CN115517991B - 一种三剂型安全无毒染发剂及其制备方法 - Google Patents
一种三剂型安全无毒染发剂及其制备方法 Download PDFInfo
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- CN115517991B CN115517991B CN202210089554.8A CN202210089554A CN115517991B CN 115517991 B CN115517991 B CN 115517991B CN 202210089554 A CN202210089554 A CN 202210089554A CN 115517991 B CN115517991 B CN 115517991B
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Abstract
本发明涉及A61K，更具体地，本发明涉及一种三剂型安全无毒染发剂及其制备方法。包括苏木素、儿茶酚胺、氧化剂、金属离子；本发明提供的染发剂通过使用润湿渗透剂暂时打开头发中的二硫键，使苏木素分子渗透并吸附在头发内部后，加入含有儿茶酚胺和金属离子的复合体系，利用金属离子和苏木素、儿茶酚胺的强螯合作用作为桥接，促进儿茶酚胺附着在头发内部，形成大分子结构，从而解决了以儿茶酚胺类物质(尤其是盐酸多巴胺)作为染发剂主要成分上染白发效果不佳的问题。具有优良的耐洗性，能耐受超过三十次的洗发且无明显褪色。染发方法简单，无需加热，染发效果可靠，安全无毒，具有较大的商业价值和良好的开发前景。
Description
技术领域
本发明涉及A61K，更具体地，本发明涉及一种三剂型安全无毒染发剂及其制备方法。
背景技术
目前市面上大多数染发剂为氧化型染发剂，其主要由染色前体，如苯二胺及苯二酚类等高毒性化合物，和氧化剂等小分子组成，其中苯二胺等染色前体当吸入呼吸道或接触皮肤时，可能会引发过敏和其他疾病，甚至存在诱导基因突变和致癌的风险，因此多年来以苯二胺类为主的永久性染发剂饱受诟病，故需要研发更佳安全无毒的染发剂。
此外，随着我国化妆品行业质量管理体制的日益完善以及人们健康和环保意识的不断深入，对染色剂的过敏性、刺激性、污染性的要求逐渐增加，并开发了许多绿色、低毒的染色前体，如植物色素或者纳米金颗粒等，但普遍存在提取率低、原料成本高昂、上染率低、牢固性差、色调单一以及步骤繁琐等缺点，限制了其商业化推广和使用。
专利号ZL201811362985.7、CN109846742A、CN11920695等报道了利用儿茶酚胺类物质自聚合生成黑色素类似物进行染发的方法，但是目前儿茶酚胺只能用于化纤类假发或漂白后的头发，而对自然老化褪色的白发染色效果较差，甚至几乎没有效果；且目前染发往往需要苛刻的染发条件，如在60℃左右染发，制备过程繁琐，难以达到商用目的。究其原因是传统的以儿茶酚胺为主要着色成分的各类染发方法存在涂层显色性差，覆盖率低等问题。因此，将儿茶酚胺类物质作为着色剂以替代传统染发剂的技术仍很不成熟，亟待突破。
发明内容
为了解决上述问题，本发明第一个方面提供了一种三剂型安全无毒染发剂，由A剂、B剂、C剂组成：
A剂包括苏木素；
B剂包括儿茶酚胺；
C剂包括氧化剂、金属离子。
作为本发明一种优选的技术方案，所述A剂的pH为9-11，苏木素占A剂的1-3wt％。所述A剂用pH调节剂调节pH，其中pH调节剂选自乙酸钠、乙酸、抗坏血酸、磷酸氢二钠、磷酸二氢钠、磷酸二氢钾、4-羟乙基哌嗪乙磺酸、巴比妥钠、柠檬酸、柠檬酸钠、甘氨酸、硼酸、硼砂、碳酸钠、碳酸氢钠、三羟甲基氨基甲烷、氢氧化钠和盐酸中的一种或多种。所述pH调节剂在A剂中的质量百分数根据pH来确定，如0.1-0.6wt％。
作为本发明一种优选的技术方案，所述儿茶酚胺占B剂的1-2wt％，氧化剂占C剂的2-3wt％，金属离子占C剂的2-4wt％。
作为本发明一种优选的技术方案，所述儿茶酚胺和金属离子的重量比为1-2：2-4。
作为本发明一种优选的技术方案，所述儿茶酚胺选自多巴胺或多巴胺的衍生物、左旋多巴或左旋多巴的衍生物、肾上腺素或肾上腺素的衍生物、去甲肾上腺素或去甲肾上腺素的衍生物中的一种或多种。
作为本发明一种优选的技术方案，所述金属离子选自二价金属离子和/或三价金属离子，可列举的有，Fe2+、Cu2+、Fe3+、Ca2+、Al3+、Mg2+、Zn2+，如氯化铁、氯化镁、硫酸锌、硫酸铜、氯化亚铁、明矾和硝酸铜等。
作为本发明一种优选的技术方案，所述A剂的溶剂为水相；B剂的溶剂为水相、油相和有机溶剂；C剂的溶剂为水相、油相和有机溶剂。本发明A剂、B剂、C剂中水相、油相和有机溶剂的种类可相同或不同，不做具体限定。
作为本发明一种优选的技术方案，所述氧化剂选自高碘酸钠、偏高碘酸钠、高碘酸钾、四丁基高碘酸铵、碘酸铵、碘酸钾等高碘酸或碘酸盐、过氧化氢等常规氧化剂中的一种或多种。
作为本发明一种优选的技术方案，所述水相为水或缓冲液，如有机酸盐缓冲液或无机酸盐缓冲液，可列举的有，乙酸盐缓冲液、磷酸盐缓冲液、柠檬酸盐缓冲液、硼酸盐缓冲液，所述缓冲液的pH为4-6。
作为本发明一种优选的技术方案，所述油相选自鲸蜡硬脂醇、石蜡、蜂蜡高级脂肪醇、凡士林、液体石蜡、植物油中的一种或多种。
作为本发明一种优选的技术方案，所述有机溶剂选自醇类溶剂、砜类溶剂、酮类溶剂中的一种或多种，所述醇类溶剂如乙醇、丁醇、戊醇、异丙醇、丙二醇、1，4-丁二醇等，所述砜类溶剂如二甲基亚砜等，所述酮类溶剂如二甲酮、甲乙酮等。
作为本发明一种优选的技术方案，所述B剂中有机溶剂的质量百分数为10-15wt％，油相的质量百分数为30-40wt％；所述C剂中有机溶剂的质量百分数为10-15wt％，油相的质量百分数为30-40wt％。
作为本发明一种优选的技术方案，所述A剂还包括助剂A，所述助剂A包括润湿渗透剂、表面活性剂、增稠剂、抗氧化剂、消泡剂中的至少一种；所述B剂还包括助剂B，所述助剂B包括表面活性剂、增稠剂、柔顺剂、消泡剂、染料中的至少一种；所述C剂还包括助剂C，所述助剂C包括增稠剂、表面活性剂、消泡剂中的至少一种。本发明所述A剂、B剂、C剂中助剂的具体种类可相同或不同，不做具体限定。
作为本发明一种优选的技术方案，所述助剂A包括润湿渗透剂，所述润湿渗透剂占助剂A的8-10wt％，所述润湿分散剂选自半胱氨酸或半胱氨酸酯类衍生物、谷胱甘肽中的至少一种。
作为本发明一种优选的技术方案，所述表面活性剂选自十二烷基硫酸钠、十二烷基磺酸钠、单硬脂酸甘油酯、鲸蜡醇、月桂基磺化琥珀酸单酯二钠、磺基琥珀酸单酯二钠，爱玛膏、吐温80、泊洛沙姆等表面活性剂中的一种或多种。所述A剂中表面活性剂的质量百分数为0.5-1wt％。
作为本发明一种优选的技术方案，所述增稠剂选自羧甲基纤维素、羧甲基纤维素钠、羟乙基纤维素、壳聚糖、海藻酸钠、瓜尔胶、泊洛沙姆、大豆蛋白胶、黄原胶、聚乙二醇、卡波姆、聚乙烯吡咯烷酮等常用增稠剂中的一种或多种。所述A剂、B剂、C剂中表面活性剂的质量百分数分别为1-2wt％、3-5wt％、3-5wt％。
作为本发明一种优选的技术方案，所述抗氧化剂选自亚硫酸氢钠、焦亚硫酸钠、亚硫酸钠、硫代硫酸钠、二丁基羟基甲苯、抗坏血酸、丁基羟基茴香醚等常用抗氧化剂中的一种或多种。所述A剂中抗氧化剂的质量百分数分别为0.5-1wt％。
作为本发明一种优选的技术方案，所述柔顺剂选自鲸蜡硬脂醇、椰油醇、甜菜碱等常用护发柔顺剂中的一种或多种。所述B剂中柔顺剂的质量百分数分别为1-3wt％。
作为本发明一种优选的技术方案，所述染料选自人工色素或天然色素中的一种或两种以上混合组成，人工色素或天然色素包括但不限于苋菜红、靛蓝、胭脂红、新红、柠檬黄、日落黄、亮蓝、赤红、诱惑红、β胡萝卜素、黑色素、甜菜红、姜黄素、红花黄、辣椒红、辣椒橙、焦糖色、玉米黄、萝卜红、红曲红、胭脂虫红、桅子黄、桅子兰、玫瑰茄红、芥菜红、藻兰、炭黑、红木素、降红木素。儿茶酚胺类染料前体经氧化剂氧化为黑色，为了实现其他颜色的染色，如金色、灰褐色、黑棕色、黑色等，本发明可控制儿茶酚胺的浓度，以及染料添加，使得染料和儿茶酚胺氧化中间体结合，如201910111411.0所示，本发明不对染料做具体限定，可根据染发颜色进行选择，其中染料在B剂的质量百分数为0-3wt％。
本发明第二个方面提供了一种所述的三剂型安全无毒染发剂的制备方法，包括：
A剂制备：将A剂原料混合，调节pH至9-11，得到A剂；
B剂制备：将B剂原料混合，得到B剂；
C剂制备：将C剂原料混合，得到C剂。
作为本发明一种优选的技术方案，所述A剂制备包括：将A剂溶剂加热至65-75℃后，依次将苏木素、润湿渗透剂、表面活性剂加入搅拌混匀、等待混合溶液降至室温时，依次加入抗氧化剂、增稠剂搅拌混匀。原料混合，调节pH至9-11，得到A剂；
作为本发明一种优选的技术方案，所述B剂制备包括：将表面活性剂加入水或缓冲液后混匀并加热到70-80℃，加入70-80℃油相和增稠剂的混合物，在70-80℃下保温10-25min后，加入儿茶酚胺搅拌溶解、加入柔顺剂和有机溶剂混匀后，得到B剂。
作为本发明一种优选的技术方案，所述C剂制备包括：将表面活性剂、金属离子依次加入水或缓冲液后混匀并加热到70-80℃，加入70-80℃油相和增稠剂的混合物，在70-80℃下保温10-25min后，温度降低到35-45℃后加入氧化剂搅拌溶解、加入有机溶剂混匀后，得到C剂。
本发明第三个方面提供了一种所述的三剂型安全无毒染发剂的使用方法，包括：将A剂涂抹在头发上10-20min后，清洗，涂抹B剂、C剂混合物，40-60min后清洗。
本发明与现有技术相比具有以下有益效果：
(1)本发明提供的染发剂通过使用润湿渗透剂暂时打开头发中的二硫键，使苏木素分子渗透并吸附在头发内部后，加入含有儿茶酚胺和金属离子的复合体系，利用金属离子和苏木素、儿茶酚胺的强螯合作用作为桥接，促进儿茶酚胺附着在头发内部，形成大分子结构，从而解决了以儿茶酚胺类物质(尤其是盐酸多巴胺)作为染发剂主要成分上染白发效果不佳的问题。
(2)此外，在儿茶酚胺附着在头发内部过程中，利用B/C混合制剂的有机溶剂和水/缓冲液的复合体系，尤其是醇类和水/缓冲液的混合体系，进一步促进金属离子桥接对儿茶酚的涂覆作用，且增强了儿茶酚胺类物质在头发表面原位涂覆类黑色素涂层显色程度，得到呈色效果均匀的棕黑色。
(3)此外，发明人也发现，控制B剂和C剂中金属离子和儿茶酚胺的螯合体系用量，可有效调控在有机溶剂和水/缓冲液的复合膏状体系中氧化剂的氧化速率，使得氧化剂缓慢可控地氧化儿茶酚胺或儿茶酚胺的衍生物产生黑色素类似物，并使其原位涂层于头发内部，达到染色的同时，金属离子与预先进入头发内部的苏木素分子可络合生成黑色大分子封锁固定在头发内部，从而进一步增强染黑效果和着色持久性。
(4)此外，发明人发现，相比于不使用苏木素、儿茶酚胺或金属离子的染色剂，本发明提供的苏木素/金属离子复合物辅助增强着色方案可先使苏木素进入头发内部，再与金属离子络合形成黑色大分子作为儿茶酚胺染发过程中的助色剂，可明显发挥强增色效果，着色和染黑效果能与苯二胺类商用染发剂相媲美。
(5)且本发明使用的有机溶剂优选无毒或低毒醇类，在促进调控原位涂层反应速率和反应程度的同时，得到的染发剂具有涂层和亮黑色效果优异、安全无毒、染色效果持久、生物相容性好、染发操作简便等优点。
(6)且在B/C制剂中使用pH调节剂制成的缓冲液作为水相，有利于维持整个反应体系的长期稳定性。此外，还可通过柔顺剂等闭合毛鳞片，修复头发表面结构。
(7)本发明提供的染发剂不含有对苯二胺、间苯二酚、氢醌、氨水等化学致癌物和刺激性成分，同时也不含有铅、汞、砷等有毒重金属，因此更加绿色安全的同时，通过本发明染色剂染发后，头发具有优良的耐洗性，能耐受超过三十次的洗发且无明显褪色。
(8)本发明的染发剂在生产及其使用过程中使用的各种组分均廉价易得，其制作方法简单，染发工艺容易形成规模化，无苛刻的合成条件。且染发方法简单，无需加热，染发效果可靠，安全无毒，具有较大的商业价值和良好的开发前景。
附图说明
图1为经本发明染发剂和商业染发剂染发后的效果对比图。
图2为经本发明染发剂和商业染发剂染发后的明度对比图。
图3为经本发明染发剂染发再洗涤后的效果对比图。
图4为经本发明染发剂染发再洗涤后的明度对比图。
具体实施方式
实施例
本例提供一种染发剂，包括：
所述A剂包括：十二烷基硫酸钠0.05g，L-半胱氨酸1g，羧甲基纤维素0.1g，抗坏血酸0.05g，碳酸氢钠0.06g，乙酸钠缓冲液8.74g，各组分质量合计为10g。
所述B剂包括：盐酸多巴胺0.1g，十二烷基硫酸钠0.1g，鲸蜡硬脂醇0.6g，硬脂酸0.3g，液体石蜡2.4g，吐温-80 1g，羟乙基纤维素0.3g，乙醇1g，甜菜碱0.2g，乙酸钠缓冲液(pH＝5)4g,各组分质量合计为10g。
所述C剂包括：高碘酸钠0.15g，氯化铁0.3g，十二烷基硫酸钠0.1g，鲸蜡硬脂醇0.6g，硬脂酸0.3g，羟乙基纤维素0.3g，液体石蜡2.4g，吐温80 1g，乙醇1g，乙酸钠缓冲液(pH＝5)3.85g，各组分质量合计为10g。
制作方法为：
A1、先将乙酸钠缓冲液加热至65-75℃后，依次将苏木素、L-半胱氨酸、十二烷基硫酸钠搅拌混匀、等待混合溶液降至室温时，依次加入抗坏血酸，羧甲基纤维素搅拌混匀。
A2、用碳酸氢钠调pH为9-11，得到A剂。
B1、将十二烷基硫酸钠加入乙酸钠缓冲液(pH＝5)后加入吐温80混匀并加热到70-80℃，得水相；
B2、将鲸蜡硬脂醇、硬脂酸、羟乙基纤维素和液体石蜡混合后加热到70-80℃，得油相；
B3、将油相加入到水相中搅拌、并在70-80℃下保温10-25min，随后加入盐酸多巴胺搅拌溶解、加入甜菜碱和乙醇混匀后，得到B剂。
C1、将十二烷基硫酸钠加入乙酸钠缓冲液(pH＝5)混匀后，加入氯化铁充分溶解，随后加入吐温80混匀并加热到70-80℃，得水相；
C2、将鲸蜡硬脂醇、硬脂酸、羟乙基纤维素和液体石蜡混合后加热到70-80℃，得油相；
C3、将油相加入到水相中搅拌、并在70-80℃下保温10-25min，随后待温度降低到35-45℃后加入高碘酸钠搅拌溶解、加入乙醇混匀后，得到C剂。
性能评价
将本实施例提供的染发剂进行染色：先将A剂涂抹在自然白发上等待10-20min后洗净，随后将B剂、C剂按照1：1的比例混匀后涂抹在头发上等待40-60min后洗净即可，并对染色后的头发和市售商业染发剂染色后的头发进行染发效果、明度值，以及洗涤后染色效果、明度值的测试。其中明度值测试方法为：用手持便携精密色差仪测量头发颜色的相关参数，每个头发样品测量十次求平均值，测量内容包括L*在内的颜色坐标值(其中L*表示明度，纯黑色明度最低，纯白色明度最高。通常明度值≤30的头发视为黑色，明度值≥60的头发被视为白色)。洗涤方法为：取一50mL离心管，加入40mL的5vol％市售洗发水，将头发样品完全浸泡其中，然后在涡旋混合器上剧烈振摇5min，随后用自来水冲洗，并用吹风机吹干。上述整个过程为一个洗发周期，本实验重复该过程30次，如图1-4所示。
从图1、2可看出，相比于市售染发剂，本发明提供的染发剂具有更好的染黑效果的同时，其明度值也相应下降，且从图2、3可看出，经本发明染发后的头发具有优良的耐洗性，能耐受超过三十次的洗发过程且无明显褪色。
Claims (1)
1.一种三剂型安全无毒染发剂，其特征在于，由A剂、B剂、C剂组成：
所述A剂包括：苏木素，十二烷基硫酸钠，L-半胱氨酸，羧甲基纤维素，抗坏血酸，碳酸氢钠和乙酸钠缓冲液，乙酸钠缓冲液pH=5；其中苏木素占A剂的1-3wt％；
所述B剂包括：盐酸多巴胺0.1g，十二烷基硫酸钠0.1g，鲸蜡硬脂醇0.6g，硬脂酸0.3g，液体石蜡2.4g，吐温-80 1g，羟乙基纤维素0.3g，乙醇1g，甜菜碱0.2g，乙酸钠缓冲液4g，各组分质量合计为10g，其中乙酸钠缓冲液pH=5；
所述C剂包括：高碘酸钠0.15g，氯化铁0.3g，十二烷基硫酸钠0.1g，鲸蜡硬脂醇0.6g，硬脂酸0.3g，羟乙基纤维素0.3g，液体石蜡2.4g，吐温80 1g，乙醇1g，乙酸钠缓冲液3.85g，各组分质量合计为10g，乙酸钠缓冲液pH=5；
所述A剂制备包括：先将乙酸钠缓冲液加热至65-75℃后，依次将苏木素、L-半胱氨酸、十二烷基硫酸钠搅拌混匀、等待混合溶液降至室温时，依次加入抗坏血酸，羧甲基纤维素搅拌混匀，然后用碳酸氢钠调pH为9-11；
所述B剂制备包括：将十二烷基硫酸钠加入乙酸钠缓冲液后加入吐温 80混匀并加热到70-80 ℃，得水相；将鲸蜡硬脂醇、硬脂酸、羟乙基纤维素和液体石蜡混合后加热到70-80℃，得油相；将油相加入到水相中搅拌、并在70-80 ℃下保温10-25 min，随后加入盐酸多巴胺搅拌溶解、加入甜菜碱和乙醇混匀；
所述C剂制备包括：将十二烷基硫酸钠加入乙酸钠缓冲液混匀后，加入氯化铁充分溶解，随后加入吐温80混匀并加热到70-80℃，得水相；将鲸蜡硬脂醇、硬脂酸、羟乙基纤维素和液体石蜡混合后加热到70-80 ℃，得油相；将油相加入到水相中搅拌、并在70-80 ℃下保温10-25 min，随后待温度降低到35-45℃后加入高碘酸钠搅拌溶解、加入乙醇混匀；
所述的三剂型安全无毒染发剂的使用方法为：将A剂涂抹在头发上10-20min后，清洗，涂抹B剂、C剂混合物，40-60 min后清洗。
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