CN101541938A - 生物抛光和漂白清洁组合的方法 - Google Patents
生物抛光和漂白清洁组合的方法 Download PDFInfo
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- 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
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
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Abstract
本发明提供用于处理纺织品的方法和组合物,其中在一个步骤内通过用于去除过氧化氢的系统和用于生物抛光的酶系统来处理所述纺织品,以实现生物抛光和漂白清洁的效果。本发明进一步提供实现生物抛光的一步方法。
Description
参考序列表
本申请含有计算机可读形式的序列表。将所述计算机可读形式通过参考并入本文。
发明领域
本发明涉及处理纺织品(textile)的方法和组合物,更具体地说,本发明涉及把生物抛光和漂白清洁(bleach clean-up)组合为一步(one-step)的方法和组合物,其包含使用用于去除过氧化氢的系统和用于生物抛光的酶系统来处理纺织品。
发明背景
通常,存在有用于在漂白后去除残余过氧化氢的方法。有三种方式可以实现这个目的。一种是用水洗涤几次,一种是用还原剂来处理浴器(bath),而另一种是借助过氧化氢酶的使用。过氧化氢酶的使用已经变得越来越流行。准备工艺,其可以涉及脱浆(对于纺织物品(woven goods))、煮练(scouring)、漂白和漂白清洁,产生适合于染色的纺织品。生物抛光在染色之前或之后完成。到目前为止,所述漂白清洁、生物抛光和染色是在分开的步骤中完成。
A.生物抛光:生物抛光是纱线表面(yarn surface)的特定处理,其在触感(handle)和外观(appearance)方面改进织物的质量。生物抛光最重要的效果的特征在于减少起毛(fuzz)和起球(pilling),增加光彩(gloss)/光泽(luster),提高织物触感,增加持久柔软性(durable softness)和改进吸水性。生物抛光通常在制造编织的(knitted)或纺织的(woven)织物的湿加工(wet processing)中进行。湿加工包含这样的步骤,例如脱浆、煮练、漂白、洗涤、染色/印刷和整理(finishing)。
B.漂白清洁:漂白的目的是为了完全去除有色的杂质(colored impurities)、改进吸收性、和实现足够的洁白度和可染性(dyeability)。为了获得多种纤维上(特别在天然纤维上)鲜明的、纯的色调(tones),有必要在染色前漂白它们。这能使其获得好的底色纤维(ground fibre)。从生态学和技术的视角看,过氧化氢,其衍生物和释放过氧化物的加成产物(addition products)通常用于所述漂白加工。但是,通常,多余的过氧化物产品残留在纤维上,并且当这种残留发生时,其能够在随后的用阴离子染料染色时干扰染色并对其产生不良影响,所述阴离子染料例如,其中染料遭到部分或全部破坏的活性染料。把漂白后破坏多余的H2O2称为漂白清洁方法。这可以通过把过氧化氢酶施于底物来完成。由于涉及到pH的加工限制,就很难组合多种酶促方法,因此为了以商业化的纺织品量获得稳定的、高质量的结果,漂白清洁或生物抛光步骤通常分开实施。
C.染色:在纺织品织物和衣物制造中,常把纺织品染色看作是最重要和最昂贵的单一步骤。染料的主要种类是偶氮(单、二、三,等等)、羰基(蒽醌和靛青衍生物(indigo derivative))、花菁(cyanine)、二和三苯甲烷和酞菁染料。所有这些染料都含有发色团,其能产生色彩。正如在比色指数中所定义,这些化学结构组成几种纤维素染料种类,即瓮(还原)染料、硫磺染料、偶氮染料、直接染料和活性染料。这些染料类型中的三种涉及氧化/还原机制,即瓮(还原)染料、硫磺染料和偶氮染料。在这些染色过程中氧化/还原步骤的目的是将染料在不可溶形式和可溶形式之间变换。
加工和染色过程以分批的或连续的方式实施,其将织物以平幅(openwidth)或绳状的形式(rope form)与液体加工流(liquid processing stream)接触。在连续的方法中,使用饱和器(saturator)将化学物施于所述织物,之后在发生化学反应的容器(chamber)中加热织物。然后清洗环节将制备用于下个加工步骤的织物。分批加工通常在一个加工浴(processing bath)中进行,由此使织物在这个浴中循环。在反应时段过后,将化学物排干,漂洗织物,并且施用下个化学物。非连续的填料分批(pad-batch)加工涉及加工化学物的连续应用,接着是停止时段(dwell period),其在冷填料分批的情况下可能是一或数日。
不管分批、连续或非连续的填料分批方法是否使用,由于存在于每一步骤中的条件的广泛变化,漂白清洁、生物抛光和染色步骤迄今为止仍不兼容。因此,在漂白清洁、生物抛光和染色之间需要漂洗或在以其它方式处理织物或置换处理溶液。因此,为了缩短加工时间、节约材料、和减少废液流(wastestream),在本技术领域存有将这三个步骤调和化的需要,以便能在单一浴(single bath)中实施所述步骤,不管是同时地或顺序地实施。
发明概述
因此,本发明提供生物抛光和漂白清洁组合的处理纺织品的一步方法,其包含用(i)用于去除过氧化氢的系统,和(ii)用于生物抛光的酶系统来处理纺织品,其中将所述用于去除过氧化氢的系统和所述用于生物抛光的酶系统同时地或顺序地加到单一溶液(single solution)中。
所述生物抛光和漂白清洁的方法可进一步与染色步骤组合并且可以在单一溶液中进行。漂白清洁、生物抛光和染色组合的处理纺织品的方法,其包括(i)把用于去除过氧化氢的酶系统加到水溶液中,(ii)添加用于生物抛光的酶系统,其中步骤(i)和步骤(ii)在含有纺织品的单一溶液中同时地或顺序地进行,和(iii)为水溶液补充一种或多种染料并将所述纺织品温育足够的时间,以实现纺织品的染色。
优选地,染料是活性染料。优选地,用于去除过氧化氢的系统是包含过氧化氢酶的酶系统,并且用于生物抛光的酶系统包含纤维素酶和/或蛋白酶。
优选地,用于去除过氧化氢的系统是化学还原剂,并且用于生物抛光的酶系统是纤维素酶和/或蛋白酶。
优选地,所述纺织品是含纤维素的(cellulose-containing)织物或纤维素织物(cellulosic fabric),例如棉、粘胶纤维(viscose)、人造纤维(rayon)、苎麻(ramie)、亚麻织物(linen)、溶解性纤维(lyocell,或其混合物,或任何这些纤维与合成纤维或其他天然纤维一起的混合物。
优选地,所述纤维素酶源自腐质霉属(Humicola)、嗜热霉属(Thermomyces)、芽孢杆菌属(Bacillus)、木霉属(Trichoderma)、镰孢属(Fusarium)、毁丝霉属(Myceliophthora)、平革菌属(Phanerochaete)、耙菌属(Irpex)、柱顶孢属(Scytalidium)、裂褶菌属(Schizophyllum)、青霉属(Penicillium)、梭孢壳属(Thielavia)、曲霉属(Aspergillus)或地霉属(Geotricum)的菌种,和更优选地,所述纤维素酶源自土生梭孢壳(Thielavia terrestis)、嗜热毁丝霉(Myceliophthora thermophila)、特异腐质霉(Humicola insolens)、里氏木霉(Trichodermareesei)、哈茨木霉(Trichoderma harzianum)、棘孢曲霉(Aspergillusaculeatus)和黑曲霉(Aspergillus niger)。
优选地,所述过氧化氢酶源自细菌例如芽孢杆菌属、假单胞菌属(Pseudomonas)或链霉菌属(Streptomyces)的菌株;源自酵母例如假丝酵母属(Candida)、克鲁维酵母属(Kluyveromyces)、毕赤酵母属(Pichia)、酵母属(Saccharomyces)、西洋蓍霉属(Yarrowia)或裂殖酵母属(Schizosaccharomyces);源自真菌例如枝顶孢霉属(Acremonium)、曲霉属、鬼伞属(Coprinus)、短梗霉属(Aureobasidium)、烟管菌属(Bjerkandera)、腐质霉属、拟蜡菌属(Ceriporiopsis)、革盖菌属(Coriolus)、隐球菌属(Cryptococcus)、丝梗霉属(Filibasidium)、镰孢属、瘟病菌属(Magnaporthe)、毛霉属(Mucor)、毁丝霉属(Myceliphthora)、新考玛脂霉属(Neocallimastix)、脉孢菌属(Neurospora)、拟青霉属(Paecilomyces)、青霉属、平革菌属(Phanerochaete)、射脉菌属(Phlebia)、瘤胃壶菌属(Piromyces)、侧耳属(Pleurotus)、裂褶菌属(Schizophyllum)、踝节菌属(Talaromyces)、嗜热子囊菌属(Thermoascus)、梭孢壳属(Thielavia)、弯颈霉属(Tolypocladium)、栓菌属(Trametes)或木霉属的菌株;或源自动物例如猪肝脏、牛肝(beeflever)。本发明进一步提供酶组合物,其包含(i)用于去除过氧化氢的系统,和(ii)用于生物抛光的酶系统。所述用于去除过氧化氢的系统可以是过氧化氢酶,或化学还原剂。所述化学还原剂优选是连二硫酸钠(sodiumhyposulphate),而用于生物抛光的酶系统优选是纤维素酶。
当生物抛光和漂白清洁在相同的处理溶液中同时地或顺序地进行时,与包含分别生物抛光和漂白清洁的传统方法相比,在本发明中避免了pH调节步骤和温度调节步骤。因为生物抛光和漂白清洁可以同时进行,本发明的另一个优点是节省/减少了处理时间。因此,本发明把生物抛光和漂白清洁组合到一步中的方法和组合物可以节省时间、能源和水。更进一步,当把染色步骤与漂白清洁和生物抛光组合在相同的处理溶液中时,甚至使方法更有效。
发明详述
纺织品
在本发明的上下文中,术语“纺织品”指织物。
可以通过纺织(weaving)、编织(knitting)或无纺织(non-woven)操作从纤维制造织物。纺织和编织需要纱线作为投入(input),而所述无纺织物是随机连接纤维的结果(可以把纸张看作无纺织的)。在本发明的上下文中,术语“织物”还可以认为包含纤维和其它类型的加工过的织物。
纺织织物(woven fabric)是在织机上通过在以纵向拉直的(stretched)包覆纱(wrap yarn)之间纺织“纬纱(filling)”或纬线纱线制造。纺织前包覆纱必须上浆,以润滑和保护它们在纺织中高速插入纬纱(filling yarn)时免于磨损。所述纬纱可以穿过经纱(warp yarn)以“上一个-下一个(over one-under the next)”的方式纺织(平织(plain weave)),或以“上一个-下两个(over one-under two)”(斜纹织)或任何其它无数种的排列纺织。力度、纹理、图案不仅与纱线的类型/质量相关,还与纺织的类型相关。通常,衣服、衬衫、裤子、被单类、毛巾、帏帐等从纺织织物产生。
编织(knitting)是通过将连锁的纱线环连接到一起形成织物。与由两种类型的纱线制造并且具有许多“末端”(ends)的纺织相反,编织织物是从单根连续的纱线生产的。与纺织一样,有许多不同的方式把纱线环编到一起,并且最终织物的特性依赖于纱线和编织的类型。内衣、毛绒衫(sweater)、袜子、运动衫、汗衫(sweat shirt)等是从编织织物生产。
无纺织物是用机械的、热的、化学的或溶剂介导的方法通过连接和/或连锁纤维和纤丝(filament)制造的织物片。所得织物可以是以网状结构、层压材料(laminates)或膜的形式。典型实例是毛巾、抹布、手术用衣服、“环境友好”(environmental friendly)式纤维、过滤介质、寝具、屋顶材料、二维织物的背板(backing)和许多其他。
根据本发明,本发明的方法可以应用于本技术领域中已知的任何织物(纺织的、编织的和无纺织的)。特别地,本发明的方法可以应用于含纤维素的织物或纤维素织物,例如棉、粘胶纤维、人造纤维、苎麻、亚麻织物、溶解性纤维(例如天丝(Tencel),由Courtaulds Fibers制造),或其混合物,或任何这些纤维与合成纤维(例如聚酯、聚酰胺、尼龙)一起的混合物,或与其他天然纤维例如毛料(wool)和丝(silk)一起的混合物,例如粘胶纤维/棉混合物(blend)、溶解性纤维/棉混合物、粘胶纤维/毛料混合物、溶解性纤维/毛料混合物、棉/毛料混合物;亚麻(亚麻织物)、苎麻和其他基于纤维素纤维的织物,包括全部含纤维素纤维与其他纤维如毛料、聚酰胺、丙烯酸和聚酯纤维的混合物,例如,粘胶纤维/棉/聚酯混合物、毛料/棉/聚酯混合物、亚麻/棉混合物等。术语“毛料”的意思是任何商业可用的动物毛发产品,例如,来自绵羊、骆驼、兔子、山羊、美洲驼(llama)的毛料,以及被称为美利奴羊毛(merino wool)、设得兰羊毛(Shetland wool)、开士米羊毛/山羊绒(cashmere wool)、羊驼毛(alpaca wool)、马海毛等的毛料,和包括毛料纤维和动物毛发。本发明所述方法可以与毛料或动物毛发材料一起使用,以毛条(top)、纤维、纱线或纺织或编织织物的形式。酶处理还可以在松散的棉絮/毛絮(loose flock)上或在由毛料或动物毛发材料制造的纤维上进行。所述处理可在加工的许多不同阶段中实施。将要漂白的织物可以是经过染色或未经染色的。根据本发明可将纺织品在脂肪酸氧化酶存在下在水介质中进行脱浆、煮练和/或漂白。
酶组合物
如本发明中所使用,酶组合物包含生物抛光酶系统和过氧化氢去除系统,其可以配制成液体(例如水剂(aqueous))、固体、凝胶、糊剂或干产品剂型。因此,所述酶组合物可以包含一种或多种生物抛光酶,和一种或多种用于去除过氧化氢的酶或一种或多种用于去除过氧化氢的化学还原剂。
“生物抛光酶系统”包含一种或多种生物抛光酶,例如纤维素酶、蛋白酶。“过氧化氢去除系统”包含一种或多种酶,例如过氧化氢酶,和/或用于去除过氧化氢的化学还原剂,其也可以被称为“漂白清洁系统”。
生物抛光酶
本发明的方法包含对织物进行的纤维素酶和/或蛋白酶处理。
纤维素酶通常在用于以下纺织品的生物抛光方法中使用,所述纺织品如纤维素织物,和纤维素织物/合成纤维混合物;而蛋白酶在用于天然蛋白纤维例如毛料和丝的抗缩水方法(shrinkage-resistance process)中使用。优选地,可将纤维素酶与蛋白酶一起用于纤维素纤维与其它纤维的混合物的生物抛光方法中,例如纤维素织物/毛料混合物、纤维素织物/合成纤维/毛料混合物等。
纤维素酶
术语“纤维素酶”意为促使纤维素水解的酶,如纤维二糖水解酶(cellobiohydrolase)(缩写为“CBH”,酶命名法E.C.3.2.1.91)、内切葡聚糖酶(以下缩写为“EG”,E.C.3.2.1.4),或β-糖苷酶(缩写为“BG”,E.C.3.2.1.21)。纤维素酶分为一系列酶家族,其包括内部(endo-)和外部(exo-)活性以及纤维二糖水解性能。实践本发明时使用的纤维素酶可以源自微生物,已知所述微生物有能力生产分解纤维素的酶,例如,举例来说,腐质霉属、嗜热霉属、芽胞杆菌属、木霉属、镰孢属、毁丝霉属、平革菌属、耙菌属、柱顶孢属、裂褶菌属、青霉属、梭孢壳属、曲霉属或地霉属的菌种,特别是特异腐质霉、尖镰孢或里氏木霉。合适的纤维素酶的非限制性实例在美国专利编号4,435,307、欧洲专利申请号0495257、PCT专利申请号WO91/17244、WO91/17243、WO98/12307、和欧洲专利申请号EP-A2-271004中所公开。
在本发明中使用的纤维素酶可以是单组分或多组分。单组分,即基本上不含其它蛋白质,特别是其它纤维素酶的纤维素酶。多组分酶可通过重组DNA技术经济地制备,即他们可如下产生:通过克隆编码所述多组分的DNA序列,继而用所述DNA序列转化合适的宿主细胞并且在该宿主中表达所述组分。多组分的纤维素酶包含多于一种纤维素酶。多组分的纤维素酶可以是两种或更多种纤维素酶的混合物,或者可以源自野生型菌株。
编码可用的纤维素酶的DNA序列可以例如通过如下来分离:筛选所研究的(in question)微生物的cDNA文库,并且选择表达适当的酶活性(即纤维素酶活性)的克隆。
编码同源酶的DNA序列,即类似的DNA序列,可以从其它微生物获得。例如,所述DNA序列可以源自类似地筛选另一个真菌的cDNA文库,例如曲霉属菌种的菌株,特别是棘孢曲霉或黑曲霉(A.niger)的菌株,木霉属菌种的菌株,特别是里氏木霉、绿色木霉(T.viride)、长枝木霉(T.longibrachiatum)、哈茨木霉或康宁木霉(T.koningii),或者新考玛脂霉属菌种、瘤胃壶菌属菌种、青霉属菌种、伞菌属(Agaricus)菌种或平革菌属菌种的菌株。
优选地,所述纤维素酶源自或可以产生于柱顶孢属(曾用名:腐质霉属(f.Humicola))、镰孢属、毁丝霉属的菌株,更优选地源自或产生于嗜热柱顶孢(曾用名:特异腐质霉(f.Humicola insolens))、尖镰孢或嗜热毁丝霉,最优选地源自特异腐质霉,DSM 1800、尖镰孢,DSM2672或嗜热毁丝霉属,CBS117.65。
在本发明的一个实施方案中,纤维素酶是内切葡聚糖酶,优选来自家族45EG(family 45EG)的纤维素酶,例如SEQ ID No.1中所示的土生梭孢壳内切葡聚糖酶的氨基酸序列(如WO 96/29397中所描述),或是所述内切葡聚糖酶的类似物,其与SEQ ID No.1中所示的所述序列至少60%同源,并与对抗内切葡聚糖酶而产生的抗体反应,和/或由下述DNA序列编码,该DNA序列与编码所述内切葡聚糖酶的DNA序列杂交。在本发明的另一个实施方案中,纤维素酶是内切葡聚糖酶,其包含SEQ ID No.2中所示的特异腐质霉内切葡聚糖酶的氨基酸序列(如WO 91/17243中所描述),或是所述内切葡聚糖酶的类似物,其与SEQ ID No.2中所示的序列至少60%同源,并与对抗所述内切葡聚糖酶而产生的抗体反应,和/或由下述DNA序列编码,该DNA序列与编码所述内切葡聚糖酶的DNA序列杂交。在本发明的进一步实施方案中,本发明中使用的纤维素酶是可由商业途径获得的多组分纤维素酶的酶产品,例如Cellusoft L,Cellish L(Novozymes A/S,丹麦)、Primafast 100、Primafast 200(Genencor International Inc.)、Rocksoft ACE(Dyadic)和Youteer 800(YouteerCo.Ltd,中国)。
用所述DNA序列转化的宿主细胞优选是真核细胞,特别是真菌细胞例如酵母或丝状真菌细胞。特别是,所述细胞可以属于曲霉属或木霉属的菌种,最优选属于米曲霉(Aspergillus oryzae)或黑曲霉。真菌细胞可以通过下述方法转化,所述方法包括原生质体生成和转化所述原生质体,继之以本身已知方式再生细胞壁。曲霉属作为宿主微生物的用途在EP 238023(Novo Nordisk A/S)中描述,将其内容在此引入作为参考。宿主细胞也可以是酵母细胞,例如酵母属菌株,特别是啤酒酵母(Saccharomyces cerevisiae)、克鲁弗酵母(Saccharomyces kluyveri)或葡萄汁酵母(Saccharomyces uvarum),裂殖酵母属的菌种菌株,例如粟酒裂殖酵母(Saccharomycespombe),汉逊酵母属(Hansenula)的菌种菌株,毕赤酵母属的菌种菌株,西洋蓍霉属的菌种例如解脂西洋蓍霉(Yarrowia lipolytica)的菌株,或克鲁维酵母属的菌种例如乳酸克鲁维酵母(Kluyveromyces lactis)。
在上下文中,蛋白质的类似物包含“变体蛋白质”。在一些优选的实施方案中,变体蛋白质不同于亲本蛋白质(parent protein),例如野生型蛋白质,并且因少数氨基酸残基而彼此不同。在本文上下文中,术语“同源”或“同源序列”意指氨基酸序列有一种或多种氨基酸残基不同于另一个蛋白质,优选1,2,3,4,5,10,15,20,30,40,50或更多个氨基酸残基。例如,在一些实施方案中,变体蛋白质有1到10处不同于亲本蛋白质。所述同源序列可以是对显示于这些列表中的氨基酸序列进行修饰的一种结果,例如包含在所述氨基酸序列中一个或多个不同部位上的一个或多个氨基酸残基的取代,在所述酶的一端或两端或在所述氨基酸序列中的一个或多个部位上的一个或多个氨基酸残基的缺失,或在所述氨基酸序列中一个或多个部位上的一个或多个氨基酸残基的插入。
但是,对技术人员来说应该显而易见的是,优选氨基酸改变对性质是较不重要的(of a minor nature),即保守的氨基酸取代,其不显著影响蛋白质的折叠和/或活性;通常为1至大约30个氨基酸的小缺失;小的氨基或羧基末端延伸,例如氨基末端甲硫氨酸残基;多至大约20-25个残基的小接头肽;或促使纯化的小延伸,例如多组氨酸序列(poly-histidine tract)、抗原表位(antigenicepitope)或连接域(binding domain)。概括地可参见Ford et al.,Protein Expressionand Purification 2:95-107,1991。保守取代的实例是在以下组之内:碱性氨基酸组(例如精氨酸、赖氨酸和组氨酸)、酸性氨基酸组(例如谷氨酸和天冬氨酸)、极性氨基酸组(例如谷氨酰胺和天冬酰胺)、疏水性氨基酸组(例如亮氨酸、异亮氨酸和缬氨酸)、芳族氨基酸组(例如苯丙氨酸、色氨酸和酪氨酸)和小氨基酸组(甘氨酸、丙氨酸、丝氨酸、苏氨酸和甲硫氨酸)。
对所述氨基酸序列的修饰可以合适地通过修饰编码所述酶的DNA序列来实现,例如,通过定向位点诱变或通过随机诱变或根据已知方法组合这些技术。可选择地,同源序列可以是源自另一种来源的酶,所述来源不同于分别对应于下文所示各个序列表中的氨基酸序列的纤维素酶的来源。因此,例如“同源物”可以指由DNA编码的多肽,所述DNA在特定条件下与探针杂交(例如在5x SSC中预浸渍,并在包含20%甲酰胺、5x Denhardt′s溶液、pH 6.8的50mM磷酸钠和50mg经变性超声处理的小牛胸腺DNA的溶液中以~40℃预杂交1小时,接着在补充有100mM ATP的相同溶液中以~40℃杂交18小时),所述探针与编码具有所述氨基酸序列的纤维素酶的DNA相同。同源序列与下文所示的每个序列列表中所示的氨基酸序列相比通常将分别显示至少50%的同源性(按照同一性)程度,例如至少60%、65%、70%、75%、80%、85%、90%或甚至95%的同源性程度。
上文提及的同源性可以作为两个序列之间的同一性程度来测定,其说明第一序列源自第二序列。所述同源性可适当地通过本领域中已知的计算机程序例如由GCG程序包提供的GAP来测定(Needleman,S.B.and Wunsch,C.D.,Journal of Molecular Biology,48:443-453,1970)。
蛋白酶
可以使用在本发明中适合使用的任意蛋白酶。
适合的蛋白酶包括动物、植物或微生物来源的那些,优选微生物来源。优选地,所述蛋白酶可以是丝氨酸蛋白酶或金属蛋白酶,更优选地,碱性微生物蛋白酶或胰蛋白酶样蛋白酶。蛋白酶的实施例包括氨肽酶,包括脯氨酰氨肽酶(3.4.11.5)、X-pro氨肽酶(3.4.11.9)、细菌亮氨酰氨肽酶(3.4.11.10)、嗜热氨肽酶(3.4.11.12)、赖氨酰氨肽酶(3.4.11.15)、色氨酰氨肽酶(3.4.11.17)和蛋氨酰氨肽酶(3.4.11.18);丝氨酸内肽酶,包括糜蛋白酶(3.4.21.1)、胰蛋白酶(3.4.21.4)、黄瓜素(cucumisin)(3.4.21.25)、断尾素(brachyuran)(3.4.21.32)、干酵母菌(cerevisin)(3.4.21.48)和枯草芽孢杆菌素(subtilisin)(3.4.21.62);半胱氨酸内肽酶,包括木瓜蛋白酶(papain)(3.4.22.2)、无花果蛋白酶(ficain)(3.4.22.3)、糜木瓜酶(chymopapain)(3.4.22.6)、萝蘼蛋白酶(asclepain)(3.4.22.7)、猕猴桃蛋白酶(actinidain)(3.4.22.14)、番木瓜蛋白酶(caricain)(3.4.22.30)和凤梨蛋白酶(ananain)(3.4.22.31);天冬氨酸氨肽酶(aspartic endopeptidase),包括胃蛋白酶A(3.4.23.1)、曲霉胃蛋白酶I(Aspergillopepsin I)(3.4.23.18)、青霉胃蛋白酶(Penicillopepsin)(3.4.23.20)和糖胃蛋白酶(Saccharopepsin)(3.4.23.25);和金属内切蛋白酶,包括芽孢杆菌溶素(Bacillolysin)(3.4.24.28)。
可由商业途径获得的蛋白酶包括:碱性蛋白酶(Alcalase)、赛威蛋白酶(Savinase)、引发酶(Primase)、Duralase、益瑞蛋白酶(Esperase)、Kannase和Durazym(可以从Novozymes A/S获得),Maxatase、Maxacal、Maxapem、碱性蛋白酶(Properase)、Purafect、Purafect OxP、FN2、FN3和FN4(可以从Genencor International Inc.获得)。
在本发明中同样有用的是蛋白酶变体,例如以下这些所公开:EP 130,756(Genentech)、EP 214,435(Henkel)、WO 87/04461(Amgen)、WO 87/05050(Genex)、EP 251.446(Genencor)、EP 260.105(Genencor)、Thomas et al.,(1985),Nature.318,第375-376页、Thomas et al.,(1987),J.Mol.Biol.,193,第803-813页、Russel et al.,(1987),Nature,328,第496-500页、WO 88/08028(Genex)、WO 88/08033(Amgen)、WO 89/06279(Novozymes A/S)、WO 91/00345(Novozymes A/S)、EP 525610(Solvay)和WO 94/02618(Gist-Brocades N.V.)。蛋白酶活性可以由在″Methods of Enzymatic Analysis″,third edition,1984,Verlag Chemie,Weinheim,vol.5中所描述的方法来测定。
漂白清洁系统
漂白清洁系统可以是去除溶液中过氧化氢的漂白清洁酶和/或化学还原剂。
漂白清洁酶:
漂白清洁酶是指能够催化过氧化氢转化为水和氧的酶,例如过氧化氢酶(EC 1.11.1.6)。优选的过氧化氢酶,其适用于根据本发明的方法中,是源自以下的过氧化氢酶:细菌例如芽胞杆菌属、假单细胞菌属或链霉菌属菌株;酵母例如假丝酵母属、克鲁维酵母属、毕赤酵母属、酵母菌、西洋蓍霉属或裂殖酵母属;真菌例如枝顶孢酶属、柱顶孢属、曲霉属、鬼伞属、短梗霉属、烟管菌属、腐质霉属、拟蜡菌属、革盖菌属、隐球菌属、丝梗霉属、镰孢属、瘟病菌属、毛霉属、毁丝霉属、新考玛脂霉属、脉孢菌属、拟青霉属、青霉属、平革菌属、射脉菌属、瘤胃壶菌属、侧耳属、裂褶菌属、踝节菌属、子囊菌属、梭孢壳属、弯颈霉属、栓菌属或木霉属菌株;或动物例如猪肝、牛肝。合适的过氧化氢酶的非限制性实例在WO92/17571、CN1563373、US2003100112-A1、EP1336659-A、US2003074697-A1、US6201167-B1、US6022721-A、EP931831-A、JP11046760-A、WO9317721-A、WO9309219-A、JP1086879-A和/或JP63003788-A中公开。非限制性实例是:T 100;Oxy-Gone400(GCI);Fermcolase 1000(Mitsubishi Gas Chemical)或Thermocatalase CTL200或JH CT 1800(Mitsubishi Gas Chemical)。
在本发明的一个实施方案中,所使用的过氧化氢酶源自具有SEQ ID No:3(如US 5,646,025中所描述)的嗜热柱顶孢(Scytalidium thermophilum),或其类似物或特别是其变体蛋白质。
依赖于过氧化氢酶的活性和用来施用所述过氧化氢酶的溶液的pH,使用的过氧化氢酶的量优选是0.001-1g/l,特别是大约5g/l的用于施用所述过氧化氢酶的溶液。
化学还原剂
化学还原系统指用于通过催化过氧化氢转化为水和氧来去除过氧化氢的任意化学还原剂。优选地,所述还原剂可以是在纺织品工业中广泛使用的那些,例如硫代硫酸钠、亚硫酸氢钠(sodium bisulphite)、亚硫酸氢钠(sodiumhydrosulphite)和连二硫酸钠等。
染料
在本发明的实施中,可以使用与生物抛光所用条件兼容的任意染料。常规染色材料(dying stuff),其包含以下中的一种或多种:活性染料,例如,染料索引活性红(C.I.Reactive Red)1、3、6、17、120、194,蓝4、19、171和182,黑5,紫5;还原染料(vat dye),例如,染料索引还原黄28,橙11和15,蓝6、16和20,绿1和3、8,棕1,黑9、27;直接染料,例如,染料索引直接红81,黄11和28,橙39,红76,蓝78、86、106、107和108,黑22;硫化染料,例如,染料索引硫化黑1和11,棕1,红色10;和偶氮染料,例如,染料索引偶合成分(coupling component)5和13与染料索引色盐(C.I.Azoic Diazo Components)44和45组合。这些染料在本领域中是熟知的,并且,例如,在Shore,ed.,Cellulosic Dyeing,Society of Dyers and Colorists,AldenPress,1995和Colour Index,Society of Dyers and Colorists and AmericanAssociation of Textile Chemists and Colorists,Vols.1-8Supplements,1977-1988中有所描述。
附加组分(Additional components):
在本发明的一些实施方案中,水溶液或洗涤液(wash liquor)进一步包含其它组分,包括但不限于其它酶,以及表面活性剂、稳定剂、湿润剂、分散剂、消泡剂(antifoaming agent)、润滑剂、增洁剂系统(builder system)等,或其混合物,其可增强煮练和/或漂白步骤,和/或提供涉及例如强度、抗起球性(resistance to pilling)、吸水性和着色性的优良效果。
酶可以从他们的细胞来源分离或者可以通过重组方法产生,并且可以是经过化学或遗传修饰的。应理解的是,与特定生物抛光酶组合在本发明的方法中使用的每个附加酶的酶活性单位的量可以使用常规试验容易地测定。
适于在本发明中的实践中使用的表面活性剂包括但不限于,非离子的、阴离子的、阳离子的和两性离子的表面活性剂,其按重量计通常以约0.2%至约15%之间的浓度存在,优选按重量计约1%至10%。阴离子表面活性剂包括但不限于线性烷基苯磺酸盐、α-烯烃属磺酸酯、烷基硫酸盐(脂肪醇硫酸酯)、乙氧基磺酸醇酯(alcohol ethoxysulfate)、仲链烷磺酸盐、α-磺基甲基脂肪酸酯(alpha-sulfo fatty acid methyl ester)、烷基或烯基琥珀酸(alkyl-or alkenylsuccinic acid)和肥皂。非离子表面活性剂包括但不限于醇乙氧基化物、壬基酚乙氧基化物(nonylphenol ethoxylate)、烷基多糖苷(alkylpolyglycoside)、氧化烷基二甲基胺(alkyldimethylamineoxide)、乙氧基化物脂肪酸单乙醇酰胺(ethoxylated fatty acid monoethanolamide)、脂肪酸单乙醇酰胺(fatty acid monoethanolamide)、聚羟基烷基脂肪酸酰胺和葡糖胺的N-酰基N-烷基衍生物(“葡糖酰胺(glucamide)”)。
增洁剂系统包括但不限于硅铝酸盐、硅酸盐、聚羧酸盐和脂肪酸,例如乙二胺四乙酸盐的物质,和金属离子多价螯合剂例如氨基聚磷酸盐(aminopolyphosphonate),特别是乙二胺四亚甲基膦酸和二亚乙基三胺五甲基次膦酸,其以按重量计约5%至约80%的浓度,优选按重量计约5%至30%的浓度被包括在内。
消泡剂包括但不限于有机硅(silicone)(美国专利号:3,933,672;DC-544(Dow Corning)),其通常以按重量计约0.01%至约1%的浓度被包括在内。
所述组合物还可以包含悬污剂(soil-suspending agent)、脱污剂(soil-releasing agent)、荧光增白剂(optical brightener)、研磨剂和/或杀细菌剂。所有适合于纺织品使用的这些附加组合物在本技术领域中是熟知的。
单浴(single bath)漂白清洁和生物抛光的方法
将生物抛光和漂白清洁组合为一步的本发明的方法在用于处理纺织品的漂白步骤后进行。
将包含用于生物抛光和漂白清洁系统的酶系统的水溶液与纺织品接触的方式将取决于处理方案是连续的、非连续的填料分批或分批的。例如,对于连续或非连续的填料分批处理,优选将酶的水溶液装入饱和器浴(saturatorbath)中,并且在含棉的织物(cotton-containing fabric)通过该浴时将其连续施用于所述织物,在此过程中,所述含棉的织物通常吸收0.5-1.5倍于其重量的处理液。在分批操作中,以4∶1-50∶1的溶液比织物的比率使所述含棉织物暴露于酶溶液约5分钟至24小时的时间。
水溶液或洗涤液通常具有在大约4至大约11的pH。优选地,所述处理组合物的pH是大约5至大约10,优选大约5至大约9,最优选大约6至大约7。
在一个实施方案中,用于处理含棉织物的单浴方法在9以下的pH进行,更优选8以下,甚至更优选7以下。
进行所述漂白清洁和生物抛光组合方法的温度将取决于所使用的方法。在冷填料分批方法的情况下,用于所述漂白清洁和生物抛光组合方法的温度优选是大约15℃至大约65℃,并且最优选大约25℃至大约60℃。对于连续方法和其它分批方法,用于进行漂白清洁和生物抛光组合方法的温度优选是大约35℃至大约75℃,并且最优选大约45℃至大约65℃。
用于生物抛光的酶通常以对于纺织品材料有效产生足够生物抛光效果的量添加。所述酶可以优选以0.01mg蛋白质/l-1g蛋白质/l总溶液的量投配,更优选0.1mg蛋白质/l-300mg蛋白质/l,最优选1mg蛋白质/l-150mg蛋白质/l。
用于漂白清洁的酶通常以有效去除过氧化氢的量添加。所述酶可以优选地以0.001mg蛋白质/l-1g蛋白质/l总溶液的量投配,优选0.01mg蛋白质/l-100mg蛋白质/l,最优选0.15mg蛋白质/l-1mg蛋白质/l。
用于漂白清洁的化学还原剂可以以约0.01g/l至约10g/l总溶液的量投配,更优选约0.1g/l至约3g/l,最优选约0.5g/l至1g/l。
可以理解的是,所述酶、漂白化合物、漂白稳定剂的最优剂量和浓度,水溶液或洗涤液的体积,以及pH和温度将依赖于以下因素而有所不同:(i)纤维的性质,即粗纤维(crude fibre)、纱线或纺织品的性质;(ii)使用的具体的酶,和所述酶的比活性;(iii)在处理进行时的温度、pH、时间等的条件;(iv)在所述洗涤液中其它组分的存在;和(v)所使用处理方案的类型,即连续的、非连续的填料分批或分批的。对所述方法条件的优化可以使用常规实验法来测定,例如,通过建立条件矩阵并且测定矩阵中不同的点。例如,可以改变酶的量、接触发生时的温度,和处理的总时间,之后评估所得纤维素材料或纺织品的(a)起球结果;和(b)残留H2O2ppm。
此外,根据本发明,漂白清洁、生物抛光和染色步骤可以在单浴中实现。在一个实施方案中,(i)添加过氧化氢酶和纤维素酶用于漂白清洁和生物抛光,将第一次温育进行足够长的时间来去除残余的过氧化氢,(ii)然后向洗涤液补充染料,然后将第二次温育进行足够长的时间且在合适的条件下以实现有效染色。优选地,在添加过氧化氢酶和纤维素酶之后,所述步骤(i)的温育时间不少于5分钟,从而将大多数的过氧化氢去除。更优选地,所述步骤(i)的温育时间不少于10分钟,甚至更优选地不少于15分钟且不超过2个小时。最优选地,所述步骤(i)的温育时间是10-20分钟,以便去除几乎所有的过氧化氢和缩短整个处理时间。
可以理解的是,在进行染色的步骤(ii)之前或之间,其进一步包含调节洗涤液组合物的一种或多种性质,例如通过添加盐来调节离子强度。而且在染色步骤中的温育条件还可以在温度、搅拌、pH、时间等方面有所不同。所述酶的生物抛光作用在进行染色处理的温育中仍然继续,从而将使整个处理时间缩短。
优选地,本发明中使用的染料是活性染料,其能很好地与本文中公开的纤维素共同作用。
在染料添加之前或之后添加的盐优选是NaCl或Na2SO4,其可以控制纤维上染料的吸收。洗涤液中盐的浓度取决于染料的浓度和所使用染料的类型。通常而言,染料的浓度要求越高,盐的浓度就需求越高。通常来说,洗涤液中的染料是织物重量的0.001-15%,优选0.001-9%。盐(例如Na2SO4)的浓度是10-100g/l。
染色步骤中的洗涤液优选具有在约5和约8之间的pH,最优选在约6和约7之间。
进行后续染色时的温度可以是在约30℃和约100℃之间,优选在约40℃和约90℃之间,和最优选在约40℃和约80℃之间。
可以理解的是在大多数情况下,在漂白清洁和生物抛光步骤中的pH和温度对于染色步骤是适合的,特别是对于活性染料。因此,在染色时不需要调节pH和温度。
以下内容可以作为对本发明的非限制性例证说明。
实施例
材料和方法
酶
-过氧化氢酶A:具有SEQ ID NO.:3的过氧化氢酶
-过氧化氢酶T 100(Genencor international Inc)
-过氧化氢酶ASC 200(Mitsubishi)
-具有SEQ ID NO.:2的中性纤维素酶B
-具有SEQ ID NO.:1中的中性纤维素酶A
-酸性纤维素酶C:CELLUSOFT LTM(Novozymes A/S)
-Primafast Luna RL(Genencor international Inc)
-IndiAge Max L(Genencor international Inc)
织物
-460-60漂白的连锁编织物(Interlock Knits)(Testfabrics,Inc.)
-染色的织物(购自家乐福(Carrfour)的衣物)
染料
-活性红BF-3B(Arugs textile auxiliary CO.LTD)
-活性黄BF-3R(Arugs textile auxiliary CO.LTD)
-活性TQ蓝G(Arugs textile auxiliary CO.LTD)
缓冲液
将2.716g的磷酸二氢钾和0.201g的氢氧化钠溶于1L去离子水中。
用HAC将1g/l NAAC调节到pH 5
方法:
过氧化氢酶活性(KCIU测定)
当根据本发明使用时,过氧化氢酶活性可以用KCIU来测量。一个CIU在pH 7.0,25℃可以每分钟分解1微摩尔的H2O2,同时H2O2浓度从每毫升反应混合物10.3微摩尔降到9.2微摩尔。
过氧化氢酶催化一级反应:
2H2O2→2H2O+O2
使用分光光度法在240nm监控过氧化氢的降解。在特定H2O2浓度下,吸光率上减少特定量的时间长度是过氧化氢酶活性的量度。
反应
酶浓度........约100CIU/ml
底物浓度......10.3mM H2O2
pH............7.0±0.05
缓冲液...........50mM磷酸盐
温度.............25℃
检测
波长...............240nm
吸收间隔......0.450-0.400
时间间隔..........0.267-0.400分钟(16-24秒)
更详细地描述了本分析方法的文件可以向丹麦Novozymes A/S请求索取,将该文件在此引入作为参考。
纤维素酶活性(ECU)
将纤维素酶样本与羧甲基纤维素(CMC)底物一起温育。所述底物的降解导致粘度的降低,其可以用振动轴粘度计(vibrating-spindle viscometer)来测定。所述粘度的降低与内切纤维素酶(endo-cellulase)活性成比例。
以ECU表示的内切纤维素酶活性是相对于Novozymes A/S酶标准品来测定的。
更详细地描述了本分析方法的文件可以向丹麦Novozymes A/S请求索取,将该文件在此引入作为参考。
纤维素酶活性(EGU)
将纤维素酶样本与羧甲基纤维素(CMC)底物一起温育。所述底物的降解导致粘度的降低,其可以用振动轴粘度计来测定。所述粘度的降低与内切葡聚糖酶活性成比例。
更详细地描述了本分析方法的文件可以向丹麦Novozymes A/S请求索取,将该文件在此引入作为参考。
漂白清洁(过氧化物试验条)
过氧化物酶将过氧化物氧传递到有机氧化还原指示剂。这产生蓝色氧化产物。这种过氧化物浓度可通过对具有色彩标度区(fields of a colour scale)的分析试验条的反应区进行视觉对比来半定量地测定。通过将分析试验条的反应区在测量样本中浸渍1秒钟来测定过氧化氢。允许过量液体通过试验条的长边流到吸收纸巾上,且在15秒后通过在反应区色彩的标签上的哪个色彩区最精确重叠来进行测定。读出以mg/l H2O2表示的相应结果,或如果需要,估算出中间值。
起球检验
马丁达里(Martindale)
起球检验的原理是使检验织物的两个样本以连续变化的模式(continuously changing pattern)相互摩擦,确保将所述样本的表面纤维在每个方向都进行了弯曲(flex)。在预设的摩擦周期数之后,通过与EMPA相片标度标准比较,在视觉上评估所述样本的耐磨性。起球检验结果有5个等级。
注解(Note)5:没有起球
注解4:轻微起球
注解3:适度起球
注解2:明显起球
注解1:严重起球
可允许1/2注解
所述检验方法参见GB/T 4802.2-1997。
ICI起球检验器
ICI起球检验器是最适合的检验,其用在大多数类型的织物上,既有纺织的也有编织的,并且其检验方法与BS EN ISO 12945-1(在其它标准之间)保持一致。起球检验器由两个盒子组成,每一个均衬有(being lined with)金属板支撑的3.2mm厚打磨抛光的(buffed-finish)软木连接材料。所述检验器的特征在于具有自动计数器,其在任何预设的转数之后可以停止所述机器。
起球标准的评定是视觉上的,使用标准相片或评级图(Rating Scheme)。将检验过的样本固定在标度盘(card)上,然后相对于标准相片或未检验过的样本来评级。
等级 | 描述 | 在评定中将要考虑的点 |
5 | 没有变化 | 没有视觉上的变化 |
4 | 轻微变化 | 轻微表面起毛 |
3 | 适度变化 | 检验标本可显示适度的起毛和/或分离的完全形成的球 |
2 | 显著变化 | 明显起毛和/或起球 |
1 | 严重变化 | 覆盖样本的密集的起毛和/或起球 |
蛋白质含量
使用BCA试剂盒(可从PIERCE获得)来检测酶产品中的蛋白质含量。
实施例1
将生物抛光和漂白清洁组合到一个方法中用洗衣仪(Laundry-meter)实施
100%460-60漂白的连锁棉织物购自Test Fabrics。将织物样本切割成约每个5g。
将一种pH 6.5的缓冲液用于此研究。在1L去离子水中溶解2.716g磷酸二氢钾和0.201g氢氧化钠。所述方法用洗衣仪来实施。把100ml缓冲液和两片预先切割的织物注入所述烧杯。
1)主洗涤(Main washing):把100ml缓冲液注入烧杯。按照说明将一些过氧化氢与20个钢球一起加入每个烧杯。同时,定量加入中性纤维素酶A到一定浓度,并加入过氧化氢酶A,然后使温度上升到55℃并保持60分钟。
2)用过氧化物试验条检验残余的过氧化氢。
3)失活:在检验之后,添加1g/l Na2CO3到机器/烧杯中,然后使温度上升到80℃并运行10分钟,排干。
4)冷漂洗:注入冷水并漂洗10分钟。
5)旋转甩掉(spin off)织物和滚筒干燥机(tumble dryer)上的水。
6)测定经处理的织物的重量损失和起球结果。
所述检验的结果示于表1。
表1
开始时的H2O2 | 过氧化氢酶A(mg蛋白质/l) | 中性纤维素酶A(mg蛋白质/l) | 处理后的残余H2O2 | 起球结果 |
0 | 0 | 0 | 0 | 1.5-2 |
0 | 0 | 7 | 0 | 4-4.5 |
100ppm | 0 | 7 | >25ppm | 4-4.5 |
0 | 0.34 | 7 | 0 | 4.5 |
100ppm | 0.34 | 0 | 0 | 1.5-2 |
100ppm | 0.34 | 7 | 0 | 4.5 |
350ppm | 0.34 | 4.2 | 0 | 4-4.5 |
如从表中可见,在本发明的组合了过氧化氢酶和纤维素酶的组合方法中处理的织物具有较少的起球,并且在溶液中没有可探测到的残余H2O2。
实施例2
将生物抛光和漂白清洁组合到一个方法中用wascator实施
100%460-60漂白的连锁棉织物购自Test Fabrics。织物样本的重量是1kg。
将一种pH 6.5的缓冲液用于此研究。在1L去离子水中溶解2.716g磷酸二氢钾和0.201g氢氧化钠。所述方法用wascator来实施。在所述方法开始时,把1kg织物放入wascator中。
1)主洗涤:把10L水注入wascator中。使温度上升到55℃。同时,加入36g K2HPO4和14.5g KH2PO4调节pH到6.5。按照说明把一些过氧化氢加入wascator。定量加入中性纤维素酶到一定浓度并加入过氧化氢酶,并保持60分钟。
2)在20分钟后,用过氧化物试验条检验残余的过氧化氢。
3)失活:在主洗涤之后,排干并再注满wascator,并在wascator中添加1g/l Na2CO3,然后使温度上升到80℃并运行10分钟,排干。
4)冷漂洗:注入冷水并漂洗10分钟。
5)旋转甩掉织物和滚筒干燥机上的水。
6)测定经处理的织物上的起球结果。
所述检验的结果示于表2。
表2
开始时的H2O2 | 过氧化氢酶A(mg蛋白质/l) | 中性纤维素酶A(mg蛋白质/l) | 处理20分钟后的残余H2O2 | 起球结果 |
100ppm | 0.34 | 7 | 0 | 4.5 |
如从表中可见,在本发明的组合了过氧化氢酶A和中性纤维素酶A的组合方法中处理的织物有较少的起球,并且在溶液中没有可探测到的残余H2O2。
实施例3
将生物抛光和漂白洗涤组合到一个方法中用洗衣仪对染色织物实施
购买100%染色的棉织物。将织物样本切割至约每个10g。
将一种pH 6.5的缓冲液用于此研究。在1L去离子水中溶解2.716g磷酸二氢钾和0.201g氢氧化钠。所述方法用洗衣仪来实施。将100ml缓冲液和一片预先切割的织物注入烧杯。
1)主洗涤:把100ml缓冲液注入烧杯中。按照说明将一些过氧化氢与20个钢球一起加入每个烧杯。同时,定量加入中性纤维素酶A到一定浓度并加入过氧化氢酶A,然后使温度上升到55℃并保持20分钟。
2)用过氧化物试验条检验残余的过氧化氢。
3)失活:在检验之后,加1g/l Na2CO3到所述机器/烧杯中,然后使温度上升到80℃并运行10分钟,排干。
4)冷漂洗:注入冷水并漂洗10分钟。
5)旋转甩掉织物和滚筒干燥机上的水。
6)测定经处理的织物上的起球结果。
所述检验的结果示于表3。
表3
开始时的H2O2 | 过氧化氢酶A(mg蛋白质/l) | 中性纤维素酶A(mg蛋白质/l) | 处理后的残余H2O2 | 起球结果 |
0 | 0 | 0 | 0 | 2-2.5 |
350ppm | 0 | 0 | >25ppm | 2-2.5 |
0 | 0 | 4.2 | 0 | 4 |
350ppm | 0 | 4.2 | >25ppm | 3.85 |
350ppm | 0.34 | 4.2 | 0 | 4 |
0 | 0 | 21 | 0 | 4.5-5 |
350ppm | 0 | 21 | >25ppm | 4.5-5 |
350ppm | 0.34 | 21 | 0 | 4.5-5 |
如从上表中可见,在本发明的组合了过氧化氢酶和纤维素酶的组合方法中处理的织物有较少的起球,并且在溶液中没有可探测到的残余H2O2。与那些单独使用过氧化氢酶或纤维素酶的方法相比,本发明显示更多的有利效果。
实施例4
将生物抛光和漂白清洁组合到一个使用酸性纤维素酶的方法中
100%460-60漂白的连锁棉织物购自Test Fabrics。将织物样本切割至约每个5g。
将一种pH 5的缓冲液用于此研究。在1L去离子水中溶解1g乙酸钠并用乙酸调节pH至5。所述方法用洗衣仪来实施。将100ml缓冲液和两片预先切割的织物注入烧杯。
1)主洗涤:将100ml缓冲液注入烧杯中。按照说明将一些过氧化氢与20个钢球一起加入每个烧杯。同时,定量加入酸性纤维素酶C到一定浓度并加入过氧化氢酶A,然后使温度上升到55℃并保持60分钟。
2)用过氧化物试验条检验残余过氧化氢。
3)失活:在检验之后,添加1g/l Na2CO3到所述机器/烧杯中,然后使温度上升到80℃并运行10分钟,排干。
4)冷漂洗:注入冷水并漂洗10分钟。
5)旋转甩掉在所述织物和滚筒干燥机上的水。
6)测定经处理织物的重量损失和起球结果。
所述检验的结果示于表4。
表4
开始时的H2O2 | 过氧化氢酶A(mg蛋白质/l) | 酸性纤维素酶C(mg蛋白质/l) | 处理后的残余H2O2 | 起球结果 |
0 | 0 | 0 | 0 | 1.5-2 |
0 | 0 | 120 | 0 | 4-4.5 |
100ppm | 0.34 | 120 | 0 | 3.5-4 |
实施例5
将生物抛光和漂白清洁组合到一个使用Primafast luna RL的方法中
所述过程与实施例4中所描述的相同,同时使用的纤维素酶是Primafastluna RL,并且使用的过氧化氢酶独立地是过氧化氢酶A或过氧化氢酶T100、ASC 200。所述检验的结果示于表5。
实施例6
将生物抛光和漂白清洁组合到一个使用IndiAge Max L的方法中
所述过程与实施例4中所描述的相同,同时使用的纤维素酶是Primafastluna RL,并且使用的过氧化氢酶独立地是过氧化氢酶A或过氧化氢酶T100、ASC 200。所述检验的结果示于表5。
实施例7
将生物抛光和漂白清洁组合到一个使用中性纤维素酶A的方法中
所述过程与实施例1中所描述的相同,同时使用的过氧化氢酶是过氧化氢酶T 100或ASC 200。所述检验的结果示于表5。
实施例8
将生物抛光和漂白清洁组合到一个使用酸性纤维素酶C的方法中
所述过程与实施例4中所描述的相同,同时使用的过氧化氢酶是过氧化氢酶T 100或ASC 200。所述检验的结果示于表5。
表5
开始时的H2O2 | 纤维素酶 | 剂量(mg蛋白质/l) | 过氧化氢酶 | 剂量(mg蛋白质/l) | 起球结果 | 处理后的残余H2O2 |
/ | PrimafastlunaRL | 41.88 | / | / | 3.85 | 0 |
350ppm | PrimafastlunaRL | 41.88 | 过氧化氢酶A | 0.34 | 4-4.5 | 0 |
350ppm | PrimafastlunaRL | 41.88 | 过氧化氢酶T 100 | 1 | 3.85 | 0 |
350ppm | PrimafastlunaRL | 41.88 | ASC 200 | 0.58 | 3.85 | 0 |
/ | IndiAgeMax L | 69 | / | / | 4.5-5 | 0 |
350ppm | IndiAgeMax L | 69 | 过氧化氢酶A | 0.34 | 4-4.5 | 0 |
350ppm | IndiAgeMax L | 69 | 过氧化氢酶T 100 | 1 | 4-4.5 | 0 |
350ppm | IndiAgeMax L | 69 | ASC 200 | 0.58 | 4-4.5 | 0 |
/ | 中性纤维素酶A | 1.75 | / | / | 4-4.5 | 0 |
350ppm | 中性纤维素酶A | 1.75 | 过氧化氢酶T 100 | 1 | 3.5-4 | 0 |
350ppm | 中性纤维素酶A | 1.75 | ASC 200 | 0.58 | 4-4.5 | 0 |
/ | 酸性纤维素酶C | 120 | / | / | 3.5-4 | 0 |
350ppm | 酸性纤维素酶C | 120 | 过氧化氢酶T100 | 1 | 3.5-4 | 0 |
350ppm | 酸性纤维素酶C | 120 | ASC 200 | 0.58 | 3.5-4 | 0 |
实施例9
将生物抛光和漂白清洁组合到一个方法中使用洗衣仪在较低温度实施
100%460-60漂白的连锁棉织物购自Test Fabrics。将织物样本切割至约每5g。
将一种pH 6.5的缓冲液用于此研究。在1L去离子水中溶解2.716g磷酸二氢钾和0.201g氢氧化钠。所述方法用洗衣仪来实施。将100ml缓冲液和两片预先切割的织物注入烧杯。
1)主洗涤:将100ml缓冲液注入烧杯中。按照说明将一些过氧化氢与20个钢球一起加入每个烧杯。同时,定量加入中性纤维素酶B到一定浓度并加入过氧化氢酶A,然后使温度上升到30℃并保持60分钟。
2)用过氧化物试验条检验残余过氧化氢。
3)失活:在检验之后,添加1g/l Na2CO3到所述机器/烧杯中,然后使温度上升到80℃并运行10分钟,排干。
4)冷漂洗:注入冷水并漂洗10分钟。
5)旋转甩掉在所述织物和滚筒干燥机上的水。
6)测定经处理织物的重量损失和起球结果。
表6
开始时的H2O2 | 纤维素酶 | 剂量(mg蛋白质/l) | 过氧化氢酶 | 剂量(mg蛋白质/l) | 起球结果 | 处理后的残余H2O2 |
/ | / | / | / | / | 1.5-2 | 0 |
/ | 中性纤维素酶B | 6 | / | / | 4 | 0 |
350ppm | 中性纤维素酶B | 6 | 过氧化氢酶A | 0.34 | 4 | 0 |
/ | 中性纤维素酶B | 12 | / | / | 4-4.5 | 0 |
350ppm | 中性纤维素酶B | 12 | 过氧化氢酶A | 0.34 | 4.5 | 0 |
350ppm | 中性纤维素酶A | 7 | 过氧化氢酶A | 0.34 | 4 | 0 |
实施例10
将生物抛光和使用还原剂的漂白清洁组合到一个方法中用洗衣仪实施
100%460-60漂白的连锁棉织物购自Test Fabrics。将织物样本切割至约每个5g。
将一种pH 6.5的缓冲液用于此研究。在1L去离子水中溶解2.716g磷酸二氢钾和0.201g氢氧化钠。所述方法用洗衣仪来实施。将100ml缓冲液和两片预先切割的织物注入烧杯。
1)主洗涤:将100ml缓冲液注入烧杯中。按照说明将一些过氧化氢与20个钢球一起加入每个烧杯。同时,定量加入中性纤维素酶B到一定浓度并加入还原剂(连二硫酸钠:缩写为Hypo),然后使温度上升到55℃并保持60分钟。
2)用过氧化物试验条检验残余过氧化氢。
3)失活:在检验之后,添加1g/l Na2CO3到所述机器/烧杯中,然后使温度上升到80℃并运行10分钟,排干。
4)冷漂洗:注入冷水并漂洗10分钟
5)旋转甩掉在所述织物和滚筒干燥机上的水。
6)测定经处理织物的重量损失和起球结果。
所述检验的结果示于表7。
表7
开始时的H2O2 | 酶 | 剂量(mg蛋白质/l) | 还原剂 | 重量损失% | 残余H2O2 | 起球结果 |
/ | 空白 | / | -0.6 | 0 | 1.625 | |
H2O2350PPM | 中性纤维素酶B | 3 | / | 2.9 | >25ppm | 4.875 |
H2O2350PPM | 中性纤维素酶B | 6 | / | 4.3 | >25ppm | 5 |
H2O2350PPM | 中性纤维素酶B | 12 | / | 6.5 | >25ppm | 5 |
H2O2100PPM | 中性纤维素酶B | 3 | 1g/l Hypo | 3.4 | 0 | 5 |
H2O2100PPM | 中性纤维素酶B | 6 | 1g/l Hypo | 4.9 | 0 | 5 |
H2O2100PPM | 中性纤维素酶B | 12 | 1g/l Hypo | 6.6 | 0 | 5 |
实施例11
用洗衣仪实施的单浴生物抛光、漂白清洁和染色
100%460-60漂白的连锁棉织物购自Test Fabrics。将织物样本切割至约每个5g。
表8:染色配方
Owf:织物的重量
将pH 6.5的水溶液用于此研究。将乙酸溶于1L去离子水中来调节pH至6.5。所述方法用洗衣仪来实施。将100ml溶液和两片预先切割的织物注入烧杯。
1)单浴漂白清洁、生物抛光和染色方法:
将100ml用乙酸调节的pH 6.5的水溶液注入烧杯。按照说明将一些过氧化氢与20个钢球一起加入每个烧杯。同时,定量加入中性纤维素酶A到一定浓度并加入过氧化氢酶A,接着加入一定量的硫酸钠,然后使温度上升到60℃并保持15分钟。用过氧化物试验条检验残余的过氧化氢。
2)添加染料和碳酸钠:在检验之后,添加一定浓度的染料(来自Argus的三种染料)到所述机器/烧杯中并运行10分钟,然后定量加一定量的碳酸钠并运行45分钟/60分钟。排干。
3)皂洗:通过以下染色方法来实施皂洗方法的两个步骤。注入冷水并添加1g/l皂洗剂Dekol SNS(BASF),然后使温度上升到90℃,保持10分钟。排干。注入冷水并添加1g/l皂洗剂Dekol SNS(BASF),然后使温度上升到90℃,保持10分钟。排干。
4)热漂洗:注入冷水,并且使温度上升到70℃,保持15分钟。
5)冷漂洗:注入冷水并漂洗10分钟。
6)旋转甩掉在所述织物和滚筒干燥机上的水。
7)测定经处理的织物上的起球结果。
所述检验的结果示于表9。
表9
样本号 | 样本1 | 样本2 | 样本3 | 样本4 | 样本5 | 样本6 |
添加染料前的残余H2O2 | 0 | n/a | 0 | n/a | 0 | n/a |
起球 | 4.5 | 1.5 | 4.25 | 1.5 | 4.25 | 1.5 |
如从上表中可见,与分开的方法相比,在使用过氧化氢酶和纤维素酶组合的本发明的单浴漂白清洁、生物抛光和染色方法中处理的织物有较少的起球并极大地缩短了处理时间。
所有专利、专利申请和此处提及的文献资料参考全部在此引入参考。根据上述详细描述的说明书的启示,本发明的许多变化对于本领域的技术人员是不言自明的。这些明显的变化均在本发明所附权利要求全部预期的范围内。
序列表
<110>诺维信公司(Novozymes A/S)
<120>生物抛光和漂白清洁组合的方法
<130>11222.204-WO
<160>3
<170>PatentIn version 3.4
<210>1
<211>299
<212>PRT
<213>土生梭孢壳(Thielavia terrestis)
<400>1
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Gln Cys Asp Ser Phe Pro Ala Pro Leu Lys Pro Gly Cys Gln Trp Arg
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Pro Gly Gly Gly Ser Gly Cys Thr Ser Gln Lys Trp Ala Gln Cys Gly
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Gly Ile Gly Phe Ser Gly Cys Thr Thr Cys Val Ser Gly Thr Thr Cys
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Gln Lys Leu Asn Asp Tyr Tyr Ser Gln Cys Leu
290 295
<210>2
<211>305
<212>PRT
<213>特异腐质霉(Humicola insolens)
<400>2
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Cys Lys Pro Ser Cys Gly Trp Ala Lys Lys Ala Pro Val Asn Gln Pro
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Thr Pro Trp Ala Val Asn Asp Asp Phe Ala Leu Gly Phe Ala Ala Thr
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Ser Ile Ala Gly Ser Asn Glu Ala Gly Trp Cys Cys Ala Cys Tyr Glu
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Ser Thr Ser Thr Gly Gly Asp Leu Gly Ser Asn His Phe Asp Leu Asn
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Ile Pro Gly Gly Gly Val Gly Ile Phe Asp Gly Cys Thr Pro Gln Phe
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Ser Ser Pro Pro Val Gln Pro Thr Thr Pro Ser Gly Cys Thr Ala Glu
260 265 270
Arg Trp Ala Gln Cys Gly Gly Asn Gly Trp Ser Gly Cys Thr Thr Cys
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Val Ala Gly Ser Thr Cys Thr Lys Ile Asn Asp Trp Tyr His Gln Cys
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Leu
305
<210>3
<211>717
<212>PRT
<213>嗜热柱顶孢(Scytalidium thermophilum)
<400>3
Met Asn Arg Val Thr Asn Leu Leu Ala Trp Ala Gly Ala Ile Gly Leu
1 5 10 15
Ala Gln Ala Thr Cys Pro Phe Ala Asp Pro Ala Ala Leu Tyr Ser Arg
20 25 30
Gln Asp Thr Thr Ser Gly Gln Ser Pro Leu Ala Ala Tyr Glu Val Asp
35 40 45
Asp Ser Thr Gly Tyr Leu Thr Ser Asp Val Gly Gly Pro Ile Gln Asp
50 55 60
Gln Thr Ser Leu Lys Ala Gly Ile Arg Gly Pro Thr Leu Leu Glu Asp
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Phe Met Phe Arg Gln Lys Ile Gln His Phe Asp His Glu Arg Val Pro
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Glu Arg Ala Val His Ala Arg Gly Ala Gly Ala His Gly Thr Phe Thr
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Ser Tyr Ala Asp Trp Ser Asn Ile Thr Ala Ala Ser Phe Leu Asn Ala
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Thr Gly Lys Gln Thr Pro Val Phe Val Arg Phe Ser Thr Val Ala Gly
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Pro Val Phe Phe Ile Gln Asp Ala Ile Gln Phe Pro Asp Leu Ile His
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Ser Val Lys Pro Arg Pro Asp Asn Glu Ile Pro Gln Ala Ala Thr Ala
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His Asp Ser Ala Trp Asp Phe Phe Ser Gln Gln Pro Ser Thr Met His
210 215 220
Thr Leu Phe Trp Ala Met Ser Gly His Gly Ile Pro Arg Ser Tyr Arg
225 230 235 240
His Met Asp Gly Phe Gly Val His Thr Phe Arg Phe Val Lys Asp Asp
245 250 255
Gly Ser Ser Lys Leu Ile Lys Trp His Phe Lys Ser Arg Gln Gly Lys
260 265 270
Ala Ser Leu Val Trp Glu Glu Ala Gln Val Leu Ser Gly Lys Asn Ala
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Asp Phe His Arg Gln Asp Leu Trp Asp Ala Ile Glu Ser Gly Asn Gly
290 295 300
Pro Glu Trp Asp Val Cys Val Gln Ile Val Asp Glu Ser Gln Ala Gln
305 310 315 320
Ala Phe Gly Phe Asp Leu Leu Asp Pro Thr Lys Ile Ile Pro Glu Glu
325 330 335
Tyr Ala Pro Leu Thr Lys Leu Gly Leu Leu Lys Leu Asp Arg Asn Pro
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Thr Asn Tyr Phe Ala Glu Thr Glu Gln Val Met Phe Gln Pro Gly His
355 360 365
Ile Val Arg Gly Ile Asp Phe Thr Glu Asp Pro Leu Leu Gln Gly Arg
370 375 380
Leu Phe Ser Tyr Leu Asp Thr Gln Leu Asn Arg Asn Gly Gly Pro Asn
385 390 395 400
Phe Glu Gln Leu Pro Ile Asn Met Pro Arg Val Pro Ile His Asn Asn
405 410 415
Asn Arg Asp Gly Ala Gly Gln Met Phe Ile His Arg Asn Lys Tyr Pro
420 425 430
Tyr Thr Pro Asn Thr Leu Asn Ser Gly Tyr Pro Arg Gln Ala Asn Gln
435 440 445
Asn Ala Gly Arg Gly Phe Phe Thr Ala Pro Gly Arg Thr Ala Ser Gly
450 455 460
Ala Leu Val Arg Glu Val Ser Pro Thr Phe Asn Asp His Trp Ser Gln
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Pro Arg Leu Phe Phe Asn Ser Leu Thr Pro Val Glu Gln Gln Phe Leu
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Val Asn Ala Met Arg Phe Glu Ile Ser Leu Val Lys Ser Glu Glu Val
500 505 510
Lys Lys Asn Val Leu Thr Gln Leu Asn Arg Val Ser His Asp Val Ala
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Val Arg Val Ala Ala Ala Ile Gly Leu Gly Ala Pro Asp Ala Asp Asp
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Thr Tyr Tyr His Asn Asn Lys Thr Ala Gly Val Ser Ile Val Gly Ser
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Gly Pro Leu Pro Thr Ile Lys Thr Leu Arg Val Gly Ile Leu Ala Thr
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Thr Ser Glu Ser Ser Ala Leu Asp Gln Ala Ala Gln Leu Arg Thr Arg
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Leu Glu Lys Asp Gly Leu Val Val Thr Val Val Ala Glu Thr Leu Arg
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Glu Gly Val Asp Gln Thr Tyr Ser Thr Ala Asp Ala Thr Gly Phe Asp
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Gly Val Val Val Val Asp Gly Ala Ala Ala Leu Phe Ala Ser Thr Ala
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Ser Ser Pro Leu Phe Pro Thr Gly Arg Pro Leu Gln Ile Phe Val Asp
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Ala Tyr Arg Trp Gly Lys Pro Val Gly Val Cys Gly Gly Lys Ser Ser
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Glu Val Leu Asp Ala Ala Asp Val Pro Glu Asp Gly Asp Gly Val Tyr
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Ser Glu Glu Ser Val Asp Met Phe Val Glu Glu Phe Glu Lys Gly Leu
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Ala Thr Phe Arg Phe Thr Asp Arg Phe Ala Leu Asp Ser
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Claims (32)
1.生物抛光和漂白清洁组合的处理纺织品的一步方法,其包括用(i)用于去除过氧化氢的系统,和(ii)用于生物抛光的酶系统来处理纺织品的步骤,其中将所述用于去除过氧化氢的系统和用于生物抛光的酶系统同时或顺序地加至含有纺织品的单一溶液。
2.权利要求1的方法,其中所述用于去除过氧化氢的系统包含过氧化氢酶或化学还原剂。
3.权利要求1的方法,其中所述纺织品包含含纤维素的织物或纤维素织物。
4.权利要求1-3任一项的方法,其中所述用于生物抛光的酶系统包含纤维素酶。
5.前述权利要求中任一项的方法,其中所述纺织品包含天然蛋白织物,例如毛料和丝。
6.权利要求5的方法,其中所述用于生物抛光的酶系统包含蛋白酶。
7.前述权利要求中任一项的方法,其中所述纤维素酶源自腐质霉属、嗜热霉属、芽孢杆菌属、木霉属、镰孢属、毁丝霉属、平革菌属、耙菌属、柱顶孢属、裂褶菌属、青霉属、梭孢壳属、曲霉属或地霉属的菌种。
8.权利要求7的方法,其中所述纤维素酶源自选自下组的菌种:土生梭孢壳、嗜热毁丝霉属、特异腐质霉、里氏木霉、哈茨木霉、棘孢曲霉和黑曲霉。
9.权利要求4或7的方法,其中所述纤维素酶是家族45纤维素酶。
10.权利要求9的方法,其中所述纤维素酶选自下组:包含SEQ ID NO:1或SEQ ID NO.2的序列的多肽,或其变体。
11.权利要求2的方法,其中所述过氧化氢酶源自细菌、酵母、真菌或动物。
12.权利要求11的方法,其中所述过氧化氢酶源自细菌,例如芽孢杆菌属、假单胞菌属或链霉菌属菌株;源自酵母,例如假丝酵母属、克鲁维酵母属、毕赤酵母属、酵母菌、西洋蓍霉属或裂殖酵母属;源自真菌,例如枝顶孢霉属、柱顶孢霉属、曲霉属、鬼伞属、短梗霉属、烟管菌属、腐质霉属、拟蜡菌属、革盖菌属、隐球菌属、丝梗霉属、镰孢属、瘟病菌属、毛霉属、毁丝霉属、新考玛脂霉属、脉孢菌属、拟青霉属、青霉属、平革菌属、射脉菌属、瘤胃壶菌属、侧耳属、裂褶菌属、踝节菌属、嗜热子囊菌属、梭孢壳属、弯颈霉属、栓菌属、微球菌属(Micrococcus)或木霉属的菌株;或源自动物,例如猪肝、牛肝。
13.权利要求12的方法,其中所述过氧化氢酶是SEQ ID No:3的嗜热柱顶孢过氧化氢酶,或其变体。
14.权利要求2的方法,其中所述还原剂是连二硫酸钠。
15.前述权利要求中任一项的方法,其中所述过氧化氢酶的浓度是0.001mg蛋白质/l至1g蛋白质/l的总溶液,优选0.01mg蛋白质/l至100mg蛋白质/l,最优选0.15mg蛋白质/l至约1mg蛋白质/l。
16.前述权利要求中任一项的方法,其中所述化学还原剂的浓度是0.01g/l至10g/l的总溶液,优选0.1g/l至3g/l,最优选0.5g/l至1g/l。
17.前述权利要求中任一项的方法,其中所述用于生物抛光的酶浓度是0.01mg蛋白质/l至1g蛋白质/l的总溶液,更优选0.1mg蛋白质/l至300mg蛋白质/l,最优选1mg蛋白质/l至150mg蛋白质/l。
18.前述权利要求中任一项的方法,其中所述溶液的pH为大约4-大约12,优选为大约6-大约8。
19.前述权利要求中任一项的方法,其中所述方法在20摄氏度至80摄氏度的温度进行,优选在50摄氏度至60摄氏度进行。
20.在单浴中组合漂白清洁、生物抛光和染色的处理纺织品的一步方法,其包括:
i)将用于去除过氧化氢的酶系统加入水溶液,
ii)添加用于生物抛光的酶系统,其中步骤(i)和(ii)在包含纺织品的单一溶液中同时或顺序地发生,和
iii)将一种或多种染料补充到所述水溶液并将纺织品温育足够的时间以获得染色的纺织品。
21.权利要求20的方法,其中所述用于去除过氧化氢的酶系统包含过氧化氢酶。
22.权利要求20的方法,其中所述用于生物抛光的酶系统包含纤维素酶。
23.权利要求20的方法,其中在添加用于去除过氧化氢的酶系统的步骤(i)之后,温育时间不少于5分钟。
24.权利要求20的方法,其中所述染料是活性染料。
25.酶组合物,其包含(i)用于去除过氧化氢的系统,和(ii)用于生物抛光的酶系统。
26.权利要求25的酶组合物,其中所述用于去除过氧化氢的系统包含过氧化氢酶或化学还原剂。
27.权利要求25或26的酶组合物,其中所述用于生物抛光的酶系统包含纤维素酶和/或蛋白酶。
28.权利要求25-27中任一项的酶组合物,其中所述酶组合物包含一个或多个附加组分,其选自表面活性剂、稳定剂、湿润剂、分散剂、消泡剂、润滑剂和增洁剂系统,或它们的混合物。
29.权利要求26的酶组合物,其中所述过氧化氢酶源自细菌、酵母、真菌或动物。
30.权利要求29的酶组合物,其中所述过氧化氢酶源自柱顶孢属。
31.权利要求27的酶组合物,其中所述纤维素酶是家族45纤维素酶。
32.权利要求26的酶组合物,其中所述还原剂是连二硫酸钠。
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- 2008-06-02 SG SG200804173-3A patent/SG148934A1/en unknown
- 2008-06-06 CN CN2008800000926A patent/CN101541938B/zh active Active
- 2008-06-06 PT PT87606760T patent/PT2164943E/pt unknown
- 2008-06-06 EP EP13196997.4A patent/EP2712916A3/en not_active Withdrawn
- 2008-06-06 CN CN2012103571852A patent/CN102943391A/zh active Pending
- 2008-06-06 EP EP08760676.0A patent/EP2164943B2/en active Active
- 2008-06-06 BR BRPI0809305A patent/BRPI0809305B1/pt active IP Right Grant
- 2008-06-06 WO PCT/EP2008/057106 patent/WO2008151999A1/en active Application Filing
- 2008-06-06 ES ES08760676.0T patent/ES2455242T5/es active Active
- 2008-06-06 PL PL08760676T patent/PL2164943T5/pl unknown
- 2008-06-11 PE PE2008001002A patent/PE20090272A1/es active IP Right Grant
- 2008-06-11 US US12/136,841 patent/US20080301882A1/en not_active Abandoned
-
2009
- 2009-10-22 HK HK09109779.9A patent/HK1133438A1/xx unknown
-
2011
- 2011-07-21 US US13/187,776 patent/US20110271464A1/en not_active Abandoned
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CN102121197A (zh) * | 2010-12-31 | 2011-07-13 | 山东滨州亚光毛巾有限公司 | 一种毛巾处理工艺 |
CN102787503A (zh) * | 2011-05-17 | 2012-11-21 | 上海市纺织科学研究院 | 溶剂法竹纤维织物用复合生物酶及织物表面光洁整理方法 |
CN102787503B (zh) * | 2011-05-17 | 2015-02-25 | 上海市纺织科学研究院 | 溶剂法竹纤维织物用复合生物酶及织物表面光洁整理方法 |
CN102433774A (zh) * | 2011-09-06 | 2012-05-02 | 珠海建轩服装有限公司 | 一种成衣染色与消毛一浴法工艺 |
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CN102493217A (zh) * | 2011-11-24 | 2012-06-13 | 上海皮皮狗毛纺织有限公司 | 一种生物复合型天然染料在羊绒制品染整应用 |
CN104583394A (zh) * | 2012-08-16 | 2015-04-29 | 诺维信公司 | 用内切葡聚糖酶处理纺织品的方法 |
CN104583394B (zh) * | 2012-08-16 | 2019-06-07 | 诺维信公司 | 用内切葡聚糖酶处理纺织品的方法 |
CN107287271A (zh) * | 2017-05-12 | 2017-10-24 | 正和清生命科技实业有限公司 | 一种微生物发酵法制备纺织品用纤维的方法 |
Also Published As
Publication number | Publication date |
---|---|
US20140007357A1 (en) | 2014-01-09 |
HK1133438A1 (en) | 2010-03-26 |
CN101541938B (zh) | 2012-11-14 |
US20080301882A1 (en) | 2008-12-11 |
EP2164943B2 (en) | 2017-09-20 |
BRPI0809305B1 (pt) | 2018-11-21 |
SG148934A1 (en) | 2009-01-29 |
ES2455242T3 (es) | 2014-04-15 |
EP2164943A1 (en) | 2010-03-24 |
WO2008151999A1 (en) | 2008-12-18 |
EP2164943B1 (en) | 2014-03-12 |
PL2164943T3 (pl) | 2014-06-30 |
EP2712916A2 (en) | 2014-04-02 |
EP2712916A3 (en) | 2014-05-21 |
PT2164943E (pt) | 2014-05-07 |
PL2164943T5 (pl) | 2018-05-30 |
ES2455242T5 (es) | 2018-01-12 |
CN102943391A (zh) | 2013-02-27 |
PE20090272A1 (es) | 2009-03-19 |
BRPI0809305A2 (pt) | 2014-10-14 |
US20110271464A1 (en) | 2011-11-10 |
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