CN116033825A - 含有抗菌活性物质的可溶性固体制品 - Google Patents
含有抗菌活性物质的可溶性固体制品 Download PDFInfo
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- CN116033825A CN116033825A CN202180054617.XA CN202180054617A CN116033825A CN 116033825 A CN116033825 A CN 116033825A CN 202180054617 A CN202180054617 A CN 202180054617A CN 116033825 A CN116033825 A CN 116033825A
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- 238000005406 washing Methods 0.000 description 1
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- 235000021119 whey protein Nutrition 0.000 description 1
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- A—HUMAN NECESSITIES
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
- A01N37/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
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Abstract
本发明公开了一种可溶性固体制品,该可溶性固体制品包含按制品的重量计:约10%至约50%的水溶性聚合物;约20%至约80%的表面活性剂;约0.5%至约2%的处于酸形式时具有约250道尔顿至约450道尔顿的平均分子量并且在pH 4下具有约‑12至约‑7的加权logP值的二氨基羧酸螯合剂及其盐;约0.1%至约6%的处于酸形式时具有约100道尔顿至约400道尔顿的平均分子量并且在pH 4下具有约‑2至约4的加权logP值的芳族羧酸及其盐;约0.1%至约18%的非芳族有机α羟基酸及其盐;其中当用30份水对1份可溶性固体制品溶解时,该可溶性固体制品具有约3至约5.1的pH。本发明提供了可溶性固体制品,该可溶性固体制品甚至在制品溶解后仍提供抗菌益处,同时控制抗菌活性成分在固体制品中的浓度。
Description
技术领域
本发明涉及一种可溶性固体制品,该可溶性固体制品包含按制品的重量计:约10%至约50%的水溶性聚合物;约20%至约80%的表面活性剂;约0.5%至约2%的处于酸形式时具有约250道尔顿至约450道尔顿的平均分子量并且在pH 4下具有约-12至约-7的加权logP值的二氨基羧酸螯合剂及其盐;约0.1%至约6%的处于酸形式时具有约100道尔顿至约400道尔顿的平均分子量并且在pH 4下具有约-2至约4的加权logP值的芳族羧酸及其盐;约0.1%至约18%的非芳族有机α羟基酸及其盐;其中当用30份水对1份可溶性固体制品溶解时,所述可溶性固体制品具有约3至约5.1的pH。本发明提供了可溶性固体制品,其甚至在制品溶解后仍提供抗菌益处,同时控制抗菌活性成分在固体制品中的浓度。
背景技术
在水溶性聚合物载体或基质中包含表面活性剂和/或其他活性成分的柔性且可溶解的固体制品是众所周知的。此类制品特别可用于在水中溶解时递送表面活性剂和/或其他活性成分。相比于相同产品类别的传统颗粒或液体形式,此类制品具有较好的结构完整性,更为浓缩,并且易于储存、运送/运输、搬运和处理。相比于相同产品类别的固体片剂形式,此类制品可为消费者提供更快的溶解和/或更美观的吸引力。
此类可溶性固体制品通常通过用例如10-30份水对1份制品水溶解制品来使用。制品中所含成分的浓度在溶解期间和之后被稀释。当可溶性固体制品为个人护理产品时,需要制品向所施用的基底(例如皮肤和/或毛发)提供抗菌益处。然而,当以足以在固体制品溶解后提供抗菌益处的水平包含抗菌活性成分时,此类活性成分在固体制品(在溶解前)中的浓度变得太高。一些国家的法规要求此类抗菌活性成分在制品(在溶解前)中的浓度上限。
因此,需要可溶性固体制品,其甚至在制品溶解后仍提供抗菌益处,同时控制抗菌活性成分在固体制品中的浓度。
发明内容
本发明涉及一种可溶性固体制品,该可溶性固体制品包含按制品的重量计:
a.约10%至约50%的水溶性聚合物;
b.约20%至约80%的表面活性剂;
c.约0.5%至约2%的处于酸形式时具有约250道尔顿至约450道尔顿的平均分子量并且在pH 4下具有约-12至约-7的加权logP值的二氨基羧酸螯合剂及其盐;
d.约0.1%至约6%的处于酸形式时具有约100至约400道尔顿的平均分子量并且在pH 4下具有约-2至约4的加权logP值的芳族羧酸及其盐;
e.约0.1%至约18%的非芳族有机α羟基酸及其盐;
其中当用30份水对1份可溶性固体制品溶解时,所述可溶性固体制品具有约3至约5.1的pH。
在一个实施方案中,当用30份水对1份可溶性固体制品溶解时,具有上述特征的可溶性固体制品具有约3.5至约4.9的pH。
在一个实施方案中,当用30份水对1份可溶性固体制品溶解时,具有上述特征中任一特征的可溶性固体制品具有约3.8至约4.8的pH。
在一个实施方案中,具有上述特征中任一特征的可溶性固体制品还包含约0.1%至约2.0%的具有约90道尔顿至约500道尔顿的平均分子量和在pH 4下约-1至约12加权logP值的二醇。
在一个实施方案中,具有上述特征中任一特征的可溶性固体制品包含两个或更多个柔性可溶性多孔片材。
在一个实施方案中,具有上述特征中任一特征的可溶性固体制品具有在约0.050g/cm3至约0.380g/cm3范围内的密度。
本发明提供了可溶性固体制品,其甚至在制品溶解后仍提供抗菌益处,同时控制抗菌活性成分在固体制品中的浓度。通过特定抗菌活性成分的组合和在特定pH下使用此类组合,甚至在制品溶解后仍可提供抗菌益处,同时控制每种抗菌活性成分在固体制品中的浓度。
在阅读本发明的以下具体实施方式时,本发明的这些和其他方面将变得更明显。
具体实施方式
虽然本说明书以特别指出并清楚地要求保护本发明的权利要求书作为结尾,但据信通过下列说明可更好地理解本发明。
本文中“包括/包含”是指可添加不影响最终结果的其它步骤和其它成分。该术语涵盖术语“由……组成”和“基本上由……组成”。
除非另外说明,否则所有百分比、份数和比率均基于本发明的组合物的总重量。所有涉及所列成分的这些重量均基于活性物质的含量,并且因此不包括可能包含在可商购获得的物质中的载体或副产物。
本文中,“混合物”是指包括物质的简单组合以及可由它们的组合产生的任何化合物。
除非另外指明,否则如本文所用,术语“分子量”或“M.Wt.”是指重均分子量。可通过凝胶渗透色谱法来测量重均分子量。
“QS”是指足量至100%。
二氨基羧酸螯合剂
本发明的可溶性固体制品包含二氨基羧酸螯合剂及其盐。二氨基羧酸螯合剂及其盐以按制品的重量计约0.5%至约2%、优选地约0.75%至约1.5%的含量包含于制品中。
可用于本文的二氨基羧酸螯合剂及其盐是具有约250道尔顿至约450道尔顿、优选地约250道尔顿至350道尔顿的平均分子量(处于酸形式时)并且在pH 4下具有约-12至约-7、约-10至约-8的加权logP值的那些。
此类二氨基羧酸螯合剂包括例如下表中的那些及其盐。
其中,优选的是下表中的那些及其盐。
在pH4下的LogP | MW | |
乙二胺四乙酸 | -9.312 | 292.24 |
2-[3-[双(羧甲基)氨基]丙基-(羧甲基)氨基]乙酸 | -9.864 | 306.27 |
1,2-二氨基丙烷-N,N,N',N'-四乙酸 | -8.945 | 306.27 |
1,3-二氨基-2-丙醇-N,N,N',N'-四乙酸 | -10.843 | 322.27 |
2-[2-[2-[双(羧甲基)氨基]乙氧基]乙基-(羧甲基)氨基]乙酸 | -10.601 | 336.3 |
其中,更优选的是下表中的那些及其盐。
在pH4下的LogP | MW | |
乙二胺四乙酸 | -9.312 | 292.24 |
芳族羧酸
本发明的可溶性固体制品包含芳族羧酸及其盐。芳族羧酸及其盐以按制品的重量计约0.1%至约6%、优选地约0.2%至约5%、更优选地约0.3%至约4%的含量包含于制品中。
可用于本文的芳族羧酸及其盐是具有约100道尔顿至约400道尔顿、优选地约105道尔顿至约200道尔顿、更优选地约110道尔顿至约150道尔顿的平均分子量(处于酸形式时)并且在pH 4下具有约-2至约4、约-0.5至约2、更优选地约0至约1.5的加权logP值的那些。
此类芳族羧酸包括例如下表中的那些及其盐。
其中,优选的是下表中的那些及其盐。
在pH4下的LogP | MW | |
水杨酸(水杨酸钠/水杨酸钾) | 0.289 | 138.1207 |
苯甲酸(苯甲酸钠) | 0.91 | 122.1213 |
羟基肉桂酸 | 1.593 | 164.16 |
辛酰基水杨酸 | 3.27 | 264.32 |
迷迭香酸 | 2.535 | 360.3148 |
吡啶二羧酸 | -0.935 | 167.1189 |
阿魏酸 | 1.571 | 194.184 |
没食子酸 | 0.573 | 170.1195 |
对茴香酸 | 1.321 | 152.1473 |
肉桂酸 | 1.709 | 148.1586 |
松萝酸 | 1.228 | 344.3154 |
咖啡酸 | 1.353 | 180.1574 |
龙胆酸 | 0.07 | 154.1201 |
其中,更优选的是下表中的那些及其盐。
在pH4下的LogP | MW | |
水杨酸(水杨酸钠/水杨酸钾) | 0.289 | 138.1207 |
苯甲酸(苯甲酸钠) | 0.91 | 122.1213 |
如上所示,芳族羧酸及其盐优选地选自:至少一种选自水杨酸及其盐的物质、至少一种选自苯甲酸及其盐的物质、以及它们的混合物,更优选地选自它们的混合物。水杨酸及其盐可以按制品的重量计约0.1%至约2.5%、优选地约0.2%至约2%、更优选地约0.3%至约1.5%的含量包含于制品中。苯甲酸及其盐可以按制品的重量计约0.1%至约5%、优选地约0.2%至约3%、更优选地约0.3%至约2.5%的含量包含于制品中。
非芳族有机α羟基酸
本发明的可溶性固体制品包含非芳族有机α羟基酸(有机AHA)及其盐。非芳族有机AHA及其盐以按制品的重量计约0.1%至约18%、优选地约0.5%至约12%、更优选地约1%至约6%、还更优选地1%至约4%、甚至更优选约1%至约3%的含量包含于制品中。
可用于本文的有机AHA包括例如下表中的那些及其盐。
柠檬酸 |
乳酸 |
苹果酸 |
酒石酸 |
葡糖酸 |
甘油酸 |
木糖酸 |
半乳糖二酸 |
其中,优选的是下表中的那些及其盐。
柠檬酸 |
乳酸 |
葡糖酸 |
其中,更优选的是下表中的那些及其盐。
柠檬酸 |
非AHA非芳族酸
本发明的可溶性固体制品还可包含非AHA非芳族酸及其盐。非AHA非芳族酸及其盐可以按制品的重量计约0.1%至约10%、优选地约0.1%至约5%、更优选地约0.1%至约3%的含量包含于制品中。
可用于本文的非AHA非芳族酸包括例如下表中的那些及其盐。
山梨酸 |
琥珀酸 |
植酸 |
乙酸 |
丙二酸 |
富马酸 |
水合乙醛酸 |
HCl |
其中,优选的是有机酸及其盐,并且更优选的是下表中的那些及其盐。
山梨酸 |
琥珀酸 |
植酸 |
乙酸 |
二醇
本发明的可溶性固体制品还可包含二醇。二醇可以按制品的重量计约0.1%至约2%、优选地约0.25%至约1.5%的含量包含于制品中。
可用于本文的二醇是具有约90道尔顿至约500道尔顿、优选地约100道尔顿至约250道尔顿、更优选地约110道尔顿至约160道尔顿的平均分子量并且在pH 4下具有约-1至约12、约0至约7、更优选地约0.5至约4的加权logP值的那些。
可用于本文的此类二醇包括例如下表中的那些。
在pH4下的LogP | MW | |
1,2-己二醇 | 0.92 | 118.17 |
1,2-辛二醇 | 1.83 | 146.23 |
1,2-二十八烷二醇 | 10.952 | 426.76 |
1,2-十八烷二醇 | 6.39 | 286.4931 |
1,2-十六烷二醇 | 5.478 | 258.44 |
1,2-十四烷二醇 | 4.565 | 230.3868 |
1,2-癸二醇 | 2.741 | 174.2805 |
1,2-十二烷二醇 | 3.653 | 202.3336 |
1,2-二十六烷二醇 | 10.04 | 398.71 |
花生甘醇 | 7.302 | 314.55 |
1,2-戊二醇 | 0.459 | 104.1476 |
1,3-庚二醇 | 0.978 | 132.2007 |
1,5-己二醇 | 0.578 | 118.1742 |
1,3-己二醇 | 0.522 | 118.1742 |
1,2,6-己三醇 | -0.31 | 134.1736 |
2-氨基-5-甲基-1-己醇 | -0.127 | 131.216 |
7-辛烯-1,2-二醇 | 1.437 | 144.21144 |
1-甲基-1-辛醇 | 3.172 | 144.2545 |
辛-2-醇 | 2.716 | 130.22792 |
壬醇-3 | 3.24 | 144.2545 |
其中,优选的是下表中的那些。
在pH4下的LogP | MW | |
1,2-己二醇 | 0.92 | 118.17 |
1,2-辛二醇 | 1.83 | 146.23 |
1,2-二十八烷二醇 | 10.952 | 426.76 |
1,2-十八烷二醇 | 6.39 | 286.4931 |
1,2-十六烷二醇 | 5.478 | 258.44 |
1,2-癸二醇 | 2.741 | 174.2805 |
1,2-二十六烷二醇 | 10.04 | 398.71 |
1,2-戊二醇 | 0.459 | 104.1476 |
1,2,6-己三醇 | -0.31 | 134.1736 |
7-辛烯-1,2-二醇 | 1.437 | 144.21144 |
其中,更优选的是下表中的那些。
在pH4下的LogP | MW | |
1,2-己二醇 | 0.92 | 118.17 |
1,2-辛二醇 | 1.83 | 146.23 |
水溶性聚合物(“聚合物结构剂”)
本发明包含用作结构剂的水溶性聚合物。水溶性聚合物以按制品的重量计约10%至约50%、优选地约15%至约40%、更优选地约18%至约30%的含量包含于制品中。如本文所用,术语“水溶性聚合物”足够广义以包括水溶性和水分散性聚合物,并且定义为,在25℃下测定,水中溶解度为至少约0.1克/升(g/L)的聚合物。在一些实施方案中,所述聚合物具有在25℃下测量的约0.1克/升(g/L)至约500克/升(g/L)的水中溶解度。(这表明制得宏观各向同性的或透明的有色或无色的溶液)。用于制备这些固体的聚合物可源自合成或天然,并且可经由化学反应改性。它们可成膜或不可成膜。这些聚合物应是生理学上可接受的,即它们应与皮肤、粘膜、毛发和头皮相容。
术语“水溶性聚合物”和“聚合物结构剂”在本文中可互换使用。此外,当陈述单数术语“聚合物”时,应理解该术语足够广义以包括一种聚合物或者多于一种聚合物的混合物。例如,如果使用聚合物的混合物,则本文所指的聚合物溶解度将是指聚合物混合物的溶解度,而不是指每种聚合物单独的溶解度。
选择本发明的一种或多种水溶性聚合物,使得它们的重均分子量为约40,000至约500,000,在一个实施方案中为约50,000至约400,000,在另一个实施方案中为约60,000至约300,000,并且在又一个实施方案中为约70,000至约200,000。通过计算每种聚合物原材料的重均分子量与它们相应的按多孔固体内存在的聚合物总重量计的相对重量百分比的乘积的和来计算重均分子量。
在本发明中可使用多种水溶性聚合物,如下所示。其中,高度优选的是聚乙烯醇。
本发明的水溶性聚合物可包括但不限于合成聚合物,包括聚乙烯醇、聚乙烯吡咯烷酮、聚环氧烷、聚丙烯酸酯、己内酰胺、聚甲基丙烯酸酯、聚甲基丙烯酸甲酯、聚丙烯酰胺、聚甲基丙烯酰胺、聚二甲基丙烯酰胺、丙烯酸和甲基丙烯酸甲酯的共聚物、单甲基丙烯酸聚乙二醇酯、聚氨酯、聚羧酸、聚乙酸乙烯酯、聚酯、聚酰胺、聚胺、聚乙烯亚胺、马来酸/(丙烯酸酯或甲基丙烯酸酯)共聚物、甲基乙烯基醚与马来酸酐的共聚物、乙酸乙烯酯与巴豆酸的共聚物、乙烯吡咯烷酮与乙酸乙烯酯的共聚物、乙烯吡咯烷酮与己内酰胺的共聚物、乙烯吡咯烷酮/乙酸乙烯酯共聚物、阴离子、阳离子和两性单体的共聚物、以及它们的组合。
本发明的水溶性聚合物还可选自源自天然的聚合物,包括植物源的那些,其示例包括刺梧桐树胶、黄蓍胶、阿拉伯树胶、乙酰吗喃、魔芋葡苷聚糖、金合欢胶、达瓦树胶、乳清分离蛋白、和大豆分离蛋白;种子提取物,包括瓜尔胶、刺槐豆胶、温柏树籽和车前籽;海藻提取物诸如角叉菜胶、海藻酸盐和琼脂;果实提取物(果胶);微生物源的那些,包括黄原胶、结冷胶、普鲁兰、透明质酸、硫酸软骨素和葡聚糖;和动物源的那些,包括酪蛋白、胶质、角蛋白、角蛋白水解产物、磺基角蛋白、白蛋白、胶原、谷蛋白、高血糖素、谷胶、玉米蛋白和紫胶。
改性的天然聚合物也可用作本发明中的水溶性聚合物。适宜的改性天然聚合物包括但不限于,纤维素衍生物如羟丙基甲基纤维素、羟甲基纤维素、羟乙基纤维素、甲基纤维素、羟丙基纤维素、乙基纤维素、羧甲基纤维素、乙酸邻苯二甲酸纤维素、硝化纤维以及其他纤维素醚/酯;和瓜尔胶衍生物诸如羟丙基瓜尔胶。
合适的本发明水溶性聚合物包括聚乙烯醇、聚乙烯吡咯烷酮、聚环氧烷、淀粉和淀粉衍生物、普鲁兰、胶质、羟丙基甲基纤维素、甲基纤维素、和羧甲基纤维素。
更优选的本发明水溶性聚合物包括聚乙烯醇和羟丙基甲基纤维素。合适的聚乙烯醇包括可以Celvol商品名从Celanese Corporation(Dallas,TX)获得那些,包括但不限于Celvol 523、Celvol 530、Celvol 540、Celvol 518、Celvol、513、Celvol 508、Celvol 504、以及它们的组合。合适的羟丙基甲基纤维素包括以Methocel商品名从Dow ChemicalCompany(Midland,MI)获得那些,包括但不限于Methocel E50、Methocel E15、MethocelE6、Methocel E5、Methocel E3、Methocel F50、Methocel K100、Methocel K3、MethocelA400、以及它们的组合,包括与上述羟丙基甲基纤维素的组合。
最优选的本发明水溶性聚合物是聚乙烯醇,该聚乙烯醇的特征在于水解度在约40%至约100%、优选地约50%至约95%、更优选地约70%至约92%、最优选地约80%至约90%的范围内。可商购获得的聚乙烯醇包括以CELVOL商品名得自Celanese Corporation(Texas,USA)的那些,包括但不限于CELVOL 523、CELVOL 530、CELVOL 540、CELVOL 518、CELVOL 513、CELVOL 508、CELVOL 504;以和POVALTM商品名得自Kuraray EuropeGmbH(Frankfurt,Germany)的那些;以及PVA 1788(也称为PVA BP17),其可商购获自各种供应商,包括Lubon Vinylon Co.(Nanjing,China),例如,BP-17(其具有86-90%的水解度,近似MW(重均)=70,000道尔顿-120,000道尔顿,可获自Liwei Chemical Co.Ltd.,China);以及它们的组合。在本发明的一个特别优选的实施方案中,柔性多孔可溶性固体片材制品包含按此类制品总重量计约10%至约25%,更优选地约15%至约23%的具有80,000道尔顿至约150,000道尔顿的重均分子量和约80%至约90%的水解度的聚乙烯醇。
表面活性剂
本发明的可溶性固体制品包含表面活性剂。表面活性剂以按制品的重量计约20%至约80%、优选地约23%至约75%、更优选地约35%至约65%的含量包含于制品中。
表面活性剂包含I组表面活性剂和II组表面活性剂的共混物。本发明的表面活性剂的共混物包含来自I组的一种或多种表面活性剂和来自II组的一种或多种表面活性剂。I组表面活性剂包括阴离子表面活性剂,并且II组表面活性剂包括两性表面活性剂、两性离子表面活性剂以及它们的组合。在本发明的一个实施方案中,I组表面活性剂与II组表面活性剂的比率为约90:10至约55:45。在本发明的又一个实施方案中,I组表面活性剂与II组表面活性剂的比率为约85:15至约65:35。
I组表面活性剂
本发明的I组表面活性剂包括一种或多种阴离子表面活性剂。用于本文可溶性制品中的合适阴离子表面活性剂组分包括已知用于毛发护理或其他个人护理清洁组合物中的那些。组合物中阴离子表面活性剂组分的浓度应足以提供所需的清洁和发泡性能,为I组表面活性剂的干固体的约6.5重量%至约71重量%。
适用于所述组合物中的阴离子表面活性剂包括不含硫酸盐的表面活性剂。此类不含硫酸盐的表面活性剂可包括衍生自氨基酸的物质,诸如单羧酸盐和二羧酸盐,诸如谷氨酸盐、甘氨酸盐、牛磺酸盐、丙氨酸盐或肌氨酸盐。示例包括月桂酰谷氨酸钠、椰油基谷氨酸钠、月桂酰谷氨酸钾、椰油基丙氨酸钠、椰油基甘氨酸钠、月桂酰肌氨酸钠、椰油基肌氨酸钠、椰油基甲基牛磺酸钠、月桂基甲基羟乙基磺酸钠、椰油基羟乙基磺酸钠、或油酰肌氨酸钠。
适用于所述组合物中的阴离子表面活性剂包括烷基硫酸盐和烷基醚硫酸盐。这些材料分别具有式ROSO3M和RO(C2H4O)xSO3M,其中R是约8至约18个碳原子的烷基或烯基,x是值为1至10的整数,并且M是阳离子,诸如铵、链烷醇胺(诸如三乙醇胺)、单价金属(诸如钠和钾)和多价金属阳离子(诸如镁和钙)。优选地,在烷基和烷基醚硫酸盐中,R具有约8至约18个碳原子、更优选地约10至约16个碳原子、甚至更优选地约11至约14个碳原子。烷基醚硫酸盐通常制备成环氧乙烷和具有约8至约24个碳原子的一元醇的缩合产物。醇可以是合成的,或者它们可以衍生自脂肪,例如椰子油、棕榈仁油、牛脂。合成醇可包括可经由ShellChemical Co.以NEODOL商品名(NEODOL 91(C9-11醇)、NEODOL 23(C12-13醇)、NEODOL 25(C12-15醇)、NEODOL 45(C14-15醇)和NEODOL 135(C11-C13-C15醇))获得的等级。月桂醇和衍生自椰子油或棕榈仁油的直链醇是优选的。此类醇与约0至约10(在一个实施方案中为约2至约5,在另一个实施方案中为约3)摩尔比例的环氧乙烷反应,并且将所得分子种类的混合物(例如每摩尔醇具有平均3摩尔环氧乙烷)硫酸化并中和。
其他合适的阴离子表面活性剂是符合式[R1-SO3-M]的有机硫酸反应产物的水溶性盐,其中R1是具有约8至约24、优选地约10至约18个碳原子的直链或支链饱和脂族烃基;并且M是上文所述的阳离子。
其他合适的阴离子表面活性剂是用羟乙磺酸酯化并用氢氧化钠中和的脂肪酸的反应产物,其中例如脂肪酸衍生自椰子油或棕榈仁油;氨基乙磺酸甲酯的脂肪酸酰胺的钠盐或钾盐,其中脂肪酸例如衍生自椰子油或棕榈仁油。其他类似的阴离子表面活性剂描述于美国专利号2,486,921、2,486,922和2,396,278中。
适用于组合物中的其他阴离子表面活性剂是琥珀酸盐,其示例包括N-十八烷基磺基琥珀酸二钠;月桂基磺基琥珀酸二钠;月桂基磺基琥珀酸二铵;N-(1,2-二羧基乙基)-N-十八烷基磺基琥珀酸四钠;磺基琥珀酸钠的二戊基酯;磺基琥珀酸钠的二己基酯;和磺基琥珀酸钠的二辛基酯。
其他合适的阴离子表面活性剂包括具有约10至约24个碳原子的烯烃磺酸盐。除真正的烯烃磺酸盐和一定比例的链烷烃磺酸盐外,烯烃磺酸盐还可以含有微量其他物质,诸如烯烃二磺酸盐,这取决于反应条件、反应物的比例、初始烯烃的性质和烯烃原料中的杂质以及磺化过程期间的副反应。此类α-烯烃磺酸盐混合物的非限制性示例描述于美国专利3,332,880中。
适用于组合物中的另一类阴离子表面活性剂是β-烷氧基链烷烃磺酸盐。这些表面活性剂符合下式
其中R1是具有约6至约20个碳原子的直链烷基基团,R2是具有约1至约3个碳原子、优选地1个碳原子的低级烷基基团,并且M是如上文所述的水溶性阳离子。
适用于组合物中的其他阴离子表面活性剂包括月桂基硫酸铵、月桂基醚硫酸铵、月桂基醚-1硫酸铵、月桂基醚-2硫酸铵、月桂基醚-3硫酸铵、月桂基硫酸三乙醇胺、月桂基醚硫酸三乙醇胺、月桂基醚-1硫酸三乙醇胺、月桂基醚-2硫酸三乙醇胺、月桂基醚-3硫酸三乙醇胺、月桂基硫酸单乙醇胺、月桂基醚硫酸单乙醇胺、月桂基硫酸二乙醇胺、月桂基醚硫酸二乙醇胺、月桂基单甘油酯硫酸钠、月桂基硫酸钠、月桂基醚硫酸钠、月桂基硫酸钾、月桂基醚硫酸钾、月桂基肌氨酸钠、月桂酰基肌氨酸钠、月桂基肌氨酸、椰油基肌氨酸、椰油酰基硫酸铵、月桂酰基硫酸铵、椰油酰基硫酸钠、月桂酰基硫酸钠、椰油酰基硫酸钾、月桂酰基硫酸钾、椰油酰基硫酸单乙醇胺、月桂酰基硫酸单乙醇胺、十三烷基苯磺酸钠、十二烷基苯磺酸钠、椰油酰基羟乙基磺酸钠、癸基硫酸铵、癸基硫酸钠、十一烷基硫酸铵和十一烷基硫酸铵以及它们的组合。
在本发明的一个实施方案中,表面活性剂中的一种或多种是烷基硫酸盐。在一个实施方案中,一种或多种烷基硫酸盐具有约0.0至约1.9的平均乙氧基化摩尔数,在另一个实施方案中,一种或多种烷基硫酸盐具有约0.0至约1.5的平均乙氧基化摩尔数,并且在又一个实施方案中,一种或多种烷基硫酸盐具有约0.0至约1.0的平均乙氧基化摩尔数。在一个实施方案中,一种或多种烷基硫酸盐包括铵抗衡离子。具有铵抗衡离子的此类表面活性剂的合适示例包括但不限于月桂基硫酸铵、月桂基醚-1硫酸铵、月桂基醚-2硫酸铵以及它们的组合。
在一个实施方案中,一种或多种I组表面活性剂选自具有以下结构的烷基硫酸盐:
其中R1选自C连接的单价取代基,这些单价取代基选自由包含平均9.0至11.9个碳原子的取代或未取代的直链或支链烷基或不饱和烷基系统组成的组;R2选自由包含2至3个碳原子的C连接的二价直链或支链烷基系统组成的组;M+是选自钠、铵或质子化三乙醇胺的单价抗衡离子;并且x为0.0至3.0。在一个实施方案中,根据以上结构的烷基硫酸盐表面活性剂中的一种或多种包括约0.0至约1.9的平均乙氧基化摩尔数,在另一个实施方案中,根据以上结构的烷基硫酸盐表面活性剂包括约0.0至约1.5的平均乙氧基化摩尔数,并且在又一个实施方案中,根据以上结构的烷基硫酸盐表面活性剂包括约0.0至约1.0的平均乙氧基化摩尔数。合适的示例包括癸基硫酸铵、癸基硫酸钠、十一烷基硫酸铵、十一烷基硫酸钠、癸基硫酸三乙醇胺或十一烷基硫酸三乙醇胺。在一个实施方案中,本发明的阴离子表面活性剂包括十一烷基硫酸铵。
II组表面活性剂
本发明的II组表面活性剂包括一种或多种两性表面活性剂、两性离子表面活性剂和/或它们的组合。适用于本文组合物中的两性表面活性剂或两性离子表面活性剂包括已知用于毛发护理或其他个人护理清洁中的那些。此类两性表面活性剂、两性离子表面活性剂和/或它们的组合的浓度在干燥固体的约1.0重量%至约52.5重量%的范围内。合适的两性离子或两性表面活性剂的非限制性示例描述于美国专利号5,104,646(Bolich Jr.等人)、5,106,609(Bolich Jr.等人)中。
适用于组合物中的两性表面活性剂是本领域熟知的,并且包括广泛描述为脂族仲胺和叔胺衍生物的那些表面活性剂,其中脂族基团可以是直链或支链的,并且其中一个脂族取代基包含约8至约18个碳原子,并且一个脂族取代基包含阴离子基团,诸如羧基、磺酸根、硫酸根、磷酸根或膦酸根。此类两性表面活性剂的合适示例包括但不限于椰油氨基丙酸钠、椰油氨基二丙酸钠、椰油酰两性基乙酸钠、椰油酰两性基羟丙基磺酸钠、椰油酰两性基丙酸钠、玉米油酰两性基丙酸钠、月桂氨基丙酸钠、月桂酰两性基乙酸钠、月桂酰两性基羟丙基磺酸钠、月桂酰两性基丙酸钠、玉米油酰两性基丙酸钠、月桂亚氨基二丙酸钠、椰油氨基丙酸铵、椰油氨基二丙酸铵、椰油酰两性基乙酸铵、椰油酰两性基二乙酸铵、椰油酰两性基羟丙基磺酸铵、椰油酰两性基丙酸铵、玉米油酰两性基丙酸铵、月桂氨基丙酸铵、月桂酰两性基乙酸铵、月桂酰两性基二乙酸铵、月桂酰两性基羟丙基磺酸铵、月桂酰两性基丙酸铵、玉米油酰两性基丙酸铵、月桂亚氨基二丙酸铵、椰油氨基丙酸三乙醇胺、椰油氨基二丙酸三乙醇胺、椰油酰两性基乙酸三乙醇胺、椰油酰两性基羟丙基磺酸三乙醇胺、椰油酰两性基丙酸三乙醇胺、玉米油酰两性基丙酸三乙醇胺、月桂氨基丙酸三乙醇胺、月桂酰两性基乙酸三乙醇胺、月桂酰两性基羟丙基磺酸三乙醇胺、月桂酰两性基丙酸三乙醇胺、玉米油酰两性基丙酸三乙醇胺、月桂亚氨基二丙酸三乙醇胺、椰油酰两性基二丙酸、癸酰两性基二乙酸二钠、癸酰两性基二丙酸二钠、辛酰两性基二乙酸二钠、辛酰两性基二丙酸二钠、椰油酰两性基羧乙基羟丙基磺酸二钠、椰油酰两性基二乙酸二钠、椰油酰两性基二丙酸二钠、二羧乙基椰油基丙二胺二钠、月桂基聚氧乙烯醚-5羧基两性基二乙酸二钠、月桂亚氨基二丙酸二钠、月桂酰两性基二乙酸二钠、月桂酰两性基二丙酸二钠、油基两性基二丙酸二钠、PPG-2-异癸醇聚醚-7羧基两性基二乙酸二钠、月桂氨基丙酸、月桂酰两性基二丙酸、月桂基氨基丙基甘氨酸、月桂基二亚乙基二氨基甘氨酸以及它们的组合。
在一个实施方案中,两性表面活性剂是根据以下结构的表面活性剂:
其中R1为C-连接的一价取代基,该取代基选自包含9至15个碳原子的取代的烷基体系、包含9至15个碳原子的未取代的烷基体系、包含9至15个碳原子的直链烷基体系、包含9至15个碳原子的支链烷基体系、和包含9至15个碳原子的不饱和烷基体系;R2、R3和R4各自独立地选自包含1至3个碳原子的C-连接的二价直链烷基体系和包含1至3个碳原子的C-连接的二价支链烷基体系;并且M+为一价抗衡离子,该一价抗衡离子选自钠、铵和质子化三乙醇胺。合适的表面活性剂的具体示例包括椰油酰两性基乙酸钠、椰油酰两性基二乙酸钠、月桂酰两性基乙酸钠、月桂酰两性基二乙酸钠、月桂酰两性基乙酸铵、椰油酰两性基乙酸铵、月桂酰两性基乙酸三乙醇胺和椰油酰两性基乙酸三乙醇胺。
适用于组合物中的两性离子表面活性剂在本领域中是已知的,并且包括被广泛地描述为脂族季铵、鏻和锍化合物的衍生物的那些表面活性剂,其中脂族基团可为直链或支化的,并且其中脂族取代基之一包含约8至约18个碳原子,并且一个脂族取代基包含阴离子基团诸如羧基、磺酸根、硫酸根、磷酸根或膦酸根。合适的两性离子表面活性剂包括但不限于椰油酰胺基乙基甜菜碱、椰油酰胺基丙基氧化胺、椰油酰胺基丙基甜菜碱、椰油酰胺基丙基二甲基氨基羟丙基水解胶原、椰油酰胺基丙基二甲基铵羟丙基水解胶原、椰油酰胺基丙基羟基磺基甜菜碱、椰油甜菜碱酰胺基两性基丙酸盐、椰油基甜菜碱、椰油基羟基磺基甜菜碱、椰油基/油基酰胺基丙基甜菜碱、椰油基磺基甜菜碱、月桂酰胺基丙基甜菜碱、月桂基甜菜碱、月桂基羟基磺基甜菜碱、月桂基磺基甜菜碱以及它们的组合。
任选的表面活性剂
本发明的组合物还可包含附加的表面活性剂以用于与上文所述的阴离子去污表面活性剂组分组合。合适的任选表面活性剂包括非离子和阳离子表面活性剂。可使用本领域已知的用于毛发或个人护理产品中的任何此类表面活性剂,前提条件是任选的附加表面活性剂也与组合物的基本组分在化学上和物理上相容,或者不会不适当地削弱产品性能、美观性或稳定性。任选的附加表面活性剂在组合物中的浓度可随所需的清洁或发泡性能、所选的任选表面活性剂、所需的产品浓度、组合物中其他组分的存在、以及本领域熟知的其他因素而变化。
其他适用于组合物中的阴离子表面活性剂、两性离子表面活性剂、两性表面活性剂或任选的附加表面活性剂的非限制性示例描述于McCutcheon的《Emulsifiers andDetergents》(1989年鉴,由M.C.Publishing Co.出版)和美国专利号3,929,678、2,658,072、2,438,091、2,528,378中。
增塑剂
本发明的可溶性固体制品还可包含适用于个人护理组合物中的水溶性增塑剂。水溶性增塑剂可以按制品的重量计约0.1%至约25%的含量包含于制品中。合适的增塑剂的非限制性示例包括多元醇、共聚多元醇和聚酯。可用的多元醇的示例包括但不限于:甘油、双甘油、丙二醇、乙二醇、丁二醇、戊二醇、聚乙二醇(200-600)、多元低分子量醇(例如,C2-C8醇);单糖、二糖和低聚糖,诸如果糖、葡萄糖、蔗糖、麦芽糖、乳糖,以及高果糖玉米糖浆固体。
任选成分
可溶性固体制品还可包含已知用于或可用于组合物中的其他任选成分,前提条件是此类任选物质与本文描述的所选基本物质相容,或者不会不适当地削弱产品的性能。
上述任选成分最典型地为那些被认可用于化妆品中并描述于参考书诸如“CTFACosmetic Ingredient Handbook”第二版(The Cosmetic,Toiletries,and FragranceAssociation,Inc.1988,1992)中的材料。
适用作本文任选成分的乳化剂包括甘油一酯和甘油二酯、脂肪醇、聚甘油酯、丙二醇酯、脱水山梨糖醇酯、以及已知的或以其他方式常用于稳定空气界面的其他乳化剂,如例如在充气食料诸如糕饼和其他烤焙物以及糖果产品制备期间或在稳定化妆品诸如毛发摩丝期间使用的那些。
此类任选成分的另外的非限制性示例包括防腐剂、香料或芳香剂、着色剂或染料、调理剂、毛发漂白剂、增稠剂、保湿剂、润肤剂、药物活性物质、维生素或营养物质、防晒剂、除臭剂、感觉剂、植物提取物、营养物质、收敛剂、化妆品颗粒、吸收剂颗粒、粘合剂颗粒、固发剂、纤维、反应剂、亮肤剂、皮肤美黑剂、去头皮屑剂、香料、去角质剂、酸、碱、湿润剂、酶、悬浮剂、pH调节剂、毛发着色剂、烫发剂、颜料颗粒、抗痤疮剂、抗微生物剂、防晒剂、美黑剂、去角质颗粒、毛发生长剂或恢复剂、驱虫剂、剃刮洗剂、共溶剂或其它附加的溶剂、以及类似的其它材料。
可以0.15%至约1.5%的含量添加附加的抗菌活性物质。此类抗菌活性物质是,例如:氯咪巴唑、吡罗克酮乙醇胺、氯己定、氯己定二盐酸盐、己脒定二羟乙基磺酸盐、氯苯甘醚、水杨酸钾、吡啶硫酮锌、苯氧乙醇、以及它们的组合。
可溶性固体制品
当用30份水对1份可溶性固体制品(基于重量)溶解时,可溶性固体制品具有约3至约5.1、优选地约3.5至约4.9、更优选地约3.8至约4.8的pH。
如本文所用,术语“固体”是指当没有向其施加外部力时制品在20℃和大气压下基本上保持其形状(即,其形状没有任何可见变化)的能力。
如本文所用,术语“柔性”是指当制品沿垂直于其纵向的中心线弯曲90°时制品承受应力而不破损或显著破裂的能力。优选地,此类制品可经历显著的弹性变形并且特征在于不大于5GPa、优选地不大于1GPa、更优选地不大于0.5GPa、最优选地不大于0.2GPa的杨氏模量。
可用于本文的可溶性固体制品能够溶解于液体,尤其是水性载体,更具体地是水。可向1份制品中加入约1份至100份、优选地约5份至约50份、更优选地约10份至约40份的水。
如本文所用,“可溶性”意指可溶性固体制品完全可溶于水中,或者其在根据手动溶解测试在水中混合时提供均匀的分散体。由手动溶解方法测量,所述可溶性固体制品具有约0个冲程至约30个冲程、另选地约0个冲程至约25个冲程、另选地约0个冲程至约20个冲程、并且另选地约0个冲程至约15个冲程的手动溶解值。“0个冲程”意指仅通过添加水,制品在没有任何剪切或手动冲程的情况下溶解。
可溶性固体制品优选为多孔的,并且其特征在于处于在如下范围内的密度:0.050g/cm3至约0.380g/cm3,优选地0.06克/cm3至0.3克/cm3,更优选地0.07克/cm3至0.2克/cm3,最优选地0.08克/cm3至0.15克/cm3。本发明的可溶性固体结构可以可溶性固体制品的形式提供,所述可溶性固体制品包含一个或多个柔性可溶性多孔片材,其中所述两个或更多个片材各自的特征在于为开孔泡沫、纤维结构等。所述多孔片材可任选地经由粘结方法(例如,热、水分、超声、压力等)而粘结在一起。
如本文所用,术语“开孔泡沫”或“开孔孔结构”是指限定空间或泡孔网络的含聚合物的固体连通基质,该空间或泡孔包含气体,通常为气体(诸如空气),同时保持固体的物理强度和粘结性。结构的互连性可通过开孔百分含量来描述,其通过下文公开的测试1测量。可用于本文的可溶性固体制品的特征在于开孔百分含量为80%至100%。
手动溶解测试方法
所需材料:
待测试的可溶性固体结构:测试3-5个可溶性固体结构(成品样品),使得如果计算单独可溶性固体结构样品,则记录每个可溶性固体样品的冲程数的平均值作为该可溶性固体结构的平均手动溶解值。对于这一方法,测试整个消费者可销售的或消费者使用的可溶性固体结构。如果整个消费者可销售的或消费者使用的可溶性固体结构具有大于5cm2的占有面积,则首先切割可溶性固体结构以具有5cm2的占有面积。
丁腈手套
5ml注射器
塑料称量舟皿(约3in×3in)
50mL玻璃烧杯
水(具有以下特性的新加坡城市水或等同物:按CaCO2计,总硬度=64mg/L;钙含量=23mg/L;镁含量=1.58mg/L;磷酸盐含量=0.017mg/L)
所用水为3gpg硬度和23℃+/-2℃
方案:
·将10mL水添加到玻璃烧杯中。
·使烧杯中的水冷却直至水处于23℃+/-2℃的温度。
·经由注射器将4mL水从烧杯转移到称量舟皿中。
·在将水转移到称量舟皿10秒内,将可溶性固体结构样品置于带手套的手掌中(以非惯用手保持可溶性固体结构样品,手处于托起位置)。
·使用惯用手,将水快速地从称量舟皿添加到可溶性固体结构样品中,并且允许立即润湿5-10秒的时间。
·在2个快速圆形冲程中,利用相对的惯用手(也带手套)摩擦。
·在2个冲程之后在手中从视觉上检查可溶性固体结构样品。如果可溶性固体结构样品完全溶解,则记录冲程数=2个溶解冲程。如果未完全溶解,则将剩余的可溶性固体结构样品揉搓2个以上的圆形冲程(总共4个)并观察溶解度。如果在2个附加的冲程之后可溶性固体结构样品不含有固体碎片,则记录冲程数=4个溶解冲程。如果在总共4个冲程之后,可溶性固体结构样品仍含有未溶解的可溶性固体结构样品的固体碎片,则在附加的2个圆形冲程中继续揉搓剩余的可溶性固体结构样品,并且在每次附加的2个冲程之后检查是否存在任何剩余的可溶性固体结构样品的固体碎片,直至可溶性固体结构样品完全溶解或直至达到总共30个冲程(无论哪个先发生)。记录冲程总数。记录30个溶解冲程,即使在最多30个冲程之后仍保留固体可溶性固体结构样品碎片。
·对附加的4个可溶性固体结构样品中的每一个重复该过程。
·为5个单独可溶性固体结构样品计算溶解冲程的记录值的算术平均值,并且将其记录为可溶性固体结构的平均手动溶解值。将平均手动溶解值记录至最接近的单个溶解冲程单元。
测试1:片材制品的开孔百分含量
经由气体测比重法测量开孔百分含量。气体测比重法是使用气体置换方法精确测定体积的常见分析技术。使用惰性气体如氦气或氮气作为置换介质。将本发明的固体片材制品样品密封于已知体积的仪器隔室中,导入适当的惰性气体,并且然后膨胀至另一个精确的内部体积。测量膨胀前后的压力,并且用于计算样品制品体积。
ASTM标准测试方法D2856使用较老的空气对比比重计模型,提供了测定开孔百分比的程序。该装置已不再制造。然而,通过执行使用Micromeritics的AccuPyc比重计的测试能够方便且精确地测定开孔百分比。ASTM程序D2856描述了用于测定泡沫材料开孔百分比的5种方法(A、B、C、D和E)。就这些实验而言,可使用氮气与ASTM foampyc软件,采用Accupyc1340来分析样品。ASTM程序中的方法C用于计算开孔百分比。该方法简单地将如使用厚度和标准体积计算测得的几何体积与如由Accupyc测得的开孔体积进行比较,根据以下等式:
开孔百分比=样品的开孔体积/样品的几何体积*100
推荐由Micromeretics Analytical Services,Inc.(One Micromeritics Dr,Suite 200,Norcross,GA 30093)进行这些测量。与该技术相关的更多信息可见于Micromeretics Analytical Services网站(www.particletesting.com或www.micromeritics.com),或公布于Clyde Orr和Paul Webb的“Analytical Methods inFine particle Technology”中。
可溶性固体制品的特征在于总体平均孔径为100μm至2000μm,如由下文测试2中所述的微-CT方法所测。总体平均孔径限定可溶性固体制品的孔隙率。
可溶性固体制品的特征可在于平均孔壁厚度或平均长丝直径为1μm至200μm,优选地10μm至100μm,更优选地20μm至80μm,还更优选地约25μm至60μm,如由下文测试2所测。
测试2:用于确定开孔泡沫(OCF)的总体或区域平均孔尺寸和平均孔壁厚度的微计
算机断层摄影术(μCT)方法
孔隙率是空隙空间与由OCF占据的总空间之间的比率。经由阈值来分割空隙空间并确定空隙体素与总体素的比率,可从μCT扫描计算孔隙率。类似地,固体体积分数(SVF)是固体空间与总空间之间的比率,并且SVF可被计算为所占据的体素与总体素的比率。孔隙率和SVF两者为平均标量值,其不提供结构信息,诸如OCF高度方向上的孔尺寸分布或OCF撑条的平均孔壁厚度。
为了表征OCF的3D结构,使用能够以高各向同性空间分辨率获取数据集的μCT X射线扫描仪器对样品成像。合适的仪器的一个示例是SCANCO系统模型50μCT扫描仪(ScancoMedical AG,Brüttisellen,Switzerland),其以以下设定操作:在133μA下45kVp的能量水平;3000个投影;15mm视野;750ms积分时间;取5次的平均;以及每像素3μm的体素大小。在扫描和随后的数据重建完成之后,扫描仪系统创建一个16位数据集,称为ISQ文件,其中灰度级反映x射线衰减的变化,而x射线衰减继而与材料密度有关。然后使用比例因子将ISQ文件转换为8位。
扫描的OCF样品通常通过冲压直径为大约14mm的核来制备。将OCF冲头平放在低衰减泡沫上,并且然后安装在15mm直径的塑料圆柱形管中进行扫描。获取样本的扫描,使得所有安装的切割样本的整个体积包括在数据集中。从这个较大的数据集中,从扫描的OCF的总横截面中提取样品数据集的较小子体积,创建3D数据板,其中可定性评估孔而没有边缘/边界效应。
为了表征高度方向上的孔尺寸分布和撑条尺寸,在子体积数据集上实施局部厚度图算法或LTM。LTM方法以欧几里德距离映射(EDM)开始,该映射指定灰度级值等于每个空体素距其最近边界的距离。基于EDM数据,表示孔的3D空隙空间(或表示撑条的3D实体空间)被镶嵌成尺寸与EDM值匹配的球体。由球体包围的体素被指定为最大球体的半径值。换句话说,每个空体素(或撑条的实体素)被指定最大球体的径向值,其既适合空隙空间边界(或撑条的实体空间边界)并且包括指定的体素。
来自LTM数据扫描的3D标记球体分布输出可被视为高度方向(或Z方向)上的二维图像的堆叠,并且用于估计作为OCF深度的函数的从切片到切片的球体直径的变化。将撑条厚度视为3D数据集,并且可评估子体积的全部或部分的平均值。使用来自Thermo FisherScientific的AVIZO Lite(9.2.0)和来自Mathworks的MATLAB(R2017a)进行计算和测量。
可溶性固体制品的特征可在于比表面积为0.03m2/g至0.25m2/g,优选地0.04m2/g至0.22m2/g,更优选地0.05m2/g至0.2m2/g,最优选地0.1m2/g至0.18m2/g,如由下文所述的测试3所测。本发明的固体片材的比表面积可表示其孔隙率并且可影响其溶解速率,例如,比表面积越大,片材的孔越多并且其溶解速率越快。
测试3:片材制品的比表面积
经由气体吸附技术测量柔性多孔可溶性固体片材制品的比表面积。表面积是分子级的固体样品暴露表面的量度。BET(Brunauer,Emmet,和Teller)理论是用于测定表面积的最流行模型,并且它基于气体吸附等温线。气体吸附使用物理吸附和毛细管冷凝来测量气体吸附等温线。该技术由以下步骤概述;将样品置于样品管中,并且在真空或流动的气体下加热以去除样品表面上的污物。通过从脱气样品和样品管总重量中减去空样品管的重量,获得样品重量。然后将样品管置于分析端口并且开始分析。分析方法中的第一步是将样品管排空,然后在液氮温度下使用氦气来测量样品管的自由空间体积。然后将样品第二次排空以去除氦气。然后仪器通过以使用者指定的间隔定量投入氪气,直到实现所需的压力量度,开始收集吸附等温线。然后可使用ASAP 2420和氪气吸附来分析样品。推荐由Micromeretics Analytical Services,Inc.(One Micromeritics Dr,Suite 200,Norcross,GA 30093)进行这些测量。与该技术相关的更多信息可见于MicromereticsAnalytical Services网站(www.particletesting.com或www.micromeritics.com),或公布于Clyde Orr和Paul Webb的书籍“Analytical Methods in Fine particleTechnology”中。
可溶性固体制品的特征可在于最终含水量为按所述制品的重量计0.5%至25%,优选地1%至20%,更优选地3%至10%,如由下文的测试4所测。所得固体片材中适当的最终含水量可确保片材期望的柔性/可变形性,以及为消费者提供柔软/光滑的感官感觉。如果最终含水量太低,则片材可能太脆或太硬。如果最终含水量太高,则片材可能太粘,并且其总体结构完整性可能受损。
测试4:片材制品的最终含水量
通过使用Mettler Toledo HX204水分分析仪(S/N B706673091)获得本发明的固体片材制品的最终含水量。将最少1g干燥的片材制品放在测量托盘上。然后执行标准程序,其中附加的程序设定为10分钟分析时间和110℃的温度。
产品
可溶性固体制品可为任何产品,包括例如个人护理产品、家庭护理产品、表面清洁产品、一般清洁产品。优选地,该产品为个人护理产品。此类个人产品包括例如个人清洁产品诸如身体、面部和/或手部清洁产品,皮肤护理产品诸如洗剂、面部喷雾、凝胶、霜膏,毛发护理产品诸如洗发剂和调理剂。
使用方法
可溶性固体制品的使用方法可包括以下步骤:a)将有效量的可溶性多孔固体施用于手,b)用水润湿可溶性多孔固体并摩擦以溶解固体,c)将溶解的物质施用于对象诸如毛发和/或皮肤,以及d)用水从对象冲洗掉溶解的物质。
实施例
以下实施例进一步描述并展示了本发明范围内的实施方案。这些实施例仅为了例证目的而给出并且不可被理解为是对本发明的限制,因为在不脱离本发明的实质和范围的情况下可能有许多变型。此处适用的成分均以化学名或CTFA名来识别,除非下文另外限定。
可溶性固体制品组成
可溶性固体制品组成
C4结果(革兰氏阴性菌)
细菌悬浮液的制备
通过用0.03M磷酸盐缓冲溶液(PBS)从琼脂平板上洗下细菌来制备1×106~9×106CFU/mL的金黄色葡萄球菌(S.aureus)ATCC6538或大肠杆菌(E.coli)ATCC25922细菌悬浮液。
对照样品的制备
使用5mL盐水溶液(0.85%w/v NaCl)作为测试的对照样品。
测试样品的制备
用30份水溶解并稀释1份上表中的组合物以制备测试样品。
测试
将100μl细菌悬浮液加入到5mL样品中以获得1×104~9×104CFU/mL以制备混合物,并且将该混合物涡旋并静置2分钟。然后,将1.0mL混合物转移到含有9.0mL的0.03M PBS的试管中并混合以稀释。用0.03M PBS进行系列稀释以将混合物的浓度稀释10000倍。通过将1.0mL的此系列稀释的混合物加入到2个陪替氏培养皿中来将该系列稀释的混合物铺板。
将熔融的(~20mL,40~45℃)胰酶大豆琼脂(TSA)倒入陪替氏培养皿中并涡旋混合。使琼脂冷却并硬化,然后翻转,并且在35±2℃下温育48小时。
如下计算杀菌率:
其中:
X4=杀菌率,%
A=对照样品上的平均细菌计数
B=测试样品上的平均细菌计数
评价标准
如果杀菌率≥50~90%,则可以报告所测试的产品具有抑菌作用。
如果杀菌率≥90%,则可以报告所测试的产品具有强效抑菌作用。
Ex.1至Ex.7的组合物是本发明实施例。CEx.i至CEx.iii的组合物是对比实施例。组合物CEx.i不含抗菌活性物质,组合物CEx.ii包含更高%的柠檬酸及其盐,并且CEx.iii的组合物具有更高的pH。
作为本发明实施例的Ex.1至Ex.7的组合物甚至在制品溶解后仍提供抗菌益处,同时控制抗菌活性成分在固体制品中的浓度。作为对比实施例的CEx.i至CEx.iii的组合物不提供抗菌益处。
本文所公开的量纲和值不应理解为严格限于所引用的精确数值。相反,除非另外指明,否则每个此类量纲旨在表示所述值以及围绕该值功能上等同的范围。例如,公开为“40mm”的量纲旨在表示“约40mm”。
除非明确排除或以其他方式限制,本文中引用的每一篇文献,包括任何交叉引用或相关专利或专利申请以及本申请对其要求优先权或其有益效果的任何专利申请或专利,均据此全文以引用方式并入本文。对任何文献的引用不是对其作为与本发明的任何所公开或本文受权利要求书保护的现有技术的认可,或不是对其自身或与任何一个或多个参考文献的组合提出、建议或公开任何此类发明的认可。此外,当本发明中术语的任何含义或定义与以引用方式并入的文献中相同术语的任何含义或定义矛盾时,应当服从在本发明中赋予该术语的含义或定义。
虽然已举例说明和描述了本发明的具体实施方案,但是对于本领域技术人员来说显而易见的是,在不脱离本发明的实质和范围的情况下可作出各种其他变化和修改。因此,本文旨在于所附权利要求中涵盖属于本发明范围内的所有此类变化和修改。
Claims (6)
1.一种可溶性固体制品,所述可溶性固体制品包含按所述制品的重量计:
a.约10%至约50%的水溶性聚合物;
b.约20%至约80%的表面活性剂;
c.约0.5%至约2%的处于酸形式时具有约250道尔顿至约450道尔顿的平均分子量并且在pH 4下具有约-12至约-7的加权logP值的二氨基羧酸螯合剂及其盐;
d.约0.1%至约6%的处于酸形式时具有约100道尔顿至约400道尔顿的平均分子量并且在pH 4下具有约-2至约4的加权logP值的芳族羧酸及其盐;
e.约0.1%至约18%的非芳族有机α羟基酸及其盐;
其中当用30份水对1份所述可溶性固体制品溶解时,所述可溶性固体制品具有约3至约5.1的pH。
2.根据权利要求1所述的可溶性固体制品,其中当用30份水对1份所述可溶性固体制品溶解时,所述可溶性固体制品具有约3.5至约4.9的pH。
3.根据前述权利要求中任一项所述的可溶性固体制品,其中当用30份水对1份所述可溶性固体制品溶解时,所述可溶性固体制品具有约3.8至约4.8的pH。
4.根据前述权利要求中任一项所述的可溶性固体制品,所述可溶性固体制品还包含约0.1%至约2.0%的具有约90道尔顿至约500道尔顿的平均分子量和在pH 4下约-1至约12的加权logP值的二醇。
5.根据前述权利要求中任一项所述的可溶性固体制品,其中所述可溶性固体制品包含两个或更多个柔性可溶性多孔片材。
6.根据前述权利要求中任一项所述的可溶性固体制品,其中所述可溶性固体制品具有在约0.050g/cm3至约0.380g/cm3范围内的密度。
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