CN105960379A - 六方板状氧化锌颗粒、其制造方法、化妆料、填料、树脂组合物、红外线反射材料和涂料组合物 - Google Patents
六方板状氧化锌颗粒、其制造方法、化妆料、填料、树脂组合物、红外线反射材料和涂料组合物 Download PDFInfo
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- CN105960379A CN105960379A CN201480074888.1A CN201480074888A CN105960379A CN 105960379 A CN105960379 A CN 105960379A CN 201480074888 A CN201480074888 A CN 201480074888A CN 105960379 A CN105960379 A CN 105960379A
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- Prior art keywords
- zinc oxide
- oxide particles
- tabular
- acid
- slurry
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- 239000011787 zinc oxide Substances 0.000 title claims abstract description 169
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Abstract
本发明的课题在于提供一种可以适合用于化妆料、填料、树脂组合物、红外线反射材料和涂料组合物的六方板状氧化锌颗粒及其制造方法。一种六方板状氧化锌颗粒,其特征在于,一次粒径为1.1μm以上,粒度分布中的D90/D10为3.0以下。
Description
技术领域
本发明涉及六方板状氧化锌颗粒、其制造方法、化妆料、填料、树脂组合物、红外线反射材料和涂料组合物。
背景技术
粉底及其它美容化妆料强调使用感,近年来也要求具有紫外线屏蔽性。为了提高紫外线屏蔽性,需要混配紫外线屏蔽用的材料,但迄今为止广泛用于防晒霜用途的微粒氧化锌及微粒二氧化钛的滑动性差,具有阻碍使用感的问题。因此,需要使用感高的紫外线屏蔽材料。
另外,氧化锌颗粒还被用作混配于树脂组合物、涂料中的无机填料。这种使用包括利用了氧化锌颗粒的高导热性的散热性填料;及以紫外线屏蔽、红外线反射为目的的填料等用途。
此外,近年来,作为具有红外线反射性的无机颗粒的氧化锌颗粒也受到关注。通过吸收红外线,各种物品的温度上升,因而,利用混配了可反射/屏蔽红外线的无机颜料的涂料来制造隔热涂料,可抑制各种物品及建筑物的温度上升,实现节能。
氧化锌颗粒具有红外线反射性能,但由于颗粒形状、颗粒大小等的不同,吸收波长的图案发生变化。因此,若想提高红外线区域的吸收波长,则至可见光区域为止会产生吸收区域,由此会产生着色。在隔热涂料的用途中,若隔热用的颜料着色则会对所得到的涂料的色调产生影响,从这点来看是不优选的。
专利文献1中记载了一种对颗粒形状进行了控制的六方板状氧化锌颗粒。在使用0.5μm以上的六方板状氧化锌颗粒的情况下,滑动良好,使用感优异,可以适合用作粉底用途中的颗粒。但是,在专利文献1中记载的平均粒径为0.5μm~1μm的六方板状氧化锌颗粒的情况下,虽然不存在现有的超微粒氧化锌那样的滑动性的恶化,但是作为混配于目前的美容化妆料中的原料的使用感不足,进而需要粒径大且粒度均匀的六方板状氧化锌颗粒。
专利文献2中记载了一种具有多层结构的10μm的六方板状氧化锌颗粒。但是,这种氧化锌颗粒在混配于化妆料中时,滑动性等方面不具有足够良好的性能。
专利文献3中记载了平均粒径为3μm~20μm的氧化锌颗粒及其红外线反射性能和滑动性。但是并未记载颗粒形状,所得到的颗粒为不定形的氧化锌颗粒。对于这种氧化锌颗粒来说,红外线反射性能及混配于化妆料中时的滑动性等方面并不具有足够良好的性能。
现有技术文献
专利文献
专利文献1:国际公开2012/147886
专利文献2:日本特开2013-245139号
专利文献3:国际公开2012/036082
发明内容
发明要解决的课题
本发明的目的在于提供一种可以适合用于美容化妆料等化妆料的六方板状氧化锌颗粒及其制造方法。另外,进一步地,本发明的目的还在于提供一种能够用作无着色的红外线反射剂的六方板状氧化锌颗粒。
用于解决课题的方案
本发明涉及一种六方板状氧化锌颗粒,其特征在于,一次颗粒的平均粒径(一次粒径)为1.1μm以上,粒度分布中的D90/D10为3.0以下。
上述六方板状氧化锌颗粒优选粉体的MIU(平均摩擦系数)为0.87以下,MMD(摩擦系数的平均偏差)为0.035以下。
本发明还涉及上述六方板状氧化锌颗粒的制造方法,其特征在于,包括下述工序:
制备pH为10以上的原料氧化锌的水浆料的工序(1);
将通过上述工序(1)制备的浆料与锌盐水溶液在35℃以下混合的工序(2);和
将所混合的浆料加热熟化的工序(3)。
本发明还涉及一种化妆料,其特征在于,其含有上述的六方板状氧化锌颗粒。
本发明还涉及一种填料,其特征在于,其由上述的六方板状氧化锌颗粒构成。
本发明还涉及一种树脂组合物,其特征在于,其含有上述的六方板状氧化锌颗粒。
本发明还涉及一种红外线反射材料,其特征在于,其由上述的六方板状氧化锌颗粒构成。
本发明还涉及一种涂料组合物,其特征在于,其含有上述的六方板状氧化锌颗粒。
发明的效果
本发明的六方板状氧化锌颗粒在混配于化妆料中时,可成为能够适合用于美容化妆料的紫外线屏蔽材料。另外,在作为填料使用的情况下,还可发挥出优异的散热性能及红外线反射能力。
附图说明
图1是示出实施例1的氧化锌颗粒的扫描型电子显微镜照片的图。
图2是示出实施例1的氧化锌颗粒的X射线衍射的光谱的图。
图3是示出实施例2的氧化锌颗粒的扫描型电子显微镜照片的图。
图4是示出实施例3的氧化锌颗粒的扫描型电子显微镜照片的图。
图5是示出实施例4的氧化锌颗粒的扫描型电子显微镜照片的图。
图6是示出实施例5的氧化锌颗粒的扫描型电子显微镜照片的图。
图7是示出比较例1的氧化锌颗粒的扫描型电子显微镜照片的图。
图8是示出比较例2的氧化锌颗粒的扫描型电子显微镜照片的图。
图9是示出比较例3的氧化锌颗粒的扫描型电子显微镜照片的图。
图10是示出比较例4的氧化锌颗粒的扫描型电子显微镜照片的图。
图11是示出比较例5的氧化锌颗粒的扫描型电子显微镜照片的图。
图12是示出比较例6的氧化锌颗粒的扫描型电子显微镜照片的图。
图13是示出比较例7的氧化锌颗粒的扫描型电子显微镜照片的图。
具体实施方式
本发明的六方板状氧化锌颗粒为下述六方板状氧化锌颗粒,其具有六方板状形状,一次粒径为1.1μm以上,具有较窄的粒度分布,从而可以适合用作美容化妆料等化妆料的混配成分或填料。
该六方板状氧化锌颗粒由于颗粒形状均匀,因而能够以高浓度混配于基质成分中,所以还可以适合用作填料。在作为填料使用的情况下,除了可以用作利用了氧化锌颗粒的高导热性的散热性填料以外,还可以用作红外线反射性的填料。本发明的六方板状氧化锌颗粒具有比以往的氧化锌颗粒优异的红外线反射能力,并且透明性也优异,因而还可以适合用作混配于隔热涂料等中的红外线反射性填料。
本发明的六方板状氧化锌颗粒的D90/D10为3.0以下。该值越大则意味着粒度分布越宽,该值越小则意味着粒度分布越窄。
需要说明的是,D10、D90分别是通过测定粒径的分布而得到的值。D10是指以体积基准计的10%累积粒径,D90是指以体积基准计的90%累积粒径。上述D90/D10更优选为2.8以下。D90/D10为3.0以下的六方板状氧化锌颗粒在混配于化妆料中并涂布至肌肤时,颗粒大小相同,阻碍触感的微小颗粒及粗大颗粒少,因而可实现优异的粉体触感。需要说明的是,本发明的D90、D10是利用以下的实施例中记载的方法所测定的值。
本发明的六方板状氧化锌颗粒的一次粒径为1.1μm以上。该一次粒径更优选为1.3μm以上、进一步优选为2.0μm以上。另外,一次粒径的上限没有特别限定,优选为50μm以下、进一步优选为30μm以下。通过形成一次粒径为1.1μm以上的颗粒,可以使用作化妆料时的粉体触感良好。需要说明的是,本发明的一次粒径是利用以下的实施例中记载的方法所测定的值。
本发明的六方板状氧化锌颗粒的MIU(平均摩擦系数)优选为0.87以下。MIU(平均摩擦系数)的值越小则意味着滑动性越好,越容易滑动。在混配于化妆料中时,MIU(平均摩擦系数)超过0.87的六方板状氧化锌颗粒的滑动性有时会变差。此外,MMD(摩擦系数的平均偏差)优选为0.035以下。MMD(摩擦系数的平均偏差)的值越小则意味着粗糙感越少、光滑性越高。MMD(摩擦系数的平均偏差)超过0.035的六方板状氧化锌颗粒的粗糙感增大,从这点出发,混配于化妆料中时使用感有时会变差。上述MIU(平均摩擦系数)更优选为0.85以下,MMD(摩擦系数的平均偏差)更优选为0.03以下。需要说明的是,本说明书中的MIU(平均摩擦系数)、MMD(摩擦系数的平均偏差)是通过实施例中详细说明的方法所测定的。
此外,本发明的六方板状氧化锌颗粒的纵横比优选为2.5以上。即,优选为具有可形成这种纵横比的六方板状形状的六方板状氧化锌颗粒。通过为这种形状,特别是在用于化妆料中的情况下,滑动良好,可以得到优异的使用感。上述纵横比更优选为2.7以上、进一步优选为3.0以上。需要说明的是,本说明书中的纵横比是利用以下的实施例中记载的方法所测定的值。
本发明中的Dmin/Dmax优选为0.3以上。Dmax意味着六方板状氧化锌颗粒的六边形状面的3条对角线中的最长对角线的长度,Dmin意味着六方板状氧化锌颗粒的六边形状面的3条对角线中的最短对角线的长度。在将Dmax作为正六边形的对角线的长度时,Dmin/Dmax意味着相对该正六边形的对角线的长度的偏差,该值越接近于1则相对正六边形的偏差越小,越接近0则偏差越大。Dmin/Dmax更优选为0.5以上、进一步优选为0.7以上。需要说明的是,本发明中的Dmin/Dmax是利用以下的实施例中记载的方法所测定的值。
另外,本发明的六方板状氧化锌颗粒的BET比表面积优选为1.9m2/g以下。通过为该范围,粒径大、微粒少,因而从形成良好的粉体触感的方面出发是优选的。需要说明的是,本发明中的BET比表面积是利用以下的实施例中记载的方法所测定的值。
本发明的六方板状氧化锌颗粒优选在1000nm所测定的分光反射率为10%以上、且在2000nm所测定的分光反射率为8%以上。特别是在上述隔热涂料中使用的情况下,优选具有高红外线反射能力。需要说明的是,该分光反射率是利用以下的实施例中记载的方法所测定的值。
本发明的六方板状氧化锌颗粒优选在400nm所测定的平行光线透过率为30%以上。上述平行光线透过率若小于30%,则氧化锌颗粒会着色,因此在化妆料或涂料中色调有可能发生变化,从这点出发是不优选的。此处,使用400nm的平行光线透过率作为指标是因为,在可见光区域中400nm的可见光透过率是最能够反映实际外观的透明性的波长。需要说明的是,该平行光线透过率是利用以下的实施例中记载的方法所测定的值。
本发明的六方板状氧化锌颗粒在红外线反射能力方面优异,另一方面还具有可见光区域的屏蔽小的特征。由此,涂膜的透明性优异,因而在如化妆料或隔热涂料等那样重视色调的用途中使用的情况下,不会对色调产生影响,从这点出发是优选的。
具有上述形状的六方板状氧化锌颗粒的制造方法没有特别限定,例如可以通过具有下述工序的制造方法来获得:
制备pH为10以上的原料氧化锌的水浆料的工序(1);
将通过上述工序(1)制备的浆料与锌盐水溶液在35℃以下混合的工序(2);和
将所混合的浆料加热熟化的工序(3)。
下面,对该制造方法进行详细说明。
上述工序(1)是将原料氧化锌制备成pH为10以上的水浆料的工序。由此,原料氧化锌在水中的分散性提高,原料氧化锌与锌盐水溶液的反应性提高,从而能够控制粒径、粒度分布。
上述原料氧化锌的水浆料中使用的原料氧化锌没有特别限定,优选使用粒径为0.005μm以上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法所求出的比表面积相同的表面积的球的直径。即,粒径是由通过全自动BET比表面积测定装置Macsorb HM-1200型(Mountech社制造)测定求出的比表面积:Sg、和氧化锌的真比重:ρ,并通过下述计算式求出的值。
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,对于颗粒的真比重:ρ而言,是以5.6作为氧化锌的真比重来用于上述计算中的。
作为上述原料氧化锌没有特别限定,可以使用通过公知方法制造的氧化锌。作为市售的氧化锌,可以举出堺化学工业社制造的FINEX-75、FINEX-50、FINEX-30、SF-15、微细氧化锌等。
上述原料氧化锌浆料优选原料氧化锌的浓度相对于浆料总量为10g/l~500g/l。
上述浆料的制备方法没有特别限定,例如可以举出下述方法:将原料氧化锌添加至水中后,加入碱性水溶液而调整为pH10以上的方法;将原料氧化锌添加至碱性水溶液中并调整为pH10以上的方法。另外,例如在调整pH后,在35℃以下分散10分钟以上,从而可以制成均匀的浆料。
作为上述原料氧化锌浆料的pH调整中使用的碱性水溶液,没有特别限定,例如可以使用氢氧化钠水溶液、氢氧化钾水溶液、氨水等。
上述原料氧化锌浆料也可以在不损害本发明的效果的范围内少量添加原料氧化锌、水、碱性水溶液以外的成分。例如还可以添加分散剂等。
本发明的制造方法中,进行将上述工序(工序(1))中制备的原料氧化锌的浆料与锌盐水溶液在35℃以下混合的工序(工序(2))。通过在35℃以下混合,可以控制原料氧化锌与锌盐水溶液的反应,可以促进颗粒生长,从这点出发是优选的。上述反应温度更优选为30℃以下、进一步优选为20℃以下。
上述锌盐水溶液没有特别限定,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的水溶液。在锌盐水溶液中,特别是使用乙酸锌水溶液的情况下可以恰当地得到本发明的特定的六方板状氧化锌颗粒。
另外,这些锌盐水溶液也可以通过将氧化锌、酸和水进行混合来对氧化锌进行酸水解从而来制备。对于利用氧化锌、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,但是从尽量减少杂质的方面考虑,氧化锌的Zn纯度优选为95%以上。另外,作为酸,可以举出乙酸、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,特别是使用乙酸的情况下可以恰当地得到本发明的特定的六方板状氧化锌颗粒。在这些锌盐水溶液中,可以合用2种来进行使用。
锌盐水溶液中的锌盐浓度优选超过0.1mol/l且为4.0mol/l以下,特别优选乙酸锌水溶液中的锌盐浓度超过0.2mol/l且为2.0mol/l以下。
上述锌盐水溶液也可以在不损害本发明的效果的范围内少量添加锌盐、水以外的成分。例如,也可以添加分散剂等。
关于上述2液的混合,可以举出下述方法:在对温度进行管理的水中同时添加原料氧化锌的水浆料和锌盐水溶液的方法;在维持温度的同时,向锌盐水溶液中添加原料氧化锌的水浆料的方法;在维持温度的同时,向原料氧化锌的水浆料中添加锌盐水溶液的方法;等等。
本发明的制造方法中,进行将通过上述工序(工序(1)和(2))得到的混合浆料加热熟化的工序(3)。
通过该加热熟化,可以得到具有目标形状和粒径的六方板状氧化锌颗粒。
熟化优选在45℃~110℃进行。熟化时间可以举出0.5小时~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,优选根据作为目标的六方板状氧化锌颗粒来适当设定。
对于如此得到的六方板状氧化锌颗粒,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方板状氧化锌颗粒,还可以根据需要进行利用筛的分级。作为利用筛的分级方法,可以举出湿式分级、干式分级。另外,还可以进行湿式粉碎、干式粉碎等处理。
如上所述,本发明的六方板状氧化锌颗粒的制造方法可以不进行烧制处理而得到六方板状氧化锌颗粒,但即使对通过上述方法得到的六方板状氧化锌颗粒实施烧制处理也无妨。进行烧制时,可以举出利用了公知的任意装置的方法,对于处理条件等也没有特别限定。
本发明的六方板状氧化锌颗粒也可以进一步实施表面处理。作为上述表面处理没有特别限定,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种化合物形成皮膜的表面处理;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。
关于上述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种化合物形成皮膜,可以利用通过水解或加热分解等使Si源化合物和/或Al源化合物析出至粉体表面等方法来进行。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、铝酸钠等容易转换为SiO2、Al(OH)3、Al2O3的化合物等。
作为上述水解没有特别限定,可以举出使用硫酸、盐酸、乙酸、硝酸等酸的方法。使用了该水分散体的二氧化硅的处理方法中的中和方法可以为下述任一方法:向含有六方板状氧化锌颗粒的分散体中加入酸,之后添加Si源化合物和/或Al源化合物的方法;向分散体中加入Si源化合物和/或Al源化合物,之后添加酸的方法;向分散体中同时添加Si源化合物和/或Al源化合物以及酸的方法。
作为上述利用疏水性有机化合物的处理没有特别限定,例如可以举出硅油、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,从化学稳定性的方面出发优选硅油。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、Wacker Asahikasei Silicone Co.,Ltd.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、Wacker Asahikasei Silicone Co.,Ltd.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-氨基丙基三甲氧基硅烷、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、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的情况下,表面处理优选相对于处理后的粉体总量以1重量%~10重量%的比例进行。通过为该范围内,滑动性提高且耐湿性提高,在树脂中的分散性提高,从这点出发是优选的。
本发明的六方板状氧化锌颗粒也可以与其它成分混合,混配于化妆料、油墨、涂料、塑料等中。特别是,由于具有上述特性,因而可以得到滑动性好、粗糙也少的具有优异的粉体触感的化妆料,从这点出发是优选的。
作为上述化妆料没有特别限定,通过根据需要在这样的粉体中混合化妆品原料,可以得到防晒霜等紫外线防御用化妆料;粉底等底妆化妆料;口红等彩妆化妆料等。另外,本发明的六方板状氧化锌颗粒除了上述优异的粉体触感以外,还具有紫外线屏蔽能力,因而在用于化妆品的情况下具有优异的性能。
上述化妆料可以形成为油性化妆料、水性化妆料、O/W型化妆料、W/O型化妆料的任意形态。
上述化妆料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调节剂、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,还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(モノステアリン酸グリセリンリンゴ酸)等甘油聚甘油脂肪酸(グリセリンポリグリセリン脂肪酸)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单二油酸酯(POEモノジオレエート)、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;聚丙二醇与环氧乙烷的加聚物(ブルロニック)等普流尼克(プルアロニック)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;テトロニック等四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。
作为其它表面活性剂,可以以在稳定性和皮肤刺激性方面没有问题的范围混配例如脂肪酸皂、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、多元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。
作为上述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、栝楼酸(カロニン酸)、去端肽胶原、胆甾醇基-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、双甘油(EO)PO加成物、缫丝花(イサイヨバラ)提取物、西洋蓍草(セイヨウノキギリソウ)提取物、草木犀(メリロート)提取物等。
作为上述高级醇没有特别限定,例如可以举出月桂醇、十六烷基醇、硬脂醇、山嵛醇、肉豆蔻醇、油烯醇、鲸蜡硬脂醇等直链醇;单硬脂基甘油醚(鲨肝醇)、2-癸基十四醇、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-1,1-二磷酸、1-羟基乙烷-1,1-二磷酸酸四钠盐、柠檬酸钠、多磷酸钠、偏磷酸钠、葡萄糖酸、磷酸、柠檬酸、抗坏血酸、琥珀酸、EDTA酸等。
作为上述天然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、卡罗布胶、刺梧桐树胶、卡拉胶、果胶、琼脂、榅桲籽(marmelo,榅桲)、褐藻胶(褐藻提取物)、淀粉(稻米、玉米、马铃薯、小麦)、甘草酸等植物系高分子;黄原胶、葡聚糖、琥珀酸葡聚糖、支链淀粉等微生物系高分子;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、硝酸纤维素、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;藻酸钠、藻酸丙二醇酯等藻酸系高分子;等等。
作为合成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。
作为无机水溶性高分子没有特别限定,例如可以举出膨润土、硅酸铝镁(VEEGUM)、合成锂皂石、锂蒙脱石、硅酸酐等。
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乙基酯、N,N-二乙氧基PABA乙基酯、N,N-二甲基PABA乙基酯、N,N-二甲基PABA丁基酯等苯甲酸系紫外线屏蔽剂;高薄荷基-N-乙酰基邻氨基苯甲酸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、对异丙醇苯基水杨酸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-羧酸酯、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、二苄肼(ジベンザラジン)、二茴香酰基甲烷(ジアニソイルメタン)、4-甲氧基-4’-叔丁基二苯甲酰基甲烷、波尼酮(5-(3,3-Dimethyl-2-norbornylidene)-3-penten-2-one)等。
作为其它药剂成分没有特别限定,例如可以举出维生素A油、视黄醇、棕榈酸视黄醇酯、肌醇、盐酸吡哆醇、烟酸苄酯、烟酰胺、DL-α-生育酚烟酸酯、抗坏血酸(アルコルビン酸)磷酸镁、2-O-α-D-吡喃葡萄糖基-L-抗坏血酸、维生素D2(麦角钙化醇)、dL-α-生育酚、dL-α-生育酚乙酸酯、泛酸、生物素等维生素类;雌二醇、乙炔雌二醇等激素;精氨酸、天冬氨酸、胱氨酸、半胱氨酸、甲硫氨酸、丝氨酸、亮氨酸、色氨酸等氨基酸;尿囊素、甘菊环等抗炎剂;熊果素等美白剂;丹宁酸等收敛剂;L-薄荷醇、樟脑等清凉剂;硫、氯化溶菌酶、氯化吡哆醇;等等。
作为各种提取液没有特别限定,例如可以举出鱼腥草(ドクダミ)提取物、黄檗树皮(オウバク)提取物、草木犀提取物、白荨麻(オドリコソウ)提取物、甘草(カンゾウ)提取物、芍药(シャクヤク)提取物、肥皂草(サボンソウ)提取物、丝瓜(ヘチマ)提取物、奎宁(キナ)提取物、虎耳草(ユキノシタ)提取物、苦参(クララ)提取物、日本萍蓬草(コウホネ)提取物、茴香(ウイキョウ)提取物、樱草(サクラソウ)提取物、蔷薇(バラ)提取物、地黄(ジオウ)提取物、柠檬提取物、紫草根(シコン)提取物、芦荟提取物、菖蒲(ショウブ)根提取物、尤加利提取物、问荆(スギナ)提取物、鼠尾草(セージ)提取物、百里香(タイム)提取物、茶提取物、海藻提取物、黄瓜提取物、丁香花(チョウジ)提取物、覆盆子(キイチゴ)提取物、蜂蜜花(メリッサ)提取物、人参提取物、娑罗果(マロニエ)提取物、桃树提取物、桃叶提取物、桑树提取物、矢车菊(ヤグリマギク)提取物、金缕梅(ハマメリス)提取物、胎盘提取物、胸腺提取物、蚕丝提取液、甘草提取物等。
作为上述各种粉体,可以举出氧化铁红、氧化铁黄、黑氧化铁、云母钛、氧化铁被覆云母钛、二氧化钛被覆玻璃鳞片等光亮性着色颜料;云母、滑石、高岭土、绢云母、二氧化钛、二氧化硅等无机粉末;聚乙烯末、尼龙末、交联聚苯乙烯、纤维素粉末、硅酮末等有机粉末;等等。为了提高官能特性、及提高化妆持续性,优选通过公知的方法并利用硅酮类、氟化物、金属皂、油剂、酰基谷氨酸盐等物质对粉末成分的一部分或全部进行疏水化处理由此来进行使用。另外,也可以混合不属于本发明的其它复合粉体来使用。
将本发明的六方板状氧化锌颗粒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。
将本发明的六方板状氧化锌颗粒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。另外,涂料中的树脂可以具有固化性,也可以不具有固化性。
本发明还涉及含有上述六方板状氧化锌颗粒的树脂组合物。对于这种树脂组合物来说,通过六方板状氧化锌颗粒作为散热性填料发挥作用,从而具有优异的散热性。此外,在红外线反射能力方面优异,因而还可以作为具有这些性能的树脂组合物使用。
如上所述,本发明的六方板状氧化锌颗粒具有红外线反射性能,因而还能够作为各种领域中的红外线屏蔽材料使用。
实施例
下面,基于实施例来更详细地说明本发明。需要说明的是,本发明不限定于以下的实施例。
(实施例1)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆而得到浆料,在该浆料中添加30%氢氧化钠水溶液8ml,调整为pH=13。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为15℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用160分钟的时间升温至95℃,在搅拌下于95℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为3.13μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图1。另外,用X射线衍射装置UltimaIII(Rigaku社制造)对所得到的颗粒进行分析,将所得到的X射线衍射的光谱示于图2。另外,将所得到的颗粒的物性的评价结果示于表1。
(实施例2)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆而得到浆料,在该浆料中添加30%氢氧化钠水溶液8ml,调整为pH=13。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为30℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用130分钟的时间升温至95℃,在搅拌下于95℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为1.89μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图3。另外,将所得到的颗粒的物性的评价结果示于表1。
(实施例3)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆而得到浆料,在该浆料中添加30%氢氧化钠水溶液70ml,调整为pH=14。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为30℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用130分钟的时间升温至95℃,在搅拌下于95℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为1.48μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图4。另外,将所得到的颗粒的物性的评价结果示于表1。
(实施例4)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆而得到浆料,在该浆料中添加30%氢氧化钠水溶液0.1ml,调整为pH=10。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为15℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用160分钟的时间升温至95℃,在搅拌下于95℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为1.32μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图5。另外,将所得到的颗粒的物性的评价结果示于表1。
(实施例5)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆而得到浆料,在该浆料中添加30%氢氧化钠水溶液8ml,调整为pH=13。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为15℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用160分钟的时间升温至95℃,在搅拌下于95℃熟化5小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为2.94μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图6。另外,将所得到的颗粒的物性的评价结果示于表1。
(比较例1)
在以乙酸锌计的浓度为1mol/l的乙酸锌水溶液1200ml中添加原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)80g而制成浆料,在25℃混合0.5小时。接着,在搅拌下将该浆料用60分钟的时间升温至100℃,在搅拌下于100℃熟化7小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为1.00μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图7。另外,将所得到的颗粒的物性的评价结果示于表2。
(比较例2)
在以乙酸锌计的浓度为1mol/l的乙酸锌水溶液1200ml中添加原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)80g而制成浆料,在25℃混合0.5小时。接着,在搅拌下将该浆料用60分钟的时间升温至100℃,在搅拌下于100℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为0.31μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图8。另外,将所得到的颗粒的物性的评价结果示于表2。
(比较例3)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆而得到浆料,在该浆料中添加30%氢氧化钠水溶液8ml,调整为pH=13。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为40℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用110分钟的时间升温至95℃,在搅拌下于95℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为0.97μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图9。另外,将所得到的颗粒的物性的评价结果示于表2。
(比较例4)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆,制成pH=8的浆料。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为30℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用130分钟的时间升温至95℃,在搅拌下于95℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为1.12μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图10。另外,将所得到的颗粒的物性的评价结果示于表2。
(比较例5)
将原料氧化锌(堺化学工业社制造FINEX-50粒径0.02μm)40g在430.49ml的水中再制浆而得到浆料,在该浆料中添加90%乙酸水溶液10ml,调整为pH=6。一边混合,一边将上述的浆料和以乙酸锌计的浓度为1.61mol/l的乙酸锌水溶液563.24ml用120分钟的时间全部添加到控制为30℃的水200ml中,制成以乙酸锌计的浓度为0.75mol/l的乙酸锌水溶液与原料氧化锌的混合浆料。接着,在搅拌下将该混合浆料用130分钟的时间升温至95℃,在搅拌下于95℃熟化1小时。熟化后马上进行骤冷,之后进行过滤、清洗,在110℃干燥12小时,由此得到一次粒径为0.96μm的六方板状氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图11。另外,将所得到的颗粒的物性的评价结果示于表2。
(比较例6)
将原料氧化锌(堺化学工业社制造氧化锌1种粒径0.6μm)放入方形匣钵中,在电炉中于750℃进行烧制,由此得到一次粒径为2.21μm的氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图12。另外,将所得到的颗粒的物性的评价结果示于表2。
(比较例7)
将原料氧化锌(堺化学工业社制造氧化锌1种粒径0.6μm)放入方形匣钵中,在电炉中于800℃进行烧制,由此得到一次粒径为2.93μm的氧化锌颗粒。利用扫描型电子显微镜JSM-6510A(日本电子社制造)对所得到的颗粒的尺寸/形态进行观察,所得到的电子显微镜照片示于图13。另外,将所得到的颗粒的物性的评价结果示于表2。
(评价方法)
(所得到的颗粒的组成)
关于图2中所示的X射线衍射的光谱和表1、表2中的所得到的颗粒的组成,示出了利用具有铜管球的X射线衍射装置UltimaIII(Rigaku社制造)进行分析的结果。根据这些结果可知,实施例和比较例的样品得到了氧化锌。
(一次粒径)
本说明书中的一次粒径是以扫描型电子显微镜JSM-6510A(日本电子社制造)拍摄的照片的2000倍~50000倍的视野中的对角线径(六方板状氧化锌颗粒的六方板状面的3条对角线中任意一条对角线的长度)所定义的粒径(μm),在SEM照片内计测100个颗粒的对角线径,求出其累积分布的平均值。
(纵横比)
本说明书中的六方板状氧化锌颗粒的纵横比是如下求出的值:在利用扫描型电子显微镜JSM-6510A(日本电子社制造)拍摄的照片的2000~50000倍的视野中,对于六方板状氧化锌颗粒的六方板状面朝向正面的颗粒,计测100个颗粒的由其对角线径(六方板状氧化锌颗粒的六方板状面的3条对角线中任意一条对角线的长度)所定义的粒径(μm),将其平均值设为L,对于六方板状氧化锌颗粒的侧面朝向正面的颗粒(视为长方形的颗粒),计测100个颗粒的厚度(μm)(长方形的短边的长度),将其平均值设为T时,这些值之比L/T即为纵横比。
(Dmin/Dmax)
关于本说明书中的Dmin/Dmax,在利用扫描型电子显微镜JSM-6510A(日本电子社制造)拍摄的照片的2000倍~50000倍的视野中,计测六方板状氧化锌颗粒的六方板状面的3条对角线,将其中最长对角线的长度设为Dmax,将最短对角线的长度设为Dmin,以这些值之比Dmin/Dmax求出,计测100个颗粒的Dmin/Dmax,平均值即为上述Dmin/Dmax。
(D10、D90和D90/D10)
本说明书中,D10、D90是利用激光衍射/散射式粒度分布测定装MicrotrackMT-3300EXII(日机装社制造)所测定的值。使用将实施例、比较例的氧化锌颗粒0.1g分散到以六偏磷酸钠计的浓度为0.025重量%的六偏磷酸钠水溶液50ml中而成的浆料,进行测定。测定前,用超声均质器US-600T(日本精机制作所制造)将浆料超声分散2分钟,将测定时的循环速度设为50%、超声输出设为40W、超声分散时间设为2分钟,由此进行测定。将实施例和比较例的氧化锌的折射率设为1.95,将0.025重量%的六偏磷酸钠水溶液的折射率设为1.333,由此进行测定。
(MIU(平均摩擦系数))
表1和表2的MIU(平均摩擦系数)是利用KES-SE摩擦感测试器(Kato Tech社制造)对上述实施例、比较例中得到的氧化锌颗粒进行测定而得到的值。在载玻片粘贴宽25mm的双面胶带,放置粉体,用化妆用粉扑展开,利用KES-SE摩擦感测试器(KatoTech社制造)测定MIU(平均摩擦系数)。在摩擦测定负荷25gf、表面测定试样移动速度1mm/sec、测定距离范围20mm的条件下进行测定。作为传感器,使用硅酮触头(带有假设为人类手指的凹凸的硅酮橡胶制的摩擦件)。
(MMD(摩擦系数的平均偏差))
表1和表2的MMD(摩擦系数的平均偏差)是利用KES-SE摩擦感测试器(KatoTech社制造)对上述实施例、比较例中得到的氧化锌颗粒进行测定而得到的值。在载玻片粘贴宽25mm的双面胶带,放置粉体,用化妆用粉扑展开,利用KES-SE摩擦感测试器(Kato Tech社制造)测定MMD(摩擦系数的平均偏差)。在摩擦测定负荷25gf、表面测定试样移动速度1mm/sec、测定距离范围20mm的条件下进行测定。作为传感器,使用硅酮触头(带有假设为人类手指的凹凸的硅酮橡胶制的摩擦件)。
(BET比表面积)
表1和表2的BET比表面积(m2/g)是通过全自动BET比表面积测定装置MacsorbModel HM-1200(Mountech社制造)所测定的值。
(1000nm分光反射率和2000nm分光反射率)
表1和表2的1000nm分光反射率、2000nm分光反射率是通过分光光度计(日本分光制造V-570型)所测定的值。将实施例和比较例中得到的氧化锌颗粒10g、醇酸树脂20.4g、丁基化三聚氰胺树脂8.7g、二甲苯5.4g、玻璃珠30g放入75ml蛋黄酱瓶中,用涂料调节器振荡60分钟,得到分散液。用棒涂机#20将所得到的分散液涂布至对比率试纸,在50℃干燥10分钟后,在110℃干燥20分钟,得到试验片。对于所得到的试验片,利用分光光度计(日本分光制造V-570型)测定波长1000nm和2000nm下的分光反射率。
(310nm全光线透过率、350nm全光线透过率和400nm平行光线透过率)
表1和表2的310nm全光线透过率、350nm全光反射率、400nm平行光线透过率是通过分光光度计(日本分光制造V-570型)所测定的值。将实施例和比较例中得到的氧化锌颗粒2g、丙烯酸多元醇树脂10g、二甲苯5g、乙酸丁酯5g、玻璃珠38g放入75ml蛋黄酱瓶中,用涂料调节器振荡90分钟,得到分散液。用棒涂机#6将所得到的分散液涂布至载玻片,利用利用分光光度计(日本分光制造V-570型)测定波长310nm下的全光线透过率、波长350nm下的全光线透过率和波长400nm下的平行光线透过率。
【表1】
【表2】
由实施例1、2、3、4和5的结果可知,本发明的六方板状氧化锌颗粒的一次粒径大,且具有较窄的粒度分布,MIU和MMD的值均小。
另一方面,比较例4中是一次粒径大、为1.12μm的颗粒,但D90/D10为3.1,粒度分布变差,MIU的值大。
另外,比较例5中,D90/D10小、为2.8,可以说粒度分布窄,一次粒径小、为0.96μm,MIU和MMD的值均大。
由比较例4和5的结果可知,仅通过粒径的大小和粒度分布的宽窄中任一者无法减小MIU和MMD的值,无法得到优异的粉体触感。
由此可知,本发明的六方板状氧化锌颗粒通过具有1.1μm以上的一次粒径和较窄的粒度分布,从而MIU和MMD的值均小,能够得到优异的粉体触感。
另外可知,为六方板状的本申请发明的氧化锌颗粒与现有的不定形的氧化锌颗粒相比具有更优异的红外线反射性能。此外,即便是六方板状氧化锌颗粒,若在本发明的范围外则在可见光区域也产生吸收,与此相对,本申请发明的六方板状氧化锌颗粒在可见光区域不产生吸收,是具有优异的透明性的颗粒。
工业实用性
本发明的六方板状氧化锌颗粒能够混配于化妆料、油墨、涂料、树脂组合物等中。此外,在各种领域中可以作为红外线反射剂使用。
Claims (9)
1.一种六方板状氧化锌颗粒,其特征在于,一次粒径为1.1μm以上,粒度分布中的D90/D10为3.0以下。
2.如权利要求1所述的六方板状氧化锌颗粒,其中,粉体的平均摩擦系数MIU为0.87以下,摩擦系数的平均偏差MMD为0.035以下。
3.如权利要求1或2所述的六方板状氧化锌颗粒,其中,一次粒径为1.3μm以上30μm以下。
4.权利要求1、2或3所述的六方板状氧化锌颗粒的制造方法,其特征在于,包括下述工序:
制备pH为10以上的原料氧化锌的水浆料的工序(1);
将通过所述工序(1)制备的浆料与锌盐水溶液在35℃以下混合的工序(2);和
将所混合的浆料加热熟化的工序(3)。
5.一种化妆料,其特征在于,其含有权利要求1、2或3所述的六方板状氧化锌颗粒。
6.一种填料,其特征在于,其由权利要求1、2或3所述的六方板状氧化锌颗粒构成。
7.一种树脂组合物,其特征在于,其含有权利要求1、2或3所述的六方板状氧化锌颗粒。
8.一种红外线反射材料,其特征在于,其由权利要求1、2或3所述的六方板状氧化锌颗粒构成。
9.一种涂料组合物,其特征在于,其含有权利要求1、2或3所述的六方板状氧化锌颗粒。
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CN110740975A (zh) * | 2017-06-12 | 2020-01-31 | 堺化学工业株式会社 | 六角板状氧化锌的制造方法 |
CN110198699A (zh) * | 2017-06-15 | 2019-09-03 | 狮王株式会社 | 口腔用组合物 |
CN111527048A (zh) * | 2017-11-30 | 2020-08-11 | 堺化学工业株式会社 | 含有角蛋白和六角板状氧化锌的粒状复合体 |
CN111527048B (zh) * | 2017-11-30 | 2023-11-17 | 堺化学工业株式会社 | 含有角蛋白和六角板状氧化锌的粒状复合体 |
CN112166039A (zh) * | 2018-04-06 | 2021-01-01 | 聚合-医药有限公司 | 用于光致聚合增材制造的方法和组合物 |
CN112166039B (zh) * | 2018-04-06 | 2023-09-05 | 聚合-医药有限公司 | 用于光致聚合增材制造的方法和组合物 |
US11639416B2 (en) | 2018-04-19 | 2023-05-02 | Poly-Med, Inc. | Macromers and compositions for photocuring processes |
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US20160347624A1 (en) | 2016-12-01 |
TW201542467A (zh) | 2015-11-16 |
EP3103769A4 (en) | 2017-08-09 |
ES2682042T3 (es) | 2018-09-18 |
KR20160115926A (ko) | 2016-10-06 |
WO2015118777A1 (ja) | 2015-08-13 |
KR102206346B1 (ko) | 2021-01-22 |
EP3103769B1 (en) | 2018-06-20 |
JPWO2015118777A1 (ja) | 2017-03-23 |
CN105960379B (zh) | 2018-04-17 |
TWI664147B (zh) | 2019-07-01 |
EP3103769A1 (en) | 2016-12-14 |
US10696563B2 (en) | 2020-06-30 |
JP6493227B2 (ja) | 2019-04-03 |
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