CN111065665A - 颜色保护剂组合物 - Google Patents

颜色保护剂组合物 Download PDF

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CN111065665A
CN111065665A CN201880058933.2A CN201880058933A CN111065665A CN 111065665 A CN111065665 A CN 111065665A CN 201880058933 A CN201880058933 A CN 201880058933A CN 111065665 A CN111065665 A CN 111065665A
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molar ratio
product formed
monomers
cationic polyurethane
hair
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CN111065665B (zh
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S-Y·康
计朝霞
S·A·特纳
曾铃方
D·A·维拉诺瓦
E·G·斯宾格勒
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Living Proof Inc
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Abstract

本文提供的是用于染色的人类毛发的颜色保护剂组合物，以及用于测定其的方法。

Description

颜色保护剂组合物
相关申请
本申请要求2018年4月10日提交的美国临时申请号62/655,275和2017年9月13日提交的美国临时申请号62/557,825的优先权，其各自通过引用全文并入本文。
背景技术
即使在漫长、昂贵的染色阶段后，对他们的毛发进行染色的消费者也报告说，毛发染料的很大一部分在最初的几次洗涤中损失。最常见的商业毛发染料由大的发色团(染料分子)组成，其通过毛发膨胀和染料沉积的过程而沉积在毛发纤维内。由于这些发色团未共价地附着于毛发本身，因此它们通常在常规洗涤和调理过程中从毛发中滤出。这对于消费者是麻烦事，需要日常前往沙龙和彻底使用化学品，其中的一些可对毛发造成永久性损伤并危害环境。在持续探索更有吸引力和更环保的染发方式时，仍然需要可以减少颜色损失量的制剂，从而导致较少去沙龙并减少有害化学品的使用。
发明内容
本文提供了保持毛发的颜色染料的方法，其包括施加某些基于阳离子聚氨酯的组合物。例如，图2a和2b显示，与可商购颜色保护剂树脂相比，包含所公开的阳离子聚氨酯的洗涤溶液导致很小的染料损失。
本文还提供了用于通过使用透析技术，测定和评估化妆品组合物的颜色保留能力的方法。
附图说明
图1a是模仿毛发染料颜色损失的透析实验，其中含有从透析管滤出的染料的储存样品显示，含有毛发染料的透析管浸没在0.8重量％的阳离子WBPU溶液中(左)，导致与毛发染料浸没在MerquatTM2003PR(Polyquaternium-53，Lubrizol Advanced Materials)和MerquatTM100(Polyquaternium-6，Lubrizol Advanced Materials)的0.8重量％溶液中(右)相比，更少的染料从管子损失。图1b是使用比色法对颜色损失的量化，显示当浸没在0.8重量％的阳离子WBPU储液中时，与浸没在0.8重量％的MerquatTM2003PR和MerquatTM100的储液中相比，更少的颜色从透析管损失。图1c是模拟毛发染料颜色损失的透析实验，其中含有从透析管滤出的染料的储存样品显示，含有毛发染料的透析管浸没在5％的阳离子WBPU溶液中，导致与毛发染料浸没在N-DurhanceTMA-1000(聚丙烯酰胺丙基三甲基氯化铵，Ashland)的5％溶液中相比，更少的染料从管子损失。图1d是使用比色法对颜色损失的量化，显示当浸没在5重量％的阳离子WBPU储液中时，与浸没在N-DurhanceTMA-1000的5重量％溶液的储液中相比，更少的颜色从透析管损失。图1e是模拟毛发染料颜色损失的透析实验，其中含有从透析管滤出的染料的调理剂储存样品显示，含有毛发染料的透析管浸没在含有0.3重量％的阳离子WBPU的调理剂中，导致与毛发染料浸没在商业调理剂中相比，更少的染料从管子损失。图1f是使用比色法对颜色损失的量化(总色度变化(ΔC))，显示当浸没在含有0.3重量％的阳离子WBPU储液的调理剂中时，与浸没在含有空白调理剂或商业调理剂的储液中相比，更少的颜色从透析管损失。图1g是使用比色法对颜色损失的量化(红色的总变化(Δa))，显示当浸没在含有0.3重量％的阳离子WBPU储液的调理剂中时，与浸没在含有空白调理剂或商业调理剂的储液中相比，更少的颜色从透析管损失。
图2a说明了颜色从用所公开的阳离子聚氨酯(左)处理并在水中蘸20次的发束的损失，以及颜色从可商购颜色保护剂聚合物MerquatTM2003PR和MerquatTM100的损失(右)。当在水中蘸之前用阳离子WBPU处理毛发，而非用MerquatTM混合物处理时，颜色损失明显更少。图2b说明了颜色从用所公开的阳离子聚氨酯(左)处理并在温和的月桂醇聚醚硫酸钠(表面活性剂)溶液中蘸15次的毛发的损失，以及颜色从可商购颜色保护剂聚合物N-DurhanceTMA-1000当在温和的月桂醇聚醚硫酸钠(表面活性剂)溶液中蘸15次时的损失(右)。当在表面活性剂溶液中蘸之前用阳离子WBPU处理毛发时，颜色损失明显更少。
图3说明了来自体内研究的颜色损失数据，其中具有新鲜染色的毛发的消费者在其头部的一侧上用含有所公开的阳离子聚氨酯的制剂进行了长时间的洗涤和调理，并且在其头部的另一侧上用没有所公开的阳离子聚氨酯的制剂进行了长时间的洗涤和调理。比色数据显示，颜色在11天洗涤期间的损失(如ΔE所指示的)当使用含有阳离子WBPU进行处理时有所减少。遮盲的、受过训练的感官评估者确定，当使用含有阳离子WBPU的处理时，没有观察到有害的视觉或感官效果。
具体实施方式
1.定义
本文所述的“基本上由”阳离子聚氨酯和其它组分“组成”的组合物、工艺或方法是指所记载的阳离子聚氨酯是唯一存在于所记载的组合物、工艺或方法中的聚氨酯。因此，“基本上由...组成(consists essentially of)”或“基本上由...构成(consistingessentially of)”对于除包含另外的聚氨酯之外的所有其它术语是开放式的，，即仅存在所记载的阳离子聚氨酯。
本文所述的“由”阳离子聚氨酯和其它组分“组成”的组合物、工艺或方法是指仅有所记载的组分存在。换句话说，“由...组成”排除了未指定的任何要素、步骤或成分。“由...组成(consists of)”和“由...构成(consisting of)”可互换使用。
“包含”是包括性或开放式的，不排除另外的、未记载的要素或方法步骤。
如本文所用，“阳离子聚氨酯”是指包含氨基甲酸酯(carbamate)(尿烷，urethane)基团的热塑性聚合物，其在pH≤7下携带总体净正电荷。在一些方面中，本文所述的阳离子聚氨酯在约3.7至约6.5、约3.7至约6.0或约3.7至约5.5的pH下携带总体净正电荷。除非另有说明，否则阳离子聚氨酯在本文中使用时包括两性/阳离子聚氨酯。然而，在一个方面，阳离子聚氨酯不涵盖两性/阳离子聚氨酯。
如本文所用，“两性聚氨酯”是指包含氨基甲酸酯(尿烷)基团的热塑性聚合物，且其可以充当阳离子或阴离子聚氨酯两者，取决于中和方法。“两性/阳离子聚氨酯”是指所描述的两性物质是当用酸(例如乳酸)中和时充当阳离子聚氨酯的两性物质。
“杨氏模量(或弹性模量，拉伸模量)”是固体聚合物膜的刚度的量度。杨氏模量E可以通过将应力-应变曲线的弹性(初始，线性)部分中的拉伸应力除以延伸应变来计算。阳离子聚氨酯的杨氏模量可以通过定义以测量机械性质的方案来测定，其是参照ASTM D638、ASTM D412、下文实施例2中所述的测试指南来开发的。
“断裂伸长率(也称为断裂应变，极限伸长率)”是固体聚合物膜断裂后的变化长度与初始长度之间的比率。阳离子聚氨酯的断裂伸长率可以通过定义以测量机械性质的方案来确定，其是参照ASTM D638、ASTM D412、下文实施例2中所述的测试指南来开发的。
“水分摄取”是固体聚合物膜吸附的水的量度。实施例3提供了用于测定固体聚合物膜的水分摄取的方法。
“感官分数”是通过毛发固定剂的性能来测定的。特别是，施加有组合物的发束被吹干90秒。将发束一式两份制备，随机遮盲，并由受过训练的感官分析师在遮盲条件下以-2至2的等级评估自然感觉和整体感官属性。感官分析者是获得许可的发型师和化妆品科学家，在评估毛发的感官属性方面具有显著的长期经验。感官分析者给被认为完全不合需要的发束-2分，给完全柔软、自然感觉和有表现力的毛发+2分，给这两个极端之间的毛发中间分。
如本文所用，“保留毛发颜色”，“减少毛发颜色的损失”，“减少染色的毛发的颜色损失”，或类似的意思，即由于用所公开的组合物处理的染色样品的毛发染料损失，如通过比色法测量的总颜色变化(ΔE)或总色度变化(ΔC)小于已经染色但未使用所公开的组合物处理的毛发的总颜色变化(ΔE)或总色度变化(ΔC)。
2.选择标记
本文提供的是已发现导致能够减少染色的毛发(例如，人的毛发)的颜色损失的化妆品组合物(例如，毛发产品)的WBPU性质的特定组合。这些性质包括，例如，某些机械性质的组合，某些化学性质的组合，或机械和化学性质两者的组合。
杨氏模量、断裂伸长率和水分摄取
本文所述的机械性质的组合包括杨氏模量(例如，高于150MPa)、断裂伸长率(例如，约15％至约300％)，以及疏水性(水分摄取，例如，小于10％)。
在一个方面，阳离子聚氨酯的杨氏模量应高于约150MPa。例如，所公开的组合物中的阳离子聚氨酯的杨氏模量可以是高于约160MPa，高于约170MPa，高于约180MPa，高于约190MPa，高于约200MPa，高于约210MPa，高于约220MPa，高于约230MPa，高于约240MPa，高于约250MPa，高于约260MPa，高于约270MPa，高于约280MPa，高于约290MPa，高于约300MPa，高于约310MPa，高于约320MPa，高于约330MPa，高于约340MPa，高于约350MPa，高于约360MPa，高于约370MPa，高于约380MPa，高于约390MPa，高于约400MPa，高于约410MPa，高于约420MPa，高于约430MPa，高于约440MPa，高于约450MPa，高于约460MPa，高于约470MPa，高于约480MPa，高于约490MPa，高于约500MPa，高于约510MPa，高于约520MPa，高于约530MPa，高于约540MPa，或高于550MPa。在其它方面，阳离子聚氨酯的杨氏模量应在约150MPa至约500MPa之间。例如，所公开的组合物中的阳离子聚氨酯的杨氏模量可以是在约150MPa至约400MPa之间，约150MPa至约350MPa之间，约170MPa至约390MPa之间，约180MPa至约320MPa之间，约190MPa至约300MPa之间，约200MPa至约290MPa之间，或约210MPa至约280MPa之间。
在一个方面，阳离子聚氨酯的断裂伸长率应为15％至约300％。例如，所公开的组合物中的阳离子聚氨酯的断裂伸长率可以是约20％至约300％，约25％至约300％，约40％至约280％，约100％至约280％，约100％至约250％，约150％至约250％，约200％至约250％，约210％至约250％，约30至约150％，约15％至约150％，约150％至约300％，约50％至约250％；约75％至约225％，或约100％至约200％。断裂伸长率可以任选地与上文段落中描述的一个或多个杨氏模量值或在本公开的其余部分中描述的任何一个杨氏模量值组合。
在一个方面，阳离子聚氨酯的水分摄取应小于约10％。例如，所公开的组合物中的阳离子聚氨酯的水分摄取可以是小于约9.5％，小于约9％，小于约8.5％，小于约8％，小于约7.5％，小于约7％，小于约6.5％，小于约6％，小于约5.5％，小于约5％，小于约4.5％，小于约4％，小于约3.5％，小于约3％，小于约2.5％，小于约2％，小于约1.5％，小于约1％，小于约0.5％，或为约0％。在一个方面，所公开的组合物中的阳离子聚氨酯的水分摄取应为约0％至约10％。例如，水分摄取可为约0％至约8％、约2％至约8％或约3％至约7％。水分摄取可以任选地与上文段落中或在本公开的其余部分中描述的一个或多个杨氏模量值、一个或多个断裂伸长率值、或两者组合。
如下文实施例部分所示，具有上述杨氏模量、断裂伸长率和水分摄取的阳离子聚氨酯使例如通过化学方法染色的毛发的颜色损失最小化。
3.使用方法
一种保持染色的人类毛发的毛发颜色的方法，所述方法包括向所述毛发施用包含阳离子聚氨酯的组合物，所述阳离子聚氨酯具有高于150MPa的杨氏模量，约15％至约300％的断裂伸长率，以及小于10％的水分摄取。还提供的是保持染色的人类毛发的毛发颜色的方法，所述方法包括向所述毛发施用基本上由阳离子聚氨酯、中和剂和油组成的组合物，所述阳离子聚氨酯具有高于150MPa的杨氏模量，约15％至约300％的断裂伸长率，以及小于10％的水分摄取。
在一些方面，所提供的方法中的阳离子聚氨酯是式[W，V，Y和Z]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；X是中和离子；W的分子量为约1,000g/mol；V:W的摩尔比为1:0.18至约1:0.32；V:Y的摩尔比为1:0.24至约1:0.72；和V:Z的摩尔比为1:0.08至约1:0.47。在一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y和Z]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；X是中和离子；W的分子量为约2,000g/mol；V:W的摩尔比为1:0.08至约1:0.18；V:Y的摩尔比为1:0.36至约1:0.82；和V:Z的摩尔比为1:0.08至约1:0.49。在另一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y和Z]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；X是中和离子；W的分子量为约3,000g/mol；V:W的摩尔比为1:0.05至约1:0.13；V:Y的摩尔比为1:0.4至约1:0.85，和V:Z的摩尔比为1:0.08至约1:0.49。
在一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y，Z和Z1]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；Z1是从乙氧基化多元醇单体形成的产物；X是中和离子；W的分子量为约1,000g/mol；V:W的摩尔比为1:0.19至约1:0.33；V:Y的摩尔比为1:0.19至约1:0.7；V:Z的摩尔比为1:0.08至约1:0.49；和V:Z1的摩尔比为1:0至约1:0.03。在另一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y，Z，和Z1]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；Z1是从乙氧基化多元醇单体形成的产物；X是中和离子；W的分子量为约2,000g/mol；V:W的摩尔比为1:0.09至约1:0.18；V:Y的摩尔比为1:0.31至约1:0.8；V:Z的摩尔比为1:0.09至约1:0.51；和V:Z1的摩尔比为1:0至约1:0.03。在另一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y，Z，和Z1]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；Z1是从乙氧基化多元醇单体形成的产物；X是中和离子；W的分子重量为约3,000g/mol；V:W的摩尔比为1:0.05至约1:0.13；V:Y的摩尔比为1:0.36至约1:0.83；V:Z的摩尔比为1:0.09至约1:0.52；和V:Z1的摩尔比为1:0至约1:0.03。
在另一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y，Z和Z2]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；Z2是从羟化烷基酸单体形成的产物；X是中和离子；W的分子量为约1,000g/mol；V:W的摩尔比为1:0.19至约1:0.33；V:Y的摩尔比为1:0.14至约1:0.44；V:Z的摩尔比为1:0.08至约1:0.47；和V:Z2的摩尔比为1:0.05至约1:0.33。在另一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y，Z，和Z2]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；Z2是从羟化烷基酸单体形成的产物；X是中和离子；W的分子量为约2,000g/mol；V:W的摩尔比为1:0.09至约1:0.18；V:Y的摩尔比为1:0.26至约1:0.53；V:Z的摩尔比为1:0.09至约1:0.49；和V:Z2的摩尔比为1:0.05至约1:0.35。在另一个替代方案中，所提供的方法中的阳离子聚氨酯是式[W，V，Y，Z，和Z2]X-的盐，其中W是从聚碳酸酯多元醇单体形成的产物；V是从多异氰酸酯单体形成的产物；Y是从C1-8烷基二醇单体形成的产物；Z是从C1-8氨基烷基二醇单体形成的产物；Z2是从羟化烷基酸单体形成的产物；X是中和离子；和W的分子量为约3,000克/摩尔；V:W的摩尔比为1:0.05至约1:0.13；V:Y的摩尔比为1:0.3至约1:0.56；V:Z的摩尔比为1:0.09至约1:0.5；和V:Z2的摩尔比为1:0.05至约1:0.35。
在又一个替代方案中，V是从异佛尔酮二异氰酸酯单体形成的产物；Y是从1,4-丁二醇单体形成的产物；和Z是从3-(二甲基氨基)-1,2-丙二醇单体形成的产物。在又一个替代方案中，所提供的方法中的阳离子聚氨酯是下式的盐
Figure BDA0002407310790000091
其中n为6至21，并且m为19至31。
在一些方面，所提供的方法中的阳离子聚氨酯选自PU-363、PU-399、PU-400、PU-377、PU-404、PU-378、PU-383、PU-398、PU-401、PU-402、PU-403、PU-385、PU-376、PU-408、PU-409、PU-396、PU-413、PU-414、PU-362和PU-372。在另一个方面，所提供的方法中的阳离子聚氨酯选自PU-362、PU-376、PU-377、PU-378和PU-404。在又一个方面，所提供的方法中的阳离子聚氨酯选自PU-363、PU-377和PU-378。
在一些方面，所提供的方法中的阳离子聚氨酯分散在水中。
在一些方面，所提供的方法中的阳离子聚氨酯是颗粒的形式。
在一些方面，所提供的方法中的阳离子聚氨酯包括具有约20至约80nm的平均颗粒直径的均匀颗粒。
在一些方面，所提供的方法中的阳离子聚氨酯包括具有约100至约300nm的平均颗粒直径的双峰或多峰颗粒。
在一些方面，所提供的方法中的阳离子聚氨酯基于组合物的总重量以25％至35％的量存在。
在一些方面，所提供的方法中描述的组合物还包含中和剂。中和剂可以是例如酸中和剂，例如乳酸。在一些方面，中和剂:C1-8氨基烷基二醇单体的比率为约0.8至约1.2。
在一些方面，所提供的方法中描述的组合物还包含油。油可以选自矿物油、动物油、植物油或合成油。在一个方面，油是亚油酸，或者脂肪酸的混合物。实例包括但不限于芳香油，润肤剂，类单萜，脂肪醇，脂肪酸，脂肪酯，脂肪醚，氟化小分子(例如，全氟甲基环戊烷，全氟全氢菲，全氟-1,3-二甲基环己烷，全氟甲基十氢化萘和全氟全氢苄基四氢萘)，及其混合物。在另一方面，基于组合物的总重量，油以约0.2至约1.65％的量存在。在另一方面，基于组合物的总重量，油以约0.2至约0.25％的量存在。
在所公开的方法的一个方面，在毛发被染色之前、期间或之后施用组合物。在另一方面，在毛发被染色之前或之后施用组合物。在又一方面，在毛发已经被染色之后施用组合物。
在所公开的方法的一个方面，所公开的组合物与水一起施加于毛发。
在所公开的方法的一个方面，所公开的组合物当施用于毛发时改变质地和外观。
在所公开的方法的一个方面，所公开的组合物当施用于毛发时还改善维持性(hold)，即，形成为给定的卷曲或造型的毛发随时间保持该卷曲或造型。
在所公开的方法的一个方面，所公开的组合物当施加于毛发时还提供足够的定型性，即，施加于毛发的组合物提供足够的刚度和柔性以形成和保持发型。
在所公开的方法的一个方面，所公开的组合物当施用于毛发时还最小化凌乱度(flyaway)，即，很少有个体毛发纤维不符合给定的卷曲或发型。
在所公开的方法的一个方面，所公开的组合物当施用于毛发时还保持卷曲形状，即，形成为给定的卷曲的毛发随时间保持该卷曲。
在所公开的方法的一个方面，所公开的组合物当施用于毛发时还提供自然卷曲的增强，即，自然地倾向于卷曲的毛发表现出更明确和更少弥散的卷曲模式。
所公开的方法中的组合物可以进一步包含抗氧化剂。可能合适的抗氧化剂包括但不限于番红花油(
Figure BDA0002407310790000113
oil)，α硫辛酸，绿茶和白茶，视黄醇，维生素C，维生素E，丁基化羟基甲苯，丁基化羟基苯甲醚，辅酶Q10(CoQ-10)，异黄酮，多酚，姜黄素，姜黄，石榴，迷迭香，谷胱甘肽，硒和锌。
在一个示例性方面，有效量的本文所述的组合物可以在毛发被染色之前、期间和/或之后被喷雾或施用于干燥或潮湿的毛发。如本文所用，“有效量”是指足以提供颜色保护的量。
本文还提供了一种用于测定化妆品组合物的颜色保留性质的方法，所述方法包括以下步骤：对包含所述化妆品组合物和至少一种颜色染料的溶液进行透析；并定量评估在一段时间内的颜色损失。在一个方面，“定量评估在一段时间内的颜色损失”是指根据实施例4所述的公式来评估总颜色损失ΔE或总色度损失ΔC，即
Figure BDA0002407310790000111
或
Figure BDA0002407310790000112
在一个方面，进行透析的步骤包括将感兴趣的毛发染料放入透析管中，然后将包含毛发染料的透析管放入包含感兴趣的组合物的储槽中。
实施例
实施例1.阳离子水性聚氨酯的化学组合物
阳离子水性聚氨酯主要使用聚碳酸酯二醇、1,4-丁二醇(BD)、异佛尔酮二异氰酸酯(IPDI)和3-(二甲基氨基)-1,2-丙二醇(DMAPD)来合成；选择性地，非离子链增长剂Tegomer D3403(乙氧基化聚醚-1,3-二醇)和2,2-双(羟甲基)丁酸(DMBA)被分别引入阳离子水性聚氨酯中以实现期望的物理性质。温和的酸——乳酸——被用作中和剂。对于每种单体，与NCO的摩尔比列于表1中。此外，有益油也可引入阳离子水性聚氨酯中，以提供改善的感官属性。
表1
Figure BDA0002407310790000121
PCD1K＝分子量为1,000g/mol的聚碳酸酯二醇；PCD3K＝分子量为3,000g/mol的聚碳酸酯二醇。
总体地，本发明的阳离子水性聚氨酯具有如本文定义的最佳物理性质：(1)杨氏模量>150MPa，(2)断裂伸长率在15％和300％之间，和(3)水摄取：(a)对于WBPU且无添加剂，低于10％；(b)对于WBPU且有添加剂，低于8％。参见表2。
表2
Figure BDA0002407310790000131
阳离子水性聚氨酯的粒度和分布可以划分为两种类型。取决于化学组成，一种类型的阳离子水性聚氨酯显示均匀的粒度分布和约20至约80nm范围内的平均颗粒直径。另一种类型的阳离子水性聚氨酯显示较大的粒度和双峰/多峰粒度分布，如100至约300nm范围内的平均粒度所示，以及较大的粒度标准偏差。参见表3。
表3
PU名称 粒度(TEM，nm)
363 29.8±3.9
399 29.9±4.3
400 29.6±5.0
377 34.1±7.5
378 36.6±10.7
383 150.3±112.9
398 111.2±45.4
402 139.6±50.6
376 21.3±4.5
355 41.3±18.3
362 57.0±15.6
372 79.7±29.7
413 60.1±16.7
414 106.2±25.2
实施例2.机械性能
杨氏模量是材料当在单轴拉伸或压缩下时承受长度变化的能力的量度。较高的杨氏模量通常表明该材料是更刚性的。断裂伸长率，也称为断裂应变，是试样断裂后的变化长度与初始长度之间的比率。较高的断裂伸长率表示材料抗断裂的能力。
将本文公开的一些聚氨酯的杨氏模量和断裂伸长率与若干种可商购聚氨酯产品进行比较。杨氏模量和断裂伸长率可以通过定义以测量机械性质的方案来测定，其是根据ASTM D638，ASTM D412，测试指南开发的。特别地，以下方案可用于测定聚氨酯的干膜的杨氏模量和断裂伸长率(或极限伸长率)。测试对每个样品需要大约10-20分钟以完成。
材料：
>25g聚氨酯水分散体
每个样品1个在Teflon片材上开槽的干净长方形模具(2mm×20mm×45mm)
1个干净的剃刀刀片
透明胶带
安装有延伸手柄几何结构的通用测试机
样品制备：
1.从其各自的储备溶液制备25g的10重量％WBPU溶液。
2.在每个模具(2mm×20mm×45mm)中施加2.5mL制备的溶液并允许干燥2天以给出WBPU膜。
3.在其变干后，用刮刀从模具移除膜。
4.使用剃刀刀片来切除角落并获得约15mm宽和约150-300微米厚的膜。确保膜没有气泡。
5.标记测试膜。
6.每个样品切成四块条带(20mm)，将它们粘贴到试样条的两侧并制成狗骨形状样品以改善手柄中的样品的维持性。将制备的测试膜在干燥器中存放1-2小时以使其完全干燥。一次从干燥器中取出一个样品进行测试。
样品测试
1.使通用测试机上记录的负载平衡，使得其读数为0牛顿。
2.使用卡尺将顶部和底部延伸手柄几何结构之间的距离设置为20mm。
3.将样品安装在延伸手柄中并牢固固定，确保透明胶带不可见，并且样品在两个垂直平面中尽可能接近垂直。
4.通过分开所述几何结构直至记录到2-5N的力为止，略微拉伸样品。
5.在通用测试机上以100mm/分钟的速度开始拉伸测试运行，在样品断裂时停止测试。
6.断裂伸长率是在材料于其处断裂的伸长处计算。
7.杨氏模量计算为在变形的初始、弹性部分期间的模量，这通过计算对该区域进行线性拟合的斜率(R值>0.99)来实现。
a)低模量和高伸长率(Avalure UR 450(PPG-17/IPDI/DMPA共聚物)，C1004(聚氨酯-35)，Polyderm PE/PA ED(聚氨酯-58)，Polyderm PE/PA(聚氨酯-18)，其导致较差的卷曲保持(例如，保持是临时的、短暂的或短命的)；或
b)高模量和低伸长率(DynamX(聚氨酯14和AMP-丙烯酸酯类共聚物)，DynamX/H2O(聚氨酯-14和AMP-丙烯酸酯类共聚物/水)，Luviset PUR(聚氨酯-1)，其导致在操作后具有低性能的脆性材料(例如，树脂是脆性的或断裂)。
实施例3.聚氨酯的疏水性/水摄取
WBPU干膜在高度湿润环境下的水分摄取性质已经与其持久保持性能相关联。因此，重要的是能够可再现地和准确地评估这样的水分摄取性质以使得能够在体外和体内预测性地评估WBPU干膜。以下方案可用于测定WBPU干膜在高度湿润环境下的水分摄取能力。测试对每个样品组需要约2-3天来完成。
材料
>15g WBPU溶液
每个样品1个干净的细胞培养皿(60mm直径×15mm高)
湿度室具有控制温度和相对湿度(RH)的灵活性
样品测试
1.从其各自的储备溶液制备15g的10重量％WBPU溶液。
2.对每个样品标记细胞培养皿并测量其空重(Wpd)。
3.在每个培养皿中施加4mL制备的溶液(3个样品/WBPU，并允许在25℃和50％RH下的湿度室中平衡20小时。
4.在平衡后，测量并记录样品重量(Wi)。
5.将样品置于在25℃和90％RH下的湿度室中，并允许平衡到高湿度达20小时。
6.测量并记录最终样品重量(Wf)。
样品分析
使用以下公式计算水分摄取％：
Figure BDA0002407310790000161
实施例4.染料保持
收集在本文公开的聚氨酯的存在下的毛发染料损失的比色数据，并与在若干种可商购颜色保护剂树脂下的毛发染料损失进行比较。通过评估每个样品的L*、a*和b*值的变化来测定颜色损失，其是可以被分配以按白色/黑色标度(L*)、红色/绿色标度(a*)和蓝色/黄色标度(b*)指示样品的颜色的数值。根据以下一般程序，使用所述方案测定使用色度计收集到的颜色损失。测试对每个样品需要大约5分钟来完成。
1.将色度计对纯白色校准标准品进行校准。
2.为了分析溶液，将包含溶液的闪烁管放在比色计样品台上，记录L*、a*和b*值。
3.对所有感兴趣的样品重复。
4.总颜色损失ΔE根据下式计算：
Figure BDA0002407310790000171
其中Lx是感兴趣的L*值，L0是初始L*值
其中ax是感兴趣的a*值，a0是初始a*值
其中bx是感兴趣的b*值，b0是初始b*值
5.总色度损失ΔC根据以下公式计算：
Figure BDA0002407310790000172
其中ax是感兴趣的a*值，a0是初始a*值
其中bx是感兴趣的b*值，b0是初始b*值
发现所公开的阳离子聚氨酯使各种聚合物体系中的染料损失最小化，因此具有足以延迟或防止染料从颜色处理的毛发损失的性质。在此，使用用于评估颜色保留的新型方法——透析——对获自阳离子WBPU的体外和体内颜色保护结果建模。在每个透析实验中，将感兴趣的毛发染料(15g)悬浮在孔径为0.5-1kDa的透析管中，以模仿生物材料(例如毛发角蛋白)的孔径。然后将透析管浸没在含有感兴趣的树脂(例如阳离子WBPU或商业颜色保护剂树脂)的大型储槽(300g)中。在一个实验中，制备含有红色毛发染料的透析管样品，然后浸没在0.8重量％的阳离子WBPU或0.8重量％的MerquatTM2003PR和MerquatTM100中。在不同时间点处采集的储器的样品在视觉上显示，与Merquat混合物相比，在阳离子WBPU的存在下，更少的毛发染料从透析管损失(图1a)。结果通过损失到储器中的染料的定量比色法评估来确认(图1b)。在另一个实验中，制备含有红色毛发染料的透析管样品，然后浸没到5重量％的阳离子WBPU或5重量％的N-DurHanceTMA-1000中。在不同时间点处采集的储器的样品在视觉上显示，与N-DurHanceTMA-1000相比，在阳离子WBPU的存在下，更少的毛发染料从透析管损失(图1c)。结果通过损失到储器中的染料的定量比色法评估来确认(图1d)。
在模拟典型染料清洗的受控体外研究过程中，用红色毛发染料染色的发束用含有阳离子聚氨酯或N-DurHanceTMA-1000的溶液处理。预先用红色毛发染料染色的1.5g发束用0.5g的5％阳离子WBPU或N-DurHanceTMA-1000溶液涂覆并静置30秒，然后在50mL DI水的广口瓶中蘸10次。与常见的颜色保护聚合物N-DurHanceTMA-1000(右)相比，阳离子WBPU处理导致少得多的染料损失(左)。参见图2a和2b。结果清楚地表明，与N-DurHanceTMA-1000发束溶液相比，含有阳离子WBPU的洗涤溶液导致很少的染料损失。
图3说明了来自体内研究的颜色损失数据，其中具有新鲜染色的毛发的消费者在其头部的一侧上用含有所公开的阳离子聚氨酯的制剂进行了长时间的洗涤和调理，并且在其头部的另一侧上用没有所公开的阳离子聚氨酯的制剂进行了长时间的洗涤和调理。比色数据显示，颜色在11天洗涤期间的损失当使用含有阳离子WBPU的处理时有所减少，如ΔE所指示的那样。遮盲的、受过训练的感官评估者确定，当使用含有阳离子WBPU的处理时，没有观察到有害的视觉或感官效果。
在本申请各处引用的所有参考文献(包括文献参考文献、授权专利、公布专利申请和共同待决的专利申请)的内容在此明确地通过引用以其全文并入本文。除非另有定义，否则本文中使用的所有技术和科学术语均与本领域普通技术人员通常已知的含义相符。

Claims (33)

1.一种保持染色的人类毛发的毛发颜色的方法，所述方法包括向所述毛发施用包含阳离子聚氨酯的组合物，所述阳离子聚氨酯具有高于150MPa的杨氏模量，约15％至约300％的断裂伸长率，以及小于10％的水分摄取。
2.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y和Z]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
X是中和离子；
W的分子量为约1,000g/mol；
V:W的摩尔比为1:0.18至约1:0.32；
V:Y的摩尔比为1:0.24至约1:0.72；和
V:Z的摩尔比为1:0.08至约1:0.47。
3.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y和Z]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
X是中和离子；
W的分子量为约2,000g/mol；
V:W的摩尔比为1:0.08至约1:0.18；
V:Y的摩尔比为1:0.36至约1:0.82；和
V:Z的摩尔比为1:0.08至约1:0.49。
4.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y和Z]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
X是中和离子；
W的分子量为约3,000g/mol；
V:W的摩尔比为1:0.05至约1:0.13；
V:Y的摩尔比为1:0.4至约1:0.85；和
V:Z的摩尔比为1:0.08至约1:0.49。
5.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y，Z和Z1]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
Z1是从乙氧基化多元醇单体形成的产物；
X是中和离子；
W的分子量为约1,000g/mol；
V:W的摩尔比为1:0.19至约1:0.33；
V:Y的摩尔比为1:0.19至约1:0.7；
V:Z的摩尔比为1:0.08至约1:0.49；和
V:Z1的摩尔比为1:0至约1:0.03。
6.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y，Z和Z1]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
Z1是从乙氧基化多元醇单体形成的产物；
X是中和离子；
W的分子量为约2,000g/mol
V:W的摩尔比为1:0.09至约1:0.18；
V:Y的摩尔比为1:0.31至约1:0.8；
V:Z的摩尔比为1:0.09至约1:0.51；和
V:Z1的摩尔比为1:0至约1:0.03。
7.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y，Z和Z1]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
Z1是从乙氧基化多元醇单体形成的产物；
X是中和离子；
W的分子量为约3,000g/mol
V:W的摩尔比为1:0.05至约1:0.13；
V:Y的摩尔比为1:0.36至约1:0.83；
V:Z的摩尔比为1:0.09至约1:0.52；和
V:Z1的摩尔比为1:0至约1:0.03。
8.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y，Z和Z2]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
Z2是从羟化烷基酸单体形成的产物；
X是中和离子；
W的分子量为约1,000g/mol；
V:W的摩尔比为1:0.19至约1:0.33；
V:Y的摩尔比为1:0.14至约1:0.44；
V:Z的摩尔比为1:0.08至约1:0.47；和
V:Z2的摩尔比为1:0.05至大约1:0.33。
9.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y，Z和Z2]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
Z2是从羟化烷基酸单体形成的产物；
X是中和离子；
W的分子量为约2,000g/mol；
V:W的摩尔比为1:0.09至约1:0.18；
V:Y的摩尔比为1:0.26至约1:0.53；
V:Z的摩尔比为1:0.09至约1:0.49；和
V:Z2的摩尔比为1:0.05至约1:0.35。
10.根据权利要求1所述的方法，其中所述阳离子聚氨酯是式[W，V，Y，Z和Z2]X-的盐，其中
W是从聚碳酸酯多元醇单体形成的产物；
V是从多异氰酸酯单体形成的产物；
Y是从C1-8烷基二醇单体形成的产物；
Z是从C1-8氨基烷基二醇单体形成的产物；
Z2是从羟化烷基酸单体形成的产物；
X是中和离子；
W的分子量为约3,000g/mol；
V:W的摩尔比为1:0.05至约1:0.13；
V:Y的摩尔比为1:0.3至约1:0.56；
V:Z的摩尔比为1:0.09至约1:0.5；和
V:Z2的摩尔比为1:0.05至约1:0.35。
11.根据权利要求2至10中任一项所述的方法，其中
V是从异佛尔酮二异氰酸酯单体形成的产物；
Y是从1,4-丁二醇单体形成的产物；和
Z是从3-(二甲基氨基)-1,2-丙二醇单体形成的产物。
12.根据权利要求1所述的方法，其中所述阳离子聚氨酯是下式的盐：
Figure FDA0002407310780000051
其中n为6至21，并且m为19至31。
13.根据权利要求1所述的方法，其中所述阳离子聚氨酯选自PU-363、PU-399、PU-400、PU-377、PU-404、PU-378、PU-383、PU-398、PU-401、PU-402、PU-403、PU-385、PU-376、PU-408、PU-409、PU-396、PU-413、PU-414、PU-362和PU-372。
14.根据权利要求1所述的方法，其中所述阳离子聚氨酯选自PU-362、PU-376、PU-377、PU-378和PU-404。
15.根据权利要求1所述的方法，其中阳离子聚氨酯选自PU-363、PU-377和PU-378。
16.根据权利要求1至15中任一项所述的方法，其中所述阳离子聚氨酯分散在水中。
17.根据权利要求1至16中任一项所述的方法，其中所述阳离子聚氨酯是颗粒的形式。
18.根据权利要求1至17中任一项所述的方法，其中所述阳离子聚氨酯包括具有约20至约80nm的平均颗粒直径的均匀颗粒。
19.根据权利要求1至18中任一项所述的方法，其中所述阳离子聚氨酯包括具有约100至约300nm的平均颗粒直径的双峰或多峰颗粒。
20.根据权利要求1至19中任一项所述的方法，其中基于所述组合物的总重量，所述阳离子聚氨酯以25％至35％的量存在。
21.根据权利要求1至19中任一项所述的方法，其中所述组合物还包含中和剂。
22.根据权利要求21所述的方法，其中所述中和剂是酸中和剂。
23.根据权利要求22所述的方法，其中所述中和剂是乳酸。
24.根据权利要求21至23中任一项所述的方法，其中所述中和剂:C1-8氨基烷基二醇单体的比率为约0.8至约1.2。
25.根据权利要求1至23中任一项所述的方法，其中所述组合物还包含油。
26.根据权利要求25中任一项所述的方法，其中所述油选自矿物油、动物油、植物油或合成油。
27.根据权利要求25或26所述的方法，其中所述油是亚油酸，或者脂肪酸的混合物。
28.根据权利要求25至27中任一项所述的方法，其中基于所述组合物的总重量，所述油以约0.2至约1.65％的量存在。
29.根据权利要求25至28中任一项所述的方法，其中基于所述组合物的总重量，所述油以约0.2至约0.25％的量存在。
30.根据权利要求1至29中任一项所述的方法，其中在所述毛发被染色之前、期间或之后施用所述组合物。
31.根据权利要求1至30中任一项所述的方法，其中在所述毛发已经被染色之后施加所述组合物。
32.根据权利要求1至31中任一项所述的方法，其中所述组合物与水一起施用于所述毛发。
33.一种用于测定化妆品组合物的颜色保留性质的方法，所述方法包括以下步骤：对包含所述化妆品组合物和至少一种颜色染料的溶液进行透析；并定量评估在一段时间内的颜色损失。
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WO2019055445A3 (en) 2019-04-25
CA3074845A1 (en) 2019-03-21
US20220105021A1 (en) 2022-04-07
JP7244494B2 (ja) 2023-03-22
JP2020533359A (ja) 2020-11-19
US10842729B2 (en) 2020-11-24
WO2019055445A2 (en) 2019-03-21
AU2018332820B2 (en) 2024-04-18
AU2018332820A1 (en) 2020-03-12
EP3681921A2 (en) 2020-07-22
BR112020004127A2 (pt) 2020-09-01
CN111065665B (zh) 2023-03-17
US11707426B2 (en) 2023-07-25

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