CN114349987B - 有机硅颗粒、配伍有其的化妆品、涂料及树脂 - Google Patents
有机硅颗粒、配伍有其的化妆品、涂料及树脂 Download PDFInfo
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- CN114349987B CN114349987B CN202210037689.XA CN202210037689A CN114349987B CN 114349987 B CN114349987 B CN 114349987B CN 202210037689 A CN202210037689 A CN 202210037689A CN 114349987 B CN114349987 B CN 114349987B
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Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/50—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms by carbon linkages
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- A—HUMAN NECESSITIES
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明提供一种有机硅粒子的制造方法,通过所述方法制备的有机硅粒子中,单位质量的硅原子键合氢原子的含量为300ppm以下,构成有机硅粒子的硅氧烷中的硅原子通过碳原子数4~20的亚烷基而与其他硅原子交联。所述有机硅粒子的分散性优异,可提供含有所述有机硅粒子的、使用感良好的化妆品、高功能涂料及电子材料。
Description
技术领域
本发明涉及一种有机硅颗粒,即便其不配伍无机物微粒或倍半硅氧烷颗粒等第三成分,仍具有低经时凝聚性及高亲油性。本发明还涉及含有该有机硅颗粒的、使用感良好的化妆品及其化妆品原料、涂料以及树脂配合剂。
背景技术
有机硅颗粒常被用作化妆品、涂料、油墨、热固性有机树脂、热塑性有机树脂等的添加剂,尤其适宜用作热固性有机树脂的内部应力缓和剂及有机树脂薄膜的表面润滑剂。
有机硅颗粒是对加成反应固化性有机硅组合物以及缩合反应固化性有机硅组合物进行固化而成者,其粒径、吸油性会因制造方法而异。一般而言,粉碎固化物制成粒状物时微细化有限度,因此,优选采用使交联性有机硅组合物的粒状物发生固化反应,获得小粒径有机硅颗粒的制造方法。
但是,虽然一次颗粒较为微细,但随着时间的变化,容易凝聚为二次颗粒,并且凝聚颗粒难以再分散为一次颗粒。这是源于如下现象:一旦一次颗粒彼此之间相互结合为凝聚颗粒,则该结合就很难再分裂(解离)。
为了发挥其作为化妆品原料的有用性,公开有一种方法,即在制造有机硅颗粒时,还加入己二烯、环己烷二甲醇二乙烯醚等具有脂肪族不饱和键的有机化合物进行固化。(日本专利4371480号公报)然而,应用该方法时,有机化合物无法充分地掺入到有机硅颗粒中,未反应的SiH会变为残基,还会导致经时凝聚。
将强凝聚性有机硅颗粒配伍到溶媒等之后,可能会出现以下情况:有机硅颗粒并不以一次粒径分散,而是变为二次凝聚颗粒或其聚集体,分散不充分,无法制备均匀的混合物。因此,存在以下问题,即含有有机硅颗粒的组合物无法充分地发挥有机硅颗粒的特征。另外,如我们所知,一般情况下例如硅橡胶粒状物等的低硬度的颗粒容易发生经时凝聚。
已知这种经时凝聚会对有机硅颗粒的吸油性产生影响,如何控制这种吸油性是其用作化妆品时所要解决的问题。为此,曾尝试对制造后的温度进行控制,以期控制吸油性。(日本专利5185111号公报)然而,存在一个主要问题,即在制造后需要确保留有控制时间。
以往在制造有机硅颗粒时,使用乙烯基作为烯基。使用乙烯基对于节约成本而言非常有效,并且也容易推断出反应后的形状。但是,使用乙烯基制造有机硅颗粒虽然能够改善上述种种问题,但无法解决相关问题,这一根本性的问题仍然存在。
现有技术文献
专利文献
专利文献1:日本专利4371480号公报
专利文献2:日本专利5185111号公报
专利文献3:日本专利特开2014-122316号公报
发明内容
发明所要解决的技术问题
本发明的目的之一在于提供一种分散性良好、具有高亲油性和高保存稳定性的有机硅颗粒及其优选的制造方法。此外,本发明的目的之一还在于提供一种使用感良好的化妆品、具有高功能性的树脂及其原料。
解决技术问题所采用的技术方案
本发明一实施方式的有机硅颗粒特征在于,单位质量的硅原子键合氢原子含量为300ppm以下,构成有机硅颗粒的硅氧烷中的硅原子通过碳原子数4~20的亚烷基而与其他硅原子交联。
本发明一实施方式的化妆品原料及树脂配合剂特征在于,由上述有机硅颗粒组成。本发明一实施方式的化妆品、涂料及电子材料特征在于,含有上述有机硅颗粒。
本发明一实施方式的有机硅颗粒形成用交联性组合物特征在于,含有以下(A)~(C)成分:
(A):一分子中具有2个以上碳原子数在4以上且20以下的烯基的有机聚硅氧烷,以及
(B):一分子中存在的硅原子键合氢原子为2个以上,且为一分子中硅原子数的40%以下的硅有机化合物,以及/或者
一分子中存在的硅原子键合氢原子为2个以上,含有三官能度硅氧烷单元或四官能度硅氧烷单元的硅有机化合物,
并且,(A)成分中的烯基含量(Alk)和(B)成分中的硅原子键合氢原子含量(H)的摩尔比为H/Alk=0.7~1.2。
本发明一实施方式的有机硅颗粒的制造方法特征在于,使上述有机硅颗粒形成用交联性组合物发生乳化,在催化剂存在的条件下使其固化。
发明效果
本发明一实施方式的有机硅颗粒具有如下特征:经时凝聚性低,保存稳定性较高。并且,有机硅颗粒自身具有舒适的触感,能够提高化妆品的使用感及涂料、树脂、电子材料的功能性。此外,本发明一实施方式的组合物能够提供该有机硅颗粒。另外,本发明一实施方式的有机硅颗粒制造方法具有以下特征,能够有效制造此种有机硅颗粒。
具体实施方式
以下,对本发明的有机硅颗粒及其制造方法以及使用该成分的化妆品、涂料、树脂进行详细说明。
本发明一实施方式的有机硅颗粒特征在于,单位质量的硅原子键合氢原子含量为300ppm以下,构成有机硅颗粒的硅氧烷中的硅原子通过碳原子数4~20的亚烷基而与其他硅原子交联。
本发明一实施方式的有机硅颗粒中硅原子键合氢含量优选为300ppm以下,更优选为250ppm以下,尤其优选为200ppm以下。进而,优选为150ppm以下,更优选为100ppm以下、50ppm以下,尤其优选为20ppm以下。本实施方式中,如果该硅原子键合氢变多,则会和其他有机硅颗粒发生交联,导致经时凝聚。此外,在本实施方式中,如果有机硅颗粒的硅原子键合氢有残留,则保存时会产生氢气。优点在于通过减少或消除这些氢气,能够更安全地制造有机硅颗粒。
作为测定该有机硅颗粒中的硅原子键合氢的方法,接触碱并采用气相色谱法(顶空法)的方法最具代表性。例如,相对于有机硅颗粒,按单位质量计算,添加等量的40%浓度氢氧化钾乙醇溶液,静置1小时,捕集反应终点前所产生的氢气,并利用顶空气相色谱法进行定量,从而能够进行鉴定。
关于构成本发明有机硅颗粒的硅氧烷中的硅原子和其他与硅原子交联的亚烷基,优选碳原子数为4~20。该碳原子数更优选为5以上、6以上;另一方面,优选为16以下、12以下、8以下。
本发明一实施方式的有机硅颗粒可使含有以下(A)成分及(B)成分的组合物反应而制成,即:
(A):一分子中具有2个以上碳原子数在4以上且20以下的烯基的有机聚硅氧烷,
(B):一分子中存在的硅原子键合氢原子为2个以上,且为一分子中硅原子数的40%以下的硅有机化合物,以及/或者
一分子中存在的硅原子键合氢原子为2个以上,含有三官能度硅氧烷单元或四官能度硅氧烷单元的硅有机化合物,
并且,(A)成分的烯基含量(Alk)和(B)成分的硅原子键合氢原子含量(H)的摩尔比为
H/Alk=0.7~1.2。
关于(A)成分中碳原子数在4以上且20以下的烯基,可列举丁烯基、戊烯基、己烯基、庚烯基、辛烯基、壬烯基、癸烯基、十一烯基、十二烯基、十三烯基、十四烯基、十五烯基、十六烯基、十七烯基、十八烯基、十九烯基、icosynyl。考虑到反应性,烯基的碳原子数优选为5以上,更优选为6以上。另外,同样考虑到反应性及凝聚性,烯基的碳原子数优选为16以下,更优选为12以下,尤其优选为8以下。特别地,优选为己烯基。并且,烯基优选位于有机聚硅氧烷的分子链末端,但也可以位于侧链,或者位于分子链末端和侧链。此外,关于除烯基以外的、和硅原子键合的基团,可列举甲基、乙基、丙基、丁基等烷基;环戊基、环己基等环烷基;苯基、甲苯基、二甲苯基等芳基;苄基、苯乙基、3-苯丙基等芳烷基;3-氯丙基、3,3,3-三氟丙基等卤代烷基等未取代或取代的一价烃基。作为其分子结构,可列举直链状、环状、网状、部分带分支的直链状,尤其优选为直链状、部分带分支的直链状。另外,其粘度优选为能够使硅氢化反应交联性有机硅组合物分散于水中的粘度。具体而言,25℃条件下,优选为20~100,000mPa·s范围内,尤其优选为20~10,000mPa·s范围内。
进而,考虑到所获得的有机硅粉末的吸油性,在(A)成分的有机聚硅氧烷中,由下式:-(CH3)2SiO-表示的二甲基硅氧烷单元含量优选为除分子末端硅氧烷单元以外的所有硅氧烷单元的90摩尔百分比以上。同样,考虑到改善所获得的硅氢化反应交联性硅橡胶粉末的吸油性,优选事先通过汽提等方式除去低聚合度(聚合物3~20)环状或链状有机聚硅氧烷。
此外,在有机聚硅氧烷1分子中,(A)成分中的烯基含量优选为0.50重量百分比以上,更优选为0.60重量百分比以上、0.70重量百分比以上、0.80重量百分比以上、0.90重量百分比以上。另一方面,其上限优选为5重量百分比以下,更优选为4重量百分比以下。
(B)成分是(i)一分子中存在的硅原子键合氢原子为2个以上,且为一分子中硅原子数的40%以下的硅有机化合物,以及/或者(ii)一分子中存在的硅原子键合氢原子为2个以上,含有三官能度硅氧烷单元或四官能度硅氧烷单元的硅有机化合物。(i)硅有机化合物,一分子中的硅原子键合氢原子优选为2个以上。并且,一分子中所具有的硅原子键合氢原子,优选为一分子中硅原子数的40%以下,更优选为30%以下、25%以下、20%以下、15%以下,尤其优选为10%以下。关于(ii)硅有机化合物,由于具有三官能度硅氧烷单元或四官能度硅氧烷单元,因此从立体结构而言,即便残留有SiH的未反应部分,也很难对有机硅颗粒的经时凝聚产生影响。考虑到反应性,则优选为三官能度硅氧烷单元。作为(B)成分的分子结构,可列举直链状、环状、网状、部分带分支的直链状。另外,其粘度优选为能够使硅氢化反应交联性有机硅组合物分散于水中的粘度。具体而言,25℃条件下,优选为1~10,000mPa·s范围内。
关于(A)成分及(B)成分在组合物中的比率,(A)成分的烯基含量(Alk)和(B)成分的硅原子键合氢原子含量(H)的摩尔比为
H/Alk=0.7~1.2
按此比率进行反应即可制成本发明的有机硅颗粒。关于H:Alk的摩尔比,优选的下限范围为H/Alk=0.8以上,更优选为0.85以上、0.90以上、0.95以上、以及1.0以上。如果超过该下限,则会有烯基残留。有机硅颗粒粉末的优选上限范围为1.15以下,更优选为1.10以下、1.05以下、以及1.00以下。如果超过该上限,则反应后容易残留有未反应的硅原子键合氢原子。另一方面,如果超过下限,则反应后容易残留有未反应的烯基。残留有这些未反应物质,则会导致有机硅颗粒凝聚,以及吸附的油脂残留,可能会对使用该有机硅颗粒作为原料的物质的物理性质造成不良影响。上述烯基为己烯基,H/Alk为0.9~1.1,尤其是接近1.0时,能够最有效地抑制有机硅颗粒的经时凝聚。
粉末粒径是对干燥后成为粉末的有机硅颗粒进行测定得出的数值,以乙醇等作为分散介质,利用激光衍射粒度分布仪鉴定的有机硅颗粒的中位粒径(相当于累计分布50%的粒径,D50),据此测定粉末粒径。本发明所涉及的有机硅颗粒是多个有机硅一次颗粒凝聚而成的二次颗粒形态,粉末粒径是直接测定有机硅颗粒的二次粒径而得出的数值。
本发明所涉及的有机硅颗粒的粉末粒径取决于构成粉末颗粒的一次颗粒的粒径大小,优选范围为0.5~50μm。该优选范围的下限优选为1μm,更优选为2μm、3μm。并且,该优选范围的上限优选为45μm,更优选为40μm、35μm、30μm、25μm以及20μm。如果小于该范围,则难以进行交联反应,而且容易附着于其他颗粒上,只能获得凝聚的交联物。如果大于该范围,则颗粒相对于化妆品、涂料的配伍性会受损,使用感也会变差。
另一方面,本发明所涉及的有机硅颗粒在制造时的水分散形态下,为凝聚前的一次颗粒,其粒径优选为1~10μm。一次粒径的下限如果低于上述数值,则交联反应性不能充分进行;如果一次粒径的上限超过上述数值,则使用感及配伍稳定性会受损。
关于有机硅颗粒的硬度,在将有机硅颗粒组合物固化为薄片状的情况下,利用JISK6301规定的JIS A硬度计测定,优选为5~70的范围。更优选为60以下,尤其优选为50以下。尤其是当橡胶硬度在所述范围内时,所获得的有机硅颗粒的凝聚性得到充分抑制,容易成为富有流动性、分散性、顺畅感、光滑性、柔软触感的物质。
本发明的有机硅颗粒是单位质量的硅原子键合氢原子含量为300ppm以下,构成有机硅颗粒的硅氧烷中的硅原子通过碳原子数4~20的亚烷基而与其他硅原子交联的物质(上述第一实施方式),或者按特定比率使(A)一分子中具有2个以上碳原子数在4以上且20以下的烯基的有机聚硅氧烷和(B)特定有机氢聚硅氧烷进行交联反应而获得的物质(上述第二实施方式),考虑到抑制有机硅颗粒的凝聚,上述有机硅颗粒的JIS-A硬度(Vα)和粉末粒径(Vβ)μm优选满足以下关系式。
Vα×Vβ≤1,200
关于本发明的上述实施方式所涉及的有机硅颗粒,如果硬度和粒径满足上述关系,则能有效地抑制有机硅颗粒的凝聚。另外,如果不满足上述实施方式,即便硬度和粒径满足上述关系,也不一定能抑制有机硅颗粒的凝聚。
对有机硅颗粒形成用交联性组合物进行乳化并固化,从而容易调整有机硅颗粒的粒径。该乳化的方法包括使用表面活性剂的方法、使用搅拌装置及超声波振动机等混合装置等的机械剪切法进行乳化的方法等。此时,在制备有机硅颗粒形成用交联性组合物的水系分散液之前,预先对固化性有机硅组合物进行冷却,抑制其固化性较为理想。使用表面活性剂时,作为该表面活性剂,可列举非离子类、阴离子类、阳离子类、甜菜碱类。所获得的有机硅颗粒的粒径会因表面活性剂的种类、含量而异。为了制备小粒径的有机硅颗粒,相对于有机硅颗粒形成用交联性组合物100质量份,该表面活性剂的添加量优选为0.5~50质量份的范围内。另一方面,为了制备大粒径的有机硅颗粒,相对于有机硅颗粒形成用交联性组合物100质量份,该表面活性剂的添加量优选为0.1~10质量份的范围内。另外,作为分散介质,相对于有机硅颗粒形成用交联性组合物100质量份,水的添加量优选为20~1,500质量份、50~1000质量份的范围内。另外,由于这些表面活性剂可以直接配伍到化妆品中,因此,本发明所涉及的有机硅颗粒可以用作化妆品原料。
此外,为了均匀地分散有机硅颗粒形成用交联性组合物,优选使用乳化器。作为该乳化器,可列举均匀混合器、桨叶式搅拌机、亨舍尔混合器、均质分散器、胶体研磨器、螺旋桨式搅拌器、均质机、连续式乳化器、超声波乳化器、真空混捏机。
接着,对根据上述方法制备的包含有机硅颗粒形成用交联性组合物的水系分散液进行加热或于室温下放置,从而能够使该水分散液中的有机硅颗粒形成用交联性组合物固化,制备有机硅颗粒的水系分散液。加热有机硅颗粒形成用交联性组合物的水系分散液时,其加热温度优选为100℃以下,尤其优选为10℃~95℃。此外,关于加热有机硅颗粒形成用交联性组合物的水系分散液的方法,例如可列举直接加热该水系分散液的方法、将该水系分散液添加到热水中的方法。然后,可以通过将水从有机硅颗粒的水系分散液中去除,从而制备有机硅颗粒。关于该除去方法,例如可列举使用真空干燥器、热风循环式烘箱、喷雾干燥器进行干燥的方法。将如上所述有机硅颗粒形成用交联性组合物放置于室温下或者通过加热,使其进行固化反应,形成有机硅颗粒。
此外,为了能在水系分散液中将有机硅颗粒形成用交联性组合物制成粒状并保持稳定,优选使用表面活性剂的水溶液。相对于有机硅颗粒形成用交联性组合物100质量份,表面活性剂的添加量优选为0.1~20质量份,更优选为0.2~10质量份,尤其优选为0.2~5质量份。相对于有机硅颗粒形成用交联性组合物100质量份,水的添加量优选为40~2000质量份,尤其优选为40~1000质量份。其原因在于,相对于有机硅颗粒形成用交联性组合物100质量份,如果水的添加量少于40质量份,则难以形成均匀的有机硅颗粒形成用交联性组合物的水系分散液;如果水的添加量超过2000质量份,则有机硅颗粒的生产力会显著降低。
另一方面,在利用上述方法除去水分的工序中,现有技术是通过加热工序使残存的有机硅颗粒表面硅原子键合氢基进行甲基化。然而,已知经过这种加热工序后,有机硅颗粒中仍然会残留有未反应硅原子键合氢基。虽然理论上没有限制,但即便颗粒表面的硅原子键合氢基全部被甲基化,颗粒内部仍然会有硅原子键合氢基残留,随着时间的变化,可能会对有机硅颗粒的粉末粒径产生影响。因此,根据现有技术,无法获得如本申请发明般硅原子键合氢基含量被抑制得极低的有机硅颗粒。
另外,无论是利用研磨机等粉碎机使有机硅颗粒形成用交联性组合物固化而获得的有机硅颗粒进行粉碎的方法,还是利用真空干燥器、热风循环式烘箱、喷雾干燥器等喷雾器在热风中喷雾使其固化的方法,有机硅颗粒中硅原子键合氢基含量都不会降低。
由于有机硅颗粒形成用交联性组合物的水系分散液容易稳定,要使用的水优选为如下所述的离子交换水,即:金属离子及卤素离子少,电导率优选为1μS/cm以下,电导率尤其优选为0.5μS/cm以下。
制成(A)成分和(B)成分混合物微粒化的水分散性液体后,向该微粒分散液中配伍(C)成分即硅氢化反应用催化剂,制备有机硅颗粒形成用交联性组合物的微粒,则能改善作业性,水分散液中的微粒也难以发生凝聚。
然后,对根据上述方法制备的有机硅颗粒形成用交联性组合物的水系分散液进行加热或于室温下放置,从而能够使该水分散液中的有机硅颗粒形成用交联性组合物固化,制备有机硅颗粒的水系分散液。
加热有机硅颗粒形成用交联性组合物的水系分散液时,其加热温度优选为100℃以下,尤其优选为10℃~95℃。此外,关于加热有机硅颗粒形成用交联性组合物的水系分散液的方法,例如可列举直接加热该水系分散液的方法、将该水系分散液添加到热水中的方法。
关于用于形成有机硅颗粒的固化反应,可使用硅氢化反应用催化剂(C)成分。该催化剂可以促进有机硅颗粒形成用交联性组合物的固化,优选为铂族金属(元素周期表中的Ⅷ族)或其化合物。优选为铂以及/或者铂化合物,例如微粉化的铂;氯铂酸或氯铂酸的酒精溶液;氯铂酸和烯基硅氧烷的合成物;铂-二酮的合成物;铂-烯基硅氧烷络合物;铂-烯烃络合物;二氧化硅、氧化铝、碳或同样载体的铂金属;或者包含铂化合物的热塑性树脂。作为其他铂族金属催化剂,可列举铑、钌、铱或者钯化合物。此外,为了进行硅氢化反应,还可以使用过氧化氢溶液作为催化剂。进而,还能使用铁、铁/钴等非铂类硅氢化催化剂。
有机硅颗粒的形状及性质并无特别限制,可以是弹性体(橡胶)颗粒,可以是树脂(resin)颗粒,也可以是同种或异种的有机硅复合颗粒。作为本发明的有机硅颗粒,更优选为具有弹性的有机硅弹性体颗粒。有机硅弹性体颗粒作为触感改善剂被用于化妆品、涂层剂等。有机硅树脂颗粒及被有机硅树脂或二氧化硅微粒包覆的有机硅弹性体颗粒很少发生凝聚,但触感较硬,可能无法获得像有机硅弹性体颗粒一样柔软的触感。
可以根据需要,对本发明的有机硅颗粒进行表面处理。具有代表性的处理是包覆二氧化硅,能够进一步改善本发明的有机硅颗粒的抑制凝聚效果。再者,也可以利用其他已知的亲水性处理剂或疏水性处理剂等进行表面处理。
本发明的有机硅颗粒可以是干燥的粉末颗粒形态,也可以是分散于水、酒精或多元醇等亲水性分散介质中的水系悬浮液形态。还可以是在油剂中分散或溶胀的油性有机硅颗粒组合物形态。
以下对本发明的化妆品进行详细说明。
该化妆品的特征在于,含有上述有机硅颗粒。关于该化妆品,可列举肥皂、沐浴露、洗面奶等清洁用化妆品;化妆水、乳霜乳液、面膜等基础化妆品;香粉、粉底等底妆化妆品;口红、腮红、眼影粉、眼线液、睫毛膏等眼眉部化妆品;指甲油等美甲化妆品;洗发水、护发素、整发液、育发剂、防脱发剂、染发剂等头发用化妆品;香水、古龙水等芳香性化妆品;牙膏;沐浴用剂;脱毛膏、剃须用须后水、止汗香体剂、防晒霜等特殊化妆品。另外,关于该化妆品的剂型,可列举水性液状、油性液状、乳液状、乳霜状、泡沫状、半固体状、固体状、粉状。还能通过喷雾的方式使用该化妆品。
在该化妆品中,上述有机硅颗粒含量优选为化妆品中的0.5~99.0质量百分比的范围内,尤其优选为1.0~95质量百分比的范围内。其原因在于,如果上述有机硅颗粒含量超过上述范围上限,则会丧失作为化妆品的效果;如果低于上述范围的下限,则难以改善化妆品的使用感等。
作为化妆品原料,还可以将颗粒以下段落中所述的化妆品成分作为介质(水性介质或油性介质),使有机硅分散于水相或油相中。作为水性介质,可以使用纯水、离子交换水、碱性离子水、深层水、波动水、天然水等水;乙醇、丙醇、异丙醇等低级醇;甘油、1,3-丁二醇、异戊二醇、二丙二醇等多元醇等能够和水混合的水性溶媒。
作为油性介质(油剂),可列举硅油、烃油、高级脂肪酸、高级醇、酯油(包括油脂)、醚油、矿物油、氟油等。其中,考虑到使用感,更优选为硅油、烃油、酯油。具体可列举二甲基聚硅氧烷、甲基氢聚硅氧烷、甲基苯基聚硅氧烷、聚醚改性有机聚硅氧烷、氟烷-聚氧化烯共改性有机聚硅氧烷、烷基改性有机聚硅氧烷、末端改性有机聚硅氧烷、氟改性有机聚硅氧烷、氨端聚二甲基硅氧烷、氨基改性有机聚硅氧烷、丙烯酸有机硅、三甲基硅烷氧基硅酸酯等硅油;液体石蜡、凡士林、角鲨烷等烃油;肉豆蔻醇肉豆蔻酸酯、月桂酸己酯、油酸癸酯、肉豆蔻酸异丙酯、二甲基辛酸己基癸酯、单硬脂酸甘油酯、邻苯二甲酸二乙酯、乙二醇单硬脂酸酯、羟基硬脂酸乙基己酯、异壬酸异壬酯、异十三醇异壬酸酯等酯油。这些油剂可以使用1种或2种以上。此外,相对于本发明所使用的油包水型乳化化妆品整体,油剂含量优选为10~50质量百分比,考虑到使用感、保存稳定性,更优选为20~40质量百分比。
在不妨碍本发明效果的范围内,本发明的化妆品能够添加常规的用于化妆品的成分、水、着色剂、醇类、水溶性高分子、皮膜形成剂、油剂、油溶性凝胶剂、有机改性粘土矿物、表面活性剂、树脂、盐类、保湿剂、防腐剂、抗菌剂、抗氧化剂、pH调节剂、螯合剂、清凉剂、抗炎剂、美肌成分(美白剂、细胞赋活剂、皮肤粗糙改善剂、血液循环催化剂、紧肤剂及抗皮脂溢出剂等)、维生素类、氨基酸类、核酸、激素、包合物等、生理活性物质、医药有效成分以及香料,并无特别限定。另外,除水以外,这些化妆品成分分别优选为化妆品的0.5~99.0质量百分比的范围内,尤其优选为1.0~95质量百分比的范围内。其原因在于,如果化妆品成分中1个成分的含量超过上述范围上限,则化妆品的使用感并不理想。此外,在添加时如果低于上述范围的下限,则难以获得提高化妆品使用感等的效果。另外,对于化妆品成分及其配伍量,将引入日本专利特开2015-113303号公报中公开的内容作为参考。
水只要是不含对人体有害的物质、洁净即可,可列举自来水、精制水、矿物质水及海洋深层水。本发明的化妆品为水系时,在不损害本发明效果的范围内,能在水相中任意配伍水溶性添加成分。另外,为了改善化妆品的保存稳定性等,还能适当配伍已知的pH调节剂、防腐剂、抗菌剂或抗氧化剂。
作为着色剂,可列举氧化铁红、氧化铁、氢氧化铁及钛酸铁等无机红色颜料,γ-氧化铁等无机褐色系颜料,黄色氧化铁及黄土等无机黄色系颜料;黑色氧化铁及碳黑等无机黑色颜料,锰紫及钴紫等无机紫色颜料,氢氧化铬、氧化铬、氧化钴及钛酸钴等无机绿色颜料,铁蓝及群青等无机蓝色系颜料,赤色3号、赤色104号、赤色106号、赤色201号、赤色202号、赤色204号、赤色205号、赤色220号、赤色226号、赤色227号、赤色228号、赤色230号、赤色401号、赤色505号、黄色4号、黄色5号、黄色202号、黄色203号、黄色204号、黄色401号、青色1号、青色2号、青色201号、青色404号、绿色3号、绿色201号、绿色204号、绿色205号、橙色201号、橙色203号、橙色204号、橙色206号及橙色207号等焦油系色素色淀化而成者,胭脂红酸、紫胶色酸、红花素、巴西木素、藏红花素等天然色素色淀化而成者等有色颜料;氧化钛包覆云母、云母钛、氧化铁处理云母钛、氧化钛包覆云母、氯氧化铋、氧化钛包覆氯氧化铋、氧化钛包覆滑石粉、银色素及氧化钛包覆着色云母等珠光颜料;铝、金、银、铜、铂、不锈钢等金属粉末。
优选对这些着色剂实施防水处理。也可以使用这些着色剂彼此之间的复合物,或者用一般油剂、有机硅化合物、氟化合物或表面活性剂等进行表面处理者,根据需要可以使用一种或两种以上。
作为这种防水处理的示例,可列举用各种防水表面处理剂处理着色剂,例如甲基氢聚硅氧烷处理、有机硅树脂处理、硅橡胶处理、丙烯酸有机硅处理、氟化有机硅处理等有机硅氧烷处理,硬脂酸锌处理等金属皂处理,硅烷偶联剂处理及烷基硅烷处理等硅烷处理,全氟烷基硅烷、全氟烷基磷酸酯盐及全氟聚醚处理等氟化合物处理及月桂酰赖氨酸处理等氨基酸处理,角鲨烷处理等油剂处理,以及丙烯酸烷基酯处理等丙烯酸处理等,可以组合其中的1种以上使用。
作为醇类,可以使用选自低级醇、糖醇及高级醇中的1种或多种。具体可列举乙醇及异丙醇等低级醇;山梨糖醇及麦芽糖等糖醇;以及月桂醇、肉豆蔻醇、棕榈醇、硬脂醇、山嵛醇、十六醇、油醇、异硬脂醇、己基十二醇、辛基十二醇、十八十六醇、2-癸基十四碳炔醇、胆甾醇、β-谷甾醇、植物甾醇、羊毛甾醇、POE胆甾醇醚、甘油单硬脂基醚(鲨肝醇)以及单油基甘油醚(鲨油醇)等高级醇。
为提高化妆品的使用感而配伍有水溶性高分子,只要是用于常规的化妆品的物质,即可使用两性、阳离子性、阴离子性、非离子性或遇水溶胀性粘土矿物中的任一个,也可以同时使用1种或2种以上的水溶性高分子。这些水溶性高分子对含水成分具有增黏效果,因此尤其适合用于获得凝胶状含水化妆品、油包水型乳液化妆品、水包油型乳液化妆品的情况。
作为两性水溶性高分子,可列举两性淀粉、二甲基二烯丙基氯化铵衍生物(例如,丙烯酰胺-丙烯酸-二甲基二烯丙基氯化铵共聚物、丙烯酸-二甲基二烯丙基氯化铵共聚物)及甲基丙烯酸衍生物(例如,聚甲基丙烯酰氧乙基二甲基甜菜碱、N-甲基丙烯酰氧乙基N,N-二甲基铵-α-甲基羧基甜菜碱与甲基丙烯酸烷基酯共聚物等)。
作为阳离子性水溶性高分子,可列举第4级氮改性多糖(例如,阳离子改性纤维素、阳离子改性羟乙基纤维素、阳离子改性瓜儿豆胶、阳离子改性槐豆胶、阳离子改性淀粉等)、二甲基二烯丙基氯化铵衍生物(例如,二甲基二烯丙基氯化铵-丙烯酰胺共聚物、聚二甲基亚甲基氯化哌啶等)、乙烯基吡咯烷酮衍生物(例如,乙烯基吡咯烷酮-甲基丙烯酸二甲氨基乙酯共聚物盐、乙烯基吡咯烷酮-甲基丙烯酰丙基三甲基氯化铵共聚物、乙烯基吡咯烷酮-甲基乙烯基咪唑氯化物共聚物等)、以及甲基丙烯酸衍生物(例如,甲基丙烯酰氧乙基二甲基甜菜碱-甲基丙烯酰氧乙基三甲基氯化铵-甲基丙烯酸2-羟乙酯共聚物、甲基丙烯酰氧乙基二甲基甜菜碱-甲基丙烯酰氧乙基三甲基氯化铵-甲基丙烯酸甲氧基聚乙二醇酯共聚物等)。
作为阴离子性水溶性高分子,可列举聚丙烯酸或其碱金属盐、聚甲基丙烯酸或其碱金属盐、透明质酸或其碱金属盐、乙酰化透明质酸或其碱金属盐及甲乙醚-马来酸酐共聚物的水解物等脂肪族羧酸或其金属盐的水溶性聚合物,羧甲基纤维素或其碱金属盐、甲乙醚-马来酸半酯共聚物、丙烯酸树脂烷醇胺液以及羧基乙烯基聚合物。
作为非离子性水溶性高分子,可列举聚乙烯基吡咯烷酮、高聚合度聚乙二醇、乙烯基吡咯烷酮/乙酸乙烯酯共聚物、乙烯基吡咯烷酮/甲基丙烯酸二甲氨基乙酯共聚物、乙烯基己内酰胺/乙烯基吡咯烷酮/甲基丙烯酸二甲氨基乙酯共聚物、纤维素或其衍生物(例如,甲基纤维素、乙基纤维素、羟乙基纤维素、羟丙基纤维素、羧甲基纤维素)、角蛋白及胶原或其衍生物、海藻酸钙、普鲁兰多糖、琼脂、明胶、罗望子多糖类、黄原胶、卡拉胶、高甲氧基果胶、低甲氧基果胶、瓜儿豆胶、果胶、阿拉伯树胶、结晶纤维素、阿拉伯半乳聚糖、刺梧桐树胶、黄蓍胶、藻酸、白蛋白、酪蛋白、凝胶多糖、结冷胶、葡聚糖、榅桲籽胶、黄蓍胶、甲壳素和壳聚糖衍生物、淀粉(大米、玉米、马铃薯及小麦等)以及角蛋白及胶原或其衍生物等天然高分子化合物。
遇水溶胀性粘土矿物为无机系水溶性高分子,是一种具有三层结构的含胶体硅酸铝,一般情况下,可列举由下式所示的物质:
(X,Y)2-3(Si,Al)4O10(OH)2Z1/3·nH2O
(其中,X为Al、Fe(III)、Mn(III)或者Cr(III),Y为Mg、Fe(II)、Ni、Zn或者Li,Z为K、Na或者Ca。)。
作为这种无机系水溶性高分子,具体可列举膨润土、蒙脱土、贝得石、绿脱石、皂石、水辉石、硅酸铝镁及硅酸酐,可以是天然物,也可以是合成物。
作为油剂,可以使用固体、半固体、液状中的任一个。具体可列举选自硅油、烃油、酯油、植物性油脂类、动物性油脂类、脂肪酸、高级醇、甘油三酯、人工皮脂及氟系油剂中的1种或2种以上。
关于硅油,作为环状有机聚硅氧烷可列举六甲基环三硅氧烷(D3)、八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)、十二甲基环六硅氧烷(D6)、1,1-二乙基六甲基环四硅氧烷、苯基七甲基环四硅氧烷、1,1-二苯基六甲基环四硅氧烷、1,3,5,7-四乙烯基四甲基环四硅氧烷、1,3,5,7-四甲基环四硅氧烷、1,3,5,7-四环己基四甲基环四硅氧烷、三(3,3,3-三氟丙基)三甲基环三硅氧烷、1,3,5,7-四(3-甲基丙烯酰氧丙基)四甲基环四硅氧烷、1,3,5,7-四(3-丙烯酰氧丙基)四甲基环四硅氧烷、1,3,5,7-四(3-羧丙基)四甲基环四硅氧烷、1,3,5,7-四(3-乙烯氧基丙基)四甲基环四硅氧烷、1,3,5,7-四(p-乙烯基苯基)四甲基环四硅氧烷、1,3,5,7-四[3-(p-乙烯基苯基)丙基]四甲基环四硅氧烷、1,3,5,7-四(N-丙烯酰基-N-甲基-3-氨基丙基)四甲基环四硅氧烷以及1,3,5,7-四(N,N-双(月桂酰基)-3-氨基丙基)四甲基环四硅氧烷等。作为直链状有机聚硅氧烷,可列举分子链两末端被三甲基硅氧基封端的二甲基聚硅氧烷(2cst或6cst等低粘度~100万cst等高粘度二甲基硅油)、有机氢聚硅氧烷、分子链两末端被三甲基硅氧基封端的甲基苯基聚硅氧烷、分子链两末端被三甲基硅氧基封端的二甲基硅氧烷-甲基苯基硅氧烷共聚物、分子链两末端被三甲基硅氧基封端的二苯基聚硅氧烷、分子链两末端被三甲基硅氧基封端的二甲基硅氧烷-二苯基硅氧烷共聚物、三甲基五苯基三硅氧烷、苯基(三甲基硅氧基)硅氧烷、分子链两末端被三甲基硅氧基封端的甲基烷基聚硅氧烷、分子链两末端被三甲基硅氧基封端的二甲基聚硅氧烷-甲基烷基硅氧烷共聚物、分子链两末端被三甲基硅氧基封端的二甲基硅氧烷-甲基(3,3,3-三氟丙基)硅氧烷共聚物、α,ω-二羟基聚二甲基硅氧烷、α,ω-二乙氧基聚二甲基硅氧烷、1,1,1,3,5,5,5-七甲基-3-辛基三硅氧烷、1,1,1,3,5,5,5-七甲基-3-十二基三硅氧烷、1,1,1,3,5,5,5-七甲基-3-十六基三硅氧烷、甲基三(三甲基硅氧基)硅烷、烷基三(三甲基硅氧基)硅烷、四(三甲基硅氧基)硅烷、四甲基-1,3-二羟基二硅氧烷、八甲基-1,7-二羟基四硅氧烷、六甲基-1,5-二乙氧基三硅氧烷、六甲基二硅氧烷、八甲基三硅氧烷、高级烷氧基改性硅油及高级脂肪酸改性硅油等。
作为烃油,可列举液体石蜡、轻质液体异构烷烃、重质液体异构烷烃、凡士林、正构烷烃、异构烷烃、异十二烷、异十六烷、聚异丁烯、氢化聚异丁烯、聚丁烯、地蜡、纯地蜡、微晶蜡、石蜡、聚乙烯蜡、聚乙烯-聚丙烯蜡、角鲨烷、角鲨烯、姥鲛烷及聚异戊二烯等。
作为酯油,可列举辛酸己基癸酯、辛酸十六烷基酯、肉豆蔻酸异丙酯、棕榈酸异丙酯、硬脂酸丁酯、月桂酸己酯、肉豆蔻醇肉豆蔻酸酯、油醇油酸酯、油酸癸酯、辛基十二醇肉豆蔻酸酯、二甲基辛酸己基癸酯、乳酸十六烷基酯、肉豆蔻醇乳酸酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、乙酰化羊毛脂、乙二醇单硬脂酸酯、丙二醇单硬脂酸酯、丙二醇双油酸酯、单硬脂酸甘油酯、甘油单油酸酯、2-乙基己酸三甘油酯、三羟甲基丙烷三(乙基己酸)酯、双三羟甲基丙烷三(乙基己酸)酯、双三羟甲基丙烷异硬脂酸酯/癸二酸酯、三羟甲基丙烷三(乙基己酸)酯、三羟甲基丙烷三异硬脂酸酯、己二酸二异丙酯、己二酸二异丁酯、己二酸-2-己基癸酯、己二酸二-2-庚基十一烷基酯、二异硬脂醇苹果酸酯、氢化蓖麻油单异硬脂酸酯、N-烷基二醇单异硬脂酸酯、辛基十二醇异硬脂酸酯、异硬脂酸异丙酯、异鲸蜡醇异硬脂酸酯、二-2-乙基己酸乙二醇酯、2-乙基己酸鲸蜡醇酯、季戊四醇四-2-乙基己酸酯、辛基十二醇酯、油酸乙酯、辛基十二醇油酸酯、新戊二醇二癸酸酯、柠檬酸三乙酯、柠檬酸2-乙基己酯、琥珀酸二辛酯、异鲸蜡醇硬脂酸酯、癸二酸二异丙酯、二-2-乙基己基癸二酸酯、癸二酸二乙酯、癸二酸二辛酯、癸二酸二丁基辛酯、鲸蜡醇棕榈酸酯、辛基十二醇棕榈酸酯、棕榈酸辛酯、棕榈酸2-乙基己酯、棕榈酸2-己基癸酯、棕榈酸2-庚基十一烷基酯、12-羟基硬脂酸胆甾醇酯、双季戊四醇脂肪酸酯、肉豆蔻酸2-己基癸酯、月桂酸乙酯、N-月桂酰基-L-谷氨酸-2-辛基十二醇酯、N-月桂酰基-L-谷氨酸二(胆甾醇酯/山嵛酯/辛基十二醇酯)、N-月桂酰基-L-谷氨酸二(胆甾醇酯/辛基十二醇酯)、N-月桂酰基-L-谷氨酸二(植物甾醇酯/山嵛酯/辛基十二醇酯)、N-月桂酰基-L-谷氨酸二(植物甾醇酯/辛基十二醇酯)、N-月桂酰基肌氨酸异丙酯、二异硬脂醇苹果酸酯、新戊二醇二(乙基己酸)酯、新戊酸异癸酯、异十三醇新戊酸酯、异硬脂醇新戊酸酯、异壬酸异壬酯、异十三醇异壬酸酯、异壬酸乙基己酯、异十三醇异壬酸酯、二新戊酸二乙基戊二醇酯、甲基戊二醇二新戊酸酯、辛基十二醇新癸酸酯、2-丁基-2-乙基-1,3-丙二醇二辛酸酯、季戊四醇四辛酸酯、氢化松香季戊四醇酯、三乙基己酸季戊四醇酯、二聚季戊四醇六羟基硬脂酸酯/六硬脂酸酯/六松脂酸酯、聚甘油四异硬脂酸酯、聚甘油-10九异硬脂酸酯、聚甘油-8十芥酸酯/十异硬脂酸酯/十蓖麻油酸酯、双甘油(癸二酸/异棕榈酸)酯、乙二醇二硬脂酸酯(乙二醇二硬脂酸酯)、二聚亚油酸二异丙酯、二异硬脂醇二聚亚油酸酯、植物甾醇异硬脂醇二聚亚油酸酯、山嵛醇/植物甾醇二聚亚油酸酯、植物甾醇/异硬脂醇/鲸蜡醇/硬脂醇/山嵛醇二聚亚油酸酯、二聚亚油醇二聚亚油酸酯、二聚亚油醇二异硬脂酸酯、二聚亚油醇氢化松脂酸酯、氢化蓖麻油二聚亚油酸酯、羟烷基二聚亚油基醚、三异辛酸甘油酯、三异硬脂酸甘油酯、三肉豆蔻酸甘油酯、三异棕榈酸甘油酯、三辛酸甘油酯、三油酸甘油酯、二异硬脂酸甘油酯、辛酸/癸酸甘油三酯、辛酸/癸酸/肉豆蔻酸/硬脂酸甘油三酯、氢化松香甘油三酯(氢化酯胶)、松香甘油三酯(酯胶)、甘油山嵛酸酯/二十酸酯、二-2-庚基十一酸甘油酯、异硬脂酸/肉豆蔻酸二甘油酯、胆甾醇乙酸酯、胆甾醇壬酸酯、胆甾醇硬脂酸酯、胆甾醇异硬脂酸酯、胆甾醇油酸酯、12-羟基硬脂酸胆甾醇酯、澳洲坚果油酸胆甾醇酯、植物甾醇澳洲坚果油酸酯、植物甾醇异硬脂酸酯、轻质胆甾醇羊毛脂酸酯、硬质胆甾醇羊毛脂酸酯、长链支化脂肪酸胆甾醇酯、长链α-羟基脂肪酸胆甾醇酯、辛基十二醇蓖麻油酸酯、辛基十二醇羊毛脂酸酯、辛基十二醇芥酸酯、氢化蓖麻油异硬脂酸酯、鳄梨油酸乙酯以及羊毛脂酸异丙酯等。
作为天然动植物油脂类及半合成油脂,可列举鳄梨油、亚麻籽油、甜扁桃油、虫蜡、紫苏子油、油橄榄果油、可可籽脂、木棉蜡、榧树油、巴西棕榈蜡、肝油、小烛树蜡、牛油、牛蹄油、牛骨油、氢化牛油、野杏仁油、鲸油、氢化油、小麦胚芽油、芝麻油、稻胚芽油、稻糠油、蔗蜡、落瓣油茶籽油、红花籽油、乳木果油、白花泡桐油、桂皮油、霍霍巴蜡、橄榄角鲨烷、紫虫胶蜡、海龟油、大豆油、茶籽油、山茶籽油、月见草油、玉米油、猪油、油菜籽油、日本桐油、糠蜡、胚芽油、马油、杏仁油、棕榈油、棕榈仁油、蓖麻油、氢化蓖麻油、蓖麻油脂肪酸甲酯、向日葵籽油、葡萄籽油、月桂果蜡、霍霍巴籽油、氢化霍霍巴酯、澳洲坚果籽油、蜜蜡、貂油、草棉籽油、棉蜡、木蜡、木蜡仁油、褐煤蜡、椰子油、氢化椰子油、椰油脂肪酸甘油酯、羊油、花生油、羊毛脂、液状羊毛脂、氢化羊毛脂、羊毛脂醇、硬质羊毛脂、乙酰化羊毛脂、羊毛脂酸异丙酯、POE羊毛脂醇醚、羊毛脂脂肪酸聚乙二醇酯、POE氢化羊毛脂醇醚以及蛋黄油等。这里,POE是指聚氧乙烯。
作为高级脂肪酸,例如可列举月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山嵛酸、十一烯酸、油酸、亚油酸、亚麻酸、花生四烯酸、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)、异硬脂酸以及12-羟基硬脂酸等。
作为高级醇,例如可列举月桂醇、肉豆蔻醇、棕榈醇、硬脂醇、山嵛醇、十六醇、油醇、异硬脂醇、己基十二醇、辛基十二醇、十八十六醇、2-癸基十四碳炔醇、胆甾醇、β-谷甾醇、植物甾醇、羊毛甾醇、POE胆甾醇醚、甘油单硬脂基醚(鲨肝醇)以及单油基甘油醚(鲨油醇)等。
作为氟系油剂,可列举全氟聚醚、全氟癸烷及全氟辛烷等,这些油剂可以根据需要使用一种或两种以上。
作为油溶性凝胶剂,可列举硬脂酸铝、硬脂酸镁、肉豆蔻酸锌等金属皂,N-月桂酰基-L-谷氨酸以及α,γ-二-n-丁基胺等氨基酸衍生物,糊精棕榈酸酯、糊精硬脂酸酯、糊精2-乙基己酸酯/棕榈酸酯等糊精脂肪酸酯,蔗糖棕榈酸酯及蔗糖硬脂酸酯等蔗糖脂肪酸酯,菊糖硬脂酸酯及低聚果糖2-乙基己酸酯等低聚果糖脂肪酸酯,亚苄基山梨醇、二苄基山梨醇等山梨醇的亚苄基衍生物,以及二甲基苄基十二烷基铵蒙脱石粘土及二甲基二(十八烷基)铵蒙脱石粘土等有机改性粘土矿物等,可以根据需要使用一种或两种以上。
作为表面活性剂,可以同时使用选自由有机硅系表面活性剂、阴离子性表面活性剂、阳离子性表面活性剂、非离子性表面活性剂、两性表面活性剂及半极性表面活性剂所组成的群组中的1种或2种以上表面活性剂。
有机硅系表面活性剂多被用作油剂的乳化及清洗、粉体的分散及表面处理用成分,代表性的有机硅系表面活性剂可列举聚甘油改性有机硅、甘油改性有机硅、糖改性有机硅、含氟聚醚改性有机硅、聚醚改性有机硅、羧酸改性有机硅、糖改性有机硅、直链状有机硅-聚醚嵌段共聚物(聚硅氧烷-13等)及长链烷基-聚醚共改性有机硅等。
作为阴离子性表面活性剂,可列举饱和或不饱和脂肪酸盐(例如,月桂酸钠、硬脂酸钠、油酸钠及亚麻酸钠等)、烷基硫酸盐、烷基苯磺酸(例如,己基苯磺酸、辛基苯磺酸及十二烷基苯磺酸等)及其盐、聚氧化烯烷基醚硫酸盐、聚氧化烯烯基醚硫酸盐、聚氧乙烯烷基硫酸酯盐、磺基琥珀酸烷基酯盐、聚氧化烯磺基琥珀酸烷基酯盐、聚氧化烯烷基苯基醚硫酸盐、链烷磺酸盐、辛基三甲基溴化铵、十二烷基三甲基溴化铵、烷基磺酸盐、聚氧乙烯烷基苯基醚硫酸盐、聚氧化烯烷基醚乙酸盐、烷基磷酸盐、聚氧化烯烷基醚磷酸盐、酰基谷氨酸盐、α-酰基磺酸盐、烷基磺酸盐、烷基烯丙基磺酸盐、α-烯烃磺酸盐、烷基萘磺酸盐、链烷磺酸盐、烷基或烯基硫酸盐、烷基酰胺硫酸盐、烷基或烯基磷酸盐、烷基酰胺磷酸盐、烷醇基烷基牛磺酸盐、N-酰基氨基酸盐、磺基琥珀酸盐、烷基醚羧酸盐、酰胺醚羧酸盐、脂肪酸酯α-磺酸盐、丙氨酸衍生物、甘氨酸衍生物及精氨酸衍生物。作为盐,可列举钠盐等碱金属盐、镁盐等碱土类金属盐、三乙醇胺盐等链烷醇胺盐以及铵盐。
作为阳离子性表面活性剂,可列举烷基三甲基氯化铵、十八烷基三甲基氯化铵、十二烷基三甲基氯化铵、十六烷基三甲基氯化铵、牛油烷基三甲基氯化铵、山嵛基三甲基氯化铵、十八烷基三甲基溴化铵、山嵛基三甲基溴化铵、双十八烷基二甲基氯化铵、二椰油酰基二甲基氯化铵、二辛基二甲基氯化铵、二(POE)油基甲基氯化铵(2EO)、氯化苄烷铵、烷基氯化苄烷铵、烷基二甲基氯化苄烷铵、氯化苄乙铵、十八烷基二甲基苄基氯化铵、羊毛脂衍生的季铵盐、二乙氨基乙基硬脂酸酰胺、二甲氨基丙基硬脂酸酰胺、山嵛酸酰胺丙基二甲基羟基丙基氯化铵、司吡氯铵、氯化十六烷吡啶、塔尔油烷基苄基羟乙基咪唑氯化物及苄基铵盐。
作为非离子性表面活性剂,可列举聚甘油二异硬脂酸酯、二甘油聚羟基硬脂酸酯、异硬脂基甘油醚、聚氧化烯醚类、聚氧化烯烷基醚类、聚氧化烯脂肪酸酯类、聚氧化烯脂肪酸二酯类、聚氧化烯树脂酸酯类、聚氧化烯(氢化)蓖麻油类、聚氧化烯烷基酚类、聚氧化烯烷基苯基醚类、聚氧化烯苯基苯基醚类、聚氧化烯烷基酯类、聚氧化烯烷基酯类、失水山梨醇脂肪酸酯、聚氧化烯失水山梨醇烷基酯类、聚氧化烯失水山梨醇脂肪酸酯类、聚氧化烯山梨醇脂肪酸酯类、聚氧化烯甘油脂肪酸酯类、聚甘油烷基醚类、聚甘油脂肪酸酯类、蔗糖脂肪酸酯类、脂肪酸烷醇酰胺、烷基糖苷类、聚氧化烯脂肪酸二苯基醚类、聚丙二醇、二乙二醇、聚氧乙烯-聚氧丙烯嵌段聚合物、烷基聚氧乙烯-聚氧丙烯嵌段聚合物、聚氧乙烯-聚氧丙烯嵌段聚合物、烷基聚氧乙烯-聚氧丙烯嵌段聚合物醚以及氟系表面活性剂等。
作为两性表面活性剂,可列举咪唑啉型、酰胺甜菜碱型、烷基甜菜碱型、烷基酰胺基甜菜碱型、烷基磺基甜菜碱型、酰胺基磺基甜菜碱型、羟基磺基甜菜碱型、羰基甜菜碱型、磷酸酯甜菜碱型、氨基羧酸型及酰胺氨基酸型两性表面活性剂。具体可列举2-十一烷基-N,N,N-(羟乙基羧甲基)-2-咪唑啉钠以及2-椰油酰基-2-咪唑鎓氢氧化物-1-羧基乙氧基-2-钠盐等咪唑啉型两性表面活性剂;十二烷基二甲基氨基乙酸甜菜碱及肉豆蔻基甜菜碱等烷基甜菜碱型两性表面活性剂;椰油脂肪酸酰胺丙基二甲基氨基乙酸甜菜碱、棕榈仁油脂肪酸酰胺丙基二甲基氨基乙酸甜菜碱、牛油脂肪酸酰胺丙基二甲基氨基乙酸甜菜碱、氢化牛油脂肪酸酰胺丙基二甲基氨基乙酸甜菜碱、月桂酸酰胺丙基二甲基氨基乙酸甜菜碱、肉豆蔻酸酰胺丙基二甲基氨基乙酸甜菜碱、棕榈酸酰胺丙基二甲基氨基乙酸甜菜碱、硬脂酸酰胺丙基二甲基氨基乙酸甜菜碱以及油酸酰胺丙基二甲基氨基乙酸甜菜碱等酰胺甜菜碱型两性表面活性剂;椰子油脂肪酸二甲基磺基丙基甜菜碱等烷基磺基甜菜碱型两性表面活性剂;十二烷基二甲基氨基羟基磺基甜菜碱等烷基羟基磺基甜菜碱型两性表面活性剂;十二烷基羟基磷酸酯甜菜碱等磷酸酯甜菜碱型两性表面活性剂;N-月桂酰基-N’-羟乙基-N’-羧甲基乙二胺钠、N-油酰基-N’-羟乙基-N’-羧甲基乙二胺钠、N-椰油酰基-N’-羟乙基-N’-羧甲基乙二胺钠、N-月桂酰基-N’-羟乙基-N’-羧甲基乙二胺钾、N-油酰基-N’-羟乙基-N’-羧甲基乙二胺钾、N-月桂酰基-N-羟乙基-N’-羧甲基乙二胺钠、N-油酰基-N-羟乙基-N’-羧甲基乙二胺钠、N-椰油酰基-N-羟乙基-N’-羧甲基乙二胺钠、N-月桂酰基-N-羟乙基-N’,N’-二羧甲基乙二胺单钠、N-油酰基-N-羟乙基-N’,N’-二羧甲基乙二胺单钠、N-椰油酰基-N-羟乙基-N’,N’-二羧甲基乙二胺单钠、N-月桂酰基-N-羟乙基-N’,N’-二羧甲基乙二胺二钠、N-油酰基-N-羟乙基-N’,N’-二羧甲基乙二胺二钠以及N-椰油酰基-N-羟乙基-N’,N’-二羧甲基乙二胺二钠等酰胺氨基酸型两性表面活性剂。
作为半极性表面活性剂,可列举烷基氧化胺型表面活性剂、烷基氧化胺、烷基酰胺氧化胺、烷基羟基氧化胺等,优选使用碳原子数10~18的烷基二甲基氧化胺以及碳原子数8~18的烷氧乙基二羟乙基氧化胺等。具体可列举十二烷基二甲基氧化胺、二甲基辛基氧化胺、二乙基癸基氧化胺、双-(2-羟乙基)十二烷基氧化胺、二丙基十四烷基氧化胺、甲基乙基十六烷基氧化胺、十二烷基酰胺丙基二甲基氧化胺、十六烷基二甲基氧化胺、硬脂基二甲基氧化胺、牛油基二甲基氧化胺、二甲基-2-羟基十八烷基氧化胺、十二烷基二甲基氧化胺、肉豆蔻基二甲基氧化胺、硬脂基二甲基氧化胺、异硬脂基二甲基氧化胺、椰子脂肪酸烷基二甲基氧化胺、辛酸酰胺丙基二甲基氧化胺、癸酸酰胺丙基二甲基氧化胺、月桂酸酰胺丙基二甲基氧化胺、肉豆蔻酸酰胺丙基二甲基氧化胺、棕榈酸酰胺丙基二甲基氧化胺、硬脂酸酰胺丙基二甲基氧化胺、异硬脂酸酰胺丙基二甲基氧化胺、油酸酰胺丙基二甲基氧化胺、蓖麻油酸酰胺丙基二甲基氧化胺、12-羟基硬脂酸酰胺丙基二甲基氧化胺、椰子脂肪酸酰胺丙基二甲基氧化胺、棕榈仁油脂肪酸酰胺丙基二甲基氧化胺、蓖麻油脂肪酸酰胺丙基二甲基氧化胺、月桂酸酰胺乙基二甲基氧化胺、肉豆蔻酸酰胺乙基二甲基氧化胺、椰子脂肪酸酰胺乙基二甲基氧化胺、月桂酸酰胺乙基二乙基氧化胺、肉豆蔻酸酰胺乙基二乙基氧化胺、椰子脂肪酸酰胺乙基二乙基氧化胺、月桂酸酰胺乙基二羟乙基氧化胺、肉豆蔻酸酰胺乙基二羟乙基氧化胺以及椰子脂肪酸酰胺乙基二羟乙基氧化胺。
作为盐类,可列举无机盐、有机酸盐、胺盐及氨基酸盐。作为无机盐,例如可列举盐酸、硫酸、碳酸、硝酸等无机酸的钠盐、钾盐、镁盐、钙盐、铝盐、锆盐以及锌盐等;作为有机酸盐,例如可列举乙酸、脱氢乙酸、柠檬酸、苹果酸、琥珀酸、抗坏血酸以及硬脂酸等有机酸类盐;作为胺盐及氨基酸盐,例如可列举三乙醇胺等胺类盐以及谷氨酸等氨基酸类盐等。此外,除此之外,还能使用透明质酸、硫酸软骨素等盐,铝锆甘氨酸络合物等,以及化妆品处方中使用的酸-碱中和盐等。
作为保湿剂,可列举甘油、山梨醇、丙二醇、二丙二醇、1,3-丁二醇、葡萄糖、木糖醇、麦芽糖醇及聚乙二醇等多元醇类;透明质酸、硫酸软骨素、吡咯烷酮羧酸盐、聚氧乙烯甲基葡萄糖苷、聚氧丙烯甲基葡萄糖苷以及PEG/PPG二甲基醚等。
作为防腐剂,可列举对羟基苯甲酸烷基酯、苯甲酸、苯甲酸钠、山梨酸、山梨酸钙及苯氧乙醇等;作为抗菌剂,可列举苯甲酸、水杨酸、苯酚、山梨酸、对羟基苯甲酸烷基酯、对氯间甲酚、六氯酚、氯化苄烷铵、氯化氯己定、三氯碳酰替苯胺、三氯生、光敏剂及苯氧乙醇等,如果是口红,优选不配伍。
作为抗氧化剂,例如可列举生育酚、丁基羟基茴香醚、二丁基羟基甲苯及植酸等。
作为pH调节剂,例如可列举乳酸、柠檬酸、乙醇酸、琥珀酸、酒石酸、dl-苹果酸、碳酸钾、碳酸氢钠及碳酸氢铵等。
作为螯合剂,例如可列举丙氨酸、依地酸钠盐、聚磷酸钠、偏磷酸钠及磷酸等。
作为清凉剂,可列举L-薄荷醇及樟脑等;作为抗炎剂,可列举尿囊素、甘草次酸、甘草酸、氨甲环酸及薁等。
作为美肌成分,可列举胎盘提取液、熊果苷、谷胱甘肽及草莓虎耳草提取物等美白剂,蜂王浆等细胞赋活剂,皮肤粗糙改善剂,壬酸香草基酰胺、烟酸苄酯、烟酸β-丁氧基乙酯、辣椒碱、姜酮、斑蝥酊、鱼石脂、咖啡因、单宁酸、α-冰片、生育酚烟酸酯、烟酸肌醇酯、环扁桃酯、桂利嗪、妥拉苏林、乙酰胆碱、维拉帕米、千金藤素及γ-米谷酚等血液循环催化剂,氧化锌及单宁酸等紧肤剂,硫及THIANTROL等抗皮脂溢出剂等;作为维生素类,可列举维生素A油、视黄醇、视黄醇乙酸酯、视黄醇棕榈酸酯等维生素A类,核黄素、核黄素丁酸酯及黄素腺嘌呤核苷酸等维生素B2类,吡哆醇盐酸盐、二辛酸吡哆醇酯及三棕榈酸吡哆醇酯等维生素B6类,维生素B12及其衍生物,维生素B15及其衍生物等维生素B类;L-抗坏血酸、L-抗坏血酸二棕榈酸酯、L-抗坏血酸-2-硫酸钠及L-抗坏血酸磷酸二酯二钾等维生素C类;麦角骨化醇、胆骨化醇等维生素D类;α-生育酚、β-生育酚、γ-生育酚、乙酸dl-α-生育酚、烟酸dl-α-生育酚及琥珀酸dl-α-生育酚等维生素E类;维生素H、维生素P、烟酸及烟酸苄酯等烟酸类,以及泛酸钙、D-泛酰醇、泛酰基乙基醚及乙酰泛酰基乙基醚等泛酸类等。
作为氨基酸,可列举甘氨酸、缬氨酸、亮氨酸、异亮氨酸、丝氨酸、苏氨酸、苯基丙氨酸、精氨酸、赖氨酸、天冬氨酸、谷氨酸、胱氨酸、半胱氨酸、蛋氨酸及色氨酸等氨基酸以及/或者其盐。
作为核酸,可列举脱氧核糖核酸等;作为激素,可列举雌二醇及乙烯基雌二醇等。
生理活性成分是涂布于皮肤或毛发时对皮肤或毛发赋予某种生理活性的物质,可列举亲油性生理活性成分。例如,可列举抗炎剂、抗老化剂、收敛剂、生发剂、育发剂、保湿剂、血液循环催化剂、干燥剂、发热剂、维生素类、促进伤口愈合剂、刺激缓解剂、镇痛剂、细胞赋活剂及酶成分等。同样,还能适当地配伍天然系植物提取成分、海藻提取成分以及/或者生药成分。
医药有效成分是具有治疗疾病效果的物质,例如可列举蛋白质、肽及低分子化合物。
香料只要是亲油性香料,则无特别限定,可列举从各种植物的花、种子、叶或根等部位提取的香料、由海藻类提取的香料、由动物各部位或分泌物提取的香料(例如,麝香、龙涎香)以及人工合成的香料(例如,薄荷醇、麝香、乙酸酯、香草)。为了使化妆品具有香气、香味而配伍香料。色素包括油溶性染料、体质颜料、无机颜料、有机颜料及亲油性荧光增白剂等。
制造本发明的化妆品时,仅均匀地混合上述本发明的化妆品原料和其他化妆品原料,即可轻松制成。作为混合单元,可使用用于制造常规化妆品的各种混合装置、混炼装置。作为相关装置,例如可列举均匀混合器、桨叶式搅拌机、亨舍尔混合器、均质分散器、胶体研磨器、螺旋桨式搅拌器、均质机、连续式乳化器、超声波乳化器、真空混捏机。
以下,对本发明一实施方式的涂料进行详细说明。
本发明一实施方式的涂料特征在于,含有上述有机硅粒子。作为该涂料,可列举常温固化型、常温干燥型及加热固化型,另外,根据其性状,可列举水性、油性、粉状,进而,根据漆料的树脂,可列举聚氨酯树脂涂料、丁缩醛树脂涂料、长油性邻苯二甲酸树脂涂料、醇酸树脂涂料、由氨基树脂和醇酸树脂组成的氨基醇酸树脂涂料、环氧树脂涂料、丙烯酸树脂涂料、苯酚树脂涂料、有机硅改性环氧树脂涂料、有机硅改性聚酯树脂涂料、有机硅树脂涂料。
在该涂料中,上述有机硅粒子优选与涂料中的树脂具有亲和性或者反应性,例如,在以环氧树脂为漆料的涂料中,优选为具有环氧基或氨基的有机硅粒子,在以聚氨酯树脂或氨基树脂为漆料的涂料中,优选为具有氨基的有机硅粒子。
在该涂料中,上述有机硅粒子的含量并无限定,但为了使所获得的涂膜具有均匀且柔和的消光性,相对于涂料固体部分100质量份,优选在0.1~150质量份的范围内,更优选为0.1~100质量份的范围内,尤其优选为0.1~50质量份的范围内。
在该涂料中,除了上述有机硅粒子外,还可含有甲醇、乙醇等醇类;甲基乙基酮、甲基异丁基酮等酮类;乙酸乙酯、乙酸丁酯、乙二醇单乙醚乙酸酯等酯类;N,N-二甲基甲酰胺等酰胺;己烷、庚烷、辛烷等烯烃;甲苯、二甲苯等芳香族烃等有机溶剂;颜料、由高分子化合物组成的增稠剂、阻燃剂、耐候性赋予剂。
对上述有机硅粒子形成用交联性组合物的水分散液,或者对不含(C)成分的有机硅组合物的水分散液中添加(C)成分而制备的有机硅粒子形成用交联性组合物的水分散液,在室温下放置或者加热至100℃以下、优选70℃以下,从而能够促进分散于水中的有机硅粒子形成用交联性组合物的固化。
接着,从分散于水中的有机硅粒子形成用交联性组合物固化而获得的有机硅粒子的水分散液中除去水,从而能够回收有机硅粒子。关于回收有机硅粒子的方法,可列举对该有机硅粒子的水分散液进行加热或减压,或者热风干燥或风干等方法。并且,干燥前如果能对该水分散液进行过滤或以离心、盐析的方式进行分离,则能轻松地除去水分。
上述本发明的树脂用添加剂可对树脂赋予可挠性及耐热冲击性,因此,适宜作为环氧树脂、苯酚树脂等热固性树脂的添加剂,或者聚乙烯树脂、聚丙烯树脂、尼龙树脂、聚酯树脂等热塑性树脂的添加剂。
接着,对本发明一实施方式的电子材料进行详细说明。
本发明一实施方式的电子材料特征在于,含有上述有机硅粒子形成用交联性组合物。本发明一实施方式的电子材料的该有机硅粒子形成用交联性组合物的含量并无限定,相对于固化性树脂100重量份,优选为0.1~100重量份范围内。其原因在于,如果树脂用添加剂的含量低于上述范围的下限,则所获得的固化树脂的可挠性及耐热冲击性会降低,尤其是吸湿后的耐热冲击性会有降低的趋势;另一方面,如果超过上述范围的上限,则所获得的固化树脂的机械特性会有降低的趋势。
在本方面一实施方式的电子材料中,作为其主要成分即固化性树脂,可列举苯酚树脂、甲醛树脂、二甲苯树脂、二甲苯-甲醛树脂、酮-甲醛树脂、呋喃树脂、脲醛树脂、酰亚胺树脂、三聚氰胺树脂、醇酸树脂、不饱和聚酯树脂、苯胺树脂、磺酰胺树脂、有机硅树脂、环氧树脂、这些树脂的共聚树脂,可以组合这些固化性树脂两种以上。作为固化性树脂,尤其优选选自由环氧树脂、苯酚树脂、酰亚胺树脂及有机硅树脂所组成的群组中的至少一种。作为该环氧树脂,只要是含有缩水甘油基及脂环式环氧基的化合物即可,可列举邻甲酚酚醛型环氧树脂、联苯型环氧树脂、双酚A型环氧树脂、双酚F型环氧树脂、双环戊二烯型环氧树脂、萘型环氧树脂、蒽型环氧树脂、萘酚芳烷基型环氧树脂、聚乙烯苯酚型环氧树脂、二苯甲烷型环氧树脂、二苯基砜型环氧树脂、三酚烷烃型环氧树脂、甲酚-萘酚共缩合型环氧树脂、双苯基乙烯型环氧树脂、芴型环氧树脂、芪型环氧树脂、螺环苯并呋喃型环氧树脂、降冰片烯型环氧树脂、萜烯型环氧树脂、苯酚环己烷型环氧树脂、卤化环氧树脂、含酰亚胺基的环氧树脂、含马来酰亚胺基的环氧树脂、烯丙基改性环氧树脂、有机硅改性环氧树脂。此外,作为该苯酚树脂,可列举聚乙烯苯酚型、酚醛型、萘酚型、萜烯型、苯酚双环戊二烯型、苯酚芳烷基型、萘酚芳烷基型、三酚烷烃型、双环戊二烯型、甲酚-萘酚共缩合型、二甲苯-萘酚共缩合型。此外,作为有机硅树脂,可列举使环氧树脂和有机硅树脂中的硅醇基或硅原子键合烷氧基反应而成的环氧改性有机硅树脂。作为这种固化性树脂的固化机制,可列举热固化型、紫外线或放射线等高能量线固化型、湿气固化型、缩合反应固化型、加成反应固化型。另外,这种固化性树脂于25℃时的性状并无限定,可以为液状或通过加热而软化的固体状中的任一种。
此外,在本发明一实施方式的电子材料中,作为其他任意成分,还能配伍固化剂、固化促进剂、填充剂、光敏剂、高级脂肪酸金属盐、酯类蜡、增塑剂等。作为该固化剂,可列举羧酸或磺酸等有机酸及其酐;有机羟基化合物;具有硅醇基、烷氧基或卤素基的有机硅化合物;一级或二级氨基化合物,还能对这些固化剂组合两种以上。此外,作为该固化促进剂,可列举叔胺化合物、铝或锆等有机金属化合物;膦等有机磷化合物;除此之外,还可列举异环型胺化合物、硼络合物化合物、有机铵盐、有机锍盐、有机过氧化物、硅氢化用催化剂。另外,作为该填充剂,可列举玻璃纤维、石棉、氧化铝纤维、以氧化铝和二氧化硅为成分的陶瓷纤维、硼纤维、氧化锆纤维、碳化硅纤维、金属纤维、聚酯纤维、芳纶纤维、尼龙纤维、苯酚纤维、天然动植物纤维等纤维状填充剂;熔融二氧化硅、沉淀二氧化硅、气相二氧化硅、热解二氧化硅、氧化锌、焙烧粘土、碳黑、玻璃珠、氧化铝、滑石粉、碳酸钙、粘土、氢氧化铝、硫酸钡、二氧化钛、氮化铝、碳化硅、氧化镁、氧化铍、高岭土、云母、二氧化锆等粉粒体状填充剂,还能对这些填充剂组合两种以上使用。
进而,本发明的有机硅粒子配伍到树脂中时,应力缓和作用优异,因此,可以配伍到印刷电路板用环氧树脂等,形成预浸料,再使铜箔的一面具备含有本发明有机硅粒子的树脂层,形成印刷电路板用的带含填充剂粒子树脂层的铜箔,用于覆铜箔层压板(CCL)用途。
实施例
通过实施例及比较例,对本发明的有机硅粒子及其制造方法进行详细说明。但本发明并不仅限定于这些实施例。实施例中的粘度是25℃时的值。另外,按照以下方式测定了有机硅粒子的特性。
[固化有机硅粒子的JIS A硬度]
利用加热烘箱,以150℃对作为固化有机硅粒子原料的固化性有机硅组合物加热1小时,固化成薄片状。用JIS K 6253规定的JIS A硬度计测定其硬度。
[固化有机硅粒子的SiH残存量]
相对于固化有机硅粒子,按单位质量计算,添加等量的40%浓度氢氧化钾乙醇溶液,静置1小时,捕集反应终点前所产生的氢气,并利用顶空气相色谱法测定捕集到的氢气产生量,测定单位质量的硅原子键合氢原子的残存量(ppm)。
[一次粒子的平均粒径]
利用激光衍射粒度分布仪(贝克曼库尔特公司的LS-230)对添加铂催化剂前的乳液进行测定,将其中位粒径(相当于累计分布50%的粒径,50%粒径)作为平均粒径。
[粉末粒径]
以乙醇为分散介质,利用激光衍射粒度分布仪(堀场制作所LA-500)测定固化有机硅粒子的粒径,获得乙醇中的固化有机硅粒子的中位粒径(相当于累计分布50%的粒径,D90,μm)及算术分散度(表示粒径分布的分散程度,SD,μm2)值。对于测定试样,使用搅拌叶片及超声波振动机,使固化有机硅粒子(1g)和乙醇(100mL)分散于300mL杯子中。
[混合液粘度的测定方法]
计量固化有机硅粒子(6g)和十甲基环五硅氧烷(58g)到300mL杯子中,用分散器以4000rpm搅拌2分钟。之后,用BM型旋转粘度计(东机产业公司制)在转子No.2、60rpm的条件下,将1分钟后的值设为粘度。
[粉末吸油量的测定方法]
将固化有机硅粒子5g放入100ml烧杯中,用玻璃棒缓慢地搅拌固化有机硅粒子,同时一滴滴地滴加角鲨烷、鲸蜡醇乙基己酸酯(注1)、矿油(注2)或者十甲基环五硅氧烷(注3),计算固化有机硅粒子和油变为均匀的浆糊状物所需的油滴加量。将油滴加量相对于固化有机硅粒子的比例设为有机交联粒子的吸油量(重量百分比)。
注1:高级醇工业公司制CEH
注2:KANEDA株式会社制HICALL K-230
注3:东丽道康宁公司制SH245
实施例、比较例中使用的成分(A)和成分(B)的平均式列举如下。
在以下式子中,Vi表示CH2=CH-,Me表示CH3-,He表示CH2=CH-C4H8-。
[化学式1-1]
Me2HeSiO-(Me2SiO)135-(MeHeSiO)0.25-SiHeMe2,
烯基含有率为0.97wt%。粘度为420mPa·s。
[化学式2-2]
ViMe2SiO-(Me2SiO)150-Me2Si-Vi,
烯基含有率为0.47wt%。粘度为360mPa·s。
[化学式3-3]
ViMe2SiO-(Me2SiO)130-(ViMeSiO)2-Me2Si-Vi
烯基含有率为1.08wt%。粘度为370mPa·s。
[化学式4-4]
1,5-己二烯(分子量=82.15)东京化成工业公司制
[化学式2-1]
Me3SiO-(Me2SiO)33.7-(HMeSiO)11.5-SiMe3,
硅原子键合氢原子含量为0.44wt%。粘度为50mPa·s。
[化学式2-2]
(Me3SiO1/2)2(Me2SiO2/2)7(HMeSiO2/2)11(MeSiO3/2)1,
硅原子键合氢原子含量为0.825wt%。粘度为15mPa·s。
[化学式2-3]
HMe2SiO-(Me2SiO)60-Me2SiH。
硅原子键合氢原子含量为0.043wt%。粘度为64mPa·s。
[实施例1]
按照表1中所列举的配伍量,在室温下将[化学式1-1]的平均式所表示的聚有机硅氧烷和[化学式2-1]的平均式所表示的聚有机硅氧烷均匀混合。接着,将该组合物分散于由聚氧乙烯烷基(C12-14)醚0.4质量份和纯水50质量份所组成的25℃水溶液中,再用胶体研磨器均匀地乳化后,加入纯水350质量份进行稀释,制备乳液。然后,用聚氧乙烯烷基(C12-14)醚和纯水将氯铂酸的异丙醇溶液(本组合物中,按质量单位计,铂金属为10ppm的量)制成水分散液,加入到乳液中并搅拌,然后以50℃静置该乳液3小时,制备硅橡胶粒子的均匀水系悬浮液。继而,用小型喷雾干燥器(Ashizawaniro公司制)干燥该水系悬浮液,获得有机硅粒子。其特性如表1所示。
[实施例2]~[实施例4]、[比较1]、[比较例2]
按表1记载的配伍组成,在室温下将表1中所列举的原料均匀混合,制备有机硅粒子形成用交联性组合物。然后,按照实施例1所述的方式对该组合物进行处理,获得有机硅粒子。其特性如表1所示。
表1
以下所示为能够配伍本发明一实施方式的有机硅粒子的本发明的化妆品处方例。但本发明并不限定于此。
处方例1:W/O粉底霜
(成分)
相A
十六烷基二甘油基三(三甲硅氧基)硅乙基聚二甲基硅氧烷
(注1)5.0质量份
2)聚二甲基硅氧烷(注2)4.2质量份
3)甲氧基肉桂酸乙基己酯(注3)3.3质量份
4)辛基聚甲基硅氧烷(注4)3.3质量份
5)异十二烷、(聚二甲基硅氧烷/双-异丁基PPG-20)交联聚合物(注5)1.5质量份
6)实施例的有机硅交联物2.0质量份
相B
7)氧化钛、滑石粉、聚甲基硅氧烷(注6)4.71质量份
8)云母、氢氧化铝(注7)2.46质量份
9)氧化铁黄(注8)0.66质量份
10)氧化铁红(注9)0.16质量份
11)氧化铁黑(注10)0.006质量份
12)十六烷基二甘油基三(三甲硅氧基)硅乙基聚二甲基硅氧烷(注11)0.5质量份
13)辛基聚甲基硅氧烷(注12)3.7质量份
相C
14)精制水61.5质量份
15)BG 8.0质量份
16)氯化钠1.0质量份
注1:东丽道康宁公司制ES-5600 Silicone Glycerol Emulsfier
注2:东丽道康宁公司制PMX-200 SILICONE FLUID 2CS
注3:Symrise公司制Neo Heliopan AV
注4:东丽道康宁公司制FZ-3196
注5:东丽道康宁公司制EL-8050 ID Silicone Organic Elastomer Blend
注6:三好化成公司制SA Titan CR-50
注7:三好化成公司制SA Exel Mica JP-2
注8:三好化成公司制SA Yellow UXLO
注9:三好化成公司制SA Red
注10:三好化成公司制SA Black
注11:东丽道康宁公司制ES-5600 Silicone Glycerol Emulsifier
注12:东丽道康宁公司制FZ-3196
按照以下步骤调制处方例1的W/O粉底霜。
1.混合成分1~6至均匀。
2.对成分7~13进行三辊混合。
3.混合成分14~16。
4.混合上述1和2。
5.用力搅拌上述4,同时加入上述3,使其乳化。
处方例2:O/W粉底
(成分)
相A
1)实施例的有机硅交联物18质量份
2)滑石粉(注1)18质量份
相B
3)精制水20质量份
4)甘油10质量份
相C
5)聚丙烯酸钠、聚二甲基硅氧烷(注2)1质量份
6)DMDM乙内酰脲、碘丙炔醇丁基氨甲酸酯(注3)适量
7)水杨酸乙基己酯(注4)3质量份
8)甲氧基肉桂酸乙基己酯(注5)3质量份
相D
9)精制水21质量份
相E
10)辛基聚甲基硅氧烷(注6)2质量份
11)氧化铁黑、聚二甲基硅氧烷(注7)0.05质量份
12)氧化铁红、聚二甲基硅氧烷(注8)0.1质量份
13)氧化铁黄、聚二甲基硅氧烷(注9)0.25质量份
14)氧化钛、滑石粉、聚二甲基硅氧烷(注10)3.6质量份
注1:三好化成公司制Si滑石粉
注2:东丽道康宁公司制RM 2051 Rheology Modifier
注3:Lonza公司制Glydant Plus
注4:Symrise公司制Neo Heliopan OS
注5:ISP公司制Escalol 557
注6:东丽道康宁公司制FZ-3196
注7:三好化成公司制SA-BLACK BL-100
注8:三好化成公司制SA-BENGALA七宝
注9:三好化成公司制SI-YELLOW-LLXLO
注10:三好化成公司制SI-钛CR-50
按照以下步骤调制处方例2的O/W粉底霜。
1.混合成分1和2。
2.混合成分3和4。
3.混合上述1和2。
4.混合成分5~8。
5.将成分9加入上述4中并混合。
6.混合成分10~14至均匀。
7.混合全部成分。
处方例3:W/O
BB霜
(成分)
相A
1)月桂基PEG-10三(三甲硅氧基)硅乙基聚二甲基硅氧烷(注1)3质量份
2)辛基聚甲基硅氧烷(注2)14质量份
3)甲氧基肉桂酸乙基己酯(注3)7.5质量份
4)二乙氨羟苯甲酰基苯甲酸己酯(注4)1.5质量份
5)水杨酸乙基己酯2.5质量份
6)三甲基硅烷氧基硅酸酯、聚丙基硅倍半氧烷(注5)2质量份
7)实施例的有机硅交联物4质量份
8)苯基聚三甲基硅氧烷(注6)4质量份
相B
9)甘油8质量份
10)氯化钠0.7质量份
11)精制水40.8质量份
相C
12)氧化钛5.6质量份
13)氧化铁黄(注7)0.25质量份
14)氧化铁红(注8)0.1质量份
15)氧化铁黑(注9)0.05质量份
16)苯基聚三甲基硅氧烷(注10)5.2质量份
17)氧化锌(注11)0.8质量份
18)月桂基PEG-10三(三甲硅氧基)硅乙基聚二甲基硅氧烷1质量份
注1:东丽道康宁公司制ES-5300 Formulation Aid
注2:东丽道康宁公司制FZ-3196
注3:BASF公司制Uvinul MC80N
注4:BASF公司制Uvinul A Plus Glanular
注5:东丽道康宁公司制MQ-1640 Flake Resin
注6:东丽道康宁公司制SH556
注7:三次化成公司制SA-IOY-8
注8:三次化成公司制SA-IOR-8
注9:三次化成公司制SA-IOB-8
注10:东丽道康宁公司制SH556
注11:堺化学工业公司制FINEX-30S-LPT
注12:东丽道康宁公司制ES-5300Formulation Aid
按照以下步骤调制处方例3的W/O BB霜。
1.混合成分1~8。(先溶解UV吸收剂,然后使MQ-1640溶解于FZ-3196中)
2.混合成分9~11。
3.混合成分12~18。
4.混合上述1和3。
5.用力搅拌上述1,同时缓慢地加入上述2,使其乳化。
处方例4:非水粉底
(成分)
相A
1)氧化钛、聚二甲基硅氧烷(注1)49.23质量份
2)氧化铁黄、聚二甲基硅氧烷(注2)9.86质量份
3)氧化铁红、聚二甲基硅氧烷(注3)1.97质量份
4)氧化铁黑、聚二甲基硅氧烷(注4)0.55质量份
5)十六烷基二甘油基三(三甲硅氧基)硅乙基聚二甲基硅氧烷(注5)1.58质量份
6)辛基聚甲基硅氧烷(注6)15.8质量份
相B
7)实施例的有机硅交联物2质量份
8)环五硅氧烷(注7)13质量份
9)异十二烷、丙烯酸(酯)类/聚三甲基硅氧烷甲基丙烯酸酯共聚物(注8)5质量份
10)二硬脂二甲铵锂蒙脱石(注9)1质量份
注1:三好化成公司制SI-钛CR-50
注2:三好化成公司制SI-YELLOW-LLXLO
注3:三好化成公司制SA-BENGALA七宝
注4:三好化成公司制SA-BLACK BL-100
注5:东丽道康宁公司制ES-5600 Silicone Glycerol Emulsifier
注6:东丽道康宁公司制FZ-3196
注7:东丽道康宁公司制SH245
注8:东丽道康宁公司制FA 4002 ID Silicone Acrylate
注9:Elementis公司制38 V CG
按照以下步骤调制处方例4的非水粉底。
1.混合成分1~6。
2.混合成分7~10。
3.混合上述1和2。
处方例5:粉饼
(成分)
1)滑石粉(注1)20质量份
2)云母(注2)34.6质量份
3)氧化钛(注3)10质量份
4)氧化铁红(注4)1质量份
5)氧化铁黄(注5)4质量份
6)氧化铁黑(注6)0.4质量份
7)云母(注7)15质量份
8)聚苯乙烯(注8)5质量份
9)角鲨烷3质量份
10)辛基十二醇肉豆蔻酸酯(注9)1.2质量份
11)凡士林2.5质量份
12)聚二甲基硅氧烷(注10)3.3质量份
13)实施例的有机硅交联物5质量份
注1:三好化成公司制SI Talc
注2:三好化成公司制SI-SERICITE FSE
注3:三好化成公司制SI-Titan CR-50
注4:三好化成公司制SA Red
注5:三好化成公司制SA Yellow UXLO
注6:三好化成公司制SA Black
注7:三好化成公司制SA-Excel MicaJP-2
注8:住友化学公司制Fine pearl 3000SPQ
注9:花王公司制EXCEPARL OD-M
注10:东丽道康宁公司制SH200-5000cs
按照以下步骤调制处方例5的粉饼。
1.混合上述全部成分。
处方例6:W/O护肤霜
(成分)
相A
1)月桂基PEG/PPG-18/18聚二甲基硅氧烷(注1)2质量份
2)双-羟乙氧丙基聚二甲基硅氧烷(注2)2质量份
3)棕榈酸异丙酯(注3)1质量份
4)环五硅氧烷(注4)6.5质量份
5)矿油(注5)10质量份
6)凡士林1.5质量份
7)实施例的有机硅交联物5质量份
相B
8)甘油5质量份
9)氯化钠1质量份
10)精制水66质量份
注1:东丽道康宁公司制5200 Formulation Aid
注2:东丽道康宁公司制5562 Carbinol Fluid
注3:花王公司制EXEPARL IPM
注4:东丽道康宁公司制SH245
注5:KANEDA公司制HICALL K-230
按照以下步骤调制处方例6的W/O护肤霜。
1.混合成分1~7。
2.混合成分8~10。
3.用力搅拌上述1,同时缓慢地加入上述2,使其乳化。
处方例7:非水防晒乳
(成分)
1)氧化锌(注1)6质量份
2)月桂基PEG-10三(三甲硅氧基)硅乙基聚二甲基硅氧烷(注2)0.5质量份
3)十六烷3.5质量份
4)甲氧基肉桂酸乙基己酯(注3)7.5质量份
5)聚二甲基硅氧烷、聚二甲基硅氧烷交联聚合物(注4)24质量份
6)环五硅氧烷(注5)60.5质量份
7)实施例的有机硅交联物2质量份
注1:堺化学公司制FINEX-30S-LPT
注2:东丽道康宁公司制ES-5300 Formulation Aid
注3:BASF公司制Uvinul MC80N
注4:东丽道康宁公司制9041 Silicone Elastomer Blend
注5:东丽道康宁公司制SH245
按照以下步骤调制处方例7的非水防晒乳。
1.混合成分1~3(珠磨机等)。
2.对上述成分加入成分4~7,搅拌至均匀。
处方例8:O/W抗皱护理霜
(成分)
相A
1)环五硅氧烷(注1)11质量份
2)有机硅交联物10质量份
3)月桂基PEG/PPG-18/18聚二甲基硅氧烷(注2)0.5质量份
4)PEG-12聚二甲基硅氧烷(注3)4质量份
相B
5)精制水72.5质量份
相C
6)聚丙烯酰胺、水、(C13,14)异构烷烃、月桂醇醚-7(注4)2质量份
注1:东丽道康宁公司制SH245
注2:东丽道康宁公司制5200 Formulation Aid
注3:东丽道康宁公司制OFX-5329
注4:SEPPIC S.A.公司制Simulgel 305
按照以下步骤调制处方例8的O/W抗皱护理霜。
1.混合成分1~4至均匀。
2.混合成分4和5至均匀。
3.对上述2加入1,混合至均匀。
工业上的实用性
本发明的有机硅粒子在乙醇、硅油中的分散性优异,容易作为添加剂进行配伍,作为化妆品原料配伍到化妆品中时,能够提高其触感,因此,能够用于皮肤化妆品、彩妆化妆品等。并且,关于利用其物性,将本发明的有机硅粒子应用到电子材料的情况,还能用于热固性树脂组合物、热塑性树脂组合物等的添加剂或者塑料薄膜的表面润滑剂。
Claims (7)
1.一种有机硅粒子的制造方法,其使交联性组合物发生乳化,在催化剂存在的条件下使所述交联性组合物固化;
其中,所述交联性组合物含有以下(A)成分及(B)成分:
(A):一分子中具有2个以上碳原子数在4以上且20以下的烯基的有机聚硅氧烷,
(B):一分子中存在的硅原子键合氢原子为2个以上,且为一分子中硅原子数的40%以下的硅有机化合物,以及/或者
一分子中存在的硅原子键合氢原子为2个以上,含有三官能度硅氧烷单元或四官能度硅氧烷单元的硅有机化合物;
并且,(A)成分的烯基含量(Alk)和(B)成分的硅原子键合氢原子含量(H)的摩尔比为
H/Alk=0.9~1.1;
通过所述方法制备的有机硅粒子中,单位质量的硅原子键合氢的含量为20ppm以下。
2.根据权利要求1所述的方法,其中,(A)成分中的所述烯基的碳原子数在4以上、12以下。
3.根据权利要求1所述的方法,其中,(B)成分包含一分子中存在的硅原子键合氢原子为2个以上,且为一分子中硅原子数的40%以下的硅有机化合物。
4.根据权利要求1所述的方法,其中,(B)成分包含一分子中存在的硅原子键合氢原子为2个以上,含有三官能度硅氧烷单元或四官能度硅氧烷单元的硅有机化合物。
5.根据权利要求1所述的方法,其中,通过所述方法制备的有机硅粒子中,根据激光衍射散射法测定的粉末粒径为1~50μm。
6.根据权利要求1所述的方法,其中,将所述交联性组合物固化为薄片状而测定的JIS-A硬度在70以下。
7.根据权利要求1所述的方法,其中,将所述交联性组合物固化为薄片状而测定的JIS-A硬度(Vα)及根据激光衍射散射法测定的粉末粒径(Vβ)μm满足以下关系:
Vα×Vβ≤1,200。
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CN111757917B (zh) | 2018-03-27 | 2022-06-03 | 陶氏东丽株式会社 | 含油剂的硅酮弹性体粒子以及化妆料组合物等用途 |
WO2020036063A1 (ja) * | 2018-08-15 | 2020-02-20 | ダウ・東レ株式会社 | 化粧料 |
US20220073684A1 (en) * | 2018-12-27 | 2022-03-10 | Dow Toray Co., Ltd. | Silicone resin-coated silicone elastomer particles, and applications thereof including organic resin additives |
CN111393863B (zh) * | 2020-04-14 | 2022-02-18 | 四川路友交通物资发展有限公司 | 一种橡胶粉改性沥青及其制备方法 |
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JP2023007034A (ja) * | 2021-07-01 | 2023-01-18 | 信越化学工業株式会社 | シリコーンゴム球状粒子用液状組成物、シリコーンゴム球状粒子およびその製造方法、およびシリコーン複合粒子およびその製造方法 |
KR102644636B1 (ko) * | 2021-08-09 | 2024-03-06 | 계명대학교 산학협력단 | 불소실리콘 코팅용액 제조방법 및 이에 의해 제조된 코팅용액 |
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KR102365802B1 (ko) | 2022-02-24 |
CN109153790B (zh) | 2024-02-20 |
US11643505B2 (en) | 2023-05-09 |
EP3453736A1 (en) | 2019-03-13 |
US20190144612A1 (en) | 2019-05-16 |
JP6949831B2 (ja) | 2021-10-13 |
JPWO2017191798A1 (ja) | 2019-03-07 |
CN114349987A (zh) | 2022-04-15 |
US10988580B2 (en) | 2021-04-27 |
US20210198432A1 (en) | 2021-07-01 |
CN109153790A (zh) | 2019-01-04 |
WO2017191798A1 (ja) | 2017-11-09 |
KR20190004720A (ko) | 2019-01-14 |
EP3453736A4 (en) | 2019-11-20 |
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