CN113613626B - 水性香水组合物 - Google Patents
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Abstract
根据本发明的减少乙醇的香水组合物包含在水性基质或递送媒介物中的丙烯酸酯/VA共聚物和丙烯酸酯共聚物的特定组合。根据本发明的香水组合物易于制造并提供保持芳香完整性(强度、持久性和香域)的水性香水组合物,甚至呈乳液形式。本发明的组合物的最有利的用途是作为香精、淡香精、淡香水和古龙水。然而,本发明还可用于许多类型的加香产品(例如在人类或动物的皮肤和毛发上使用的那些)、所有类型的清洁产品、空气除臭剂、空气清新剂等。
Description
技术领域
本发明属于香料组合物领域,更具体地涉及液体水性香水组合物。
背景技术
绝大多数液体香水组合物使用醇(通常乙醇)作为常以芳香油的形式包含在组合物中的芳香成分的增溶剂。常见的是乙醇浓度在50体积%至95体积%之间的产品。乙醇增溶剂的使用提供透明的香水组合物。然而,使用乙醇有其缺点。这些缺点包括但不限于急性接触性皮炎。此外,乙醇被归类为挥发性有机化合物(VOC)。一段时间以来,人们一直在努力减少周围环境中VOC的水平。在出于宗教原因而严格管制或禁止醇的使用的文化中,其它缺点是明显的。
人们已努力从香水产品减少或消除醇。例如,已知水基香水产品,但由于与性能和美学相关的原因,这些产品尚未获得广泛的接受。一个问题在于加香成分因其疏水性而倾向于不溶于水。已经尝试通过形成乳液组合物来解决此问题。参见例如US4,803,195、US5,374,614、US6,403,109、US6,774,101、US2003/0186836、US2004/0209795、US7,226,901、US7,655,613、US7,846,889、US 8,343,521、US9,301,910。然而,许多乳液香水组合物具有其自身的缺点。例如,使用太多的表面活性剂会导致皮肤刺激、发粘感,并改变对芳香成分的感觉。对于使用相对高浓度的表面活性剂的微乳液组合物,情况尤其如此,但粗乳液和纳米乳液也可能遭遇同样的问题。结果,水基香水组合物通常未能提供与传统的乙醇基香料相同的强度、持久性和香域。关于强度的损失,我们指的是水基香料的香气倾向于比传统香水弱。关于下降的持久性,我们指的是人鼻可感知水基香水组合物的时间比传统的乙醇基香水组合物显著更短。香域,如本文所用,有时被称为嗅觉线性。关于香域的损失,我们指的是在施用于皮肤或其它表面后,不保持水基香水组合物所散发的融合香调,甚至当仍能感知到一些香料时。因此,仍需要具有相对较少的乙醇但仍保持芳香完整性(强度、持久性和香域)的水基香水组合物。本发明提供了乳液形式的此类组合物。据我们所知,现有技术未公开或提出本发明的组合物,特别是如本文所公开按重量计包含4.5%至18.5%的丙烯酸酯/VA共聚物和0.25%至1.0%的丙烯酸酯共聚物的水基香水组合物。现有技术未公开如本文所公开的这些材料的比率,也未公开它们在保持香水组合物的性能方面的有用性。
发明内容
根据本发明的减少乙醇的香水组合物包含在水性基质或递送媒介物中的丙烯酸酯/VA共聚物和丙烯酸酯共聚物的特定组合。根据本发明的香水组合物易于制造并提供保持芳香完整性(强度、持久性和香域)的水性香水组合物,甚至呈乳液形式。本发明的组合物的最有利的用途是作为香精、淡香精、淡香水和古龙水。然而,本发明还可用于许多类型的加香产品(例如在人类或动物的皮肤和毛发上使用的那些)、所有类型的清洁产品、空气除臭剂、空气清新剂等。
具体实施方式
除在操作和对比实例中,或另有明确指出外,本说明书中所有表示材料或反应条件的量或比率、材料的物理性质和/或用途的数字均应理解为受词语“约”修饰。除非另有指出,否则所有的量均以最终组合物的重量百分数呈现。
在整个说明书中,“成膜剂”等是指例如在伴随成膜剂的溶剂蒸发、吸收到基材中和/或在基材上消散后,在施用其的基材上留下膜的聚合物。
“包含”指的是要素的列表可不限于明确列举的那些。
“乳液”指的是在一种或多种表面活性剂的促进下不连续相(或内相)在连续相(或外相)中的稳定分散(水包油或油包水)。为清楚起见,我们提供了个人护理领域中常见的三种主要乳液类型的定义。
粗乳液(常简称为“乳液”)是一种各向异性的两相体系,其动力学稳定但热力学不稳定,这意味着它们需要高的能量输入以形成分散在连续相中的液滴。关于内相中液滴的特征尺寸,文献提出了许多定义。国际纯粹与应用化学联合会(IUPAC)推荐10nm-100µm。这些液滴结构因凝聚和从连续相分离而随时间自然降解,但降低油水界面处表面张力的表面活性剂可延长粗乳液的寿命。
微乳液(有时称为胶束乳液)与粗乳液显著不同。微乳液是水、油和相对高浓度的表面活性剂的各向同性单相体系。微乳液是热力学稳定的,这意味着它们通过简单的低能混合而自发形成。内相结构是动态的、不断变化的形状,但尺寸范围通常为约1nm-100nm(IUPAC)。由于这种小的颗粒尺寸,微乳液通常是半透明的。
还不同的是纳米乳液(也称为细乳液或亚微乳液)。类似粗乳液,纳米乳液是两相体系,其中不连续相的液滴分散在连续相中。然而,纳米乳液的平均液滴尺寸可在直径50nm至1000nm(IUPAC)的范围内。在该范围的下端的纳米乳液是半透明的,因为液滴尺寸低于可见光的波长。纳米乳液是动力学稳定的,但热力学不稳定,必须通过表面活性剂保持在一起。它们可通过高能乳化方法形成,如用均质器或超声剪切。或者,存在相转化方法,其需要的能量非常少。
水
本发明的组合物包含水,通常占总组合物的重量的30%至70%的水,而预期50%至60%是常见的。此量的水是来自所有来源的水,如下面讨论的Vinysol 2140L和Daitosol5000AD中的水。
丙烯酸酯/VA共聚物
本发明的主要成分为丙烯酸酯/VA共聚物(INCI名称)C15H26O4,也称为乙酸乙烯酯或丙-2-烯酸2-乙基己酯(IUPAC名称);CAS号25067-02-1。有关详细信息,参见PubChem化合物数据库;CID = 168269。
在化妆品中,这种材料常用作粘结剂、成膜剂、粘合剂和/或毛发定型剂。当在水性化妆品体系中采用时,丙烯酸酯/VA共聚物可在皮肤或毛发上赋予膜。纯丙烯酸酯/VA共聚物膜具有温度依赖性的特征,使得约40℃或更高温度的水冲洗会降解膜,并允许其从表面去除,而在正常皮肤温度(即,36.5-37.5℃)或低于此的温度下保持其完整性。
本发明的香水组合物通常包含组合物的总重量的4.5%至18.5%的丙烯酸酯/VA共聚物,例如,组合物的总重量的7%至16%,例如9%至14%。
丙烯酸酯/VA共聚物可商购获得,例如从Daido Chemical Corp.以Vinysol 2140L商购获得。Vinysol 2140L为丙烯酸酯/VA共聚物的46.6%水性混合物。因此,在使用Vinysol2140L时,为了达到上述丙烯酸酯/VA共聚物的浓度,Vinysol 2140L的浓度应为组合物总重量的约10%至40%,例如15%-35%,例如20%-30%。据报道,Vinysol 2140L的pH为4.5,粘度为2,000 mPa-s,计算的玻璃化转变温度(Tg)为-9℃,同时膜的断裂伸长率为1,200%,和断裂强度为1.2MPa(当铺展到厚度0.1mm时)。
丙烯酸酯共聚物
本发明的另一主要成分为丙烯酸酯聚合物,其具有比丙烯酸酯/VA共聚物低的Tg。通常,较低的Tg为所得的膜提供更大的柔韧性。在本发明中,第二主要成分为丙烯酸酯共聚物C14H22O6,也称为丙-2-烯酸乙酯、2-甲基丙-2-烯酸甲酯或2-甲基丙-2-烯酸(IUPAC名称);CAS号25133-97-5。有关详细信息,参见PubChem化合物数据库;CID = 168299。在各种类型的化妆品制剂中,丙烯酸酯共聚物具有广泛的用途,包括作为成膜剂、毛发定型剂、粘结剂和悬浮剂、增粘剂、抗静电剂和粘合剂。在本文讨论的浓度下,丙烯酸酯/VA共聚物与丙烯酸酯共聚物的组合形成有用的水溶性复合物,当施加到表面时,其干燥成疏水膜。
在本发明中,基于组合物的总重量计,丙烯酸酯共聚物的可用浓度为0.25%至1.0%;例如0.35%至0.8%,或例如0.5%至0.7%。另外,当丙烯酸酯/VA共聚物与丙烯酸酯共聚物的重量比在10:1至30:1、优选地15:1至25:1的范围内、更优选地为约20:1时,我们已注意到特别好的结果。
丙烯酸酯共聚物可商购获得,例如从Daito Kasei Kogyo Co.以Daitosol 5000AD商购获得。Daitosol 5000AD是丙烯酸酯共聚物的50%水性混合物。因此,为了达到上述丙烯酸酯共聚物的浓度,Daitosol 5000AD的浓度应为组合物总重量的约0.5%至2%,例如0.7%至1.6%,例如1.0%至1.4%。据报道,Daitosol 5000AD的pH为5.5-7.5,粘度为50-100 mPa-s,玻璃化转变温度(Tg)为约-14℃。
增塑剂
虽然可以在不进一步改性丙烯酸酯/VA共聚物-丙烯酸酯共聚物复合物的情况下配制根据本发明的水性香水组合物,但优选的组合物可在水相中包含一种或多种能够增塑丙烯酸酯/VA共聚物的材料。这样的增塑剂将降低最终组合物的凝固点至适合于商业流通和消费者使用的温度。此外,在将香水组合物施用于表面时,这样的增塑剂将改变由丙烯酸酯/VA共聚物-丙烯酸酯共聚物复合物产生的膜的孔隙率。通常,在本文考虑的范围内,水相中更多的增塑剂倾向于增加丙烯酸酯/VA共聚物-丙烯酸酯共聚物膜中存在的表面孔隙的尺寸。控制该孔隙尺寸是控制作为时间的函数的芳香的释放以及保持组合物中加香成分的完整性的关键。在每种特定的组合物中,常规实验可表明增塑剂的最佳用量。然而,作为指导,我们发现约1:1的丙烯酸酯/VA共聚物与增塑剂的重量比给出极好的结果。我们注意到,较少的增塑剂也可给出有用的结果,例如5:1或甚至10:1重量的丙烯酸酯/VA共聚物比增塑剂。由于丙烯酸酯/VA共聚物的浓度为4.5重量%至18.5重量%,因此全部增塑剂将不超过总组合物的约4.5重量%。
可用的增塑剂包括二醇,也称为二元醇(包含两个羟基的化合物)。潜在合适的二醇包括丁二醇、丙二醇和戊二醇。优选的是1,3-丙二醇。
其它可用的增塑剂是简单的化妆品级醇(例如,乙醇或异丙醇),其量至多为最终组合物的约5重量%。虽然最优选无醇组合物,但5%相对于常规香料组合物中通常发现的量大幅减少。二醇或醇可单独使用或组合使用,其总量与上述丙烯酸酯/VA共聚物与增塑剂的重量比一致。
芳香成分
芳香成分包括一种或多种精油、馏出物、提取物、合成物以及为赋予气味或香味的唯一目的或者为抵消气味而添加的其它成分。取决于香水产品的类型,芳香成分的水平通常从最终香水组合物的约3重量%至约30重量%变化。大多数芳香成分是疏水性的,并将形成油相的一部分或全部。精油是花、草、根或树脂的纯净蒸馏物,而“香料油”通常是指合成的芳香成分的共混物或精油馏分与载体油的共混物。例如,一种或多种精油或者一种或多种香料油或者它们的组合可形成油相的大部分或全部。或者油相可包含分散在化妆品可接受的油中的其它芳香成分。
其它成分
香水组合物还可根据需要包含防腐剂,其通常至多为组合物的约2重量%。同样,可根据需要使用粘度调节剂和/或pH调节剂来产生消费者可接受的产品,其水平通常小于组合物的1重量%。在这些水平下,防腐剂、粘度调节剂和pH调节剂似乎不会不利地影响香水组合物的芳香完整性。组合物包含不大于5重量%的醇,优选小于3%,更优选不包含醇。
香水组合物的形式
本发明优选的液体香水组合物具有似水的稠度,并适合从机械喷雾泵或喷雾器分配。所述组合物为水包油乳液,但与先前的水基香水产品不同,本文公开的组合物能够使用少得多的乳化剂和/或表面活性剂,这将大大(如果不是完全的话)消除由使用高水平的这些成分而引入的问题。基于组合物的总重量计,优选香水组合物包含不大于5重量%的表面活性剂和/或乳化剂,更优选小于3%,还更优选小于1%。实施例1示出了本发明的有效的水包油粗乳液组合物。相1为连续的水相。相2为不连续的油相。在此实施例中,并优选地,在形成乳液之后添加丙烯酸酯/VA共聚物和丙烯酸酯共聚物。然而,如果将其加到水相,则也将获得有效的组合物。
1 水96.70% / 黄原胶3.10% / 防腐剂0.20%。
2 丙烯酸酯/VA共聚物的46.6%水性混合物。
3 丙烯酸酯共聚物的50%水性混合物。
组合物使用如下冷混合法:
1. 在合适的烧杯中用均质器预混合黄原胶阶段,直至均匀。
2. 在主烧杯中按所列顺序添加序列1成分,均质器速度设置为10。
3. 在所有序列1进入主烧杯中后再混合10分钟。
4. 向主烧杯中加入序列2,均质器速度设置为30。
5. 混合30分钟。
6. 在均质器速度30下加入序列3。
7. 在相同的均质器速度30下加入序列4。
8. 再混合30分钟。
芳香完整性研究
进行了八小时的研究来研究根据本发明的组合物保持芳香完整性的能力。分析并比较了两个样品:根据以上实施例1的测试配方和对照。对照是在测试配方中使用的相同的香料油。使用气相色谱法和质谱法(GC/MS)来确定总体挥发性指纹,并在各种时间间隔鉴定测试样品散发出的化合物。
首先在载玻片上准备用于分析的样品。为了保持测试样品和对照中香料油的相同浓度,调整了对照和测试样品的重量。向各个玻璃载玻片上称取大约0.09g对照和0.60g测试样品。将样品均匀铺展在载玻片上,然后置于32℃的热板上以干燥。制备干燥时间为2、4、6和8小时的样品以及初始样品。在分配的干燥时间后,将每个载玻片置于50mL的扁平试管中,通过容量移液管向其加入10mL异丙醇。然后将试管制备物声处理两个15分钟的间隔,并涡旋,以从载玻片移除所有的干燥制剂。当观察到每种制备物完全进入溶液时,通过0.45umPTFE过滤器过滤每种样品,并在GC/MS上进行分析。
色谱图
对对照样品的色谱图的评价表明,在八小时的时间内,总挥发性化合物的总浓度显著下降。相反,对测试样品的色谱图的评价表明,该制剂的挥发性芳香成分在八小时的时间内得以保留。
面积计数定量
为了表示对照样品和测试样品保留的挥发性化合物的量,记录了以下四种关键芳香成分的面积计数:柠檬烯、芳樟醇、香根草醇和乙酸香叶酯。
A. 对照样品结果
在两小时时间点,柠檬烯、芳樟醇和香根草醇低于检出限。乙酸香叶酯保留49%。
在四小时时间点,仅保留5%的乙酸香叶酯。
在六小时和八小时时间点,所有四种关键的挥发性化合物均低于检出限。
B. 测试样品结果
在两小时时间点,所有四种化合物都保留在测试样品中;柠檬烯、芳樟醇、香根草醇和乙酸香叶酯分别保留53%、58%、78%和89%。
在四小时时间点,柠檬烯、芳樟醇、香根草醇和乙酸香叶酯分别以41%、44%、68%和81%存在。
在八小时时间点,柠檬烯、芳樟醇、香根草醇和乙酸香叶酯分别以32%、40%、64%和78%存在。
C. 结论
在八小时的时间内,获得的色谱图和面积计数表明,当与对照相比时,测试样品保留了大量的芳香成分。在8小时的测试期结束时,仍然存在显著的强度,该持久性对于消费者使用来说是合适的。另外,完全保持了香调的香域(嗅觉线性)。我们怀疑挥发性芳香成分保留在丙烯酸酯/VA共聚物和/或丙烯酸酯共聚物的表面上,并且比其它水基香料组合物更缓慢地挥发。
Claims (8)
1.一种水包油粗乳液组合物,所述组合物包含:
水相,所述水相按所述组合物的总重量计包含:
30%至70%的水;
4.5%至18.5%的丙烯酸酯/VA共聚物;
0.25%至1.0%的丙烯酸酯共聚物;
一种或多种能够增塑丙烯酸酯/VA共聚物的材料,其中丙烯酸酯/VA共聚物与全部增塑剂的比率范围为1:1至10:1;
油相,所述油相按所述组合物的总重量计包含3%至30%的芳香成分;和
不超过3%的表面活性剂和/或乳化剂。
2.根据权利要求1所述的香水组合物,其中丙烯酸酯/VA共聚物与丙烯酸酯共聚物的比率为10:1至30:1。
3.根据权利要求1所述的香水组合物,其中丙烯酸酯/VA共聚物与丙烯酸酯共聚物的比率为15:1至25:1。
4.根据权利要求1所述的香水组合物,其中所述芳香成分包括一种或多种精油、提取物、合成物以及为赋予气味或香味的唯一目的或者为抵消气味而添加的其它成分。
5.根据权利要求4所述的香水组合物,其中所述提取物为馏出物。
6.根据权利要求1所述的香水组合物,其中所述一种或多种能够增塑丙烯酸酯/VA共聚物的材料包括醇。
7.根据权利要求6所述的香水组合物,其中所述醇包括二醇。
8.根据权利要求1所述的香水组合物,所述香水组合物按所述组合物的总重量计包含不超过5%的醇。
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2020
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- 2020-01-24 ES ES20752494T patent/ES2942027T3/es active Active
- 2020-01-24 BR BR112021015404-3A patent/BR112021015404B1/pt active IP Right Grant
- 2020-01-24 EP EP20752494.3A patent/EP3920882B1/en active Active
- 2020-01-24 CN CN202080026068.0A patent/CN113613626B/zh active Active
- 2020-01-24 WO PCT/US2020/015057 patent/WO2020163097A1/en unknown
- 2020-01-24 CA CA3129210A patent/CA3129210C/en active Active
- 2020-01-24 KR KR1020217027061A patent/KR20210110400A/ko not_active Application Discontinuation
- 2020-01-24 JP JP2021545789A patent/JP7178505B2/ja active Active
- 2020-02-03 TW TW109103188A patent/TWI721768B/zh active
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CN113613626A (zh) | 2021-11-05 |
WO2020163097A1 (en) | 2020-08-13 |
CA3129210A1 (en) | 2020-08-13 |
EP3920882B1 (en) | 2023-03-01 |
AU2020219720B2 (en) | 2022-10-20 |
BR112021015404A2 (pt) | 2021-10-05 |
JP7178505B2 (ja) | 2022-11-25 |
JP2022519645A (ja) | 2022-03-24 |
US10980717B2 (en) | 2021-04-20 |
TW202042779A (zh) | 2020-12-01 |
BR112021015404B1 (pt) | 2022-04-05 |
TWI721768B (zh) | 2021-03-11 |
US20200246227A1 (en) | 2020-08-06 |
EP3920882A1 (en) | 2021-12-15 |
ES2942027T3 (es) | 2023-05-29 |
EP3920882A4 (en) | 2022-05-18 |
CA3129210C (en) | 2023-10-10 |
KR20210110400A (ko) | 2021-09-07 |
AU2020219720A1 (en) | 2021-09-23 |
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