08μm的六角板状氧化锌(XZ-3000F、堺化学工业株式会社制造)150g添加至750g水中,充分搅拌,从而得到氧化锌浓度为193g/L的水性浆料。接着,一边搅拌浆料,一边添加纯度15%的阳离子化水解角蛋白水溶液(硬脂二铵羟丙基水解角蛋白:promoisWK-SAQ、成和化成社制造)52.6g,以使得角蛋白的添加量相对于氧化锌95质量%为5质量%。直接熟化60分钟,然后进行过滤、水洗,40℃下干燥16小时,从而得到一次粒径为2.15μm的含有角蛋白和氧化锌颗粒的粒状复合体。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察所得粒状复合体的尺寸和形态。
(比较例1):无处理XZ-1000F
将六角板状氧化锌(XZ-1000F、堺化学工业株式会社制造)作为比较对象的颗粒。一次粒径为0.66μm。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察颗粒的形态。需要说明的是,从上述的内容可知,该颗粒是成为实施例l、2、3、4和5中得到的含有角蛋白和氧化锌颗粒的粒状复合体的母体的氧化锌颗粒。
(比较例2):无处理XZ-3000F
将六角板状氧化锌(XZ-3000F、堺化学工业株式会社制造)作为比较对象的颗粒。一次粒径为2.08μm。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察颗粒的形态。需要说明的是,该颗粒是成为实施例6中得到的含有角蛋白和氧化锌颗粒的粒状复合体的母体的氧化锌颗粒。
(比较例3):无定形氧化锌颗粒
将无定形氧化锌(氧化锌1种:JIS标准、堺化学工业株式会社制造)作为比较对象的颗粒。一次粒径为0.48μm。用扫描型电子显微镜JSM-6510A(日本电子社制造)观察颗粒的形态。
MIU(平均摩擦系数)的测定
对于MIU(平均摩擦系数),利用KES-SE摩擦感测试器(Kato Tech公司制造)对包含角蛋白和六角板状氧化锌颗粒的粒状复合体进行测定。具体而言,将宽度25mm的双面胶带粘贴在载玻片上,载置该粒状复合体(粉体)并用化妆用海绵延展开,利用KES-SE摩擦感测试器(Kato Tech公司制造)测定MIU(平均摩擦系数)。在摩擦测定载荷25gf、表面测定试样移动速度1mm/秒、测定距离范围20mm的条件下进行测定。作为传感器,使用有机硅触头(施有设想为人的手指的凹凸的有机硅橡胶制摩擦件)。
MMD(摩擦系数的平均偏差)的测定
对于MMD(摩擦系数的平均偏差),利用KES-SE摩擦感测试器(Kato Tech公司制造)对包含角蛋白和六角板状氧化锌颗粒的粒状复合体进行测定。具体而言,将宽度25mm的双面胶带粘贴在载玻片上,载置该粒状复合体(粉体)并用化妆用海绵延展开,利用KES-SE摩擦感测试器(Kato Tech公司制造)测定MMD(摩擦系数的平均偏差)。在摩擦测定载荷25gf、表面测定试样移动速度1mm/秒、测定距离范围20mm的条件下进行测定。作为传感器,使用有机硅触头(施有设想为人的手指的凹凸的有机硅橡胶制摩擦件)。
一次粒径的测定
六角板状氧化锌颗粒和粒状复合体的一次粒径是如下得出的值:在利用扫描型电子显微镜(SEM)(JSM-6510A:日本电子社制造)拍摄到的照片的2000~50000倍的视野中,对100个颗粒测量对角线直径(六角板状氧化锌颗粒或粒状复合体为六角板状的形状时,为六角板状面的3条对角线中的任意1条的对角线的长度)(μm),并由其累积分布的50%而求出的值。
无定形颗粒的一次粒径是如下得出的值:在利用扫描型电子显微镜(SEM)(JSM-6510A:日本电子社制造)对该颗粒进行拍摄而得到的照片的2000~50000倍的视野中,对100个颗粒测量由XY轴平均径(对夹持颗粒的X轴方向和Y轴方向上分别2根平行线的间隔取平均而得到的长度)定义的粒径(μm),并由其累积分布的50%而求出的值。
粒状复合体中的角蛋白含有率的测定
在坩埚中加入粒状复合体及其原料的六角板状氧化锌颗粒分别各2g,在电炉中以500℃加热1小时。分别测定加热后的重量。按照粒状复合体所含的角蛋白全部消失、并且作为原料的六角状氧化锌颗粒的减少率在任一情况下均相同,算出粒状复合体中的角蛋白含有率(质量%)。
光谱反射率的测定
光谱反射率利用分光光度计(日本分光制造V-570型)进行测定。更具体而言,将各实施例和各比较例中得到的粒状复合体或颗粒放入专用比色皿中,安装在分光光度计上,并测定各波长下的光谱反射率。由于反射率=100-吸收率,因此,吸收越多则反射率越低,是优选的。
以上的研究结果示于下述表1~3。另外,所得颗粒的物性的评价结果也示于下述表中。另外,所使用的各角蛋白的数均分子量也示于下述表中。需要说明的是,光谱反射率测定结果示于图1~图2。
[表1]
[表2]
[表3]
对氧化锌颗粒的各种角蛋白处理2
[表4]
使用表4记载的各种角蛋白,对六角板状氧化锌颗粒的表面进行处理。更详细地,按如下进行处理。将粒径为0.66μm的六角板状氧化锌(XZ-1000F、堺化学工业株式会社制造)150g添加至750g水中,充分搅拌,从而得到氧化锌浓度为193g/L的水性浆料。接着,一边搅拌浆料,一边添加表4中记载的各种角蛋白,以使得角蛋白的添加量相对于氧化锌95质量%为5质量%(由各种角蛋白样品的角蛋白含量计算出添加量)。直接熟化60分钟,然后进行过滤、水洗,40℃下干燥16小时,从而得到含有角蛋白和氧化锌颗粒的粒状复合体(各实施例和各参考例:表4)。
需要说明的是,由实施例1~4的记载和关于表4的记载可以理解的是,实施例1与实施例1a、实施例2与实施例2a、实施例3与实施例3a、以及实施例4与参考例1a是分别相同的。
针对所得到的各粒状复合体,按照如下测定涂膜透过率。将有机硅橡胶4.27g(KE-1300T信越化学社制造)、固化剂0.47g(CAT-1300信越化学社制造)混合在一起,向其中投入各粒状复合体的粉体0.25g,利用胡佛式研磨机(Hoover Muller)进行混炼。将其用1miL(25.4μm)涂抹器在TAC薄膜上拉伸,静置并干燥一晩。对于干燥后所得的涂膜,用分光光度计测定透过率。
结果示于图3。需要说明的是,可认为透过率越低则屏蔽效果越好。另外,在图3所示的各粒状复合体中,对透过率尤其低的粒状复合体(即,涂膜透过率明显低于氧化锌颗粒XZ-1000F本身的粒状复合体)进行选拔,并示于图4。
由表4、图3和图4可知,在作为对六角板状氧化锌颗粒进行处理的角蛋白,使用数均分子量为500~2000左右的源自羊毛的阳离子化水解角蛋白、源自羊毛的甲硅烷基化水解角蛋白或源自羽毛的水解角蛋白的情况下,当所得粒状复合体与有机硅混合而制成有机硅组合物时,起到了特别优异的近红外线屏蔽效果。
各粒状复合体的特性的研究
针对实施例1a~4a的粒状复合体,用扫描型电子显微镜JSM-6510A(日本电子社制造)观察尺寸和形态。另外,与上述同样地测定MIU、MMD、一次粒径和粒状复合体中的角蛋白含有率。各测定结果示于表5。
[表5]
对氧化锌颗粒的各种角蛋白处理3
除了使用实施例2a的粒状复合体制备中所用的角蛋白作为角蛋白,并使用粒径为1.52μm的六角板状氧化锌(XZ-2000F、堺化学工业株式会社制造)作为六角板状氧化锌颗粒以外,与上述同样地制备了粒状复合体(实施例A)。对于所得到的粒状复合体,与上述同样地测定了涂膜透过率。将结果示于图5。另外,进而与上述同样地测定了所得到的粒状复合物的MIU、MMD、一次粒径和粒状复合体中的角蛋白含有率。将各测定结果示于表6。
[表6]
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Claims (9)
1.一种粒状复合体,其包含角蛋白和六角板状氧化锌颗粒,并且在六角板状氧化锌颗粒表面具备角蛋白,
所述角蛋白含量为0.8~5质量%,
角蛋白为选自由源自羊毛的阳离子化水解角蛋白、源自羊毛的甲硅烷基化水解角蛋白和源自羽毛的水解角蛋白组成的组中的至少1种,且数均分子量为500~2000。
2.根据权利要求1所述的粒状复合体,其一次粒径为0.1~5μm。
3.根据权利要求1所述的粒状复合体,其中,
角蛋白为选自由源自羊毛的阳离子化水解角蛋白、源自羊毛的甲硅烷基化水解角蛋白和源自羽毛的水解角蛋白组成的组中的至少1种,且数均分子量为500~2000,
角蛋白含量为0.8~4质量%,
所述粒状复合体的一次粒径为0.2~4μm。
4.一种外用组合物,其包含权利要求1~3中任一项所述的粒状复合体。
5.根据权利要求4所述的外用组合物,其为化妆品组合物、准药品组合物或医药品组合物。
6.一种组合物,其含有权利要求1~3中任一项所述的粒状复合体和有机硅。
7.根据权利要求6所述的组合物,其为有机硅薄膜。
8.权利要求1~3中任一项所述的粒状复合体在制造化妆品组合物、准药品组合物或医药品组合物中的用途。
9.权利要求1~3中任一项所述的粒状复合体作为近红外线反射物质或近红外线遮光物质的用途。
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- 2018-11-26 WO PCT/JP2018/043349 patent/WO2019107304A1/ja unknown
- 2018-11-26 KR KR1020207014703A patent/KR102570736B1/ko active IP Right Grant
- 2018-11-26 EP EP18884056.5A patent/EP3718971A4/en active Pending
- 2018-11-26 US US16/766,585 patent/US11179303B2/en active Active
- 2018-11-26 CN CN201880077647.0A patent/CN111527048B/zh active Active
- 2018-11-29 TW TW107142718A patent/TWI804533B/zh active
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TWI804533B (zh) | 2023-06-11 |
WO2019107304A1 (ja) | 2019-06-06 |
KR102570736B1 (ko) | 2023-08-25 |
US11179303B2 (en) | 2021-11-23 |
CN111527048A (zh) | 2020-08-11 |
KR20200093545A (ko) | 2020-08-05 |
US20200368124A1 (en) | 2020-11-26 |
EP3718971A4 (en) | 2021-09-15 |
TW201927279A (zh) | 2019-07-16 |
EP3718971A1 (en) | 2020-10-07 |
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