CN1886547A - 用抗菌剂处理的纤维 - Google Patents
用抗菌剂处理的纤维 Download PDFInfo
- Publication number
- CN1886547A CN1886547A CNA2004800348955A CN200480034895A CN1886547A CN 1886547 A CN1886547 A CN 1886547A CN A2004800348955 A CNA2004800348955 A CN A2004800348955A CN 200480034895 A CN200480034895 A CN 200480034895A CN 1886547 A CN1886547 A CN 1886547A
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- CN
- China
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- composition
- cellulosic fibre
- resin
- weight
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- Prior art date
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- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
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Abstract
一种在回潮率≤5%的非纤维素纤维上抑制微生物生长的组合物,其包括:i)1-50%重量的至少一种可自交联的树脂;ii)0.25-20%重量的至少一种催化剂;iii)0.1-4%重量与该树脂反应的至少一种抗菌活性剂;iv)98.65-26%重量的水;其中i)+ii)+iii)+iv)=100%。
Description
本发明涉及抑制在非纤维素纤维上微生物生长的组合物,该组合物包括可自交联的树脂、催化剂和与可自交联的树脂反应的活性抗菌剂;用该组合物处理非纤维素纤维的方法和用该组合物处理的非纤维素纤维。
使用抗菌活性剂处理纤维素纤维的用途是众所周知的。在处理纤维素纤维如棉和粘胶丝的过程中,发生纤维素的氧化反应,且形成羧酸基。可通过在阳离子抗菌活性剂和阴离子羧酸基之间的离子键合,将阳离子抗菌活性剂如聚(六亚甲基双胍)附着到纤维素纤维上。
JP 5-226185公开了通过用交联剂交联抗菌活性剂到具有羟基官能度的纺织品上,固定聚六亚甲基双胍类型的化合物到纺织品材料上的方法。
然而,仍需要用抗菌活性剂处理非纤维素纤维的方法。非纤维素纤维包括,但不限于,动物来源,例如羊毛、蚕丝、兽皮、皮革和毛发的蛋白质基纤维;合成纤维,例如基于聚酯、脂族聚酰胺(例如,尼龙)、芳族聚酰胺(例如,Aramid)、聚丙烯、聚乙烯、聚(氯乙烯)、氟烃(例如聚(四氟乙烯)PTFE)和聚氨酯(例如,LycraTM,SpandexTM)的纤维;矿物来源的纤维,例如玻璃、碳、陶瓷和金属纤维;和其中任何羧酸基已经化学反应了,结果不具有反应性的植物来源的纤维,例如乙酸纤维素。
可通过浸轧将抗菌活性剂施加到非纤维素纤维上,但在非纤维素纤维和抗菌活性剂之间不具有相互作用,因此对洗涤或漂洗不具有耐久性。此外,若使用可能对皮肤具有负面影响的抗菌活性剂,则这一体系在要求皮肤接触的应用中是不可行的。
我们已发现,可通过可自交联的树脂将抗菌活性剂固定到非纤维素纤维上且不需要在非纤维素纤维和抗菌活性剂之间离子键合或共价交联。
特别地,我们已发现,可在非常少或者没有活性氢的情况下将抗菌活性剂固定到非纤维素纤维上。难以测量纤维上的活性氢的浓度,然而,密切相关的性能是纤维的亲水度。可使用许多参数,其中包括纤维的酸值和或纤维的回潮率来确定纤维的亲水度。
在“Comprehensive Cellulose Chemistry”D.Klemm,B.Philipp,T.Heinze,U.Heinze和W.Wagenknecht,第1卷,Fundamentals andAnalytical Methods,Wiley-VCH,1998,ISBN 3-527-29413-9中描述了酸值的测量。以下描述测量纤维酸值所使用的技术。
回潮率是通过完全干燥的纤维吸收的水量,其详述于ASTM D2495和D1909中。以下描述测量回潮率所使用的技术。
根据本发明,提供一种抑制在回潮率≤5%的非纤维素纤维上微生物生长的组合物,其包括:
i)1-50%重量的至少一种可自交联的树脂;
ii)0.25-20%重量的至少一种催化剂;
iii)0.1-4.0%重量与该树脂反应的至少一种抗菌活性剂;
iv)98.65-26%重量的水;
其中i)+ii)+iii)+iv)=100%。
优选地,非纤维素纤维的回潮率≤4.5%,更优选≤4.0%,最优选≤3.0%。特别是≤2.0%,和最特别地为≤1.5%。
根据本发明的一个可供替代的实施方案,还提供一种抑制在酸值≤5mmol/kg的非纤维素纤维上微生物生长的组合物,其包括:
i)1-50%重量的至少一种可自交联的树脂;
ii)0.25-20%重量的至少一种催化剂;
iii)0.1-4.0%重量与该树脂反应的至少一种抗菌活性剂;
iv)98.65-26%重量的水;
优选地,非纤维素纤维的酸值≤4mmol/kg,更优选≤3mmol/kg和最优选≤2mmol/kg。
优选的非纤维素纤维是合成纤维。最优选非纤维素纤维包括聚酯、聚酰胺(尼龙)、聚丙烯、聚氨酯(LycraTM,SpandexTM)和乙酸纤维素。
优选地,该组合物包括1-40%重量,更优选2-20%重量,和最优选3-12%重量的至少一种可自交联的树脂。
优选地,该组合物包括0.25-10%重量,更优选0.5-5%重量,和最优选0.75-3%重量的至少一种催化剂。
优选地,该组合物包括0.2-4.0%重量,更优选0.2-3.0%重量,和最优选0.4-1.6%重量与该树脂反应性的至少一种抗菌活性剂。
优选地,该组合物包括60-98%重量的水,更优选75-97%重量,和最优选80-95%重量的水。
优选地,可自交联的树脂对与该可自交联的树脂反应性的抗菌活性剂的重量比范围为1∶1到20∶1,更优选范围为1∶1到15∶1,和最优选范围为2∶1到10∶1。
本发明的可自交联的树脂可基于甲醛与脲或三聚氰胺的缩合物,所述缩合物可另外改性以降低非所需的游离甲醛含量(游离甲醛产生令人讨厌的气味且可引起皮肤反应)。额外的甲醛缩合物包括亚乙基脲、苯并胍胺硫脲和乙酰基胍胺。
合适的可自交联的树脂可描述为氨基树脂,更优选醚化的氨基树脂,和最优选包括脲醛树脂和三聚氰胺甲醛树脂,和尤其甲基化和丁基化的脲醛树脂和三聚氰胺甲醛树脂。
优选掺入亚乙基且释放较低含量甲醛的可自交联的树脂,且包括二羟甲基二羟基亚乙基脲[DMDHEU]和二羟基二亚甲基脲[DHDMEU]。这种可自交联的树脂中的其余羟基可进一步用丁基或甲基醚化,仍进一步降低游离甲醛含量,且这种可自交联的树脂常常被称为无甲醛树脂。
优选使用脲醛树脂,这是由于其具有导致处理改进的较低的可交联密度。
优选使用非常低甲醛和最优选不含甲醛的树脂。
在本发明中使用的可自交联的树脂(但不限于)以下表1中所示的详述商品名获自商业供应商:
表1
可自交联的树脂的商品名 | 化学类型 | 商业供应商 |
VALREZ | 低甲醛的DMDHEU树脂 | APS Chemicals |
AIROREZ | 低到零甲醛的三聚氰胺和脲树脂 | Airedale Chemical Co Ltd |
FABRISET | 低甲醛的DMDHEU树脂 | Alphachem Specialties Ltd |
AVCO-REZ | 低甲醛的DMDHEU树脂 | Avco Chemicals Ltd |
BAYPRET | 醚化的三聚氰胺形式 | Bayer AG |
ACROFIX | 醚化的三聚氰胺形式 | Bayer AG |
AC119TO176BEETAFIN L9009-9801BEETLE RESIN PT | 甲基化DMDHEU羟甲基三聚氰胺形式 | BIP Ltd |
ELASTOFIX | 低甲醛的DMDHEU树脂 | Boehme KG Chem Fab GmbH+Co |
REACELREAPRET | UF、MF、乙二醛和DMEU树脂 | Giovanni Bozzetto Spa |
APOMUL | DMDHEU树脂,三聚氰胺和脲-甲醛树脂 | Brookstone Chemicals Ltd |
FIXAPRETKAURITHELIZARIN | HMDEU,HMUMMMMMM聚缩合物 | BASF plc |
KNITTEXLYOFIXALCOPRINT | 改性DMDHEU烷基改性的三聚氰胺/形式 | Ciba Specialty ChemicalsInc |
ARKOFIXCASSURIT | 低到零甲醛的改性DMDHEU | Clariant International AG |
REAKNITT | 醚化DMDHEU | R.Beitlich GmbH |
STABITEX | 甲氧基甲基三聚氰胺 | Cognis Deutschl and GmbH |
PERMAFRESH | DMDHEU,乙二醛,三聚氰胺和脲-甲醛树脂 | Contract Chemicals Ltd |
ALBUTEXHYCAR | 三聚氰胺和脲-甲醛树脂 | BF Goodrich CorporationNoveon Inc. |
RUCON | DMDHEU,HMUMMM | Rudolf GmbH and Co KG |
SARALINK | 低甲醛树脂 | Sarex Overseas |
RESINTEXFINTEXCHEMPERMUTEX | 羟甲基二羟基亚乙基脲MF | Texchem Ltd Dyestuffs |
TC-REAKTANT | 低甲醛的树脂 | Textilcolor AF |
SERIREZ | MF、UF、甲基化UF树脂 | York shire Chemicals plc |
EDUNINE | 低甲醛树脂 | Uniquema |
DUPRANINQUECODUR | 醚化二羟甲基乙二醛 | Thor Specialties UK Ltd |
DRYWEAR | 低甲醛树脂 | Rotte GmbH |
NOVAROL | 三聚氰胺,乙二醛树脂 | Novaria Snc |
备注:UF=脲/甲醛,MF=三聚氰胺/甲醛,DMEU=二羟甲基亚乙基脲,HMDEU=羟甲基二亚乙基脲,MMM=甲基化羟甲基三聚氰胺 |
为了引发树脂的自交联反应,要求催化剂。合适的催化剂包括金属氯化物催化剂,例如氯化镁和氯化铵;硫酸铵;强酸,例如甲酸、硼酸、磷酸、草酸的铵盐,和胺盐酸盐催化剂,例如聚六亚甲基双胍[PHMB]盐酸盐,其中氯离子充当催化剂。然而,优选具有添加的催化剂(亦即,不是PHMB)。若PHMB用作催化剂,则组分ii)和iii)所使用的用量仍然与以上所述的一样,优选地,催化剂选自氯化镁;氯化铵;硫酸铵;甲酸、硼酸、磷酸、草酸的铵盐;及其混合物。
催化剂可含有诸如柠檬酸之类的添加剂。额外的添加剂的功能可以是增加固化速度,减少发黄,和或扫除任何释放的甲醛。
使用抗菌活性剂抑制微生物,例如细菌、真菌、病毒、藻类、酵母和原生动物等的生长。本发明中使用的合适的抗菌活性剂是具有反应性羟基或胺基的试剂,该试剂与可自交联的树脂共价反应。实例包括,但不限于,季铵盐、双胍和单胍类型的抗菌活性剂,酚类,醇类和2-溴-2-硝基丙-1,3-二醇。优选地,抗菌活性剂选自季铵盐、双胍和单胍和/或其混合物。
因此,可在两方面均能使用聚六亚甲基双胍盐酸盐,即氯离子作为催化剂和聚六亚甲基双胍部分作为抗菌活性剂。
优选地,抗菌活性剂选自双胍类和单胍类。
优选地,双胍包括通过含有至少一种亚甲基的桥连基团连接的式(1)的至少两种双胍单元:
式(1)
该桥连基团优选包括聚亚甲基链,所述聚亚甲基链任选地被掺入一个或多个杂原子,例如氧、硫或氮或被其取代。该桥连基团可包括一个或多个可饱和或者不饱和的环状部分。优选地,桥连基团使得至少三个,和特别是至少四个碳原子直接插入式(1)的两个相邻的双胍单元之间。优选地,在式(1)的两个相邻的双胍单元之间插入的碳原子不大于10,和特别是不大于8。
可通过任何合适的基团,例如烃基、取代烃基、胺基或式(2)的氰基胍基封端双胍:
式(2)
当封端基是烃基时,它优选是烷基、环烷基、芳基或芳烷基。当烃基是烷基时,它可以是直链或支链的烷基,但优选是直链烷基。优选的烷基包括C1-8烷基。优选的烷基的实例包括例如甲基、乙基、正丙基、异丙基、正戊基、正丁基、异丁基、叔丁基和正辛基。
当烃基是环烷基时,它优选是环丙基、环戊基或环己基。当烃基是芳烷基时,它优选在将芳基连接到双胍的亚烷基中含有1-6,更优选1-2个碳原子。优选的芳烷基包括苄基和2-苯乙基。
优选的芳基包括苯基。当封端基是取代烃基时,取代基可以是不显示出对聚合物双胍的微生物性能具有非所需的负面影响的任何取代基。这种取代基的实例是芳氧基、烷氧基、酰基、酰氧基、卤素和腈。
当双胍含有式(1)的两个双胍基团时,则双胍是双联胍(bisbiguanide)。两个双胍基优选通过聚亚甲基,特别是六亚甲基连接。
在这种双联胍内的封端基优选是C1-10烷基(所述C1-10烷基可以是直链或支链烷基)和任选地取代的芳基,特别是任选取代的苯基。这种封端基的实例是2-乙基己基和4-氯苯基。这种双联胍的具体实例是游离碱形式的用式(3)和式(4)表示的化合物。
式(3)
式(4)
双胍优选含有大于两个式(1)的双胍单元,且优选是具有下式(5)表示的重复聚合物链的直链聚合物双胍或其盐:
式(5)
其中X和Y代表桥连基,所述桥连基可以相同或不同,和其中通过X连接的氮原子对之间直接插入的碳原子的总数加上通过Y连接的氮原子对之间直接插入的碳原子的总数之和大于9且小于17。
桥连基X和Y优选由聚亚甲基链组成,所述聚亚甲基链任选地被杂原子,例如氧、硫或氮隔开。X和Y也可掺入可饱和或者不饱和的部分,在此情况下,通过X和Y连接的氮原子对之间直接插入的碳原子数被视为包括最短的环状基团片段。因此,在下述基团中的氮原子之间直接插入的碳原子数为4,而不是8。
具有式(5)的重复聚合物单元的直链聚合物双胍典型地以其中聚合物链具有不同长度的聚合物混合物形式获得。优选地,式(5a)和(5b)中各双胍单元的数量之和为3-约80。
式(5a) 式(5b)
优选的直链聚合物双胍是其中X和Y相同的聚合物链的混合物,且不包括封端基的各聚合物链为式(6)或其盐:
式(6)
其中n为4-20,特别是4-18。特别优选n的平均值为约16。优选地,游离碱形式的聚合物的平均分子量为1100-4000。
可通过式(7)的二双氰胺:
式(7)
与二胺H2N-Y-NH2反应,其中X和Y具有以上定义的含义,或者通过使式(8)的双氰胺的二胺盐:
(H3N+-X-N+H3)(N-(CN)2)2
式(8)
与二胺H2N-Y-NH2反应,其中X和Y具有以上定义的含义,从而制备直链聚合物双胍。在GB专利No.702268和1152243中分别描述了这些制备方法,和此处所述的任何聚合物双胍可用于本发明。如前所述,直链聚合物双胍的聚合物链可或者用氨基或者用下式(9)的氰基胍基封端。
式(9)
可在制备直链聚合物双胍的过程中水解这一氰基胍基,从而得到胍端基。在每一聚合物链上的端基可以相同或不同。在制备以上所述的聚合物双胍中,可与二胺H2N-Y-NH2一起包括小比例的伯胺R-NH2,其中R代表含有1-18个碳原子的烷基。伯胺充当链终止剂,因此,可用-NHR基终止聚合物双胍的聚合物链的一个或两个端基。也可使用这些-NHR链终止的聚合物双胍。聚合物双胍容易与无机和有机酸二者形成盐。优选的聚合物双胍盐是水溶性盐。当聚合物双胍用游离碱形式的式(3)的化合物表示时,优选的水溶性盐是二葡糖酸盐。它可以以商品名VantocilTMCHG商购于Avecia Limited。当聚合物双胍是游离碱形式的式(6)表示的直链聚合物的混合物时,优选的盐是盐酸盐。
特别优选的是,本发明所使用的聚合物双胍是盐酸盐形式的直链聚合物的混合物,其中所述直链聚合物中的各聚合物链(不包括端基)用式(6)表示。这一聚(六亚甲基双胍)化合物以商品名ReputexTM20商购于Avecia Limited。
聚(C2-18烃基单胍)(“PMG”)区别于PHMB在于,它们含有单胍基,而PHMB不含单胍基,而是含有式-NHC=(NH)NHC(=NH)NH-的双胍基。
PMG优选包括多个式(10)的基团和/或式(11)的基团或其盐。
式(10)
式(11)
其中:
每一m独立地为0或1;
每一z独立地为C2-18烃基;
A和B是一起包括总计3-18个碳原子的烃基;
每一R独立地为氢、任选取代的烷基或任选取代的烷氧基。
优选每一m为0。
在PMG内且用Z、A、和B表示的烃基任选地被一个或多个杂原子或基团隔开,且任选地携带一个或多个除了氢以外的取代基。优选的隔开原子和基团是-O-、-S-、-NH-、-C(=O)-和亚苯基。优选的任选取代基是羟基;C1-4烷氧基;卤素,特别是氯或溴;硝基;氨基;取代氨基;和酸基,特别是羧基、磺基和磷酸基。
优选地,在PMG内且用Z表示的烃基是C2-18亚烷基(更优选C4-16亚烷基,特别是C6-12亚烷基,更特别地为C6亚烷基);C3-12亚芳基,更优选C6-10亚芳基,特别是亚苯基或亚萘基;C7-12亚芳烷基(更优选C7-11亚芳基,特别是亚苄基或亚二甲苯基);或其结合,其任选地被一个或多个-O-、-S-、-NH-或-C(=O)-基隔开。
优选地,用A和B表示的烃基各自独立地为C2-6亚烷基,其任选地被一个或多个-O-、-S-、-NH-或-C(=O)-基隔开,条件是A和B包括总计3-12个碳原子,优选3-6个碳原子,更优选3或4个碳原子。在特别优选的实施方案中,A或B之一是-CH2-或-(CH2)2-,和其它是-(CH2)2-,更特别地A和B二者为-(CH2)2-。
用Z表示的优选烃基的实例包括-CH2C6H4CH2-、-CH2OC6H4OCH2-、-CH2OC6H10OCH2-、-(CH2)3O(CH2)3-和-(CH2)2S(CH2)2-。
用Z表示的特别优选烃基的实例包括-(CH2)6-、-(CH2)8-、-(CH2)12-、-CH2CH(-CH3)(CH2)4CH3、1,4-、2,3-和1,3-亚丁基、2,5-亚己基、2,7-亚庚基和3-甲基-1,6-亚己基。
优选用Z表示的所有基团相同,且为C4-16亚烷基,更优选C4-12亚烷基,特别是C4-8亚烷基,更特别地为1,6-亚己基。
优选每一R独立地为H、C1-4烷基、C1-4烷氧基或C1-4烷氧基-OH,更优选H或甲基,特别是H。
优选地,PMG基本上由式(10)的基团组成。
优选地,用R表示的所有基团相同。
更优选用R表示的所有基团是H。
认为在PMG上的终止基的性质不是关键的,在PMG上的优选的终止基是氨基和胍基。
鉴于前述的择优选择,PMG优选包括一个或多个式(12)的基团或其盐。
式(12)
其中:
n为2-50,优选3-25。
优选地,PMG为盐形式。优选的盐是具有有机或无机酸的盐,特别是水溶性盐,例如葡糖酸盐、乙酸盐或磷酸盐。
可通过使盐酸胍与二胺,例如式H2N-Y-NH2、HN(-A-)(-B-)NH反应,或者与这种二胺的混合物反应,从而制备PMG,其中Z、A和B如上所定义。
要理解,PMG也可含有小量除了式(10)和(11)的重复单元以外的重复单元。然而,优选PMG基本上由式(10)和/或(11)的重复单元以及终止基组成。
实例包括聚六亚甲基单胍,例如获自于SK Corp.的SKAN BTM,和聚(氧亚乙基)胍盐酸盐,例如获自澳大利亚POC的AkacidTM。
非聚合物单胍的合适实例包括正癸基(docyl)胍盐酸盐。
该组合物可用水、含水溶剂、有机溶剂和或其混合物稀释,之后施加到非纤维素纤维上。优选地,用水和或与水混溶且具有低的挥发度的醇,尤其二元醇稀释组合物,更优选用水稀释组合物。
本发明的组合物任选地也可包括染料;除味剂;UV吸收剂;不可交联的树脂;软化剂;芯吸剂;防水剂;抗静电剂;防污剂;润滑剂,例如聚四氟乙烯(PTFE)和在纺织品工业领域中熟练的技术人员公知的其它添加剂。
在本发明的第二实施方案中,提供抑制在回潮率≤5%和或酸值≤5mmol/kg的非纤维素纤维上微生物生长的方法,该方法包括下述步骤:
A)使纤维与含下述组分的组合物接触:
i)1-50%重量的至少一种可自交联的树脂;
ii)0.25-20%重量的至少一种催化剂;
iii)0.1-4%重量与该树脂反应的至少一种抗菌活性剂;
iv)98.65-26%重量的水;
其中i)+ii)+iii)+iv)=100%。
B)任选地干燥用该组合物接触过的纤维;和
C)固化用该组合物接触过的纤维,使树脂进行交联。
可通过任何本领域已知的湿法整理技术,例如喷淋、浸渍或浸轧工艺,将根据本发明第一方面的组合物施加到非纤维素纤维(或由其制造的纱线或织物)。浸轧包括或者通过使材料经过浴,然后通过挤压辊,或者简单地通过经过挤压辊,其中下方的挤压辊之一部分或全部浸渍在组合物内,从而施加组合物到材料上。可以以单一浸渍、单一挤压操作使用这种技术,或者可更加复杂化(例如,双浸渍、双辊隙压浸或多浸渍、单辊隙(nip)等)。对于织造材料,例如床上用品和毛巾来说,优选通过在织造材料辊上压浸该组合物,从而施加该组合物。进一步的湿法施加技术涉及使用喷淋或滴流棒施加该组合物到松散纤维或复合非织造材料的移动床上。
在用组合物涂布纤维之后,通过例如挤压除去过量液体,接着处于固化状态,引起可自交联树脂交联并使抗菌活性剂与可自交联树脂之间进行反应。优选地,抗菌活性剂与树脂共价反应。优选地,在100-180℃的温度范围内,更优选在140-180℃范围内,和最优选在140-160℃范围内进行固化步骤。
显然确切的固化时间和温度取决于所使用的确切装置,然而,固化时间范围优选为30秒-5分钟。
根据本发明的第三方面,提供一种回潮率≤5%和或酸值≤5mmol/kg的非纤维素纤维,其载有含下述组分的组合物:
(a)基于非纤维素纤维计为1-10%重量至少一种可自交联树脂;和
(b)基于非纤维素纤维计为0.1-1%重量与该树脂反应的至少一种抗菌活性剂。
根据本发明的第四方面,提供用本发明第一方面的组合物处理的回潮率≤5%和或酸值≤5mmol/kg的非纤维素纤维。
根据本发明的第五方面,提供本发明第一方面的组合物在处理回潮率≤5%和或酸值≤5mmol/kg的非纤维素纤维上的用途。
通过下述实施例进一步阐述本发明,其中所有基准是重量份,除非另有说明。
试验方法
回潮率
在ASTM D 2495中描述了棉和棉的共混物回潮率的标准试验方法,并将其用于此处所述的非纤维素纤维上。回潮率定义为在预定条件下测定的材料样品内水的含量并以不含水的材料样品的质量百分数形式表达。大体上称取纤维样品,在烘箱内干燥直到达到恒重,然后以百分数形式计算起始质量与烘箱干燥质量之差。
在ASTM D 1909中给出了典型的商业回潮率值:羊毛(13.6%)、蚕丝(11%)、人造丝(11%)、棉(8.5%)、尼龙(聚酰胺)(4.5%)、聚酯(0.4%)、丙烯酸系(1.5%)、聚氨酯(Spandex)(1.3%)、聚丙烯(烯烃)(0.0%)、聚氯乙烯(Vinyon)(0.0%)和氟烃(Teflon)(0.0%)。
在下述实施例中,使用回潮率为0.4%的聚酯纤维。
酸值
通过PHMB的吸收测定纤维的酸值。
将8g待测试的纤维浸渍在120g80ppm PHMB(在蒸馏水中的)的溶液内,并在40℃下搅拌1小时。这被称为尽染。
溶液与纤维之比被称为浴比,在该方法中,浴比为120/8=15。
在纤维尽染之前和之后,在235nm下测量PHMB溶液的UV/可见光谱。根据校正图表,计算上染之前和之后PHMB的浓度。
通过方程式1给出纤维的酸值:
酸值(mmol/kg)=(PHMB的浓度差(ppm×浴比))/PHMB的分子量(方程式1)
典型酸值为:棉(30mmol/kg)、粘胶丝(60mmol/kg)、尼龙(1.6mmol/kg),聚酯(红色,针织0.91mmol/kg))、聚酯(蓝色,织造0.57mmol/kg)。
在以下的实施例中,使用酸值为1.07mmol/kg的聚酯纤维。
抗菌活性剂含量
通过用Eosin Y染色,测定在处理纤维上具有阳离子基团的抗菌活性剂,例如PHMB的含量。
Eosin Y试验溶液
通过在蒸馏水[1500cm3]内溶解Eosin Y[15g 80%2`,4`,5`,7`-四溴荧光素二钠盐指示剂等级,获自Aldrich Chemical Co.],然后用蒸馏水稀释到2500cm3,从而制备Eosin Y的储液。
混合以上制备的200cm3的Eosin Y的储液与蒸馏水[1500cm3],并添加柠檬酸钠[100g]。在完全溶解柠檬酸钠之后,进一步用蒸馏水稀释溶液到2000cm3,得到Eosin Y试验溶液。
染色工序
精确地称取待测试的纤维样品(约0.2g),将其放置在30cm3的小瓶内,并添加100倍(纤维)重量的Eosin Y试验溶液,之后密封该小瓶,并在环境温度下将该小瓶放置在辊上20分钟。
取出纤维样品,并在冷水中漂洗,然后放置在约800cm3的热水中,并搅拌5分钟。这一漂洗步骤进一步重复3次,之后在50℃下干燥纤维样品。
评价处理程度
使用X-Rite SP62分光光度计,测量染色纤维样品的反射光谱。或者,也可使用染色的纤维样品与一系列染色的参考样品的直接视觉比较,得到处理程度的可接受的评价。
抗菌活性的评估
AATCC 100试验方法(1998)是例如在由非纤维素纤维制造的纺织品材料样品上测量细菌菌落并进而测定抗菌效率的定量试验。以下概述了该工序。在5%无菌生理盐水溶液中稀释在营养肉汤中摇动过夜的肺炎克雷伯氏菌(Klebsiella pneumoniae)培养物到约1×105个细胞/cm3。从每一片处理布料中取出2块样品(每一块0.5g)并用1cm3的肺炎克雷伯氏菌悬浮液接种。在接种之后,一块布料样品立即用100cm3的中和剂溶液(CEN标准中和剂)中和,并激烈摇动60秒。通过连续稀释倾注培养方法,使用盐水溶液作为稀释剂,在营养琼脂板上计数存活的细胞。其它接种的样品在37℃下保温24小时。然后如上所述进行中和与计数技术。可在由American Association of TextileChemists and Colorists,PO Box 12215,Research TrianglePark,North Caroline 27709,USA出版的AATCC Technical Manual中找到这一技术进一步的细节。
所有计数以菌落形成单位/cm3(cfu/cm3)测量。
纤维的洗涤
使用Home Laundry Consultative Council(HLCC)的标准方法洗涤由非纤维素纤维制造的织物样品,其中United Kingdom集团公司对制定纺织品洗涤的原则负责。以规则的间隔取出样品,并进行最多25次洗涤。
所使用的方法是在40℃下6A。洗涤的细节如下所述:
1.在40℃下洗涤6分钟
2.在15℃下2次漂洗3分钟
3.1次漂洗2分钟+1分钟旋压
4.1次漂洗2分钟+2分钟旋压
洗衣机是Wascator FOM71。每次洗涤使用2kg样品和48g ECE参考洗涤剂+12g高硼酸盐漂白剂。
实施例1(E1)
TexchemTM2700是由Rochdale UK的Texchem Dyestuffs Ltd.供应的具有66%固体含量的水溶液形式的改性DMDHEU树脂,并且以供应时的形式使用。
CondensolTMFC是氯化镁和其它组分的50%水溶液,并且以德国BASF plc,Ludwigshafen供应时的形式使用。
ReputexTM20是由Blackley,UK的Avecia Ltd.供应的20%PHMB的水溶液,并且以供应时的形式使用。
制备100g TexchemTM2700、30g CondensolTMFC和40g ReputexTM20的混合物,并水补充至1000cm3,引入到实验室压浸/轧片机的贮槽中。使尺寸为25cm×25cm的一片100%的聚酯织物经过压浸,并挤压,得到50%的吸液率。然后空气干燥织物,并在160℃下热固化3分钟,在热水中漂洗并空气干燥。
实施例2(E2)
BaypretTMR是由德国Leverkusen的Bayer AG以具有60%固体含量的水溶液形式供应的改性DMDHEU树脂,并且以供应时的形式使用。
制备100g BaypretTMR、30g CondensolTMFC和40g ReputexTM20的混合物,并以水补充至1000cm3,引入到实验室压浸/轧片机的贮槽中。使25cm×25cm的一片100%的聚酯织物经过压浸,并挤压,得到50%的吸液率。然后空气干燥织物,并在160℃下热固化3分钟,在热水中漂洗并空气干燥。
对比例1(CE1)
未处理的100%聚酯织物。这一实施例是不具有额外处理的对照样品。
对比例2(CE2)
将用水补充至1000cm3的40g ReputexTM20引入到实验室压浸/轧片机的贮槽中。使25cm×25cm的一片100%的聚酯织物经过压浸,并挤压,得到50%的吸液率。然后空气干燥织物,并在160℃下热固化3分钟,在热水中漂洗并空气干燥。这一实施例是具有抗菌活性剂但不具有可自交联树脂或催化剂的对照样品。
在40℃下洗涤织物最多25次。
对比例3(CE3)
制备100g TexchemTM2700和30g CondensolTMFC的混合物,并以水补充至1000cm3,引入到实验室压浸/轧片机的贮槽中。使25cm×25cm的一片100%的聚酯织物经过压浸,并挤压,得到50%的吸液率。然后空气干燥织物,并在160℃下热固化3分钟,在热水中漂洗并空气干燥。这一实施例是具有可自交联树脂和催化剂但不具有抗菌活性剂的对照样品。
对比例4(CE4)
制备100g BaypretTMR和30g CondensolTMFC的混合物,并以水补充至1000cm3,引入到实验室压浸/轧片机的贮槽中。使25cm×25cm的一片100%的聚酯织物经过压浸,并挤压,得到50%的吸液率。然后空气干燥织物,并在160℃下热固化3分钟,在热水中漂洗并空气干燥。这一实施例是具有可自交联树脂和催化剂但不具有抗菌活性剂的对照样品。
所有织物在40℃下洗涤最多25次,并使用Eosin Y染色技术测量耐洗性,且在下表2中给出了结果。
表2
实施例 | 未洗涤 | 1次洗涤 | 10次洗涤 | 25次洗涤 |
E1 | 强的紫色染色 | 中等紫色染色 | 中等紫色染色 | 中等紫色染色 |
E2 | 强的紫色染色 | 中等紫色染色 | 中等紫色染色 | 中等紫色染色 |
CE1 | 没有染色 | 没有染色 | 没有染色 | 没有染色 |
CE2 | 强的紫色染色 | 没有染色 | 没有染色 | 没有染色 |
CE3 | 没有染色 | 没有染色 | 没有染色 | 没有染色 |
CE4 | 没有染色 | 没有染色 | 没有染色 | 没有染色 |
表2表明织物本身、可自交联的树脂和催化剂没有用Eosin Y染成紫色。
当在没有任何可自交联的树脂情况下施加抗菌活性剂时,获得紫色染色。然而,在一次洗涤之后,颜色消失,这显然表明抗菌活性剂不耐洗。
如上所述测量抗菌活性水平并在下表3中给出了结果。
表3
未洗涤 | 1次洗涤 | 10次洗涤 | 25次洗涤 | |||||
实施例 | 细菌计数cfu/cm3 | 与对照组相比的对数下降 | 细菌计数cfu/cm3 | 与对照组相比的对数下降 | 细菌计数cfu/cm3 | 与对照组相比的对数下降 | 细菌计数cfu/cm3 | 与对照组相比的对数下降 |
E1 | <100 | 5.8 | <100 | 5.9 | <100 | 6.1 | <100 | 6.3 |
E2 | <100 | 5.8 | <100 | 5.9 | <100 | 6.1 | <100 | 6.3 |
CE1 | 5.9×107 | 0 | 6.7×107 | 0 | 1.1×108 | 0 | 2.0×108 | 0 |
CE2 | <100 | 5.8 | 9.8×107 | 0 | 9.8×107 | 0 | 1.2×108 | 0 |
CE3 | 6.7×107 | 0 | - | - | 6.7×107 | 0 | 8.6×107 | 0 |
Claims (26)
1.一种抑制在回潮率≤5%的非纤维素纤维上的微生物生长的组合物,其包括:
i)1-50%重量的至少一种可自交联的树脂;
ii)0.25-20%重量的至少一种催化剂;
iii)0.1-4%重量与该树脂反应性的至少一种抗茵活性剂;
iv)98.65-26%重量的水;
其中i)+ii)+iii)+iv)=100%。
2.权利要求1的组合物,其中非纤维素纤维的酸值为≤5mmol/kg。
3.一种抑制在酸值≤5mmol/kg的非纤维素纤维上的微生物生长的组合物,其包括:
i)1-50%重量的至少一种可自交联的树脂;
ii)0.25-20%重量的至少一种催化剂;
iii)0.1-4%重量与该树脂反应性的至少一种抗茵活性剂;
iv)98.65-26%重量的水;
其中i)+ii)+iii)+iv)=100%。
4.权利要求3的组合物,其中非纤维素纤维的回潮率≤5%。
5.前述任何一项权利要求的组合物,其中非纤维素纤维选自聚酯、聚酰胺、聚丙烯、聚氨酯和乙酸纤维素。
6.前述任何一项权利要求的组合物,其中可自交联的树脂是氨基树脂。
7.权利要求6的组合物,其中可自交联的树脂是甲醛与脲或三聚氰胺的缩合物。
8.权利要求7的组合物,其中可自交联的树脂选自二羟甲基二羟基亚乙基脲和二羟基二亚甲基脲。
9.前述任何一项权利要求的组合物,其中催化剂选自氯化镁;氯化铵;硫酸铵;甲酸、硼酸、磷酸、草酸的铵盐;和聚(六亚甲基双胍)盐酸盐和或其混合物。
10.权利要求1-8任何一项的组合物,其中催化剂选自氯化镁;氯化铵;硫酸铵;甲酸、硼酸、磷酸、草酸的铵盐;和或其混合物。
11.权利要求1-9任何一项的组合物,其中催化剂是聚(六亚甲基双胍)盐酸盐。
12.前述任何一项权利要求的组合物,其中抗茵活性剂选自季铵盐、双胍、单胍和或其混合物。
13.抑制在回潮率≤5%的非纤维素纤维上的微生物生长的方法,该方法包括下述步骤:
A)使纤维与前述任何一项权利要求的组合物接触:
B)任选地干燥与该组合物接触过的纤维;和
C)固化与该组合物接触过的纤维,使树脂进行交联。
14.权利要求13的方法,其中非纤维素纤维的酸值为≤5mmol/kg。
15.抑制在酸值≤5mmol/kg的非纤维素纤维上的微生物生长的方法,该方法包括下述步骤:
A)使纤维与前述任何一项权利要求的组合物接触:
B)任选地干燥与该组合物接触过的纤维;和
C)固化与该组合物接触过的纤维,使树脂进行交联。
16.权利要求15的方法,其中非纤维素纤维的回潮率≤5%。
17.权利要求13-16任何一项的方法,其中在100-180℃的温度范围内进行步骤C)。
18.权利要求13-17任何一项的方法,其中步骤C)进行30秒-5分钟的时间。
19.一种回潮率≤5%的非纤维素纤维,其载有含下述组分的组合物:
(a)基于非纤维素纤维计为1-10%重量的至少一种可自交联树脂;和
(b)基于非纤维素纤维计为0.1-1%重量的与该树脂反应的至少一种抗茵活性剂。
20.权利要求19的非纤维素纤维,其酸值为≤5mmol/kg。
21.一种酸值≤5mmol/kg的非纤维素纤维,其载有含下述组分的组合物:
(a)基于非纤维素纤维计为1-10%重量的至少一种可自交联树脂;和
(b)基于非纤维素纤维计为0.1-1%重量的与该树脂反应的至少一种抗菌活性剂。
22.权利要求21的非纤维素纤维,其回潮率≤5%。
23.用权利要求1-11任何一项的组合物处理的回潮率≤5%的非纤维素纤维。
24.用权利要求1-11任何一项的组合物处理的酸值≤5mmol/kg的非纤维素纤维。
25.权利要求1-11任何一项的组合物在处理回潮率≤5%的非纤维素纤维中的用途。
26.权利要求1-11任何一项的组合物在处理酸值≤5mmol/kg的非纤维素纤维中的用途。
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- 2004-11-10 US US10/580,802 patent/US8147707B2/en not_active Expired - Fee Related
- 2004-11-10 BR BRPI0416710-4A patent/BRPI0416710A/pt not_active Application Discontinuation
- 2004-11-10 CN CN2004800348955A patent/CN1886547B/zh not_active Expired - Fee Related
- 2004-11-10 WO PCT/GB2004/004738 patent/WO2005054566A1/en active Application Filing
- 2004-11-10 JP JP2006540573A patent/JP2007513262A/ja active Pending
- 2004-11-10 EP EP20040798461 patent/EP1697577B1/en not_active Not-in-force
-
2006
- 2006-06-27 KR KR1020067012892A patent/KR101173150B1/ko active IP Right Grant
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111621981A (zh) * | 2015-02-27 | 2020-09-04 | 生活保卫股份公司 | 具有抗微生物性能之布料 |
CN112030552A (zh) * | 2015-02-27 | 2020-12-04 | 生活保卫股份公司 | 具有抗微生物性能之布料 |
CN108018714A (zh) * | 2016-11-04 | 2018-05-11 | 香港纺织及成衣研发中心有限公司 | 一种屏障织物制造方法及屏障织物 |
WO2018082454A1 (zh) * | 2016-11-04 | 2018-05-11 | 香港纺织及成衣研发中心有限公司 | 屏障织物制造方法及屏障织物 |
CN109652983A (zh) * | 2018-12-26 | 2019-04-19 | 绵阳佳联印染有限责任公司 | 一种织物抗菌整理液及织物抗菌整理工艺 |
CN110470564A (zh) * | 2019-08-22 | 2019-11-19 | 江苏省纺织产品质量监督检验研究院 | 用于羊毛混纺产品的超声快速定量方法 |
CN113215856A (zh) * | 2021-06-08 | 2021-08-06 | 辽宁大学 | 接触型纸质文物综合保护剂及其制备方法和应用 |
Also Published As
Publication number | Publication date |
---|---|
BRPI0416710A (pt) | 2007-01-16 |
CN1886547B (zh) | 2010-12-08 |
GB0327693D0 (en) | 2003-12-31 |
KR20060125822A (ko) | 2006-12-06 |
WO2005054566A1 (en) | 2005-06-16 |
EP1697577A1 (en) | 2006-09-06 |
EP1697577B1 (en) | 2012-10-24 |
WO2005054566A8 (en) | 2005-10-20 |
KR101173150B1 (ko) | 2012-08-16 |
JP2007513262A (ja) | 2007-05-24 |
US20070271707A1 (en) | 2007-11-29 |
GB2408516A (en) | 2005-06-01 |
US8147707B2 (en) | 2012-04-03 |
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