CN104080900A - 处理基材的组合物和方法 - Google Patents
处理基材的组合物和方法 Download PDFInfo
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- CN104080900A CN104080900A CN201380007463.4A CN201380007463A CN104080900A CN 104080900 A CN104080900 A CN 104080900A CN 201380007463 A CN201380007463 A CN 201380007463A CN 104080900 A CN104080900 A CN 104080900A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0036—Soil deposition preventing compositions; Antiredeposition agents
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/008—Polymeric surface-active agents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2079—Monocarboxylic acids-salts thereof
-
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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Abstract
本发明涉及处理基材例如织物的组合物和方法;特别是涉及使得基材防污和当随后洗涤时易于清洁。本发明已经主要研发针对织物使用,并且以下将参考这些应用加以描述。本发明的一个目的是为织物提供防污性。本发明的另一个目的是提供为织物提供改善的芳香剂输送的组合物。现已发现在包含脂肪酸,水溶性铝盐和非离子聚合物的组合物中获得改善的芳香剂输送。当聚合物的HLB为12至18时,获得改善的防污性。
Description
技术领域
本发明涉及处理基材例如织物的组合物和方法;特别是涉及使得基材防污和当随后洗涤时易于清洁。
本发明已经主要研发针对织物使用,并且以下将参考这些应用加以描述。
发明背景
织物通常用洗涤剂来清洁。标准洗涤剂组合物包括表面活性剂和助洗剂。表面活性剂清洁织物。一些洗涤剂组合物也含有苏打粉以增强清洁作用。许多洗涤剂组合物还包括帮助脱除污垢(release
stains)的特殊聚合物。这种聚合物被称作污垢脱除聚合物(SRP)。一些洗涤剂组合物还包括减少洗涤液中脱除的污垢再沉积的添加剂。这种添加剂被称作抗再沉积剂(ARD)。
织物倾向于在使用期间变脏。污垢通常是油性或水性的。水性污垢的常见来源包括茶,咖啡,饮料和油墨。油性污垢的常见来源包括腌汁,沙司和番茄酱,发动机油以及油脂。人们喜欢穿着污垢较少的服装。这特别适用于白色织物,例如白衬衫。人们还喜欢厨房,浴室表面以及窗户表面没有污垢。
防止织物和硬质表面变脏的一种方法为用在织物表面或硬质表面上形成膜的组合物处理它们。该薄膜防止或至少减少污垢附着。该膜还允许洗涤期间轻易地去除污垢,并且据称形成牺牲层(sacrificial
layer),例如我们的申请WO2009/077255中公开的。
使得后续洗涤时更容易清洁的另一种方法为降低织物变脏或着色的能力。典型地,这种组合物中通常存在金属盐。当污垢在其上铺展时,表面变脏。在此情况下,污垢使表面润湿。当污垢润湿表面时,污垢和表面之间的接触角极低,通常小于10 (°)。当表面处理组合物形成膜时,该膜使接触角增加。换言之,该膜不允许污垢润湿表面。通常,90 (°)至170 (°)的水接触角被认为是对于排斥水性污垢良好。另一方面,大于60的油接触角被认为对于排斥油性污垢良好。这种处理过的表面可以称为超疏水性或超疏油性的。为织物提供这种防污性的组合物在WO2010/069731中公开。
接触角为液体/蒸气(或两种不混溶液体)接触面接合固体表面的角度。接触角对于任何给定体系而言是特定的,并且由横跨两个接触面的相互作用决定。最经常的,用平坦的水平固体表面上静置的液滴说明该原理。液滴的形状由Young-Laplace公式确定。测量接触角的一种方法为对液体的固定液滴(sessile drop)使用接触角测角仪。该方法用来评价固体表面上固定区域的润湿性。液滴的基线和液滴边缘处的切线之间的角度为接触角。
织物处理组合物已经在共同未决未公开印度申请WO2011/134755和WO2011/134756 (都为Unilever)中公开。
WO2011/134756公开防污液体组合物及其使用方法。该组合物帮助使得基材,特别是织物排斥亲水性污垢。该组合物包括25至50 wt%的皂,10至30 wt%的锌和三乙醇胺的络合物,30至65 wt%的三价金属离子和/或四价金属离子,和低级醇和水比率为99:1至85:15的溶剂。
理想地,这种组合物在机洗循环的最终漂洗中与织物调理剂一起或者代替织物调理剂添加。
在US 4,555,349中,已经公开包含金属盐电解质和皂的织物调理剂,但是并未发现它们提供任何防污性或为随后的洗涤提供改善的清洁益处。类似的组合物在US
4,417,995中公开,其公开包含水合氯化铝(也叫做聚氯化铝)和Pristerene (牛脂酸)的织物软化剂组合物,但是所述组合物并不为随后的洗涤提供改善的清洁或者改善的防污性。此外,US 4,555,349和US 4,417,995并未提供对于织物改善的芳香剂输送。
GB
552447公开用于防水和防腐材料的永久性涂层。类似地,GB662945公开一种织物处理组合物,其用作熨烫助剂并赋予织物永久的保护性的、耐污性、防水性和淀粉整理(starchy finish)。另外,GB662945公开小于0.3%的聚合物浓度。但是就织物而论,相比永久性涂层,消费者更喜欢可去除的涂层。因此,仍然希望得到通过织物调理剂赋予改善的防污性和下次清洁益处的组合物。
WO01/07551公开聚乙烯醇(污垢脱除聚合物)在主洗洗涤剂组合物中作为洗涤剂添加剂的用途。但是,该文献中公开的组合物并未通过织物调理剂提供下次清洁益处。
US
4136038涉及包含污垢脱除聚合物的织物调理组合物。但是,该文献中公开的组合物并未通过提供下次清洁益处。因此,仍然需要通过织物调理剂的下次清洁益处。
本发明的一个目的是为织物提供防污性。
本发明的另一个目的是当随后的洗涤时提供改善的清洁。
本发明的再另一个目的是提供并不相分离的稳定组合物。
本发明的又另一个目的是提供为织物提供改善的芳香剂输送的组合物。
本发明的又另一个目的是提供提供从织物改善的芳香剂释放的组合物。
本发明的又另一个目的是提供提供织物软化度的组合物。
意外地,现已发现在包含脂肪酸、水溶性铝盐和非离子聚合物的组合物中获得改善的芳香剂输送。当聚合物的HLB为12至18时,获得改善的防污性。
发明内容
因此本发明提供处理基材的组合物,所述组合物包含2-25 wt%的C8-C24脂肪酸,2.5-40 wt%的水溶性铝盐,0.01-2.0
wt%的碱源;0.3-10 wt%的HLB值为12至20的非离子聚合物,芳香剂和水;和其中组合物的pH为1至6,其中5至50 wt%的全部脂肪酸被碱源中和。
在第二个方面,本发明提供一种处理基材的方法,包含以下步骤:制备本发明的组合物在水中的0.05-1 wt%溶液,在该溶液中漂洗织物制品,和干燥该织物制品。
在第三个方面,本发明提供一种制备本发明组合物的方法,包含以下顺序的步骤:在超过脂肪酸熔点的温度下用碱源部分中和脂肪酸,将聚合物混合在部分中和的脂肪酸混合物中,向该混合物中添加铝盐,均化该混合物,和使组合物冷却至室温;和任选添加芳香剂。
在第四个方面,本发明提供瓶装漂洗调理剂,在250 mL至5 L瓶中包含本发明的组合物。
为避免引起怀疑,当随后的洗涤时改善的清洁益处也称为下次清洁益处,同时施加于织物的组合物也称为牺牲层。减少污渍或污垢吸附到织物上或织物中的益处也称为防污性,与是否涉及特定污渍或者一般污垢无关。
通过阅读以下详细说明和所附权利要求,这些和其它方面、特征和优点对于本领域技术人员而言将变得显而易见。为了避免引起怀疑,本发明的一个方面的任何特征可以用于本发明的任何其它方面。措辞“包括”用来表示“包含”,而并不必然表示“由...构成”或“由...组成”。换言之,所列步骤或方案不必是穷举的。应注意以下说明中给出的实施例意图是澄清本发明,而并不试图将本发明限制到那些实施例本身。类似地,所有百分比为重量/重量百分比,除非另有说明。除了操作中和对比例中之外,或当另外明确指明时,表示材料量或反应条件、材料物理性能和/或用途的本说明中的所有数值应理解为由措辞‘约’所修饰。用格式“x至y”表示的数值范围理解为包括x和y。当对于特定的特征,以格式“x至y”描述多个优选范围时,应理解同样预期组合不同的端点的所有范围。
发明详述
本发明提供处理基材的组合物,包含C8-C24脂肪酸,水溶性铝盐,碱源;非离子聚合物。该组合物优选包含其它任选的成分。该组合物的余量用水补足至100 wt%。该组合物的pH为1至6。
脂肪酸
该组合物包含脂肪酸,该脂肪酸包含8至24个碳原子的碳链长度,在此之后称为C8-C24脂肪酸。该组合物优选包含具有至少10个碳原子,但是优选不超过20个,更优选不超过18个,再更优选不超过16个碳原子或甚至不超过14个碳原子的碳链长度的脂肪酸。从成本观点来看,不同脂肪酸的组合是优选的,因为市售脂肪酸通常包含具有类似链长度的不同脂肪酸的混合物。
脂肪酸可以具有或可以不具有一个或多个碳-碳双键或三键。碘值是不饱和度的指示,优选低于20,更优选低于10,和最优选低于5。没有碳-碳双键或三键的饱和脂肪酸是特别优选的。
脂肪酸是水不溶性的。根据本发明可以使用的水不溶性脂肪酸的非限制实例包括月桂酸,辛酸,肉豆蔻酸,硬脂酸,油酸和棕榈酸。
该组合物包含2-25 wt%,优选至少5 wt%,或甚至至少10 wt%的脂肪酸,但是典型地小于组合物的22
wt%。
碱源
该组合物包含碱源。碱源的目的是部分中和脂肪酸。优选5-50 wt%的全部脂肪酸被碱源中和,更优选至少10 wt%,更优选至少12
wt%,或甚至至少15 wt%,但是典型地不超过40
wt%,更优选不超过30 wt%的全部脂肪酸被中和。
碱源优选为氢氧化物盐,更优选为碱金属氢氧化物,其中氢氧化钠和氢氧化钾是最常用的。氢氧化钠是最优选的碱源。
为将脂肪酸中和至全部脂肪酸的5-50 wt%的程度,每mol脂肪酸,该组合物包含0.05-0.5 mol的氢氧化物盐。
因此,该组合物包含组合物的0.01-2.0 wt%,优选至少0.02
wt%,更优选至少0.05 wt%,更优选至少0.1
wt%,但是典型地不超过1.5 wt%,更优选不超过1.2
wt%的碱源。
铝盐
铝盐优选为水溶性铝盐,包括硝酸铝,硫酸铝和氯化铝。为避免引起怀疑,本发明的铝化合物包括聚铝盐,包括聚氯化铝和聚硫酸铝。聚氯化铝是最优选的。
聚氯化铝(PAC)可以定义为羟基氯化铝的非化学计量低聚物,具有通式[AlnCl(3n-m)(OH)m],其中m值优选为5至24,n优选为2至12。
水不溶性铝化合物,例如粘土、氧化铝和氢氧化铝排除在本发明范围之外。
当根据本发明的铝盐在20℃水中的1%溶液产生1至6,更优选2至5的pH时,获得最好的结果。
该组合物包含组合物的2.5-40 wt%,优选至少5 wt%,更优选至少10 wt%,但是典型地不超过30 wt%,更优选不超过25 wt%的水溶性铝盐。
不希望受理论束缚,据信铝盐和脂肪酸形成沉积到织物纤维上的铝皂,由此提供疏水性。
其它多价(poly-valent)金属离子
当组合物包含其它多价金属离子时可以获得其它改善的结果。从组合物成本的观点来看,多种多价金属离子也比铝便宜,因此更加优选。多价金属盐理想地是水溶性的。
金属盐为介质进一步提供离子强度,促进活性物在表面上沉积。因此,多价金属比单价金属盐更加优选。多价金属也比单价金属盐更易水解,因此倾向于进一步通过活性物在表面上的弱聚结和絮凝,促进活性物的沉积。
优选的多价金属离子选自碱土金属离子,钛和锌离子。更优选包括钙、锌、镁、钡、钛的金属盐,更优选选自钙、锌、镁或铁。这些金属盐可以在组合物中与PAC结合使用。对于家用用途而言,铬不是优选的,因为其有毒。金属盐的对应阴离子可以为氯根、硝酸根、硫酸根和乙酸根,或其它水溶性阴离子。氯根、硝酸根、硫酸根和乙酸根是最优选的。
多价金属盐优选以组合物的5至30 wt%,更优选5-25 wt%,更优选5-20 wt%,或甚至5-15 wt%的浓度存在于组合物中。
当存在多价金属盐时,水溶性铝盐和多价金属盐一起的组合量为组合物的7.5-40 wt%,优选为至少10 wt%,但是典型地不超过30 wt%,更优选不超过25 wt%。
当组合物中存在铝(Al)和其它多价金属(M)时,对于良好的芳香剂输送而言,当Al对M的摩尔比率为0.2至2.5时,获得更好的结果。0.5至2.5之间获得最好的疏水性和稳定性结果。在0.2至1,优选0.5至1的摩尔比率下获得最好的清洁结果。
脂肪酸对金属离子比率
脂肪酸对金属比率决定芳香剂的沉积,织物疏水性和清洁效能。
脂肪酸对单独的铝
对于良好的芳香剂沉积和输送而言,脂肪酸对铝盐比率(重量基准)优选为0.2至5,对于改善的疏水性和防污性而言,优选0.4至2或甚至0.6至1.5。
该组合物典型地在超过1.5 (重量基准)的脂肪酸对铝盐比率下相分离。但是,对于消费者来说,在使用之前需要摇振的2-相体系也是可接受的。
对于最好的防污性而言,脂肪酸对铝盐比率优选为,基于重量基准,0.6至1.5,或更优选为0.8至1.2。
脂肪酸对全部金属离子比率(铝+其它多价金属)
对于良好的芳香剂沉积和输送而言,脂肪酸对金属离子比率(摩尔基准)优选为0.2至2,对于改善的疏水性和防污性而言,优选0.5至1.2。
该组合物典型地在超过1.2的脂肪酸对金属离子比率(摩尔基准)下相分离或固化。
对于最好的防污性而言,脂肪酸对金属离子比率优选为,基于摩尔基准,0.6至1.5,或更优选为0.8至1.2。
聚合物
根据本发明的组合物包含非离子聚合物。非离子聚合物典型地包含亲水性和亲油性部分。为定义亲水性对亲油性平衡值(hydrophilic
to lipophilic balance),本领域中广泛使用聚合物的HLB值。
使用聚合物来稳定组合物和促进组合物在织物上的沉积。
HLB值可以如下计算,例如由Griffin的方法(Griffin
WC:“Calculation of HLB Values of Non-Ionic
Surfactants”,Journal of the Society of Cosmetic
Chemists,5 (1954):259),或Davies的基团贡献法(Davies JT:“A quantitative kinetic theory of emulsion type,I. Physical chemistry of emulsifying agent”,Gas/Liquid and Liquid/Liquid Interface。Proceedings of the International Congress of Surface
Activity (1957):426-438);或基团计算法(HLB = 7+∑(亲水性基团数)-∑(亲油性基团数))。
为了本发明目的,当HLB值为10至20时,获得为织物提供优异芳香剂输送和从织物延长的(extended)芳香剂释放的组合物。
当HLB值为10至18,优选12至18,或甚至15至17时,获得最好的防污性。
对于最好的组合物稳定性而言,和为获得不相分离的组合物,HLB优选为12至18。
本发明的非离子聚合物优选选自环氧烷,包括环氧乙烷和环氧丙烷及其共聚物的均聚物和共聚物,和聚乙烯醇,其具有12至20的HLB值。
环氧乙烷/环氧丙烷嵌段共聚物和聚乙烯醇是最优选的。
为获得最好的组合物稳定性,优选的是当使用时,聚乙烯醇聚合物(PVA)具有至少75 (%),优选至少80%,或甚至至少85%,但是优选小于95%的水解度。85-91%,或甚至87-89%的水解度是最优选的。PVA的分子量优选为10,000 u至200,000 u。
环氧乙烷/环氧丙烷嵌段共聚物(市售为Pluronic,购自BASF)是特别优选的,优选具有2500至25000 u的分子量(其中u为SI原子质量单位),和聚合物的5至30 wt%,更优选10至25 wt%,或甚至15至20 wt%的PPG嵌段。
该组合物包含组合物的0.3-10 wt%,优选至少0.5
wt%,更优选至少1 wt%或甚至至少2 wt%,但是典型地小于8 wt%的非离子聚合物。
组合物的pH
当在机洗循环的漂洗水中使用该组合物时,最好的结果为酸性。在碱性pH下,该组合物在织物上不沉积或仅部分沉积。
因此,优选的是组合物的pH为1至6。当组合物的pH小于5时获得最好的结果。
芳香剂
本发明的组合物包含组合物的0.1-10 wt%,优选至少0.2 wt%,更优选至少0.5 wt%,但是典型地不超过5 wt%的芳香剂。
用于油污去除的其它任选成分
对于随后的洗涤时最好的清洁性能而言,特别是对于改善的油性污垢和污渍清洁而言,优选的是该组合物进一步包含另外的聚合物或非离子表面活性剂。
纤维素聚合物
人们发现添加低级烷基纤维素,优选甲基纤维素改善接下来洗涤时的脂肪污垢(fatty
soils)的去除。优选的是烷基纤维素在水中的2%溶液具有2000至6000 mPa.s的粘度(20°下,布氏粘度计中测量)。该组合物优选包含组合物的0.1至2.5 wt%的烷基纤维素。
用污垢脱除聚合物,例如Rhodia的Repel-O-Tex系列(商标),即SF2,PF94,Crystal,特别是Repel-O-Tex SF2得到类似的结果。该组合物优选包含0.1至2.5
wt%的污垢脱除聚合物。
用分子量为40-200ku的羧甲基纤维素钠,分子量为2k-100ku的聚丙烯酸,和分子量为10k-100ku的聚环氧乙烷获得类似的结果。
当组合物中包括repel-o-tex聚合物和烷基纤维素两者时获得最好的结果。
脂肪酸烷基酯
脂肪酸酯可以通过脂肪或脂肪酸与甲醇/乙醇之间的碱金属催化反应来制备。优选实例包括月桂酸甲酯,辛酸乙酯,月桂酸乙酯,辛酸乙酯,己酸甲酯,肉豆蔻酸甲酯,硬脂酸甲酯。
非离子表面活性剂
非离子表面活性剂在本领域中是公知的。它们通常由水增溶聚亚烷氧基(polyalkoxylene )(优选3至10个乙氧基和/或丙氧基基团)或单或双烷醇酰胺基团与有机疏水基团的化学组合构成,所述有机疏水基团衍生自例如具有9至15个碳原子的脂肪醇(任选支化,例如甲基支化),烷基酚(优选12至20个碳原子),其中烷基含有约6至约12个碳原子,其中每个烷基含有6至12个碳原子的二烷基酚,伯、仲或叔脂族醇(或其烷基-封端衍生物),在烷基中具有10至约24个碳原子的单羧酸,以及聚氧丙烯。
其中脂肪酸基团的烷基含有10至约20个碳原子以及烷酰基基团具有1至3个碳原子的脂肪酸单和二烷醇酰胺也是常用的。在任何单和二烷醇酰胺衍生物中,任选,可以存在连接后者基团和分子的疏水性部分的聚氧化烯结构部分。
在所有含聚亚烷氧基的表面活性剂中,聚亚烷氧基结构部分通常由平均2至20个环氧乙烷基团、环氧丙烷基团或其混合组成。后者种类包括特别是用作全部或部分液相的欧洲专利说明书EP-A-0,225,654中描述的那些,在此将其引入作为参考。
特别优选的是那些乙氧基化非离子表面活性剂,其为具有9至15个碳原子的脂肪醇与3至12摩尔环氧乙烷(通常理解为平均值)缩合的缩合产物。那些的实例为C9至C15醇与3或7摩尔环氧乙烷,或其混合物的缩合产物。这些可以用作唯一的非离子表面活性剂或者与EP-A-0,225,654中描述的那些结合。
织物软化阳离子助表面活性剂
织物软化阳离子助表面活性剂为季铵盐表面活性剂,其特征在于铵盐具有通式:R1R2R3R4N+X-,其中R1至R4为烷基或芳基,X-为无机阴离子。优选使用部分硬化的三乙醇胺酯(triethanolmaine
ester)季铵盐表面活性剂。特别优选的季铵阳离子助表面活性剂为甲基二[乙基(牛脂酸酯)]-2-羟乙基甲基硫酸铵(Methyl bis[ethyl (tallowate)]-2-hydroxyethyl ammonium
methyl sulphate),甲基二[乙基(棕榈酸酯)]-2-羟乙基甲基硫酸铵(Methyl bis[ethyl (palmate)]-2-hydroxyethyl ammonium
methyl sulphate)等。
阴离子表面活性剂
阴离子表面活性剂选自线性烷基苯磺酸盐,支化烷基苯磺酸盐,烷基聚(乙氧基化物),烷基硫酸盐,甲基酯磺酸盐及其混合物。在此有用的阴离子表面活性剂的实例包括任何常用阴离子表面活性剂,例如线性或改性的,例如烷基苯磺酸盐表面活性剂,烷基聚(乙氧基化物)表面活性剂,烷基硫酸盐,甲基酯磺酸盐,或其混合物。
理想地,当存在阳离子表面活性剂和阴离子表面活性剂两者时,阳离子表面活性剂对阴离子表面活性剂的比率为5:1至1:1,优选为3:1至1:1。
其它任选的成分
该组合物典型地包含典型地全部组合物的0.1至10%,优选0.1至5%,或甚至0.3至3%的芳香剂。
该组合物可以进一步包含织物软化组合物中通常使用的软化剂。
处理织物的方法
在另一个方面,本发明提供一种处理基材的方法,包含以下步骤:制备本发明组合物在水中的0.05-1
wt%溶液,在该溶液中漂洗织物制品,和干燥该织物制品。
该溶液优选为组合物在水中的0.1-0.5 wt%。
添加到市售前装式洗涤机(front load washing machine)中的溶液通常为12-15 L漂洗水中的25至100 ml的组合物。对于顶装式洗涤机,添加量典型地为50-60
L漂洗水中50-150 ml。
制备组合物的方法
在另一个方面,本发明提供制备本发明组合物的方法,包括以下顺序步骤:在超过脂肪酸熔点的温度下用碱源部分地中和脂肪酸,将聚合物混合到部分中和的脂肪酸混合物中,向该混合物添加铝盐,均化该混合物,使组合物冷却至室温;和任选添加芳香剂。
室温表示20至25℃的温度。
优选在低于100℃的温度下,更优选低于90℃的温度下,再更优选低于80℃的温度下,或甚至低于75℃的温度下用碱溶液部分地中和脂肪酸,但是该温度典型地超过脂肪酸的熔点,典型地为至少45℃,更优选为至少50℃,再更优选为至少55℃,或甚至为至少60℃。
根据本发明,随后可以添加其它成分。
产品形式
产品典型地包装在容积为250 ml至5 L,更优选为250 ml至1.5 L的瓶子,优选塑料瓶中。常用的超市规格瓶子为250 ml,500
ml,750 ml,1 L和1.5 L。瓶子可以任选具有附带的量杯,或盖子中的量尺指示器(measuring
scale indicator),使消费者能够在洗涤机的漂洗调理剂隔室(compartment)中添加适量。
在本发明上下文中同样考虑的是包含本发明组合物、具有触发喷雾分配器的瓶子形式的产品形式。触发喷雾分配器瓶子典型地具有250
ml至1.5 L的容积。常用的容积包括400
ml,500 ml,750
ml和1 L。
本发明的范围同样包括工业规模用途的较大容器。
实施例
本发明现在通过以下非限制性实施例来说明。
制备组合物
首先,在70℃用碱溶液部分中和脂肪酸。然后,将聚乙烯醇混合到部分中和的脂肪酸中。然后,向上述混合物中添加PAC。完全添加PAC之后,将混合物均化5分钟,在室温(25℃)下使其冷却,向冷却的混合物中添加芳香剂并充分混合。随后添加在一些实施例中使用的其它成分。
织物处理规程
在具有6°fH水的5 kg前装式洗涤机(IFB制造,5 kg)中进行实施例中所有的处理过程。10个各棉、聚酯-棉(poly-cotton)和聚酯10×10 cm样品用于处理。包含棉,聚酯-棉(60:40)和聚酯衬衫的3.5 kg织物用作压仓材料(ballast material)。将织物样品钉入压仓衬衫之一。30克的Surf
Excel Matic-Front Load (购自Hindustan
Unilever Ltd,印度)用于主洗,其通过机器的洗涤剂隔室分配。在典型的方法中,40 g实施例中描述的测试配制剂用于织物表面处理,并在第三个(=最终)漂洗期间通过机器的织物调理剂隔室分配。完成整个循环(包含洗涤和3次旋转漂洗(rinses with spin))之后,取出样品,然后在干燥器中干燥并熨烫。
评价织物疏水性
从~2 cm的高度将水滴滴到保持水平的织物上,研究水滴的行为并如以下列表给出评级:
疏水性评级
织物中吸收水滴所需时间 | 疏水性评级 |
接触之后10 s织物才润湿 | 超疏水性 (SH) |
接触之后5 s织物才润湿或者接触之后5-10 s织物润湿 | 疏水性 (H) |
接触之后小于5 s织物润湿 | 吸水 (w) |
沾污规程
炭黑(Carbon soot)沾污:向1 L去离子水中添加150 mg炭黑(Cabot India),在超声处理浴中超声处理2小时。将0.2 ml该炭黑料浆滴到放置在45°斜面上的织物上。使织物整夜干燥。
红泥沾污:向1 lt去离子水中添加5 g红泥(筛分过的,<150微米),在超声处理浴中超声处理2小时。将0.2 ml该料浆滴到放置在45°斜面上的织物上。使织物整夜干燥。
茶垢沾污:将两个茶袋浸入150 ml热牛奶中泡茶。将0.2
ml该茶滴到放置在45°斜面上的织物上。使织物整夜干燥。
脏发动机油(DMO)沾污:将50 ml的脏发动机油与50 ml的新发动机油混合,获得污渍。将0.2 ml该污渍滴到放置在45°斜面上的织物上。使织物整夜干燥。
烹饪油沾污:将0.2 g的Macrolex (商标)紫色染料加入到100 ml的葵花油中并充分混合。将0.2 ml该污渍滴到放置在45°斜面上的织物上。使织物整夜干燥。
洗涤规程
将沾污的10×10 cm样品钉到压仓衬衫(如织物处理规程中所述)之一上。全部洗涤荷载为3.5 kg,包含沾污的样品和压仓衬衫。用30克Surf Excel Matic Front Load (购自Hindustan Unilever Ltd,印度)以6°fH进行洗涤。分别研究处理过的和未处理过的棉、聚酯-棉和聚酯样品。典型的洗涤循环包含洗涤和两次旋转漂洗。洗涤完成之后,取出样品,然后在干燥器中干燥。
对于每种污垢类型,以一对一的基准,相对于对照(未处理过的)织物比较去污程度。如果处理过的织物上的污垢看起来比未处理过的织物更轻,给出分数“+”。类似地,如果处理过的纤维上的污垢看起来比未处理过的织物更深,给出分数“-”。在所有情况下,由受过训练的人进行评价。
芳香剂特性的评价
50×50 cm聚酯样品用于芳香剂平价研究。5个样品以已经描述的方式用实施例中所述的各测试配制剂处理。40 g测试配制剂用于处理。作为对照,使用40 g的Comfort® (市场样品-批号B.876,蓝色变体,印度)。处理和干燥2小时之后,对于每组,基于一对一基准,相对于对照(在这种情况下处理过的Comfort)比较处理过的样品的芳香剂影响。如果处理过的织物上的芳香剂影响看起来比对照织物上的更大,给出分数“+”。类似地,如果处理过的织物上的芳香剂影响看起来比对照织物上的小,给出分数“-”。在所有情况下,由受过训练的人进行评价。
材料
Prifac 5908,(购自Croda Chemicals-55%月桂树脂酸,22%肉豆蔻酸,22%棕榈酸,1%油酸)
市售月桂酸
聚氯化铝:级别_AC/100S (购自Grasim,印度)。
聚乙烯醇(购自Sigma
Aldrich,重均MW-13-250K,87-89%水解)。
甲基纤维素(购自Sigma-Aldrich,4000 cp,2% H2O @ 20℃))
PPG/PEG共聚物:Pluronic F108和F65 (购自BASF)
污垢脱除聚合物:REPEL-O-TEX SF2 (购自Rhodia)。
实施例1:脂肪酸对聚氯化铝比率的作用
如上所述制备组合物。将月桂酸中和至大约15%。使用的聚合物为聚乙烯醇(PVA),其具有85-124k
u的Mw。氢氧化钠(NaOH)用于中和脂肪酸。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
实施例 | 脂肪酸(%w) | PAC (%w) | PVA (%w) | NaOH (%w) | FA:PAC比率 |
实施例1 | 8 | 18 | 1.5 | 0.2 | 0.44 |
实施例2 | 10 | 12 | 1.5 | 0.2 | 0.83 |
实施例3 | 20 | 20 | 1.5 | 0.6 | 1.0 |
实施例4 | 20 | 12 | 1.5 | 0.4 | 1.67 |
余量为水。
以下表格给出稳定性、疏水性和芳香剂输送的结果。
以上表格显示实施例组合物实施例1-实施例4的芳香剂输送良好。用实施例2和3获得最好的稳定性和疏水性结果。
实施例2:脂肪酸对聚氯化铝比率的作用
用市售脂肪酸混合物重复实施例1-4,所述脂肪酸混合物包含55%月桂树脂酸,22%肉豆蔻酸,22%棕榈酸和1%油酸(Prifac 5908,购自Croda),使用的聚合物为聚乙烯醇(PVA),其具有13-23k u的Mw。氢氧化钠(NaOH)用于中和脂肪酸。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
实施例 | 脂肪酸(%w) | PAC (%w) | PVA (%w) | NaOH (%w) | FA:PAC比率 |
实施例5 | 8 | 18 | 3 | 0.2 | 0.44 |
实施例6 | 20 | 25 | 3 | 0.4 | 0.80 |
实施例7 | 18 | 18 | 3 | 0.6 | 1.0 |
实施例8 | 20 | 12 | 3 | 0.4 | 1.67 |
余量为水。
以下表格给出稳定性、疏水性和芳香剂输送的结果。
以上表格显示实施例组合物实施例5-实施例8的芳香剂输送良好。用实施例6和实施例7获得最好的稳定性和疏水性结果。
实施例3:脂肪酸的中和度的作用
在该实施例中说明中和度的作用。按照实施例1进行实验。使用的聚合物为聚乙烯醇(PVA),其具有85-124k
u的Mw。氢氧化钠(NaOH)用于中和脂肪酸。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
实施例 | 月桂酸 (%w) | PAC (%w) | PVA (%w) | NaOH (%w) | FA中和度 (%) |
实施例9 | 20 | 20 | 1.5 | 0 | 0 |
实施例10 | 20 | 20 | 1.5 | 0.16 | 4 |
实施例11 | 20 | 20 | 1.5 | 0.48 | 12 |
实施例12 | 20 | 20 | 1.5 | 1.0 | 25 |
实施例13 | 20 | 20 | 1.5 | 2.4 | 60 |
实施例14 | 20 | 20 | 1.5 | 4.0 | 100 |
余量为水。
以下表格给出稳定性、疏水性和芳香剂输送的结果。
以上表格显示实施例9-实施例14的芳香剂输送良好。用实施例组合物实施例11和实施例12获得最好的稳定性和疏水性结果。
实施例4:聚合物的HLB值的作用
在该实施例中说明聚合物的HLB值的作用。按照实施例1进行实验。
本实施例中的所有组合物含有20%的月桂酸和20%的PAC;其它成分以下列出。余量为水。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
实施例 | 聚合物 (类型) | 聚合物 (Mnf) | 聚合物 (Mw) | 聚合物 (HLB) | 聚合物 (%w) | NaOH (%w) |
实施例15 | PVA | Sigma | 10-200k | 15.5-16.2 (1) | 3 | 0.6 |
实施例16 | Pluronic | BASF | 2.5-25k | 16-17 (1) | 3 | 0.6 |
实施例17 | 甲基纤维素 | Sigma | 10-12 (1) | 3 | 0.6 | |
对比A | 聚乙二醇 | Sigma | 20-100k | 86 (2) | 5 | 0.6 |
对比B | 聚丙烯酸 | Sigma | 20-100k | 5 | 0.6 | |
对比C | 羧甲基纤维素钠 | Sigma | 40-150k | 5 | 0.6 | |
对比D | 聚乙烯亚胺 | Sigma | 20-100k | 5 | 0.6 |
1) HLB由Griffin的方法计算。
2) HLB由基团计算法计算。
以下表格给出稳定性和疏水性的结果。
以上表格显示用实施例15、实施例16和实施例17获得最好的疏水性结果。实施例17显示一定相分离,但是被认为非常适合于用前摇振组合物。
实施例5:聚合物水解度的作用
重复实施例1,聚乙烯醇(PVA)聚合物的水解度不同。余量为水。
以下的所有组合物含有20%的月桂酸,20%的PAC,0.6%的NaOH。以下给出浓度、类型、HLB和水解度。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
实施例 | 分子量 (Mw) | 水解度 (%) | HLB (1) | PVA (%) | 稳定性 |
实施例18 | 89k-98k | 99 | 19.61 | 5 | 否 |
实施例19 | 146k-186k | 99 | 19.61 | 5 | 否 |
实施例20 | 85k-124k | 99 | 19.61 | 5 | 否 |
实施例21 | 31k-50k | 98-99 | 19.23 | 5 | 否 |
实施例22 | 85k-124k | 96 | 18.49 | 5 | 否 |
实施例23 | 85k-124k | 87-89 | 16.11 | 3 | 是 |
实施例24 | 13k-23k | 87-89 | 15.48 | 3 | 是 |
以上表格显示HLB低于18的组合物赋予组合物最好的稳定性(即没有相分离)。
实施例6:添加其它聚合物的作用
重复实施例1,说明对随后的洗涤的清洁效能并与没有处理的对照物相比较。
另外,用任选的其它聚合物进行一些实施例,说明油污清洁的作用。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
以下表格给出随后洗涤时的清洁结果。
以上表格显示对于炭黑,茶和泥污垢而言,当随后的洗涤时,用本发明组合物处理过的织物都比未处理过的表现更好,而具有任选的聚合物的组合物对于去除油污(脏发动机油和烹饪油)也表现更好。
实施例7:进一步的金属离子的作用。
在以下实施例中使用以下材料:
Prifac 5908,(购自Croda Chemicals-55%月桂酸,22%肉豆蔻酸,22%棕榈酸,1%油酸)。
市售月桂酸
聚氯化铝:级别_AC/100S (购自Grasim,印度)。
CaCl2.2H2O- CAS:10035-04-8
Merck India
MgCl2.6H2O- CAS:7791-18-6
Merck India
ZnCl2- CAS:7646-85-7
Merck India
NaOH- CAS:1310-73-2
Merck India
聚乙烯醇(购自Sigma
Aldrich,重均MW为85-124k
u,87-89%水解)。
首先,在70℃温度下用碱溶液部分中和脂肪酸。然后,将聚乙烯醇混合到部分中和的脂肪酸中。然后,向上述混合物中添加包含PAC (聚氯化铝)和CaCl2.2H2O的混合物的水溶液。完成添加含有Al和Ca的溶液之后,将混合物均化5分钟,使其在室温(25℃)下冷却,以及向冷却的混合物中添加芳香剂并充分混合。随后添加在一些实施例中使用的其它成分。
将月桂酸中和至20%。使用的聚合物为聚乙烯醇(PVA),其具有85-124k u的Mw。氢氧化钠(NaOH)用于中和脂肪酸。PAC用作铝源。PAC含有15%的Al (基于该基准进行摩尔计算)。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
以下表格给出稳定性、疏水性和芳香剂输送的结果:
结果显示对于al配制剂而言,芳香剂输送良好。结果进一步显示大于2.3的Al对Ca摩尔比产生稳定的配制剂但是较差的油性(DMO)污清洁,0.5至2.3的Al对Ca摩尔比产生稳定的配制剂以及更好的油性(DMO)污垢清洁,小于0.5的Al对Ca摩尔比产生不稳定的配制剂,但是油性(DMO)污垢清洁更好。
当放置一夜时,配制剂立即稳定固化。立即进行处理。
实施例8:脂肪酸对全部金属(Al + Ca)摩尔比的作用:
如上所述制备组合物。将月桂酸中和至20%。使用的聚合物为聚乙烯醇(PVA),其具有85-124k
u的Mw。氢氧化钠(NaOH)用于中和脂肪酸。PAC用作Al源。PAC含有15%的Al (基于该基准进行摩尔计算)。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
以下表格给出稳定性、疏水性和芳香剂输送的结果:
结果显示对于所有实施例而言,芳香剂输送良好。结果进一步显示大于1.2的脂肪酸对(Al +
Ca)摩尔比产生不稳定配制剂,同等/更好的DMO清洁,0.5-1.2的脂肪酸对(Al + Ca)摩尔比产生稳定配制剂以及更好的油性(DMO)污垢清洁,小于0.5的脂肪酸对(Al + Ca)摩尔比产生稳定配制剂,在所有情况下润湿,以及较差的油性(DMO)污垢清洁。
实施例9:脂肪酸的中和度的作用
如上所述制备组合物。使用的聚合物为聚乙烯醇(PVA),其具有85-124k u的Mw。氢氧化钠(NaOH)用于中和脂肪酸。PAC用作Al源。PAC含有15%的Al (基于该基准进行摩尔计算)。在以下组合物中使用1%的芳香剂。
以下表格给出稳定性、疏水性和芳香剂输送的结果:
结果显示对于所有实施例而言,芳香剂输送良好。结果进一步显示对于脂肪酸中和度低于10%和高于40%,配制剂不稳定,而配制剂在15-40%之间稳定。
实施例10:具有PAC和其它金属离子
使用CaCl2.2H2O (MW 147);MgCl2.6H2O (MW 203)和无水ZnCl2
(MW 136)。PAC用作Al源。PAC含有15%的Al (基于该基准进行摩尔计算)。
使用以下组合物(参见以下表格)。在以下组合物中使用1%的芳香剂。
以下表格给出稳定性、疏水性和芳香剂输送的结果:
结果显示不同的金属盐提供相同的作用。
实施例11:任选的除油成分
如上相同的实验设备中使用以下其它成分。
产品名称 | 说明 | 制造商 |
月桂酸甲酯 | CAS号:111-82-0 | Sigma-Aldrich |
非离子表面活性剂 | C12乙氧基化醇非离子 (EO3,EO7和EO3:EO7 = 1:1,EO5) | Galaxy Surfactants Ltd.,India |
RHODACAL SSA/R | 96% LABSA. 十二烷基苯磺酸 (线性) | Rhodia |
甲基二[乙基(棕榈酸酯)]-2-羟乙基甲基硫酸铵 | Quat (CAS: 91995-81-2) | Zenith Hygiene Systems |
CaCl2.2H2O | CAS:10035-04-8 | Merck India |
MgCl2.6H2O | CAS:7791-18-6 | Merck India |
ZnCl2 | CAS:7646-85-7 | Merck India |
NaOH | CAS:1310-73-2 | Merck India |
首先,在70℃温度下用碱溶液部分中和脂肪酸。然后,将聚乙烯醇混合到部分中和的脂肪酸中。然后,向上述混合物中添加PAC。完全添加PAC之后,将混合物均化5分钟,在室温(25℃)下使其冷却,向冷却的混合物中添加芳香剂并充分混合。随后添加在一些实施例中使用的其它成分。如下制备含有阴离子和阳离子表面活性剂的组合的用于增强的油污去除的配制剂:在高于脂肪酸熔点的温度下用碱源部分中和脂肪酸,将聚合物混合到部分中和的脂肪酸混合物中,向该混合物中添加铝盐溶液,均化该混合物,接着添加阳离子表面活性剂,然后添加阴离子表面活性剂,然后使组合物冷却至室温;和任选添加芳香剂。室温表示20至25℃的温度。使用时,用40%的NaOH溶液中和LAS酸(RHODACAL SSA/R),混合物的最终pH设置为10。该混合物用于所有实验中。
以下表格显示使用的组合物。在以下组合物中使用1%的芳香剂。
结果在以下给出。
以下表格显示对于炭黑,茶和泥污垢而言,当随后洗涤时,用本发明组合物处理过的织物都比未处理过的表现更好,而具有任选的聚合物的组合物对于去除油污表现更好。
实施例12:PVA浓度的作用
如上所述制备组合物。将月桂酸部分中和至15%。使用的聚合物为聚乙烯醇(PVA),其具有85-124k
u的Mw。氢氧化钠(NaOH)用于中和脂肪酸。脂肪酸对PAC比率固定为0.83。
以下表格显示使用的组合物。在以下组合物中使用1%的芳香剂。
实施例 | 脂肪酸 (%w) | PAC (%w) | NaOH (%w) | FA:PAC比率 | PVA (%w) |
实施例53 | 10 | 12 | 0.2 | 0.83 | 0.1 |
实施例54 | 10 | 12 | 0.2 | 0.83 | 0.2 |
实施例55 | 10 | 12 | 0.2 | 0.83 | 0.5 |
实施例56 | 10 | 12 | 0.2 | 0.83 | 3 |
实施例57 | 10 | 12 | 0.2 | 0.83 | 12 |
以下表格给出稳定性、疏水性和芳香剂输送的结果:
结果显示对于所有实施例而言,芳香剂输送良好。结果进一步显示小于0.3 %的PVA浓度产生不稳定的相分离组合物。本发明的组合物(实施例55和实施例56)显示最好的稳定性、疏水性和芳香剂输送结果。
Claims (12)
1. 处理基材的组合物,所述组合物包含:
a 2-25 wt%的C8-C24脂肪酸,
b 2.5-40 wt%的水溶性铝盐,
c 0.01-2.0 wt%的碱源;
d 0.3-10 wt%的HLB值为10至20的非离子聚合物,
e 水,和
f 芳香剂;和
其中所述组合物的pH为1至6,和其中全部脂肪酸的5至50 wt%被碱源中和。
2. 根据权利要求1的组合物,进一步包含5-30%的其它多价金属离子盐,其中铝盐和多价金属盐的总量为7.5至40 wt%。
3. 根据权利要求2的组合物,其中铝离子对多价金属离子的比率为2.5:1至1:2。
4. 根据权利要求2或3任一项的组合物,其中多价金属离子选自钙、锌、镁、钡和钛。
5. 根据在前权利要求任一项的组合物,进一步包含0.1-10 wt%的芳香剂。
6. 根据在前权利要求任一项的组合物,进一步包含0.1-2.5 wt%的甲基纤维素。
7. 根据在前权利要求任一项的组合物,进一步包含0.1-2.5 wt%的污垢脱除聚合物。
8. 根据在前权利要求任一项的组合物,其中所述非离子聚合物具有12至18的HLB值。
9. 处理基材的方法,包括以下步骤:
a 制备根据权利要求1至8任一项的组合物在水中的0.05-1 wt%溶液,
b 在该溶液中漂洗织物制品,和
c 干燥该织物制品。
10. 制备根据权利要求1至8任一项的组合物的方法,包含以下顺序的步骤:
a 在超过脂肪酸熔点的温度下用碱源部分地中和脂肪酸,
b 将所述聚合物混合到所述部分中和的脂肪酸混合物中,
c 向该混合物中添加铝盐,
d 均化该混合物,
e 使所述组合物冷却至室温;和
f 添加芳香剂。
11. 瓶装漂洗调理剂,在250 mL至5 L瓶中包含权利要求1-8任一项的组合物。
12. 触发喷雾瓶装漂洗调理剂,在250 mL至1.5 L瓶中包含权利要求1-8任一项的组合物。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IN295MU2012 | 2012-01-31 | ||
IN0295/MUM/2012 | 2012-01-31 | ||
EP12160157.9 | 2012-03-19 | ||
EP12160157 | 2012-03-19 | ||
PCT/EP2013/050546 WO2013113541A1 (en) | 2012-01-31 | 2013-01-14 | A composition and method for treating substrates |
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CN104080900A true CN104080900A (zh) | 2014-10-01 |
CN104080900B CN104080900B (zh) | 2019-02-15 |
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CN201380007463.4A Expired - Fee Related CN104080900B (zh) | 2012-01-31 | 2013-01-14 | 处理基材的组合物和方法 |
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Country | Link |
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EP (1) | EP2809757B1 (zh) |
CN (1) | CN104080900B (zh) |
AR (1) | AR089831A1 (zh) |
BR (1) | BR112014017891A8 (zh) |
ES (1) | ES2584384T3 (zh) |
IN (1) | IN2014MN01460A (zh) |
WO (1) | WO2013113541A1 (zh) |
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CN113164002A (zh) * | 2018-11-22 | 2021-07-23 | 花王株式会社 | 擦拭片及其制造方法 |
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WO2019170249A1 (en) * | 2018-03-09 | 2019-09-12 | Symrise Ag | Floating active ingredient systems |
EP3730594B1 (en) | 2019-04-24 | 2023-08-30 | The Procter & Gamble Company | Dishwashing composition having improved sudsing |
EP3730596B1 (en) | 2019-04-24 | 2021-08-11 | The Procter & Gamble Company | Liquid hand dishwashing cleaning composition |
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GB552447A (en) | 1941-10-01 | 1943-04-08 | Geigy Colour Company Ltd | Improvements in the manufacture of water-proofing compositions |
GB602109A (en) | 1944-06-14 | 1948-05-20 | E F Houghton And Co | Wax emulsions and method of preparing the same |
GB662945A (en) | 1948-09-16 | 1951-12-12 | Johnson & Son Inc S C | Fabric-treating composition and methods of preparation |
ZA72434B (en) * | 1971-01-25 | 1973-09-26 | Colgate Palmolive Co | Fabric conditioning |
US4136038A (en) | 1976-02-02 | 1979-01-23 | The Procter & Gamble Company | Fabric conditioning compositions containing methyl cellulose ether |
EP0063899B1 (en) | 1981-04-21 | 1985-03-27 | Unilever N.V. | Fabric conditioning composition |
US4555349A (en) | 1983-04-08 | 1985-11-26 | Lever Brothers Company | Fabric softening compositions |
GB8527772D0 (en) | 1985-11-11 | 1985-12-18 | Unilever Plc | Non-aqueous built liquid detergent composition |
WO2001007551A1 (de) | 1999-07-26 | 2001-02-01 | Henkel Kommanditgesellschaft Auf Aktien | Verwendung von polyvinylalkoholen als schmutzablösevermögende waschmittelzusätze |
MY153922A (en) | 2007-12-14 | 2015-04-15 | Unilever Plc | Process for treatment of a fabric |
MX2011006435A (es) | 2008-12-16 | 2011-07-19 | Unilever Nv | Metodo y composicion para el tratamiento de un substrato. |
CN102858937A (zh) | 2010-04-30 | 2013-01-02 | 荷兰联合利华有限公司 | 防污组合物 |
BR112012026467A2 (pt) | 2010-04-30 | 2016-08-09 | Unilever Nv | composição líquida, processo para preparar um substrato hidrofílico de repelência à mancha, utilização de uma composição e dispensador pulverizador |
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2013
- 2013-01-14 BR BR112014017891A patent/BR112014017891A8/pt not_active Application Discontinuation
- 2013-01-14 CN CN201380007463.4A patent/CN104080900B/zh not_active Expired - Fee Related
- 2013-01-14 WO PCT/EP2013/050546 patent/WO2013113541A1/en active Application Filing
- 2013-01-14 ES ES13700225.9T patent/ES2584384T3/es active Active
- 2013-01-14 IN IN1460MUN2014 patent/IN2014MN01460A/en unknown
- 2013-01-14 EP EP13700225.9A patent/EP2809757B1/en active Active
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CN104080900B (zh) | 2019-02-15 |
IN2014MN01460A (zh) | 2015-04-17 |
BR112014017891A8 (pt) | 2017-07-11 |
EP2809757A1 (en) | 2014-12-10 |
ES2584384T3 (es) | 2016-09-27 |
WO2013113541A1 (en) | 2013-08-08 |
BR112014017891A2 (zh) | 2017-06-20 |
AR089831A1 (es) | 2014-09-17 |
EP2809757B1 (en) | 2016-04-27 |
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