CN114423402A - 乳化组合物、化妆料组合物以及乳化组合物的制造方法 - Google Patents
乳化组合物、化妆料组合物以及乳化组合物的制造方法 Download PDFInfo
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- CN114423402A CN114423402A CN202080065987.9A CN202080065987A CN114423402A CN 114423402 A CN114423402 A CN 114423402A CN 202080065987 A CN202080065987 A CN 202080065987A CN 114423402 A CN114423402 A CN 114423402A
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Abstract
本发明提供油性成分并不限于植物油、并且不需要以黄原胶、威兰胶作为必须成分的乳化组合物、化妆料组合物以及乳化组合物的制造方法。乳化组合物包含油性成分、水系分散介质、乳化剂以及纤维素纳米纤维,纤维素纳米纤维为乳化稳定剂,是将未改性的纤维素解纤而得到的,乳化剂的混配量小于乳化组合物总量的20质量%。化妆料组合物包含上述乳化组合物。乳化组合物的制造方法具有调整油相的工序、调整水相的工序、以及将上述油相和上述水相混合的乳化工序,在水相的调整工序和乳化工序中的至少任一工序中添加将未改性的纤维素解纤而得到的纤维素纳米纤维,在油相的调成工序、水相的调整工序以及乳化工序中的至少任一工序中添加乳化剂。
Description
技术领域
本发明涉及乳化组合物、化妆料组合物以及乳化组合物的制造方法。
背景技术
在乳膏、乳液、粉底液、护发素等化妆品、油漆等涂料、蛋黄酱、色拉调料等食用品等中,使用乳化(乳液)技术以使得在将油性成分和水系介质混合时油相和水相不发生分离。另外,近年来,作为生物物质来源的纤维素的有效利用,纳米级的纤维分散而成的纤维素纳米纤维(CNF)引起了人们的关注。出于静置粘度的高低、触变性等原因,期待纤维素纳米纤维在上述化妆品、涂料、食料品等中展开应用。但是,关于混配有纤维素纳米纤维的乳液的报告和提案并不多见。
例如,作为使用了纤维素纳米纤维(分散液)的乳化液或乳化方法的提案,具有专利文献1。该提案中,将纤维素纳米纤维(分散液)作为乳化剂进行添加,施加机械剪切力使其乳化。但是,该提案中可使用的油性成分限于菜籽油、橄榄油等天然植物油。植物油具有羧酸,与纤维素具有亲和性,因此认为纤维素纳米纤维起到作为乳化剂的作用。但是,还希望使用不具有亲水基团的油性成分。
另外,专利文献2中提出了一种水包油型乳化外用剂组合物。该提案中,除了发酵纤维素和/或纤维素纳米纤维以外,还合用了相对于这些纤维素为特定量的黄原胶和/或威兰胶。但是,合用特定量的黄原胶和/或威兰胶时,其用途非常受限,期望提出其他解决方法。
现有技术文献
专利文献
专利文献1:日本特开2015-157796号公报
专利文献2:日本特开2017-222594号公报
专利文献3:日本特开2019-156824号公报
发明内容
发明所要解决的课题
本发明所要解决的主要课题在于提供油性成分并不限于植物油、并且不需要以黄原胶、威兰胶等多糖类增稠剂作为必须成分的乳化组合物、化妆料组合物以及乳化组合物的制造方法。
用于解决课题的手段
若为下述乳化组合物,则可解决上述课题,该乳化剂组合物的特征在于,其包含油性成分、水系分散介质、乳化剂以及纤维素纳米纤维,纤维素纳米纤维为乳化稳定剂,是将未改性的纤维素解纤而得到的,上述乳化剂的混配量小于乳化组合物总量的20质量%。
关于这一点,作为乳化组合物的相关提案,例如有纤维素纳米纤维“通过对于将纤维素原料进行化学处理而得到的化学改性(羧甲基化、羧基化、磷酸酯化、阳离子化等)的纤维素(改性纤维素)进行解纤而得到”的提案(日本特开2019-156824号(专利文献3))。该提案“目的在于提供乳化稳定性、特别是长期乳化稳定性优异的乳化剂组合物”。总之,从乳化稳定性的方面出发,优选使用改性纤维素。但是,本发明人将如何消除油性成分的限定(限制)也作为课题,从这方面出发查明了纤维素为未改性的纤维素是优选的。尤其还查明了,在仅使纤维素为未改性的纤维素时,从乳化稳定性的方面出发还不能说一定是优选的。因此反复进行了各种研究,从而发现了乳化剂和纤维素纳米纤维的作用差异,结果想到了上述手段。
发明效果
根据本发明,可提供油性成分并不限于植物油、并且不需要以黄原胶、威兰胶等多糖类增稠剂作为必须成分的乳化组合物、化妆料组合物以及乳化组合物的制造方法。
附图说明
图1是示出乳化的状态的照片。
具体实施方式
接着对本发明的具体实施方式进行说明。需要说明的是,本实施方式为本发明的一例。本发明的范围并不限于本实施方式的范围。
本方式的乳化组合物包含油性成分、水系分散介质、乳化剂以及未改性的纤维素纳米纤维。本方式中的乳化剂使油性成分和水系介质乳化,因此具有提高相容性的作用。另一方面,未改性的纤维素纳米纤维具有作为乳化后的稳定剂(乳化稳定剂)的作用。根据这些事实,能够使水系介质和以往未作为对象的植物油以外的油性成分进行乳化。而且,能够防止经时地发生相分离(水相和油相发生分离),能够维持乳化稳定性。以下进行详细说明。
(用途)
本方式的乳化组合物能够用作例如化妆料组合物、医药中间原料、食品原料、涂料、树脂等的成分,特别适合用作化妆料组合物的成分。
此处的化妆料组合物被用作例如皮肤用化妆料、毛发用化妆料等。作为皮肤用化妆料,例如可例示出化妆水、乳液、冷霜、雪花膏、按摩霜、润肤霜、清洁霜、美容液、面膜、粉底、防晒化妆料、晒黑化妆料、补水霜、手霜、美白乳液、各种护肤液(lotion)等。
另外,作为毛发用化妆料,例如可例示出洗发水、润丝液、护发素、洗护洗发水、头发造型剂(造型慕丝、凝胶状整发料等)、养护发剂(发膏、发妆水等)、染发剂、化妆水类型的生发剂/养发剂等。
此外,作为化妆料组合物,还可例示出例如须前化妆水、须后化妆水、牙膏剂、软膏、贴剂、洗手液等清洗剂、芳香剂等。
需要说明的是,本方式的乳化组合物的乳化稳定性优异,其用途并不限于化妆料组合物。
(油性成分)
可在本方式的乳化组合物中使用的油性成分并不限于植物油。作为油性成分,例如可以使用油脂、高级醇、高级脂肪酸、酯类、烃类等。在后述的实施例中,示出了使用蓖麻油、二甲基硅油、棕榈酸乙基己酯、庚烷的示例。
将本方式的乳化组合物作为化妆料组合物的成分使用的情况下,作为油性成分,优选使用包含选自角鲨烷、链烷烃、聚乙烯蜡、微晶蜡、液体石蜡、矿物油中的1种或2种以上的烃的成分。
另外,作为油性成分,例如可以从下述物质中选择1种或2种以上来使用:加州希蒙得木油(jojoba oil)、澳洲坚果油、鳄梨油、月见草油、貂油、菜籽油、蓖麻油、葵花籽油、玉米油、可可油、椰子油、米糠油、橄榄油、杏仁油、芝麻油、红花油、大豆油、山茶油、杏核仁油、蓖麻油、貂油、棉籽油、木蜡、棕榈油、棕榈核油、蛋黄油、羊毛脂、角鲨烯等天然动植物油脂类;合成三甘油酯、角鲨烷、液体石蜡、凡士林、纯白地蜡、微晶蜡、异链烷烃等烃类;巴西棕榈蜡、固体石蜡、鲸蜡、蜂蜡、小烛树蜡、羊毛脂等蜡类;鲸蜡醇、硬脂醇、月桂醇、鲸蜡硬脂醇、油醇、山嵛醇、羊毛脂醇、氢化羊毛脂醇、己基癸醇、辛基十二烷醇等高级醇类;月桂酸、十四酸、棕榈酸、硬脂酸、山嵛酸、异硬脂酸、油酸、亚麻酸、亚油酸、氧代硬脂酸、十一碳烯酸、羊毛脂脂肪酸、硬质羊毛脂脂肪酸、软质羊毛脂脂肪酸等高级脂肪酸类;胆甾醇基-辛基十二烷基-二十二烷基等胆固醇及其衍生物;十四异丙酸、棕榈异丙酸、硬脂异丙酸、2-乙基己酸甘油酯、硬脂酸丁酯等酯类;二甘醇单丙醚、聚氧乙烯聚氧丙烯季戊四醇醚、聚氧丙烯丁醚、亚油酸乙酯等极性油;其他氨基改性硅酮、环氧改性硅酮、羧基改性硅酮、甲醇改性硅酮、甲基丙烯酰基改性硅酮、巯基改性硅酮、苯酚改性硅酮、单末端反应性硅酮、异种官能团改性硅酮、聚醚改性硅酮、甲基苯乙烯基改性硅酮、烷基改性硅酮、高级脂肪酸酯改性硅酮、亲水性特殊改性硅酮、高级烷氧基改性硅酮、含高级脂肪酸的硅酮、氟改性硅酮等(更具体地说包括硅树脂、甲基苯基聚硅氧烷、甲基聚硅氧烷、八甲基环四硅氧烷、十甲基环五硅氧烷、十二甲基环己烷硅氧烷、甲基环聚硅氧烷、八甲基三硅氧烷、十甲基四硅氧烷、聚氧乙烯-甲基聚硅氧烷共聚物、聚氧丙烯-甲基聚硅氧烷共聚物、聚(氧化乙烯-氧化丙烯)甲基聚硅氧烷共聚物、甲基氢聚硅氧烷、四氢四甲基环四硅氧烷、硬脂氧基甲基聚硅氧烷、十六烷氧基甲基聚硅氧烷、甲基聚硅氧烷乳液、高聚合甲基聚硅氧烷、三甲基硅氧基硅酸、交联型甲基聚硅氧烷、交联型甲基苯基聚硅氧烷、交联型甲基苯基聚硅氧烷等各种衍生物的硅酮类等)。
需要说明的是,近年来已经开发出据称为富含水的配方等的水(水相)的混配量高的化妆液(乳化液)。该化妆液中,油性成分的混配比例低、为10~20质量%的程度。并且,由于像这样油性成分的混配比例低的化妆液容易发生乳化,因此乳化的问题可能不会变得明显。因此,本方式的乳化组合物中,在油性成分的混配比例多的情况下,例如在为20质量%以上、特别是30质量%以上的情况下,可以使该效果更为显著。
(水系介质)
作为本方式中的乳化组合物的水系介质,可以单独使用水,也可以使用在水中混合有特定成分的混合液。
作为在水中混合的特定成分,例如可例示出乙醇、异丙醇等水溶性醇、甘油、乙二醇、丁二醇等亲水性多元醇类等。
(乳化剂)
在本方式的乳化组合物中与纤维素纳米纤维或纤维素纳米纤维的分散液分开地混合乳化剂。
作为乳化剂,例如可以使用非离子性表面活性剂、阴离子(anion)性表面活性剂、阳离子(cation)性表面活性剂、两性表面活性剂、磷脂等。其中优选使用非离子表面活性剂的酯型或酯-醚型。使用非离子性表面活性剂酯型或酯-醚型时,乳化剂的选择范围丰富,因此用于提高油相的初期分散性的设计变得容易,用于控制乳化组合物的设计、例如乳化组合物的触感、流动性的设计变得容易。
作为非离子性表面活性剂,例如可例示出甘油脂肪酸酯、聚甘油脂肪酸酯、丙二醇脂肪酸酯、山梨聚糖脂肪酸酯和山梨糖醇的脂肪酸酯以及它们的烷撑二醇加成物、聚烷撑二醇脂肪酸酯、蔗糖脂肪酸酯、聚山梨醇酯20、聚山梨醇酯60、聚山梨醇酯80、聚氧化烯烷基醚、聚氧乙烯烷基苯基醚等。
其中,作为非离子性表面活性剂,还适于使用例如聚氧乙烯甘油脂肪酸酯、聚甘油脂肪酸酯、山梨聚糖脂肪酸酯、聚氧乙烯山梨聚糖脂肪酸酯、聚氧乙烯山梨糖醇脂肪酸酯、聚乙二醇脂肪酸酯、聚氧乙烯蓖麻油、聚氧乙烯氢化蓖麻油、聚氧乙烯植物甾醇、聚氧乙烯聚氧丙烯烷基醚、聚氧乙烯羊毛脂、聚氧乙烯羊毛脂醇、聚氧乙烯蜂蜡衍生物、聚氧乙烯烷基胺、聚氧乙烯脂肪酰胺、聚氧乙烯烷基苯基甲醛缩合物、聚氧乙烯烷基醚磷酸(盐)等非离子表面活性剂。
另外,只要为不妨碍由本发明带来的效果的范围,也可以使用例如烷基硫酸酯盐、聚氧乙烯烷基硫酸酯盐、烷基苯磺酸盐、α-烯烃磺酸盐等阴离子表面活性剂、烷基三甲基氯化铵、二烷基二甲基氯化铵、苯扎氯铵等阳离子表面活性剂、烷基二甲氨基乙酸甜菜碱、烷基酰胺二甲氨基乙酸甜菜碱等两性表面活性剂、卵磷脂、羊毛脂、胆固醇、皂甙等具有表面活性能力的天然物、磺化琥珀酸酯类或氧化乙烯-氧化丙烯嵌段共聚物等低刺激性表面活性剂。
乳化剂的混配量优选小于乳化组合物总量的20质量%、更优选为15质量%以下、特别优选为10质量%以下。乳化剂的混配量为20质量%以上时,乳化稳定性趋于变差。据知这是由于,若过量地添加乳化剂,则包含纤维素纳米纤维的水相部分的流动性趋于降低、或者趋于凝胶化,作为结果使水相与油相的均匀分散性降低。
关于纤维素纳米纤维的混配量(绝干固体成分换算),优选按照其高于乳化剂的混配量的2.0质量%的方式来调节乳化剂和/或纤维素纳米纤维的混配量,更优选按照成为2.1质量%以上的方式进行调节、特别优选按照成为2.2质量%以上的方式进行调节。另外,关于纤维素纳米纤维的混配量(2.0质量%浓度的分散液),优选按照其高于乳化剂的混配量(高于100质量%)的方式来调节乳化剂和/或纤维素纳米纤维的混配量,更优选按照成为105质量%以上的方式进行调节、特别优选按照成为110质量%以上的方式进行调节。纤维素纳米纤维的混配量相对于乳化剂的混配量若过少,则包含纤维素纳米纤维的水相的分散性变差,特别具有容易产生纤维素的凝聚或凝胶化的倾向。
需要说明的是,例如甘油、丙二醇、二十二醇等有时也作为保湿剂、粘度调整剂等辅助剂使用,这些辅助剂也起到作为乳化剂的功能。因此,本方式中,在计算乳化剂的混配量时,上述辅助剂包含在乳化剂中。
(纤维素纳米纤维)
本方式的乳化组合物中,与乳化剂分开地将作为乳化稳定剂(乳化助剂)的未改性的纤维素纳米纤维根据需要以分散液的状态进行混合。下面对纤维素纳米纤维进行详细说明。
作为纤维素原料(下文中也称为“原料纸浆”),例如可以从以阔叶树、针叶树等作为原料的木材纸浆、以稻草、甘蔗渣、绵、麻、韧皮纤维等作为原料的非木材纸浆、以回收旧纸、废纸等作为原料的旧纸纸浆(DIP)等中选择1种或2种以上来使用。需要说明的是,以上的各种原料例如可以为被称为纤维素系粉末等的粉碎物(粉状物)的状态等。
其中,出于尽量避免杂质的混入、在纤维素成分中也以高配比得到不溶于碱的α-纤维素的原因,与非木材纸浆、旧纸纸浆相比,更优选使用木材纸浆。作为木材纸浆,例如可以从阔叶树硫酸盐纸浆(LKP)、针叶树硫酸盐纸浆(NKP)等化学纸浆、机械纸浆(TMP)等中选择1种或2种以上来使用。
阔叶树硫酸盐纸浆可以为阔叶树漂白硫酸盐纸浆、可以为阔叶树未漂白硫酸盐纸浆、也可以为阔叶树半漂白硫酸盐纸浆。同样地,针叶树硫酸盐纸浆可以为针叶树漂白硫酸盐纸浆、可以为针叶树未漂白硫酸盐纸浆、也可以为针叶树半漂白硫酸盐纸浆。
作为机械纸浆,例如可以从磨石磨纸浆(SGP)、压力磨石磨纸浆(PGW)、木片磨纸浆(RGP)、化学细磨纸浆(CGP)、热磨纸浆(TGP)、磨纸浆(GP)、热磨机械浆(TMP)、化学热磨机械浆(CTMP)、盘磨机械纸浆(RMP)、漂白热磨机械浆(BTMP)等中选择1种或2种以上来使用。
本方式中,优选纤维素原料未改性,即未进行TEMPO氧化、基于磷酸、亚磷酸等磷的含氧酸的改性、氨基甲酸酯改性等化学改性。关于这一点,若纤维素原料进行了化学改性,则通常通过其后的解纤得到的纤维素纳米纤维的均匀性增高。特别是在本方式中,由于纤维素纳米纤维的混配量相对于乳化组合物总量少,因此均匀性提高是乳化稳定性的重要因素。但是,在使用经化学改性的纤维素时,通过由静电排斥带来的影响,而使乳化(混合)液的乳化稳定性变差。因此,在使用纤维素纳米纤维作为乳化稳定剂的本方式中,优选未改性。在使用未改性的纤维素纳米纤维时,还可防止乳化组合物变成糊状,在制成化妆料组合物的情况下,可提高顺滑感等使用感。需要说明的是,本发明中的未改性被定义为在纤维素的解纤工序之前纤维素表面的羟基未进行改性的含义。
纤维素原料进行解纤而制成纤维素纳米纤维。该纤维素纳米纤维通常以分散液的状态得到。
在纤维素纳米纤维解纤之前,也可以利用化学方法进行前处理。作为利用化学方法的前处理,例如可例示出利用硫酸等酸进行的多糖的水解(酸处理)、利用酶进行的多糖的水解(酶处理)。
其中,优选利用酸处理和酶处理中的至少任一方法。在利用这些方法时,能够降低纤维素纳米纤维的保水度、提高结晶度,能够提高纤维素纳米纤维的均匀性。关于这一点,若纤维素纳米纤维的保水度低则容易脱水,纤维素纳米纤维的分散液(浆料)的脱水性提高。另外,纸浆(纤维素原料)所具有的半纤维素或纤维素的非晶区域发生分解,能够降低微细化处理的能量,能够提高纤维素纤维的均匀性、分散性。需要说明的是,纤维素纤维的分散性例如有助于提高纤维素纳米纤维的均匀性。其中,前处理会降低纤维素纳米纤维的长径比,因此优选避免过度的前处理。
作为酶处理中使用的酶,优选使用纤维素酶系酶和半纤维素酶系酶中的至少任一者,更优选将两者合用。在使用这些酶时,解纤变得容易。需要说明的是,纤维素酶系酶在水共存下引起纤维素的分解。另外,半纤维素酶系酶在水共存下引起半纤维素的分解。
作为纤维素酶系酶,例如可以使用木霉菌(Trichoderma、丝状菌)属、支顶孢(Acremonium、丝状菌)属、曲霉菌(Aspergillus、丝状菌)属、原毛平革菌(Phanerochaete、担子菌)属、栓菌(Trametes、担子菌)属、腐质霉(Humicola、丝状菌)属、杆菌(Bacillus、细菌)属、裂褶菌(Schizophyllum、担子菌)属、链霉菌(Streptomyces、细菌)属、假单胞菌(Pseudomonas、细菌)属等所产生的酶。这些纤维素酶系酶可以以试剂或市售品的形式购入。作为市售品,例如可例示出Cellulosin T2(HBI公司制)、Meicelase(明治制果公司制造)、Novozyme 188(Novozyme公司制造)、Multifect CX10L(Genencor公司制造)、纤维素酶系酶GC220(Genencor公司制造)等。
另外,作为纤维素酶系酶,也可以使用EG(内切葡聚糖酶)和CBH(外切葡聚糖酶)中的任一者。EG和CBH可以分别单独使用,也可以混合使用。另外,也可以与半纤维素酶系酶混合使用。
作为半纤维素酶系酶,例如可以使用作为分解木聚糖的酶的木聚糖酶(xylanase)、作为分解甘露聚糖的酶的甘露聚糖酶(mannase)、作为分解***聚糖的酶的***聚糖酶(arabanase)等。另外,也可以使用作为分解果胶的酶的果胶酶。
半纤维素是位于植物细胞壁的纤维素微原纤维之间的除果胶类以外的多糖类。半纤维素的种类多样,并且还根据木材的种类、细胞壁的壁层间而不同。在针叶树的次生壁,葡甘露聚糖为主成分;在阔叶树的次生壁,4-O-甲基葡萄糖醛酸木聚糖为主成分。因此,在由针叶树漂白硫酸盐纸浆(NBKP)得到微细纤维的情况下,优选使用甘露聚糖酶。另外,在由阔叶树漂白硫酸盐纸浆(LBKP)得到微细纤维的情况下,优选使用木聚糖酶。
酶相对于纤维素原料的添加量例如由酶的种类、原料木材的种类(针叶树还是阔叶树)、机械纸浆的种类等来决定。其中,酶相对于纤维素原料的添加量优选为0.1~10质量%、更优选为0.2~5质量%、特别优选为0.3~3质量%。酶的添加量若低于0.1质量%,则可能不能充分得到由酶的添加所带来的效果。另一方面,酶的添加量若高于10质量%,则可能使纤维素被糖化、微细纤维的收率可能会降低。另外还具有不能观察到与添加量的增量相符的效果的提高的问题。
使用纤维素酶系酶作为酶的情况下,从酶反应的反应性的方面出发,酶处理时的pH优选为弱酸性区域(pH=3.0~6.9)。另一方面,使用半纤维素酶系酶作为酶的情况下,酶处理时的pH优选为弱碱性区域(pH=7.1~10.0)。
关于酶处理时的温度,在使用纤维素酶系酶和半纤维素酶系酶中的任一者作为酶的情况下优选为30~70℃、更优选为35~65℃、特别优选为40~60℃。若酶处理时的温度为30℃以上,则酶活性不容易降低,能够防止处理时间延长。另一方面,若酶处理时的温度为70℃以下,则能够防止酶的失活。
酶处理的时间例如通过酶的种类、酶处理的温度、酶处理时的pH等来决定。其中,一般的酶处理时间为0.5~24小时。
在酶处理后优选使酶失活。作为使酶失活的方法,例如有添加碱性水溶液(优选pH10以上、更优选pH11以上)的方法、添加80~100℃的热水的方法等。
另外,在解纤之前进行碱处理时,纸浆所具有的半纤维素、纤维素的羟基发生部分解离,分子呈阴离子化,由此使分子内和分子间氢键减弱,促进解纤中的纤维素纤维的分散,但如上所述,本方式中不优选进行纤维素的改性。
原料纸浆的解纤例如可以通过使用磨浆机、高压均化器、高压均质化装置等均化器、研磨机、磨碎机等石臼式摩擦机、单轴混炼机、多轴混练机、捏合精研机、喷射式粉碎机等将原料纸浆打浆来进行。其中优选使用精研机、喷射式粉碎机来进行。
原料纸浆的解纤优选按照所得到的纤维素纳米纤维的平均纤维径、平均纤维长度、保水度、结晶度、模拟粒度分布的峰值、纸浆粘度、聚合度、分散液的B型粘度为以下所示的所期望的值或评价的方式来进行。
纤维素纳米纤维的平均纤维径(平均纤维宽度。单纤维的直径平均)优选为10~1000nm、更优选为10~100nm、特别优选为10~80nm。纤维素纳米纤维的平均纤维径若低于10nm,则纤维素纳米纤维分散液的粘度过度上升,乳化组合物的粘度也相对地增加,可能无法混配所期望的量的纤维素纳米纤维。
另一方面,纤维素纳米纤维的平均纤维径若高于1000nm,则可能会使乳化组合物的流动性变差、并且作为触感会带来不适感。
纤维素纳米纤维的平均纤维径例如可以通过原料纸浆的选定、前处理、解纤等来进行调整。
纤维素纳米纤维的平均纤维径的测定方法如下。
首先,将固体成分浓度0.01~0.1质量%的纤维素纳米纤维的水分散液100ml用特氟龙(注册商标)制膜过滤器进行过滤,用乙醇100ml进行1次溶剂置换、用叔丁醇20ml进行3次溶剂置换。接着进行冷冻干燥,进行锇涂布,制成试样。对于该试样,根据所构成的纤维的宽度,以3,000倍~30,000倍的任一倍率利用电子显微镜SEM图像进行观察。具体地说,在观察图像上绘出两条对角线,并任意绘出三条通过对角线的交点的直线。进一步目视测量与该三条直线交错的合计100根纤维的宽度。并且将测量值的中值径作为平均纤维径。
纤维素纳米纤维的平均纤维长度(单纤维的长度)优选为0.3~200μm、更优选为0.4~200μm、特别优选为0.5~200μm。纤维素纳米纤维的平均纤维长度若高于200μm,则纤维彼此凝聚,可能会使乳化组合物的流动性变差、即触感变差。
纤维素纳米纤维的平均纤维长度例如可以通过原料纸浆的选定、前处理、解纤等来进行调整。
关于纤维素纳米纤维的平均纤维长度的测定方法,与平均纤维径的情况同样地通过目视测量各纤维的长度。将测量值的中值长作为平均纤维长度。
纤维素纳米纤维的保水度优选为500%以下、更优选为300~480%。纤维素纳米纤维的保水度若低于300%,则可能得不到乳化稳定感,并且可能导致异物感的产生。
另一方面,纤维素纳米纤维的保水度若高于500%,则尽管纤维素纳米纤维本身的保水力增高、带来乳化稳定化,但可能使水滴或油滴的均匀化变得困难。
纤维素纳米纤维的保水度例如可以通过原料纸浆的选定、前处理、解纤等来进行调整。
纤维素纳米纤维的保水度为依据JAPAN TAPPI No.26(2000)测定得到的值。
纤维素纳米纤维结晶度优选为50%以上、更优选为55%以上。另外,CNF的结晶度优选为90%以下、更优选为86%以下。CNF的结晶度为上述范围内时,不容易受到乳化中使用的除纤维素以外的材料的物理/化学性的影响,容易维持乳化稳定性。
纤维素纳米纤维的结晶度例如可以通过原料纸浆的选定、前处理、解纤等来任意地进行调整。
纤维素纳米纤维的结晶度是依据JIS K 0131(1996)测定得到的值。
纤维素纳米纤维的模拟粒度分布曲线中的峰值优选为1个峰。为1个峰的情况下,纤维素纳米纤维的纤维长度和纤维径的均匀性高,纤维素纤维浆料的脱水性优异。
纤维素纳米纤维的峰值例如为1~100μm、优选为3~80μm、更优选为5~60μm。
纤维素纳米纤维的峰值例如可以通过原料纸浆的选定、前处理、解纤等来进行调整。
纤维素纳米纤维的峰值是依据ISO-13320(2009)测定得到的值。更详细地说,首先,使用粒度分布测定装置(株式会社Seishin Enterprise的激光衍射-散射式粒度分布测定器)调查纤维素纳米纤维的水分散液的体积基准粒度分布。接着,根据该分布测定纤维素纳米纤维的中值径。将该中值径作为峰值。
纤维素纳米纤维的纸浆粘度优选为1~10cps、更优选为2~9cps、特别优选为3~8cps。纸浆粘度是将纤维素溶解在铜乙二胺液中之后的溶解液的粘度,纸浆粘度越大,表示纤维素的聚合度越大。纸浆粘度为上述范围内时,可带来乳化稳定性,能够抑制异物感的产生。
纤维素纳米纤维的纸浆粘度是依据TAPPI T 230测定得到的值。
进行解纤得到的纤维素纳米纤维可以根据需要在与其他成分混合之前预先分散在水系介质中制成所期望的分散液。水系介质特别优选全部为水(水溶液)。但是,水系介质也可以一部分为与水具有相容性的其他液体。作为其他液体,例如可以使用碳原子数3以下的低级醇类等。
纤维素纳米纤维的聚合度优选为300以上、更优选为350~1800、特别优选为400~1700。聚合度若低于300,则可能带来乳化稳定性的阻碍、乳化组合物的异物感。需要说明的是,聚合度是作为纤维素的最小结构单元的“β-葡萄糖2分子”的连结数。本方式中的聚合度通过使用铜乙二胺溶液的粘度法来求出。
纤维素纳米纤维的分散液(浓度1.5%)的B型粘度优选为1,000cps~20,000cps、更优选为1,000~10,000cps、特别优选为1,000~5,000cps。分散液的B型粘度为上述范围内时,与构成乳化组合物的其他成分的混合/分散变得容易。
纤维素纳米纤维的分散液的B型粘度(浓度1.5%)是依据JIS-Z8803(2011)的“液体的粘度测定方法”测定得到的值。B型粘度是对分散液进行搅拌时的阻力矩,该B型粘度越高,意味着搅拌所需要的能量越多。
纤维素纳米纤维的固体成分浓度优选为0.1%~5.0%、更优选为0.3~4.0%、特别优选为0.5~3.0%。纤维素纳米纤维的固体成分浓度若低于0.1%,则流动性变得过高,乳化后的分散稳定化可能会受损。另外,纤维素纳米纤维的固体成分浓度即使高于5.0质量%,流动性也会显著降低,由此可能难以与其他成分进行混合,浆料本身的流动性降低,可能无法均匀地混合。
乳化组合物中的纤维素纳米纤维(2.0质量%浓度的分散液)的含量优选为5~90质量%、更优选为5~85质量%、特别优选为5~80质量%。纤维素纳米纤维的含量若低于5质量%,则乳化稳定性可能会丧失,可能容易发生乳化组合物的沉淀/分离。
(其他成分)
作为增强乳化稳定性的成分,也可以与纤维素纳米纤维分开地合用黄原胶、羧基乙基纤维素、羧基乙烯基聚合物等高分子系成分。这些高分子系成分均使水增粘、使乳化组合物变得稳定。
将本方式的乳化组合物作为化妆料组合物的成分使用的情况下,作为功能性成分,例如可以适当地使用:对氨基苯甲酸及其衍生物、7N-乙酰基邻氨基苯甲酸高孟基酯、丁基甲氧基苯甲酰基甲烷、二对甲氧基肉桂酸-单-2-乙基己酸甘油酯、肉桂酸辛酯等对甲氧基肉桂酸衍生物、水杨酸戊酯等水杨酸衍生物、2,4-二羟基二苯甲酮等二苯甲酮衍生物、二甲氧基亚苄基二氧代咪唑啉丙酸乙基己酯、乙酸液态羊毛脂、黄芩根提取物、三苯胺基-对羰乙基己氧基三嗪等紫外线吸收剂;熊果苷、曲酸、抗坏血酸磷酸酯镁等抗坏血酸及其衍生物、谷胱甘肽、甘草提取物、丁香提取物、茶提取物、虾红素、牛胎盘提取物、生育酚及其衍生物、传明酸及其盐、甘菊环、γ-羟基丁酸等美白成分;麦芽糖醇、山梨糖醇、甘油、丙二醇、1,3-丁二醇、聚乙二醇、二醇等多元醇、吡咯烷酮羧酸钠、乳酸钠、柠檬酸钠等有机酸及其盐、透明质酸钠等透明质酸及其盐、酵母和酵母提取液的水解物、酵母培养液、乳酸菌培养液等发酵代谢产物、胶原蛋白、弹性蛋白、角蛋白、丝胶蛋白等水溶性蛋白、胶原蛋白水解物、酪蛋白水解物、丝绸水解物、聚天冬氨酸钠等肽类及其盐、海藻糖、木二糖、麦芽糖、蔗糖、葡萄糖、植物性粘质多糖等糖类/多糖类及其衍生物、水溶性壳多糖、壳聚糖、果胶、硫酸软骨素及其盐等糖胺多糖及其盐、甘氨酸、丝氨酸、苏氨酸、丙氨酸、天冬氨酸、酪氨酸、缬氨酸、亮氨酸、精氨酸、谷酰胺、脯氨酸等氨基酸、氨基羰基反应物等糖氨基酸化合物、芦荟、七叶树等的植物提取液、三甲基甘氨酸、脲、尿酸、氨、卵磷脂、羊毛脂、角鲨烷、角鲨烯、葡糖胺、肌酸酐、DNA、RNA等核酸相关物质等的保湿剂;羧甲基纤维素、羟基乙基纤维素、羟基丙基三甲基氯化铵醚、乙基纤维素、羟基丙基纤维素、甲基羟基丙基纤维素、可溶性淀粉、羧甲基淀粉、甲基淀粉、藻酸丙二醇酯、聚乙烯醇、聚乙烯吡咯烷酮、聚乙烯基甲醚、羧基乙烯基聚合物、聚丙烯酸、甲基纤维素、羟基乙基纤维素、***树胶、黄原胶、瓜尔胶、刺槐豆胶、木瓜种子、卡拉胶、半乳聚糖、果胶、甘露聚糖、淀粉、右旋糖苷、琥珀酰聚糖、可得然胶、透明质酸、明胶、酪蛋白、白蛋白、胶原蛋白、甲氧基乙烯马来酸酐共聚物、两性甲基丙烯酸酯共聚物、聚氯化二甲基亚甲基哌啶鎓、聚丙烯酸酯共聚物、聚乙酸乙烯酯、硝酸纤维素、硅氧烷树脂、聚乙二醇脂肪酸酯、二硬脂酸聚乙二醇等聚氧乙烯脂肪酸酯、聚氧乙烯二油酸甲基葡糖苷等聚氧乙烯脂肪酸酯甲基糖苷、十四烯磺酸等α-烯烃磺酸等增稠剂;乙二胺四乙酸及其盐类、羟基乙二胺3乙酸及其盐类、磷酸、抗坏血酸、琥珀酸、葡萄糖酸、多磷酸盐类、偏磷酸盐类等金属离子封锁剂;乙醇、丙二醇、1,3-丁二醇等有机溶剂、丁基羟基甲苯、生育酚、植酸等抗氧化剂;苯甲酸及其盐、水杨酸及其盐、山梨酸及其盐、对羟基苯甲酸烷基酯(对羟基苯甲酸乙酯、对羟基苯甲酸丁酯等)及其盐、脱氢乙酸及其盐类、对氯间甲酚、六氯酚、硼酸、间苯二酚、三溴沙仑、邻苯基苯酚、葡萄糖酸氯己定、得恩地、感光素201号、苯氧基乙醇、苯扎氯铵、苄索氯铵、卤卡班、氯化氯己定、三氯卡班、乙酸生育酚、吡啶硫酮锌、扁柏酚、苯酚、异丙基甲基苯酚、2,4,4-三氯-2-羟基苯酚、六氯酚等抗菌、防腐剂;柠檬酸、苹果酸、酒石酸、乳酸、己二酸、谷氨酸、天冬氨酸、马来酸等有机酸;维生素A及其衍生物;维生素B6盐酸盐、维生素6三棕榈酸酯、维生素B6二辛酸酯、维生素B2及其衍生物等维生素B类;抗坏血酸、抗坏血酸硫酸酯、抗坏血酸磷酸酯等维生素C类、α生育酚、β生育酚、γ生育酚等维生素E类、维生素D类、维生素H、泛酸等维生素类、烟酰胺、烟酸苄酯、γ-谷维素、尿囊素、甘草酸(盐)、甘草次酸及其衍生物、扁柏酚、粘液素、红没药醇、桉树脑、百里酚、肌醇、皂甙类(皂树皂角苷、红豆皂角苷、丝瓜皂角苷等)、传明酸、泛酰基***、炔雌醇、头孢菌素、胎盘提取物、当药提取物、千金藤素、维生素E及其衍生物、γ谷维素等血行促进剂、辣椒酊、生姜酊、斑蝥酊、烟酸苄酯等局部刺激剂、维生素A类、维生素B组、维生素D组、维生素E、泛酸、维生素H等各种维生素或氨基酸等营养剂、甘草次酸、甘草酸衍生物、卡普氯铵、壬酸香草酰胺、尿囊素、甘菊环、氨基己酸、氢化可的松等抗炎症剂、氧化锌、硫酸锌、尿囊素羟基铝、氯化铝、磺基苯酚锌、丹宁酸等收敛剂、薄荷醇、樟脑等清凉剂、抗组胺剂、高分子硅酮、环状硅酮等硅系物质、生育酚类、BHA、BHT、没食子酸、NDGA等抗氧化剂等各种药剂;对于酿酒酵母等酵母、丝状菌、细菌、牛胎盘、人胎盘、人脐带、酵母、牛胶原蛋白、牛乳蛋白、小麦、大豆、牛血液、猪血液、鸡冠、春黄菊、黄瓜、稻米、乳木果油、白桦、茶、番茄、蒜、金缕梅、蔷薇、丝瓜、啤酒花、桃、杏、柠檬、猕猴桃、鱼腥草、辣椒、苦参、羊蹄菜、萍蓬草、鼠尾草、欧蓍草、锦葵、川芎、当药、百里香、当归、云杉、桦木、问荆、七叶树、虎耳草、山金车花、百合、艾蒿、芍药、芦荟、芦荟胶、黄芩、黄柏、红花(コウカ)、红花(ベニバナ)、山栀子、紫草根、大枣、陈皮、胡萝卜、薏苡仁、薏苡、栀子、花柏等动植物/微生物及其一部分利用有机溶剂、醇、多元醇、水、水性醇等进行提取或水解而得到的天然提取物;色素类;碳酸钙、滑石、高岭土、云母、硫、月桂酰赖氨酸、微粒二氧化硅、二氧化钛、二氧化锌、氧化铁红、氧化铁黄、氧化铁黑、尼龙12粉末、聚甲基丙烯酸甲酯粉末、聚乙烯粉末、聚苯乙烯粉末等粉末成分;阳离子化纤维素、羧基乙烯基聚合物、聚乙烯吡咯烷酮、聚乙烯吡咯烷酮/乙酸乙烯酯共聚物、黄原胶、羟基乙基纤维素等高分子添加剂;香料类;螯合剂;三乙醇胺、氢氧化钾、硼砂等碱;抗氧化剂等。这些成分的混配量根据化妆料组合物的目的适宜地决定。
(制造方法)
本方式的乳化组合物的制造方法至少具有调整油相的工序、调整水相的工序、以及将油相和水相进行混合的乳化工序。
本方式的方法中,将纤维素纳米纤维通常以分散液的状态在水相的调整工序和乳化工序中的至少任一工序中、优选在水相工序中进行添加。另一方面,乳化剂在油相的调整工序、水相的调整工序以及乳化工序中的至少任一工序中、优选在油相工序中进行添加。
乳化处理(工序)可以考虑各种乳化处理,但作为得到乳化稳定性优异并且使用感也优异的乳化组合物的方法,例如可例示出机械乳化法、D相乳化法、转相乳化法、液晶乳化法、氨基酸凝胶乳化法。机械乳化法中,例如可使用高压均化器、胶体磨、Nanomaizer、Microfluidizer、带螺旋桨的搅拌机、均相混合机、均质分散机等。另外,在使用带螺旋桨的搅拌机、均相混合机、均质分散机等的情况下,转速为500rpm以上、优选为800rpm以上、进一步优选为2000rpm以上、特别优选为5000rpm以上。
实施例
接着对本发明的试验例进行说明。
(试验例1~4)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯、二甲基硅油、蓖麻油或庚烷132g,接着加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐油酸酯2g,利用螺旋桨搅拌机在300rpm的条件下进行搅拌。接着添加作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)66g,进行乳化。该乳化中,利用螺旋桨搅拌机在1000rpm的条件下搅拌5分钟。以质量比计,油性成分(棕榈酸乙基己酯、二甲基硅油、蓖麻油、庚烷)为66%(油相)、包含未改性的CNF(乳化稳定剂)的水系介质为33%(水相)、表面活性剂(乳化剂)为1%。
关于试验结果,作为乳化稳定性,确认了刚搅拌后的乳化稳定性(初期乳化稳定性)和24小时后的乳化稳定性(24小时后乳化稳定性)。将均匀乳化的情况记为○、有凝聚物的情况记为△、水相和油相发生了分离的情况记为×。在以下的试验例中也是同样的。需要说明的是,图1中示出了下述示例的照片:从左起第1个为均匀乳化的情况(○)的示例(试验例1),从左起第2个为具有凝聚物的情况(△)的示例(试验例11),从左起第3个为水相和油相发生了分离的情况(×)的示例(试验例14)。试验例1~4中,在为任一油性成分时,乳化组合物均未发生分离。
(试验例5)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯128g,另一方面,作为水分调整,将作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)60g和作为表面活性剂的聚氧乙烯山梨糖醇酐油酸酯12g混合搅拌后投入到油性成分中,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。乳化组合物未发生分离。
(试验例6)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯128g,另一方面,作为水分调整,将作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)60g和作为表面活性剂的聚氧乙烯山梨糖醇酐单月桂酸酯12g混合搅拌后投入到油性成分中,进行乳化。该乳化中,利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟搅拌来进行。乳化组合物未发生分离。
(试验例7)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯149g,接着向油性成分中加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐油酸酯2g,利用螺旋桨搅拌机在300rpm的条件下进行搅拌。接着添加作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)49g,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。乳化组合物未发生分离。
(试验例8)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯99g,接着向油性成分中加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐油酸酯2g,另一方面,作为水分调整,将作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)49g与纯净水50g混合,利用螺旋桨搅拌机在300rpm的条件下进行搅拌。将该搅拌物投入到上述油性成分中,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。乳化组合物未发生分离。
(试验例9)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯66g、二甲基硅酮66g,进行混合,利用螺旋桨搅拌机在300rpm的条件下进行搅拌。接着向油性成分中添加作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)66g,最后向油性成分中加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐油酸酯2g,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。乳化组合物未发生分离。
(试验例10)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯120g,向油性成分中加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐单月桂酸酯30g,利用螺旋桨搅拌机在300rpm的条件下进行搅拌。接着向油性成分中添加作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)50g,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。乳化组合物未发生分离。
(试验例11)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯132g,接着向油性成分中加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐油酸酯2g,利用螺旋桨搅拌机在300rpm的条件下进行搅拌。接着添加作为乳化稳定剂的TEMPO氧化CNF(2.0%浓度)66g,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。刚搅拌后即未均匀分散,生成了凝聚物。
(试验例12)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯132g,接着向油性成分中加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐油酸酯2g,利用螺旋桨搅拌机在300rpm的条件下进行搅拌。接着添加纯净水66g(不包含乳化稳定剂(CNF)的条件),进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。初期分散性良好,但24小时后发生了水相和油相的分离。
(试验例13)
在300ml烧杯中量取作为油性成分的蓖麻油132g,接着添加作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)66g,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。该试验中未使用乳化剂。初期分散性良好,但24小时后发生了水相和油相的分离。
(试验例14)
在300ml烧杯中量取作为油性成分的棕榈酸乙基己酯120g,接着向油性成分中加入作为表面活性剂(乳化剂)的聚氧乙烯山梨糖醇酐单月桂酸酯40g,利用螺旋桨搅拌机在300rpm条件下进行搅拌。接着添加作为乳化稳定剂的未改性的CNF分散液(2.0%浓度)40g,进行乳化。该乳化利用螺旋桨搅拌机在1,000rpm的条件下搅拌5分钟来进行。刚搅拌后即未均匀分散,从初期分散起趋于分离,发生了相分离。
需要说明的是,所使用的CNF如下所述。
未改性机械处理CNF:大王制纸公司制造的机械处理CNF
TEMPO氧化CNF:第一工业制药公司制造
(考察)
由试验例1与试验例12的对比可知,将油性成分与乳化剂混合时,暂时成为乳化状态,但不具有经时稳定性;通过混配CNF,可提高经时稳定性。
由试验例3与试验例13的对比可知,将油性成分与CNF混合时,暂时成为乳化状态,但在未混配乳化剂时,经时稳定性变差。
由本试验结果可知,为了使油性成分和水系介质进行乳化且呈稳定化,适于添加未改性的CNF作为乳化稳定剂。由这一点也可获知,改性CNF作为乳化稳定剂并不优选。
由试验例10与试验例14的对比可知,乳化剂的混配量优选小于20%。
工业实用性
本发明可用作乳化组合物、化妆料组合物以及乳化组合物的制造方法。
Claims (5)
1.一种乳化组合物,其特征在于,
其包含油性成分、水系分散介质、乳化剂以及纤维素纳米纤维,
所述纤维素纳米纤维为乳化稳定剂,是将未改性的纤维素解纤而得到的,
所述乳化剂的混配量小于乳化组合物总量的20质量%。
2.如权利要求1所述的乳化组合物,其中,所述乳化剂为包含脂肪酸和脂肪酸酯中的至少任一者的非离子表面活性剂。
3.如权利要求1或2所述的乳化组合物,其中,所述纤维素纳米纤维以绝干固体成分换算的混配量为大于所述乳化剂的混配量的2.0质量%的量。
4.一种化妆料组合物,其特征在于,其包含权利要求1~3中任一项所述的乳化组合物。
5.一种乳化组合物的制造方法,其特征在于,
该制造方法具有调整油相的工序、调整水相的工序、以及将所述油相和所述水相进行混合的乳化工序,
在所述水相的调整工序和所述乳化工序中的至少任一工序中添加将未改性的纤维素解纤而得到的纤维素纳米纤维,
在所述油相的调整工序、所述水相的调整工序、以及所述乳化工序中的至少任一工序中添加乳化剂。
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