CN101018904A - 成品纤维和纺织品组织 - Google Patents
成品纤维和纺织品组织 Download PDFInfo
- Publication number
- CN101018904A CN101018904A CNA200580026462XA CN200580026462A CN101018904A CN 101018904 A CN101018904 A CN 101018904A CN A200580026462X A CNA200580026462X A CN A200580026462XA CN 200580026462 A CN200580026462 A CN 200580026462A CN 101018904 A CN101018904 A CN 101018904A
- Authority
- CN
- China
- Prior art keywords
- active component
- textiles
- fiber
- acid
- microencapsulation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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Abstract
本发明涉及纤维和纺织品组织，其特征在于，它们由下述成分的混合物修整：(a)疏水性的活性组分、和(b)成膜聚合物。
Description
技术领域
本发明涉及纺织品领域，更具体而言，涉及具有改善了穿着舒适性的新成品纤维和纺织品组织(Textile Construction)，以及它们的制备方法及活性组分和粘合剂的混和物用于修整纺织品的用途。
背景技术
术语“穿着舒适性”特别地包括部分消费者增加的对舒适的期望，即不刺激或使皮肤变红，这些消费者不再简单地满足于穿戴紧贴皮肤的衣服，所述紧贴皮肤的衣服例如女内衣或裤袜。相反地，消费者也期望这些衣服对于皮肤状态有积极的作用，无论是在促进克服疲劳症状和给予新鲜香味方面，还是在避免皮肤粗糙方面。因此，在尝试使用能在穿着期间传递至皮肤和在那里产生预期效果的化妆品活性组分来修整纺织品，尤其是女性裤袜，其似乎是特别吸引人的消费者部分(consumer sector)，一直存在着不足。现在，很自然的是仅研究当相应活性组分从穿戴者转移到皮肤时，即，在穿戴或多或少的长时间后，不再有活性组分存在于衣服各部分上时的预期效果。这意味着当这些产品的制造商想要选择活性组分时，必须满足某些要求，因为考虑到性能、可应用的量、以及至关重要的涉及的费用，他不得不在活性成分可导致产品获得的效果和消费者准备支付的增加价格之间发现折中点(compromise)。因为具有预期效果的化妆品活性组分通常较贵，并且因为制备的最终产品也包括额外费用，所以，对制造商而言，特别重要的是，除了制备的最终产品和穿戴者的皮肤之间接触外，不想存在活性组分不需要的损耗，因为这将意味着消费者支付昂贵的费用的额外穿着舒适感只能在较短的时间有效。特别不想要的活性组分损失的形式存在于清洗纤维和由此修整的织物中。即使这些损失不能完全地避免，相应产品的制造商显然特别关注以不容易溶解或机械除去的方式将活性组分应用于纤维。
解决该问题的方法是使用微囊化的活性组分，其为给纤维纤丝之间加入粘合剂或将粘合剂应用于纤维。相应的方法是已知的，例如，来自EP0436729A1、WO 01/098578A1、US6,355,263、DE23 2318336A1和WO03/093571(Cognis)。然而，微囊化的缺点在于其给修整方法引入了另外的复杂性，当然，增加了成本。然而，更加重要的是许多胶囊不是十分稳定，释放活性组分太早，在最坏的情况下，其在本身应用过程中就释放了。相反地，如果使用以包囊系统为特征的特别稳定的胶囊来代替，活性组分可能仅在延长机械应力后才释放，因而，消费者不会立即感受到预期良好的效果。
因此，本发明解决的问题是用适宜的活性组分来修整纤维和纺织品，按这种方式，可给活性组分施加最小努力(minimal effort)，其将在第一次穿着期间逐渐释放，在洗涤5次后，至少20至50重量％的起始量将仍然存在于纤维或纺织品上。
发明内容
本发明涉及一种纤维和纺织品，其特征在于，所述混合物由下述物质修整：
(a)疏水性的活性组分，和
(b)成膜聚合物。
一般性技术偏见认为如果将活性组分预先微囊化，它们只能用于具有某些耐用性的纤维和纺织品上，与此相反，意外地发现可以应用疏水性的活性组分，即使没有包囊，只要将他们良好分散在具有成膜性能类型的高分子粘合剂中就行。本发明包括来自所谓的合成物修整的观察结果，即使在5至10次洗涤后，通常有10至50重量％的最初使用的活性组分保留在纤维上，这取决于粘合剂和活性组分的性质。另外，不存在微囊化，确保了活性组分可在第一次穿着期间缓慢释放，消费者也可以感受到预期效果。
活性组分
基本上，活性组分的选择不是关键性的，仅取决于它们在水中的溶解性，和施用于皮肤上达到的效果。在20℃下，活性组分优选在水中的溶解度小于10g/l，更加优选小于1g/l。
疏水性的活性组分是优选的，其对皮肤具有增湿性，抑制了蜂窝织炎(cellulitis)和/或具有缓解(soothing)效果。典型的实例为生育酚类、胡萝卜素化合物、甾醇、抗坏血酸棕榈酸酯、(脱氧)核糖核酸及其裂解产物、β-葡聚糖、视黄醇、没药醇、尿囊素、植烷三醇(phytantriol)、AHA酸、氨基酸、神经酰胺、拟神经酰胺、壳聚糖、薄荷醇、化妆用油和油组分、精油、植物蛋白及其水解产物、植物提取物、复合维生素、驱虫剂和纳米化的无机物或矿物及它们的混合物。
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生育酚类
生育酚类应理解为在2位用4，8，12-三甲基三癸基取代的苯并二氢吡喃-6-醇(3，4-二氢-2H-1-苯并吡喃-6-醇)。它们也被称为生物醌类。典型的实例为塑醌(plastiquinones)、生育酚醌、泛醌、boviquinones、K维生素和甲基萘醌类(例如2-甲基-1，4-萘醌)。优选使用来自维生素E族的苯醌，即和生育酚(这些中的最后一个仍然具有原始的不饱和异戊二烯基(prenyl)侧链，参见图)。
α-生育酚和α-生育醌
生育酚醌和氢醌以及醌与羧酸例如醋酸或棕榈酸的酯也是适宜的。优选使用α-生育酚、生育酚醋酸酯和生育酚棕榈酸酯及其混合物。
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胡萝卜素化合物
胡萝卜素化合物基本上可理解为胡萝卜素和类胡萝卜素。胡萝卜素为一组11x至12x-不饱和三萜。其中特别重要的是三种同分异构体α-、β-和γ-胡萝卜素，所有这三种都具有相同的基本骨架：包含9个共轭双键、8个甲基支链(包括可能的环状结构)和在分子一端的β-紫罗酮结构，其最初被认为是同类的天然材料。下面示出了许多适合作为组分(b)的胡萝卜素化合物，虽然其没有全部列出。
β-胡萝卜素
辣椒红
辣椒红素
虾青素
除了已经提及的异构体外，δ-、ε-、和ζ-胡萝卜素(番茄红素)也是适宜的，尽管β-胡萝卜素(前维生素A)必然特别重要，因为其分布广泛；在有机体中，其由酶裂解为两个视黄醛分子。类胡萝卜素为胡萝卜素的含氧衍生物，其也称为叶黄素，而且其基本骨架为8异戊二烯单元(四萜)。类胡萝卜素可能被认为由两个C20类异戊二烯(isoprenopids)通过两个彼此位于1，6-位的中心甲基连接组成。典型的实例为(3R，6’R)-β-ε-胡萝卜素-3，3’-二醇(叶黄素)、(3R，3’S，5’R)-3，3’-二羟基-β，κ-胡萝卜素-6-酮(辣椒红)、9’-顺式-6，6’-二脱胡萝卜素二酸(diapocarotendiacid)-6’-甲酯(胭脂树橙)、(3S，3’S，5R，5’R)-3，3’-二羟基-κ,κ-胡萝卜素-6，6’-二酮(辣椒红素)或3S，3’S-3，3’-二羟基-β，β’-胡萝卜素-4，4’-二酮(虾青素)。除了胡萝卜素和类胡萝卜素之外，本发明中的胡萝卜素化合物也包括解聚产物，例如3，7二甲基-9-(2，6，6-三甲基-1-环己烯基)-2，4，6，8-壬四烯-1-醇(视黄醇，维生素A1)和3，7-二甲基-9-(2，6，6-三甲基-1-环己烯基)-2，4，6，8-壬四烯醛(视黄醛，维生素A1醛)。
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甾醇
甾醇也称为固醇，为具有羟基连接到C3原子上的类固醇。甾醇通常包含27至30个碳原子和在5/6位的双键。双键的氢化导致甾醇经常被称为甾烷醇，其也包括在本发明内。下图示出了最熟知的甾醇、胆固醇的结构，其属于动物甾醇组。
由于它们优越的生理学性质，优选使用植物甾醇、所谓的植物甾醇。实例包括麦角固醇、豆甾醇，更加优选谷甾醇及其氢化产物二氢谷甾醇。本发明也包括甾醇酯，所有上述提及的具有包含6至26个碳原子和最多6个双链的饱和的或不饱和脂肪酸的甾醇缩合产物。
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壳聚糖
壳聚糖为生物聚合物，属于亲水(性)胶体组。从化学上来说，它们为部分地脱乙酰基的分子量不同的壳多糖，其包含下述理想的单体单元：
与大多数亲水(性)胶体相反，在生物学pH值下，其带负电，在该条件下，壳聚糖为阳离子生物聚合物。带正电荷的壳聚糖能够对相反的电荷表面构成影响，因此，可被用于化妆用毛发护理和身体护理产品和药物制剂。壳聚糖由壳多糖制备，优选由甲壳动物的壳残余物制备，其为大量市售的便宜的原材料。在Hackmann等人的首次报道的方法中，壳多糖通常首先通过加入碱来脱去蛋白质，再通过加入无机酸来脱矿质，最后通过加入强碱脱乙酰化，其分子量分布较广。优选的类型为具有平均分子量为10,000至500,000道尔顿或800,000至1,200,000道尔顿和/或Brookfield粘度(在乙醇酸中为1重量％)低于5,000mPas、脱乙酰度为80至88％和灰分小于0.3重量％的类型。
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化妆用油和油组分
适宜的化妆用油和油组分为，例如基于包含6至18个，优选包含8至10个碳原子的脂肪醇的Guerbet醇、具有直链或支链C6-22脂肪醇的直链C6-22脂肪酸酯或具有直链或支链C6-22脂肪醇的支链C6-13羧酸酯，例如肉豆蔻酸肉豆蔻酯、棕榈酸肉豆蔻酯、硬脂酸肉豆蔻酯、异硬脂酸肉豆蔻酯、油酸肉豆蔻酯、山嵛酸肉豆蔻酯、芥酸肉豆蔻酯、肉豆蔻酸鲸蜡酯、棕榈酸鲸蜡酯、硬脂酸鲸蜡酯、异硬脂酸鲸蜡酯、油酸鲸蜡酯、山萮酸鲸蜡酯、芥酸鲸蜡酯、肉豆蔻酸硬脂酯、棕榈酸硬脂酯、硬脂酸硬脂酯、异硬脂酸硬脂酯、油酸硬脂酯、山萮酸硬脂酯、芥酸硬脂酯、肉豆蔻酸异硬脂酯、棕榈酸异硬脂酯、硬脂酸异硬脂酯、异硬脂酸异硬脂酯、油酸异硬脂酯、山萮酸异硬脂酯、油酸异硬脂酯、肉豆蔻酸油酯、棕榈酸油酯、硬脂酸油酯、异硬脂酸油酯、油酸油酯、山萮酸油酯、芥酸油酯、肉豆蔻酸山萮酯、棕榈酸山萮酯、硬脂酸山萮酯、异硬脂酸山萮酯、油酸山萮酯、山萮酸山萮酯、芥酸山萮酯、肉豆蔻酸芥酯、棕榈酸芥酯、硬脂酸芥酯、异硬脂酸芥酯、油酸芥酯、山萮酸芥酯和芥酸芥酯。优选直链C6-22脂肪酸与支链醇，更优选与2-乙基己醇的酯、C18-38烷基羟基羧酸与直链或支链C6-22脂肪醇的酯，特别优选二辛基苹果酸酯、直链和/或支链脂肪酸与多元醇(例如丙二醇、二聚二醇或三聚三醇)和/或Guerbet醇的酯、基于C6-10脂肪酸的甘油三酯、基于C6-18脂肪酸的液态单/二/三甘油酯混合物、C6-22脂肪醇和/或Guerbet醇与芳香族羧酸，更加优选与苯甲酸的酯、C2-12二羧酸与包含1至22个碳原子的直链或支链醇或包含2至10个碳原子和2至6个羟基的多元醇的酯、植物油、支链伯醇、取代的环己烷，直链和支链C6-22脂肪醇碳酸酯，例如碳酸二辛酯(DicaprylylCarbonate)(CetiolCC)、基于包含6至18个，优选包含8至10个碳原子的脂肪醇的Guerbet碳酸酯、苯甲酸与直链和/或支链C6-22醇(例如FinsolvTN)的酯、直链或支链的，对称的或不对称的每个烷基包含6至22个碳原子的二烷基醚，例如二辛基醚(CetiolOE)、环氧化脂肪酸酯与多元醇的酯的开环产物、(聚)硅氧烷油(环甲硅油、甲硅油(silicon methicone)类型等)和/或脂肪族或环烷烃，例如角鲨烷、角鲨烯或二烷基环己烷。
纳米化的无机物质和矿物
“纳米颗粒”应理解为经过适宜的制备方法后，微粒具有的平均粒径为0.01至0.1μm。已知一种通过快速展开超临界溶液(RESS process)来制备纳米颗粒的方法(RESS process)，例如，来自S.Chihlar，M.Türk and K.Schaber在Proceedings World Congress on Particle Technology 3，Brighton，1998中的报道。为了防止纳米颗粒凝聚，建议在存在适宜的保护胶体或乳化剂条件下溶解原料，和/或展开于临界溶液中，形成保护胶体或乳化剂的含水和/或醇溶液或形成化妆用油，其可以依次包含再溶解乳化剂和/或保护胶体。适宜的保护胶体为，例如明胶、酪蛋白、壳聚糖、阿拉伯胶、卵清酸、淀粉，和聚合物例如聚乙烯醇、聚乙烯基吡咯烷酮、聚亚烷基二醇和聚丙烯酸酯。
另一种用于制备纳米颗粒的适宜方法是蒸发法。此处，首先将壳聚糖溶于适宜的有机溶剂中(例如链烷烃、植物油、醚、酯、酮、缩醛等)。然后，将溶液引入到水或另一种非溶剂中，在任选地存在溶解于其中的表面活性化合物的情况下，以便纳米颗粒通过两种不互溶溶剂的均化作用而沉淀，优选蒸发有机溶剂。O/w或o/w微乳状液可以使用水溶液来代替。开始时提到的乳化剂和保护胶体可被用作表面活性化合物。
用于制备纳米颗粒的另一种方法为所谓的GAS方法(气体抗溶剂重结晶)。该方法使用高压气体或超临界流体(例如二氧化碳)作为非溶剂来结晶溶解的物质。将压缩的气体相引入到原料的主要溶液中，吸收到其中，因此，液体体积增加，溶解性降低，沉淀出细小颗粒。
PCA法(用压缩的流体抗溶剂沉淀)也同样适宜。在该方法中，将原料的主要溶液引入到超临界流体中，导致形成非常细小的小滴，其中发生扩散过程，因此，沉淀出非常小的颗粒。
在PGSS法(从气体饱和溶液中沉淀颗粒)中，在压力下通过引入气体(例如二氧化碳或丙烷)来熔化原料。温度和压力达到接近或超临界状态。将气相溶于固体中，并降低熔化温度、粘性和表面张力。在通过喷嘴展开时，由于冷却效应形成非常小的颗粒。
制备纳米颗粒的另一种方法为GPC或PVS法(气相冷凝；物理式水蒸气合成)，其中，用氧气氧化等离子体汽化的金属并接受控制冷凝。
根据本发明，优选活性组分为纳米化的氧化锌，其比常规氧化锌具有出人意料的较高的抗神经性皮炎活性。因此，本发明还涉及任选地微囊化纳米化的氧化锌用于修整纤维和纺织品以及用于制备化妆品和/或药物制剂的用途。氧化锌纳米颗粒通常具有0.1至0.2μm的平均直径。二氧化钛及其它纳米金属氧化物和纳米混合氧化物，例如ITO和ATO也是适宜的。
根据最宽的作用特性透视可以看出，特别优选使用下述活性组分：
●生育酚、生育酚醋酸酯、生育酚棕榈酸酯，
●β-胡萝卜素、视黄醇，
●希蒙得木油，
●植物性甘油三酯，例如椰子油、棕榈油、杏仁油或榛子油，
●精油，
●角鲨烷，
●壳聚糖，
●薄荷醇，
●植物性或动物性(丝状)蛋白质及其水解产物，
●N，N-二乙基-3-甲基苯甲酰胺(DEET)和
●纳米化的氧化锌或二氧化钛
因为，分别或组合使用，它们
●有助于皮肤水油层(hydrolipid layer)的平衡，
●防止水分流失和因此产生的皱纹，
●保持皮肤柔嫩和抗疲劳症状；
●给予皮肤柔软和弹性的感觉，
●改善真皮排水，提供营养和促进循环，
●起抗氧化刺激、环境毒素、皮肤衰老和自由基的作用，
●补偿由于水和阳光引起的脂肪损失，
●抗蜂窝织炎，
●改善UV过滤器的抗水性，
●促进和延长晒黑，
●抗御或杀死昆虫，以及
●具有杀菌、抗炎症和抗神经性皮炎的性质。
活性组分在成品纤维和纺织品中的百分量，表示活性物质为0.1至10重量％，优选为0.25至7.5重量％，特别优选0.5至5重量％。
粘合剂
适于本发明目的的聚合的成膜粘合剂可选自：
●聚氨酯，
●聚乙基醋酸乙烯酯，
●聚三聚氰胺化合物，
●聚乙二醛化合物，
●聚硅氧烷化合物，
●环氧氯丙烷交联的聚酰胺基胺，
●聚(甲基)丙烯酸酯，和
●聚氟碳化合物。
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聚氨酯和聚醋酸乙烯酯
适宜的聚氨酯(PU)和聚乙基醋酸乙烯酯(EVA)为可商业获得的产品，售自Cognis Deutschland GmbH&Co.KG的Stabiflex和stabicryl系列。
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聚三聚氰胺化合物
三聚氰胺(又名：2，4，6-三氨基-1，3，5-三嗪)通常由双氰胺的三聚作用或采用二氧化碳与氨的消去反应与尿素环化而形成。在本发明中，三聚氰胺应当理解为三聚氰胺与甲醛、尿素、苯酚的寡聚或聚合缩合产物或它们的混合物。
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聚乙二醛化合物，
乙二醛(又名：oxaldehyde、ethanedial)为在存在银催化剂的情况下，乙二醇与空气气相氧化形成。本发明中的乙二醛应当理解为乙二醛(“polyglyoxals”)的自缩合产物。
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聚硅氧烷化合物
适宜的(聚)硅氧烷化合物为，例如，二甲基聚硅氧烷、甲基苯基聚硅氧烷、环状(聚)硅氧烷和氨基-、脂肪酸-、醇-、聚醚-、环氧-、氟-、糖苷-和/或烷基改性的(聚)硅氧烷化合物，其在室温下可以为液体和树脂状。适宜的(聚)硅氧烷化合物为二甲基硅油，其为具有平均链长为200至300个二甲基硅氧烷单元的二甲基聚硅氧烷和氢化硅酸酯的混合物。特别优选使用氨基硅氧烷，例如来自Cognis Deutschland GmbH&Co.KG的Cognis 3001。它们进一步地与H-硅氧烷交联，例如来自Cognis Deutschland GmbH&Co.KG的Cognis 3002，可进一步增强它们作为粘合剂的性能。
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环氧氯丙烷交联的聚酰胺基胺
环氧氯丙烷交联的聚酰胺基胺，其也称为“纤维骨架”或“湿强度树脂(wetstrength resin)”，是纺织品和造纸工艺熟知的。它们优选由两种方法制备：
i)聚氨基酰胺为(a)首先与季铵化剂反应，以用于季铵反应的氮计，季铵化剂的量为5至30mol％，和(b)然后，将得到的季铵化聚氨基酰胺与环氧氯丙烷交联，环氧氯丙烷的量相当于非季铵化氮含量的摩尔量，或
ii)聚氨基酰胺为(a)首先在10至35℃下，与环氧氯丙烷反应，以用于交联的氮计，环氧氯丙烷的量为5至40mol％，和(b)调节中间产物的pH为8至11，在20至45℃再次与环氧氯丙烷交联，以可用于交联的氮计，所有环氧氯丙烷的摩尔比为90至125mol％。
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聚(甲基)丙烯酸酯
聚(甲基)丙烯酸酯应理解为丙烯酸、甲基丙烯酸及其酯的均聚和共聚反应产物，该反应以已知的方式获得，例如通过在紫外灯下通过自由基聚合，所述酯为与下述醇形成的：低级醇，例如甲醇、乙醇、异丙醇、异构的丁醇、环己醇等。聚合物的平均分子量通常为100至10,000道尔顿，优选200至5,000道尔顿，更加优选400至2,000道尔顿。
作为活性物质的粘合剂在纤维中的用量通常为0.5至15重量％，优选1至10重量％，更优选1至5重量％。
微胶囊
在本发明优选的实施方案中，纤维和纺织品为使用提到的粘合剂由疏水性未包囊的活性组分和其它压缩的活性组分修整。如此，结合了两种作用机理的优点，抵消了它们的缺点。未包囊的活性组分直接起作用，即在第一次穿着期间起作用，提供给消费者想要的良好效果，但是在洗涤10次后，含量迅速减少，然而，然后微囊化活性组分开始释放它们的活性成分，特别是当使用高耐受性胶囊系统时。
“微胶囊”或“纳米胶囊”应理解为具有直径大约为0.0001至大约5mm，优选0.005至0.5毫米的球状凝聚体，其包含至少一个固体或液体核，被至少一层连续薄膜包围。更确切地说，它们为良好分散的液体或固体相，用成膜聚合物涂覆，在其制备中，在乳化和凝聚或界面聚合后，聚合物沉积在所述包囊的物质上。在另一种方法中，熔化的蜡被基质(“微海绵(microsponge)”)吸收，其例如微颗粒可另外用成膜聚合物涂覆。在第三种方法中，微粒可交替地用具有不同电荷的聚电解质涂覆(层对层法)。细小的胶囊可以如同粉末一样干燥。除了单核微胶囊外，还存在多核凝聚体，也称为微球体，其包含两个或更多个分配在连续薄膜物质中的核心。另外，单核或多核微胶囊可以被另外的第二个、第三个等薄膜包围。薄膜可包含天然的、半合成的或合成的材料。天然的薄膜物质为，例如阿拉伯胶、琼脂、琼脂糖、麦芽糖糊精合剂、海藻酸及其盐例如海藻酸钠或海藻酸钙、脂肪和脂肪酸、鲸蜡醇、胶原蛋白、壳聚糖、卵磷脂、明胶、白蛋白、虫胶、多糖例如淀粉或右旋糖酐、多肽、蛋白质的水解产物、蔗糖和蜡。半合成的薄膜物质优选化学改性的纤维素，更加优选纤维素酯和醚，例如醋酸纤维素、乙基纤维素、羟丙基纤维素、羟丙基甲基纤维素和羧甲基纤维素、和淀粉衍生物，特别优选淀粉醚和酯。合成的薄膜物质为，例如聚合物，如聚丙烯酸酯、聚酰胺、聚乙烯醇或聚乙烯基吡咯烷酮。
已知微胶囊的实例为下述市售产品：(薄膜物质表示在括号中)Hallcrest Microcapsules(明胶、阿拉伯胶)、Coletica Thalaspheres(海生的胶原蛋白)、Lipotec Millicapseln(海藻酸、琼脂)、Induchem Unispheres(乳糖、微晶纤维素、羟丙基甲基纤维素)、Unicerin C30(乳糖、微晶纤维素、羟丙基甲基纤维素)、Kobo Glycospheres(改性淀粉、脂肪酸酯、磷脂)、Softspheres(改性琼脂)、Kuhs Probiol Nanospheres(磷脂)、Primaspheres和Primasponges(壳聚糖、海藻酸盐)和Primasys(磷脂)。壳聚糖微胶囊和它们的制备方法为申请人较早专利申请的主题[WO 01/01926，WO 01/01927，WO 01/01928，WO01/01929]。
为了制备微胶囊，通常制备1至10重量％,优选2至5重量％的凝胶前体的水溶液，所述凝胶前体优选琼脂，并进行加热回流。第二种水溶液包含含量为0.1至2重量％，优选0.25至0.5重量％的阳离子聚合物，优选壳聚糖，在沸点温度，优选在80至100℃，加入量为0.1至25重量％，优选0.25至10重量％的活性物质；该混合物称为基质。因此，包含活性物质的微胶囊的填料可能也包含占胶囊重量的0.1至25重量％的填料。如果需要，暂时可将水不溶性组分，例如无机颜料加入以调节粘性，通常为水性或水性/醇性的分散液形式。另外，为了乳化或分散活性物质，向基质中加入乳化剂和/或增溶剂是有益的。在由凝胶前体、阳离子聚合物和活性物质制备后，在后来的包囊法中，基质可任意地非常细地分散在油相中，增强剪切以产生小颗粒。已经证实，在这点上特别有利的是将基质加热至40至60℃的温度，同时冷却油相为10至20℃。实际的包囊，即基质中的阳离子聚合物与阴离子聚合物接触形成薄膜发生在最后，其为又一个必须步骤。结束时，建议用含水大约1至50重量％，优选10至15重量％的阴离子聚合物的水溶液清洗任选的分散在油相中的基质，如有必要，同时或者随后除去油相。获得的含水制剂通常具有包含含量为1至10重量％的微胶囊。在某些情况下，包含其它成分可对聚合物溶液有利，所述成分例如乳化剂或防腐剂。过滤后，得到平均直径优选为约0.01至1mm的微胶囊。建议筛选胶囊以保证得到均匀的粒径分布。因此，获得的微胶囊可能是与产品相关限制内的任意形状，形。另外地，阴离子聚合物也可用于基质的制备，包囊可采用阳离子聚合物，尤其是壳聚糖来进行。
另外，包囊也可使用单独的阳离子聚合物并利用它们在高于pKs值的pH值凝聚的性质来进行。
根据本发明制备微胶囊的第二种方法包括：首先制备o/w乳剂，其除了包含油组分、水和活性组分外，还包含有效量的乳化剂。为了形成基质，将适宜量的含水阴离子聚合物溶液加入到制剂中，强烈搅拌。薄膜是通过加入壳聚糖溶液形成的。所有的方法优选在pH为3至4的中等条件下进行。如有必要，通过加入无机酸调节pH。在薄膜形成后，通过加入三乙醇胺或另一种碱增加pH值到5至6。这将导致粘性增加，其可通过加入其他的下述增稠剂来支持：例如多糖，更加优选黄原胶、瓜尔胶、琼脂、海藻酸盐和甲基纤维素(tyloses)、羧甲基纤维素和羟乙基纤维素、相对高分子量的脂肪酸的聚乙二醇单和二酯、聚丙烯酸酯、聚丙烯酰胺等。最后，微胶囊从含水中分离，例如通过倾泻法、过滤或离心。
在第三种方法中，形成的微胶囊优选包覆固体，例如晶质，包覆核，核心在反向电荷聚电解质层中，参见欧洲专利EP1064088 B1(Max-PlanckGesellschaft)。
制备PVMMA-基微胶囊的其它方法记载在DE 3512565 A1(BASF)和US 4,089,802(NCR Corp.)中。在这些已知的方法中，水性聚丙烯酸酯溶液，例如与石蜡混合，然后加入三聚氰胺和甲醛的预缩合物。
商业应用
疏水性活性组分和成膜聚合物制剂可用于修整纤维和各种各样的纺织品，即，在修整过程期间以至之后的最终产品和半成品都适宜改善穿着时对皮肤的舒适感。纤维或纺织品组成物质的选择是非关键性的(very largelyuncritical)。适宜的材料为任何标准的天然和合成材料及其混和物，但特别优选棉纱、聚酰胺、聚酯、粘胶、聚酰胺/弹性体(elastane)、棉纱/弹性和棉纱/聚酯。纺织品的选择同样不是关键性的(uncritical)，虽然其逻辑上是与皮肤直接接触的成品，即，特别是与内衣、泳衣、睡衣、长筒袜和裤袜。
应用方法
本发明还涉及用于修整纤维或纺织品的第一种方法，其中将基材浸润于含水制剂中，所述含水制剂包含疏水性活性组分和成膜聚合物和任选的其它的微囊化活性组分和乳化剂。纤维或纺织品的浸润可能通过例如所称的排气法进行。这可在通常用于纺织工业的市售洗衣机或染色机中进行。
另外，本发明还涉及用于修整纤维或纺织品的第二种方法，其中含水制剂是通过压力法使用的，所述含水制剂包含疏水性活性组分和成膜聚合物和任意的其它的微囊化活性组分和乳化剂。在这个方法中，用于治疗的纤维/织物都穿过浸浴，所述浸浴包含微囊化活性组分和粘合剂、在压力器中使用一定压力的制剂。本方法被称为填充法(padding)。
活性组分的浓度通常为溶液或浸浴的0.5至15重量％，优选为1至10重量％。浸润通常需要比将活性组分充填入纤维或纺织品的压力法更低的浓度。
最后，本发明涉及包含下述物质的混合物用于修整纤维和纺织品的用途：
(a)疏水性活性组分，
(b)成膜活性组分，和任选的
(c)其它微囊化活性组分
实施例
实施例1
将重量比为9∶1的Monoi de Tahiti(含有Tiara花的活性成分的精炼的椰子油)和维生素E与各种聚合的粘合剂(Stabiflex:聚氨酯，Cognis 3001，3002＝聚硅氧烷)混合，通过压力法将得到的混和物用于棉织物。以活性物质和纤维的重量计，活性组分的使用量为1重量％，粘合剂的使用量为3重量％。在140℃，干燥所有的织物样品2分钟。在40℃下，用常规洗衣机共洗涤棉织物10次，在每次洗涤周期后，测定保留在纤维上的活性组分的量。结果(三次试验系列的完整均值)示于表1中。
表1
洗涤试验
| Monoi[％] | 粘合剂 | |
| StabiflexNi(PU) | Cognis 3001/Cognis 3002(95/5) | |
| 未洗的 | 100 | 100 |
| 洗涤1次后 | 76 | 90 |
| 洗涤5次后 | 50 | 78 |
| 洗涤10次后 | 39 | 54 |
| 维生素E[％] | 粘合剂 | |
| StabiflexNi(PU) | Cognis 3001/Cognis 3002(95/5) | |
| 未洗的 | 100 | 100 |
| 洗涤1次后 | 98 | 90 |
| 洗涤5次后 | 79 | 68 |
| 洗涤10次后 | 65 | 55 |
实施例2
使用聚酰胺/Lycra(90∶10)的混和物代替棉纱重复实施例1。结果(三次试验系列的完整均值)示于表2中。
表1
洗涤试验
| 维生素E[％] | 粘合剂 | |
| StabiflexNi(PU) | Cognis 3001/Cognis 3002(95/5) | |
| 未洗的 | 100 | 100 |
| 洗涤1次后 | 75 | 89 |
| 洗涤5次后 | 66 | 77 |
| 洗涤10次后 | 53 | 69 |
实施例3
将专门的甾醇混合物(GenerolR，Cognis Deutschland GmbH&Co.KG)与各种聚合粘合剂混合，通过压力法应用至聚酰胺/Lycra混和物上。以活性物质和纤维的重量计，甾醇的使用量为1重量％，粘合剂的使用量为3重量％。在140℃，干燥所有的织物样品2分钟。在40℃，在常规洗衣机中洗涤织物共10次，在每种洗涤周期后测定保留在纤维上的甾醇量。结果(三次试验系列的完整均值)示于表3中。
表3。
洗涤试验
| 甾醇[％] | 粘合剂 | |
| StabiflexNi(PU) | Stabicryl1009(EVA) | |
| 未洗的 | 100 | 100 |
| 洗涤1次后 | 95 | 82 |
| 洗涤5次后 | 83 | 69 |
| 洗涤10次后 | 66 | 58 |
实施例4至9
为了制备纳米级的金属氧化物(实施例4至8)，在60巴的恒压下首先从储库中抽取二氧化碳，在含有活性炭和分子筛填料的柱中纯化。在液化以后，在3.51/h的恒量传送速率下通过隔膜泵将CO2压缩至需要的超临界压力。然后，在预热器中将溶剂升温至必要的温度T1，并将溶剂引入到装填有金属皂的萃取柱(钢，400ml)。在温度T2下，通过激光(laser-drawn)喷嘴(长度830μm，直径45μm)，将得到的超临界混合物，即流体，喷雾到Plexiglas膨胀室中，该膨胀室包含4重量％的乳化剂或保护胶体的水溶液。蒸发流体介质，之后，分散的纳米颗粒包囊残留在保护胶体中。为了制备根据实施例9的纳米颗粒，在40℃和在40毫巴的减压下，将1重量％的氧化锌分散液滴加到4重量％的椰子葡糖苷水溶液中，强力搅拌。当分散液包含剩余的纳米颗粒时，在冷阱中冷凝蒸发的溶剂。制备条件和平均粒度范围(PSR，如通过3-WEM法的光度测定来确定)示于下述表4中。
表4。
纳米金属氧化物
| 实施例 | 金属氧化物 | 溶剂 | pbar | T1℃ | T2℃ | 乳化剂/保护性胶体 | PSRnm |
| 4 | 氧化锌 | CO2 | 200 | 85 | 175 | 聚乙烯醇 | 60-120 |
| 5 | 氧化锌 | CO2 | 180 | 70 | 160 | 聚乙烯醇(M＝400) | 75-120 |
| 6 | 氧化锌 | CO2 | 200 | 85 | 180 | 聚乙烯醇 | 75-130 |
| 7 | 二氧化钛 | CO2 | 200 | 85 | 175 | 聚乙烯醇 | 60-140 |
| 8 | 二氧化钛 | CO2 | 200 | 85 | 175 | 椰子葡糖苷 | 55-140 |
| 9 | 氧化锌 | - | - | - | - | 椰子葡糖苷 | 60-130 |
实施例10
将分散于水中的纳米化的氧化锌(粒径0.1-0.2μm)与多种聚合粘合剂混合，通过压力法将其应用于聚酰胺/Lycra混和物上。以活性物质和纤维的重量计，氧化锌的使用量为1重量％，粘合剂的使用量为1重量％。在140℃下，所有织物样品干燥2分钟。然后，在40℃，共洗涤它们10次，在每次洗涤周期后，测定保留在纤维上的氧化锌量。结果(三次试验系列的完整均值)示于表5中。
表5。
洗涤试验
| Nano-ZnO[％] | 粘合剂 | |
| StabiflexNi(PU) | Cognis 3001/Cognis 3002(95/5) | |
| 未洗的 | 100 | 100 |
| 洗涤1次后 | 31 | 68 |
| 洗涤5次后 | 9 | 35 |
| 洗涤10次后 | 6 | 29 |
实施例11
将未包囊的维生素E和微囊化维生素E(Primaspheres，Cognis Iberia S.L.)与各种聚合粘合剂混合，通过压力法应用至棉织物。以活性物质和纤维的重量计，活性组分的使用量为1重量％，粘合剂的使用量为3重量％。在40℃，在常规洗衣机中洗涤棉织物共10次，在每次洗涤周期后，测定保留在纤维上的活性组分的含量。结果(三次试验系列的完整均值)示于表6中。
表6。
洗涤试验
| 维生素E[％] | 粘合剂 | |
| StabiflexNi(PU) | Cognis 3001/Cognis 3002(95/5) | |
| 未洗的 | 100 | 100 |
| 洗涤1次后 | 82 | 89 |
| 洗涤5次后 | 61 | 70 |
| 洗涤10次后 | 45 | 52 |
Claims (12)
1.纤维和纺织品，其特征在于，它们由下述成分的混合物修整：
(a)疏水性的活性组分，和
(b)成膜聚合物。
2.权利要求1所述的纤维和纺织品，其特征在于，它们由选自下述的活性组分修整：生育酚类、胡萝卜素化合物、甾醇、抗坏血酸、(脱氧)核糖核酸及其裂解产物、β-葡聚糖、视黄醇、没药醇、尿囊素、植烷三醇、AHA酸、氨基酸、神经酰胺、拟神经酰胺、壳聚糖、薄荷醇、化妆用油和油组分、精油、植物蛋白及其水解产物、植物提取物、复合维生素、驱虫剂、纳米化的无机物和矿物及其混合物。
3.权利要求1或2所述的纤维和纺织品，其特征在于，以活性物质计，含有0.1至10重量％的活性组分。
4.权利要求1至3中任何一项所述的纤维和纺织品，其特征在于，它们由选自下述的粘合剂修整：聚氨酯、聚醋酸乙烯酯、聚三聚氰胺化合物、聚乙二醛化合物、聚硅氧烷化合物、环氧氯丙烷交联的聚酰胺基胺、聚(甲基)丙烯酸酯和高分子氟碳化合物及其混合物。
5.权利要求1至4中任何一项所述的纤维和纺织品，其特征在于，以活性物质计，含有0.5至15重量％的粘合剂。
6.权利要求1至5中任何一项所述的纤维和纺织品，其特征在于，由其修整的所述混合物还含有作为组分(c)的微囊化活性组分。
7.一种用于修整纤维或纺织品的方法，其中，将基材用含水制剂浸润或将含水制剂通过排气法涂覆于基材，所述含水制剂包含疏水性活性组分和成膜聚合物和任选的微囊化活性组分。
8.一种用于修整纤维和纺织品的方法，其中，通过压力法来应用含水制剂，所述含水制剂包含疏水性活性组分和成膜聚合物和任选的微囊化活性组分。
9.包含下述成分的混合物用于修整纤维和纺织品的用途：
(a)疏水性的活性组分，和
(b)成膜聚合物，以及任选的
(c)其它的微囊化活性组分。
10.纳米化的锌和/或二氧化钛用于修整纤维和纺织品的用途。
11.纳米化的锌和/或二氧化钛用于制备化妆品和/或药物制剂的用途。
12.权利要求10或11所述的用途，其特征在于，纳米化的锌和/或二氧化钛为微囊化的。
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2004
- 2004-08-04 DE DE200410037752 patent/DE102004037752A1/de not_active Withdrawn
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2005
- 2005-07-26 JP JP2007524227A patent/JP2008508444A/ja active Pending
- 2005-07-26 EP EP05773891A patent/EP1774083A1/de not_active Withdrawn
- 2005-07-26 WO PCT/EP2005/008092 patent/WO2006015718A1/de active Application Filing
- 2005-07-26 BR BRPI0514110-9A patent/BRPI0514110A/pt not_active IP Right Cessation
- 2005-07-26 CN CNB200580026462XA patent/CN100572651C/zh not_active Expired - Fee Related
- 2005-07-26 US US11/659,412 patent/US20080248704A1/en not_active Abandoned
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104379010A (zh) * | 2013-03-20 | 2015-02-25 | Nom涂料有限公司 | 人造头发的组成及其制造方法 |
| CN103436982A (zh) * | 2013-09-03 | 2013-12-11 | 陈曦 | 一种改性涤纶纤维及其制备方法 |
| CN105555940A (zh) * | 2013-09-23 | 2016-05-04 | 宝洁公司 | 颗粒 |
| CN104313871A (zh) * | 2014-10-20 | 2015-01-28 | 湖州市菱湖石淙永盛丝织厂 | 一种疏水纳米纤维织物的制备方法 |
| CN114053965A (zh) * | 2021-12-08 | 2022-02-18 | 罗莱生活科技股份有限公司 | 神经酰胺微胶囊、改性粘胶纤维，及其制备方法和应用 |
| CN114053965B (zh) * | 2021-12-08 | 2024-05-14 | 罗莱生活科技股份有限公司 | 神经酰胺微胶囊、改性粘胶纤维，及其制备方法和应用 |
| CN117779355A (zh) * | 2024-02-28 | 2024-03-29 | 江苏青昀新材料有限公司 | 一种闪纺膜材及其制造方法 |
| CN117779355B (zh) * | 2024-02-28 | 2024-05-24 | 江苏青昀新材料有限公司 | 一种闪纺膜材及其制造方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100572651C (zh) | 2009-12-23 |
| WO2006015718A1 (de) | 2006-02-16 |
| BRPI0514110A (pt) | 2008-05-27 |
| DE102004037752A1 (de) | 2006-03-16 |
| EP1774083A1 (de) | 2007-04-18 |
| JP2008508444A (ja) | 2008-03-21 |
| US20080248704A1 (en) | 2008-10-09 |
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