CN1942613A - 可染色的聚烯烃纤维和织物 - Google Patents
可染色的聚烯烃纤维和织物 Download PDFInfo
- Publication number
- CN1942613A CN1942613A CNA200580011757XA CN200580011757A CN1942613A CN 1942613 A CN1942613 A CN 1942613A CN A200580011757X A CNA200580011757X A CN A200580011757XA CN 200580011757 A CN200580011757 A CN 200580011757A CN 1942613 A CN1942613 A CN 1942613A
- Authority
- CN
- China
- Prior art keywords
- additive
- fiber
- silk
- butyl
- acid
- 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.)
- Pending
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- 150000004056 anthraquinones Chemical class 0.000 claims abstract description 4
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/06—Dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
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- D06P3/794—Polyolefins using dispersed dyes
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- C—CHEMISTRY; METALLURGY
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Abstract
借助于加入可染性添加剂使得聚烯烃纤维和丝以及由其制备的织物可染色。可染性添加剂组合物包含选自聚酰胺、共聚酰胺和聚醚聚酰胺的至少一种化合物和至少一种乙烯-乙酸乙烯酯共聚物。借助于使用稳定剂的组合使得染色的聚烯烃纤维和织物是光稳定的,其中稳定剂的组合包含选自紫外光稳定剂的至少一种化合物和选自位阻胺光稳定剂的至少一种化合物。紫外线稳定剂例如是羟基苯基苯并***或三芳基-s-三嗪。位阻胺光稳定剂例如是高分子量的,例如分子量大于1000g/mol。所述染料例如蒽醌蓝染料、蒽醌红染料、重氮红染料或硝基黄染料。
Description
本发明涉及显示出优异的可染性和耐光牢度的烯烃聚合物纤维和织物。此类纤维可用于服装、毛毯、家具套、一次性医用服、尿布等。
聚烯烃,比如聚丙烯,具有许多适宜的物理性能。但是,其本身的着色能力很差。一直以来都渴求光稳定的可染色的聚烯烃组合物,特别是聚丙烯纤维。
纤维形式的着色聚丙烯在大多数情况下是通过添加固体颜料而获得的。不幸的是,含固体颜料的纤维根本不及染色纤维有竞争力。而且,同染料相比,由于种类有限,颜料可供选择的范围也相当有限。还有,使用颜料会对可以向由聚丙烯制造的衣物制品上施用的图案构成限制。另外,某些颜料会影响聚丙烯纤维的可拉伸性和最终性能。其它聚烯烃比如聚乙烯也有类似的缺点。一直存在着对可染色聚烯烃组合物,例如聚丙烯纤维的需求。特别需要可染色的光稳定的聚烯烃。
美国专利5,140,065公开了与颜料相容的热塑性模塑组合物,它包含嵌段聚醚聚酰胺、嵌段聚醚酯聚酰胺、非晶态共聚酰胺和改性共聚烯烃。
美国专利6,054,215公开了可染色的聚丙烯纤维。
美国专利5,130,069公开了包含某些聚合物添加剂的聚丙烯纤维。
WO-A-97/47684公开了对分散染料有亲和力的聚丙烯组合物,该组合物包含等规立构聚丙烯、共聚酰胺和EVA共聚物。
令人惊奇地发现,包含聚酰胺/乙烯-乙酸乙烯酯共聚物可染性添加剂共混物、至少一种紫外线吸收剂和至少一种位阻胺光稳定剂的聚烯烃组合物可有效染色且是光稳定的。
本发明涉及包含熔体共混物的可染色、光稳定的聚烯烃纤维或丝,该共混物包含
i)聚烯烃基材,
ii)有效量的选自聚酰胺、共聚酰胺和聚醚聚酰胺的至少一种可染性添加剂和选自乙烯-乙酸乙烯酯共聚物的至少一种可染性添加剂的组合,
iii)有效量的选自紫外线吸收剂的至少一种添加剂和选自位阻胺光稳定剂的至少一种添加剂的组合,和
该纤维或丝进一步包含至少一种分散染料。
本发明还涉及制备可染色、光稳定的聚烯烃纤维或丝的方法,该方法包括熔体共混一种组合物,该组合物包含
i)聚烯烃基材,
ii)有效量的选自聚酰胺、共聚酰胺和聚醚聚酰胺的至少一种可染性添加剂化合物和选自乙烯-乙酸乙烯酯共聚物的至少一种可染性添加剂的组合,
iii)有效量的选自紫外线吸收剂的至少一种添加剂化合物和选自位阻胺光稳定剂的至少一种添加剂的组合,
该方法进一步的包括用至少一种分散染料处理所述熔体共混物。
聚烯烃基材的实例是:
1.单烯烃和二烯烃的聚合物例如聚丙烯、聚异丁烯、聚丁-1-烯、聚-4甲基戊-1-烯、聚异戊二烯或聚丁二烯,以及环烯烃例如环戊烯或降冰片烯的聚合物,聚乙烯(其任选进行交联)例如高密度聚乙烯(HDPE)、高密度高分子量聚乙烯(HDPE-HMW)、高密度超高分子量聚乙烯(HDPE-UHMW)、中密度聚乙烯(MDPE)、低密度聚乙烯(LDPE)、线型低密度聚乙烯(LLDPE)、(VLDPE)和(ULDPE)。
聚烯烃,即前一段例举的单烯烃的聚合物,例如,聚乙烯和聚丙烯,可以通过不同的方法,尤其是以下方法制备:
i)自由基聚合(通常在高温高压下)。
ii)使用通常包含元素周期表IVb、Vb、VIb或VIII族的一种或多种金属的催化剂进行的催化聚合。这些金属通常具有一种或多种配体,其典型地为氧化物、卤化物、醇化物、酯、醚、胺、烷基化合物、烯基化合物和/或芳基化合物,它可以是π-配位的或者σ-配位的。这些金属配合物可以是游离形式或固定在基材上,典型地固定在活化的氯化镁、氯化钛(III),氧化铝或二氧化硅上。这些催化剂可溶于聚合介质或者不溶于聚合介质。在聚合时可以直接使用这些催化剂,或可以使用其它的活化剂,典型地是烷基金属化合物、金属氢化物、烷基金属卤化物、烷基金属氧化物或金属烷基烷,所述金属是元素周期表Ia、IIa和/或IIIa族元素。活化剂可以用其它酯、醚、胺或甲硅烷基醚基团方便地进行改性。这些催化剂体系通常被命名为Philips催化剂、Standard Oil Indiana催化剂、Ziegler(-Natta)催化剂、TNZ(DuPont)催化剂、茂金属催化剂或单位点催化剂(SSC)。
2.第1项中提到的聚合物的混合物,例如聚丙烯与聚异丁烯的混合物、聚丙烯与聚乙烯的混合物(例如PP/HDPE、PP/LDPE)、以及不同类型聚乙烯的混合物(例如LDPE/HDPE)。
3.单烯烃和二烯烃互相之间或与其它乙烯基单体之间形成的共聚物,例如乙烯/丙烯共聚物、线型低密度聚乙烯(LLDPE)和其与低密度聚乙烯(LDPE)的混合物、丙烯/丁-1-烯共聚物、丙烯/异丁烯共聚物、乙烯/丁-1-烯共聚物、乙烯/己烯共聚物、乙烯/甲基戊烯共聚物、乙烯/庚烯共聚物、乙烯/辛烯共聚物、丙烯/丁二烯共聚物、异丁烯/异戊二烯共聚物、乙烯/丙烯酸烷基酯共聚物、乙烯/甲基丙烯酸烷基酯共聚物、乙烯/乙酸乙烯酯共聚物和其与一氧化碳的共聚物或乙烯/丙烯酸共聚物及其盐(离聚物),以及乙烯与丙烯和二烯如己二烯、二环戊二烯或亚乙基降冰片烯的三元共聚物;和这种共聚物彼此之间或其与上述第1项中提到的聚合物之间的混合物,例如聚丙烯/乙烯-丙烯共聚物、LDPE/乙烯-醋酸乙烯酯共聚物(EVA)、LDPE/乙烯-丙烯酸共聚物(EAA)、LLDPE/EVA、LLDPE/EAA、和交替的或无规的聚烯烃/一氧化碳共聚物及其与其它的聚合物例如聚酰胺的混合物。
本发明的聚烯烃比如是聚丙烯均聚物和共聚物以及聚乙烯均聚物和共聚物。比如,聚丙烯、高密度聚乙烯(HDPE)、线性低密度聚乙烯(LLDPE)和聚丙烯无规和耐冲击共聚物。
采用烯烃聚合物的共混物或熔合物也是包括在本发明的范围之内。
本发明的可染性添加剂是选自聚酰胺、共聚酰胺和聚醚聚酰胺的至少一种化合物和选自乙烯-乙酸乙烯酯共聚物的至少一种化合物的组合。特别感兴趣的是共聚酰胺。
聚酰胺和共聚酰胺是例如公开在WO-A-97/47684和美国专利5,130,069中的那些。本发明的聚酰胺和共聚酰胺是例如低结晶度的。
所述聚酰胺是如下制备的那些:聚合在氨基和羧基之间具有至少2个碳原子的单氨基单羧酸或其内酰胺,聚合基本上等摩尔份的在氨基之间包含至少2个碳原子的二胺和二羧酸或聚合以上定义的单氨基羧酸或其内酰胺与基本上等摩尔份的二胺和二羧酸。术语“基本上等摩尔”份包括严格的等摩尔份和与其稍微偏离的等摩尔份,其用于稳定生成聚酰胺的粘度所用的传统方法。所述二羧酸可以以其官能性衍生物的形式(例如酯或酰基氯)使用。
用于制备所述聚酰胺的上述单氨基单羧酸或其内酰胺的例子包括在氨基和羧基之间含有2-16个碳原子的化合物,在内酰胺的情况下所述碳原子形成包含-CO-NH-基团的环。作为氨基羧酸和内酰胺的具体例子,可提及ε-氨基己酸、丁内酰胺、新戊内酰胺、ε-己内酰胺、辛内酰胺、庚内酰胺、十一烷内酰胺、十二烷内酰胺和3-和4-氨基苯甲酸。
适用于制备所述聚酰胺的二胺包括直链和支链烷基、芳基和烷芳基二胺。说明性的二胺是丙二胺、丁二胺、戊二胺、辛二胺、己二胺(其常常是优选的)、三甲基己二胺、间苯二胺和间二甲苯二胺。
所述二羧酸可以由下式表示:
HOOC-B-COOH
其中B是包含至少2个碳原子的二价脂族或芳族基团。
脂族酸的例子是癸二酸、十八烷二酸、辛二酸、戊二酸、庚二酸和己二酸。
结晶和非晶态的聚酰胺都可以使用,常常优选结晶物质,因为它们有耐溶剂性。聚酰胺(或尼龙,常常这样称呼它们)的典型实例包括,例如聚酰胺-6(聚己内酰胺)、6,6(聚己二酰己二胺)、11,12、4,6、6,10和6,12,以及源自于对苯二甲酸和/或间苯二甲酸和三甲基己二胺的聚酰胺;源自于己二酸和间二甲苯二胺的聚酰胺;源自于己二酸、壬二酸和2,2-二(对氨基苯基)丙烷或2,2-二(对氨基环己基)丙烷的聚酰胺;和源自于对苯二甲酸和4,4′-二氨基二环己基甲烷的聚酰胺。上述聚酰胺的两种或多种的混合物和/或共聚物也在本发明范围内。优选的聚酰胺是聚酰胺-6、4,6、6,6、6,9、6,10、6,12、11和12,最优选聚酰胺-6,6。
聚酰胺可以通过在分子量调节剂存在下进行聚酰胺形成组分的开环聚合或缩聚而获得。作为分子量调节剂,通常使用具有4-20个碳原子的二羧酸,更具体地说,使用脂族二羧酸,如琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一烷二羧酸和十四烷双酸;芳香二羧酸,如对苯二甲酸、间苯二甲酸、邻苯二甲酸、萘二甲酸、和3-磺基间苯二甲酸碱金属盐;和脂环族二羧酸,如1,4-环己烷二羧酸、二环己基-4,4′-二羧酸。也可以使用这些羧酸的卤代或磺基衍生物。这样的化合物的例子是脂族二羧酸和芳香二羧酸,更优选己二酸、癸二酸、对苯二甲酸、间苯二甲酸和3-磺基间苯二甲酸碱金属盐。
所述共聚酰胺由以上聚酰胺的缩聚产物组成。
共聚酰胺组分通过缩聚适合单体混合物而获得,优选包含相当太部分,例如超过约10重量%、优选约20-40重量%具有线型脂族链的单元的单体混合物,所述脂族链具有8-12个碳原子、优选12个碳原子,并且其不包含大量的任何离子基团。这些共聚酰胺是市售的。适用作本发明组合物的组分的典型共聚酰胺是例如尼龙型的聚酰胺(PA),其是重量组成为40∶20∶40或40∶40∶20的PA6/PA6,6/PA12单体混合物的缩聚产物。
例如,所述共聚酰胺包含选自6-12个碳原子的内酰胺和6-12个碳原子的氨基碳酸的至少两种化合物与等摩尔量4-12个碳原子的二胺和6-36个碳原子的二伯碳酸的缩聚产物。
例如,所述共聚酰胺包含基于该共聚酰胺为约20-90重量%的6-12个碳原子的至少一种内酰胺或氨基碳酸(例如线型的和脂族的)与基于该共聚酰胺为约80-10重量%的等摩尔量4-12个碳原子的二胺和6-36个碳原子的二伯碳酸的缩聚产物。
例如,共聚酰胺中的内酰胺或氨基碳酸的量为约20-60重量%,基于该共聚酰胺计算。
例如,所述共聚酰胺包括基于该共聚酰胺的重量为约20-90重量%的至少两种环内酰胺或至少两种氨基碳酸与约80-10重量%的等摩尔量的二胺和二碳酸的缩聚产物。
例如,所述共聚酰胺包括约20-90重量%的至少一种内酰胺或氨基碳酸与约80-10重量%的等摩尔量的哌嗪和6-36个碳原子的二碳酸的缩聚产物。
共聚酰胺组分中的二胺可以是二伯胺或二仲胺,例如哌嗪。
共聚酰胺组分例如由共聚酰胺组成,在所述共聚酰胺中,所述内酰胺或碳酸组分的量基于所述共聚物为约20-60重量%,所述内酰胺或碳酸组分包括至少两种环内酰胺或线型脂族氨基碳酸的混合物。
例如,在所述共聚酰胺中,内酰胺或碳酸组分包含基于所述共聚酰胺为约15-60%的11-氨基十一酸和/或12-氨基十二烷酸。
例如,本发明的共聚酰胺组分包含哌嗪基团。
所述共聚酰胺组分优选的相对粘度ηrel是1.4-1.9,按照DIN53727测量(间甲酚;c=0.25g/50mL,Ubbelohde粘度计;毛细管II;25℃)。
其中各个聚酰胺区段以有序还是无规形式存在的共聚酰胺的分子量分布对可染性没有重要影响,其仅对制剂的加工性能有相对小的影响。
适合的共聚酰胺是市售的。
本发明的共聚酰胺可以如美国专利5,130,069中的描述。
本发明的聚醚聚酰胺是聚醚二胺、二羧酸、二聚酸与内酰胺例如己内酰胺的缩聚产物。所述聚醚聚酰胺例如是嵌段共聚物。例如,本发明的聚醚聚酰胺由己内酰胺、二聚酸和聚醚二胺如Jeffamine D-2000的缩聚形成。
本发明的聚醚聚酰胺公开在例如美国专利5,140,065和4,356,300中。
例如,本发明的乙烯-乙酸乙烯酯共聚物在190℃和21.2N(2.16kg)压力下的MFR(熔体流动速率)为约3-8g/10min,按照ISO 1133测量;密度为约0.93-0.96g/cm3,按照DIN 53455测量;VICAT点为约35-65℃,按照DIN 53460测量。
适合的乙烯-乙酸乙烯酯共聚物(EVA)包含基于该EVA的重量为约18-33%的乙酸乙烯酯或约27-29%的乙酸乙烯酯,和/或其如上所述的MFR值为约5-8g/10min。
本发明组合物中的可染性添加剂与聚烯烃组分的重量比为约0.1∶99.9-40∶60.对于许多用途,基于聚烯烃组分的重量,存在的可染性添加剂为约0.1-15重量%,例如基于聚烯烃组分的重量为约0.5-10重量%。例如,基于聚烯烃的重量,存在的可染性添加剂为约7-9重量%或约8重量%。
选自聚酰胺、共聚酰胺和聚醚聚酰胺的添加剂与乙烯-乙酸乙烯酯共聚物的重量比为约1∶9-9∶1,例如约1∶7-7∶1,约1∶5-5∶1或约1∶3-3∶1。
本发明的紫外线吸收剂(UVA)选自羟苯基苯并***、二苯甲酮、α-氰基丙烯酸酯、N,N′-草酰二苯胺、三芳基-s-三嗪、肉桂酸酯、丙二酸酯、苯甲酸酯和水杨酸酯。
例如,本发明的UVA选自羟苯基苯并***、二苯甲酮和三芳基-s-三嗪。
例如,本发明的UVA选自羟苯基苯并***和三芳基-s-三嗪。
本发明的羟苯基苯并***紫外线吸收剂公开在例如以下美国专利中:3,004,896、3,055,896、3,072,585、3,074,910、3,189,615、3,218,332、3,230,194、4,127,586、4,226,763、4,275,004、4,278,589、4,315,848。4,347,180、4,383,863、4,675,352、4,681,905,4,853,471、5,268,450、5,278,314、5,280,124、5,319,091、5,410,071、5,436,349、5,516,914、5,554,760、5,563,242、5,574,166、5,607,987和5,977,219。
本发明的三芳基-s-三嗪紫外线吸收剂公开在例如以下美国专利中:3,843,371、4,619,956、4,740,542、5,096,489、5,106,891、5,298,067、5,300,414、5,354,794、5,461,151、5,476,937、5,489,503、5,543,518、5,556,973、5,597,854、5,681,955、5,726,309、5,736,597、5,942,626、5,959,008、5,998,116、6,013,704、6,060,543、6,242,598和6,255,483。
在本发明中有用的紫外线吸收剂的例子是:
4-辛氧基-2-羟基二苯甲酮,
4-甲氧基-2-羟基二苯甲酮,
2-(2-羟基-5-甲基苯基)-2H-苯并***,
2-(2-羟基-5-叔辛基苯基)-2H-苯并***,
2-(2-羟基-3,5-二叔戊基苯基)-2H-苯并***,
3-(苯并***-2-基)-5-叔丁基-4-羟基氢肉桂酸辛酯,
2-(2-羟基-3,5-二叔丁基苯基)-2H-苯并***,
2-(2-羟基-5-叔丁基苯基)-2H-苯并***,
5-氯-2-(2-羟基-3,5-二叔丁基苯基)-2H-苯并***,
5-氯-2-(2-羟基-3-叔丁基-5-甲基苯基)-2H-苯并***,
2-(2-羟基-3-仲丁基-5-叔丁基苯基)-2H-苯并***,
2-(2-羟基-4-辛氧基苯基)-2H-苯并***,
2-(2-羟基-3-十二烷基-5-甲基苯基)-2H-苯并***,
2-[2-羟基-3,5-二(α,α-二甲基苄基)苯基]-2H-苯并***,
2-[2-羟基-3-(α,α-二甲基苄基)-5-叔辛基苯基]-2H-苯并***,
2-(2-羟基-3-叔丁基-5-[2-(ω-羟基-八(乙烯氧基)羰基)乙基]苯基]-2H-苯并***,
2-{2-羟基-3-叔丁基-5-[2-(辛氧基)羰基)乙基]苯基}-2H-苯并***,
对甲氧基肉桂酸2-乙基己基酯,
4-甲氧基-2,2′-二羟基二苯甲酮,
4,4′-二甲氧基-2,2′-二羟基二苯甲酮,
2,4-二(2,4-二甲基苯基)-6-(2-羟基-4-辛氧基苯基)-s-三嗪,
2,4-二苯基-6-(2-羟基-4-己氧基苯基)-s-三嗪,
2,4-二(2,4-二甲基苯基)-6-[2-羟基-4-(3-二-/三-癸氧基-2-羟基丙氧基)苯基]-s-三嗪,
2,4-二(2,4-二甲基苯基)-6-[2-羟基-4-(3-二-/三-癸氧基-2-羟基丙氧基)-5-α-异丙苯基-苯基]-s-三嗪,和
2,4,6-三(2,4-二羟苯基)-s-三嗪与α-卤代乙酸辛酯的反应产物。
例如,在本发明中有用的紫外线吸收剂的例子是:
4-辛氧基-2-羟基二苯甲酮,
4-甲氧基-2-羟基二苯甲酮,
2-(2-羟基-5-叔辛基苯基)-2H-苯并***,
2-[2-羟基-3-(α,α-二甲基苄基)-5-叔辛基苯基]-2H-苯并***,
5-氯-2-(2-羟基-3,5-二叔丁基苯基)-2H-苯并***,
2-{2-羟基-3-叔丁基-5-[2-(ω-羟基-八(乙烯氧基)羰基)乙基]苯基}-2H-苯并***,
2-{2-羟基-3-叔丁基-5-[2-(辛氧基)羰基)乙基]苯基}-2H-苯并***,
2,4-二(2,4-二甲基苯基)-6-[2-羟基-4-(3-二-/三-癸氧基-2-羟丙氧基)苯基]-s-三嗪,
2,4-二苯基-6-(2-羟基-4-己氧基苯基)-s-三嗪,或
2,4,6-三(2,4-二羟苯基)-s-三嗪与α-卤代乙酸辛酯的反应产物。
例如,本发明的UVA是5-氯-2-(2-羟基-3,5-二叔丁基苯基)-2H-苯并***或2,4-二苯基-6-(2-羟基-4-己氧基苯基)-s-三嗪。
位阻胺光稳定剂(HALS)选自在N-原子上被烷氧基或环烷氧基部分取代的位阻胺、在N-原子上进一步被羟基取代的烷氧基取代的位阻胺和N-原子被氢、烷基、酰基等取代的常规位阻胺。
本发明的共聚酰胺公开在例如美国专利5,204,473、5,980,783、6,046,304、6,297,299、5,844,026和6,271,377中。
烷氧基是具有高达25个碳原子的支链或直链基团,例如甲氧基、乙氧基、丙氧基、异丙氧基、正丁氧基、异丁氧基、戊氧基、异戊氧基、己氧基、庚氧基、辛氧基、癸氧基、十四烷氧基、十六烷氧基或十八烷氧基。本发明的烷氧基可以具有1-12个、例如1-8个、例如1-6个碳原子。
环烷氧基例如是C5-C12环烷氧基,例如环戊氧基或环己氧基。
烷基是具有高达25个碳原子的支链或直链基团,例如甲基、乙基、丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、2-乙基丁基、正戊基、异戊基、1-甲基戊基、1,3-二甲基丁基、正己基、1-甲基己基、正庚基、异庚基、1,1,3,3-四甲基丁基、1-甲基庚基、3-甲基庚基、正辛基、2-乙基己基、1,1,3-三甲基己基、1,1,3,3-四甲基戊基、壬基、癸基、十一烷基、1-甲基十一烷基、十二烷基、1,1,3,3,5,5-六甲基己基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、二十烷基或二十二烷基。
在N-原子上被烷氧基或环烷氧基部分取代的位阻胺是本领域众所周知的。它们详细描述在美国专利5,204,473中,其相关部分在此引入作为参考。
在本发明中有用的在N-原子上被烷氧基、环烷氧基或苄氧基部分取代的位阻胺包括下列:
二(1-辛氧基-2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
二(1-环己氧基-2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
1-环己氧基-2,2,6,6-四甲基-4-十八烷基氨基哌啶;
2,4-二[(1-环己氧基-2,2,6,6-四甲基哌啶-4-基)丁基氨基]-6-(2-羟乙基-氨基)-s-三嗪;
二(1-环己氧基-2,2,6,6-四甲基哌啶-4-基)己二酸酯;
低聚化合物,其是4,4′-六甲撑二(氨基(1-辛氧基-2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(1-辛氧基-2,2,6,6-四甲基哌啶-4-基)丁基氨基]-s-三嗪的缩合产物;
低聚化合物,其是4,4′-六甲撑二(氨基(1-环己氧基-2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(1-环己氧基-2,2,6,6-四甲基哌啶-4-基)丁基氨基]-s-三嗪的缩合产物;
低聚化合物,其是4,4′-六甲撑二(氨基(1-丙氧基-2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(1-丙氧基-2,2,6,6-四甲基哌啶-4-基)丁基氨基]-s-三嗪的缩合产物(其为以下的相应N-H位阻胺的正丙氧基衍生物);
低聚化合物,其是4,4′-六甲撑二(氨基(1-乙酰氧基-2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(1-乙酰氧基-2,2,6,6-四甲基哌啶-4-基)丁基氨基]-s-三嗪的缩合产物;
1-甲氧基-4-羟基-2,2,6,6-四甲基哌啶;
1-辛氧基-4-羟基-2,2,6,6-四甲基哌啶;
1-环己氧基-4-羟基-2,2,6,6-四甲基哌啶;
1-甲氧基-4-氧-2,2,6,6-四甲基哌啶;
1-辛氧基-4-氧-2,2,6,6-四甲基哌啶;
1-环己氧基-4-氧-2,2,6,6-四甲基哌啶;
二(1-庚氧基-2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
二(1-壬氧基2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
二(1-十二烷氧基2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
N,N′,N″,N-四[(4,6-二(丁基-1-辛氧基-2,2,6,6-五甲基哌啶-4-基)氨基-s-三嗪-2-基]-1,10-二氨基-4,7-二氮杂癸烷;和
其中R′是
具体的烃氧基位阻胺稳定剂(CAS#191680-81-6)描述在美国专利5,844,026中。
在N-原子上被羟基-取代的烷氧基取代的位阻胺公开在美国专利6,271,377中。
在本发明中有用的在N-原子上被羟基取代的烷氧基部分取代的位阻胺包括下列:
1-(2-羟基-2-甲基丙氧基)-4-十八酰氧基-2,2,6,6-四甲基哌啶;
1-(2-羟基-2-甲基丙氧基)-4-羟基-2,2,6,6-四甲基哌啶;
1-(2-羟基-2-甲基丙氧基)-4-氧-2,2,6,6-四甲基哌啶;
二(1-(2-羟基-2-甲基丙氧基)-2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
二(1-(2-羟基-2-甲基丙氧基)-2,2,6,6-四甲基哌啶-4-基)己二酸酯;
二(1-(2-羟基-2-甲基丙氧基)-2,2,6,6-四甲基哌啶-4-基)琥珀酸酯;
二(1-(2-羟基-2-甲基丙氧基)-2,2,6,6-四甲基哌啶-4-基)戊二酸;和
2,4-二{N-[1-(2-羟基-2-甲基丙氧基)-2,2,6,6-四甲基哌啶-4-基]-N-丁基氨基]-6-(2-羟乙基氨基)-s-三嗪。
在本发明中有用的常规位阻胺包括下列:
低聚化合物,其是4,4′-六甲撑二(氨基(2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(2,2,6,6-四甲基哌啶4-基)丁基氨基]-s-三嗪的缩合产物;
二(2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
2,4-二氯-6-叔辛基氨基-s-三嗪和4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物;
1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶和琥珀酸的缩聚产物;
4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)和1,2-二溴乙烷的缩聚产物;
二(2,2,6,6-四甲基哌啶-4-基)癸二酸酯和2,4-二氯-6-叔辛基氨基-s-三嗪与4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物的混合物;
1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶与琥珀酸的缩聚产物和2,4-二氯-6-叔辛基氨基-s-三嗪与4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物的混合物;
二(1,2,2,6,6-五甲基哌啶-4-基)癸二酸酯;
二(1,2,2,6,6-五甲基哌啶-4-基)(3,5-二叔丁基-4-羟基苄基)丁基丙二酸酯;
4-苯甲酰基-2,2,6,6-四甲基哌啶;
4-硬脂酰氧基-2,2,6,6-四甲基哌啶;
三(2,2,6,6-四甲基哌啶-4-基)次氮基三醋酸酯;
四(2,2,6,6-四甲基哌啶-4-基)1,2,3,4-丁烷四羧酸酯;
四(1,2,2,6,6-五甲基哌啶-4-基)1,2,3,4-丁烷四羧酸酯;
2,4-二氯-6-吗啉代-s-三嗪和4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物;
2,4-二氯-6-吗啉代-s-三嗪和4,4′-六甲撑二(氨基-(1-甲基-2,2,6,6-四甲基哌啶)的缩聚产物;
N,N′,N″,N-四[(4,6-二(丁基-1,2,2,6,6-五甲基哌啶-4-基)氨基-s-三嗪-2-基]-1,10-二氨基-4,7-二氮杂癸烷;
八亚甲基二(2,2,6,6-四甲基哌啶-4-羧酸酯);
N-2,2,6,6-四甲基哌啶-4-基-n-十二烷基琥珀酰亚胺;
N-1,2,2,6,6-五甲基哌啶-4-基-n-十二烷基琥珀酰亚胺;
N-1-乙酰基-2,2,6,6-四甲基哌啶-4-基-n-十二烷基琥珀酰亚胺;
4-C15-C17烷酰氧基-2,2,6,6-四甲基哌啶;
2,4-二氯-6-环己基氨基-s-三嗪和4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物;
1,5-二(2,2,6,6-四甲基哌啶-4-基)-1,5-二氮杂-氧丙烷;
甲基丙烯酸甲酯、丙烯酸乙酯和丙烯酸2,2,6,6-四甲基哌啶-4-基酯的共聚物;
N-十八烷基马来酰亚胺、苯乙烯和N-(2,2,6,6-四甲基哌啶-4-基)马来酰亚胺的共聚物;
1,3,5-三[3-(2,2,6,6-四甲基哌啶-4-基氨基)-2-羟基丙基]异氰脲酸酯;
含有衍生自N-[2-(2,2,6,6-四甲基哌啶-4-基)草酰胺-1-基]马来酰亚胺的单元的烯烃聚合物;
2,2,4,4-四甲基-7-氧杂-3,20-二氮杂-21-氧二螺[5,1,11,2]二十一烷;
C12-C14烷基3-(2,2,4,4-四甲基-7-氧杂-3,20-二氮杂-21-氧二螺[5,1,11,2]二十一烷-20-基)丙酸酯;
表氯醇与2,2,4,4-四甲基-7-氧杂-3,20-二氮杂-21-氧二螺[5,1,11,2]二十一烷的反应产物;
1,3-二(2,2,6,6-四甲基哌啶-4-基)2,4-双十三烷基丁烷四羧酸酯;
1,3-二(1,2,2,6,6-五甲基哌啶-4-基)2,4-双十三烷基丁烷四羧酸酯;
3,9-二(1,1-二甲基-2-羟乙基)-2,4,8,10-四氧杂螺[5.5]十一烷、1,2,3,4-丁烷四羧酸四甲酯和2,2,6,6-四甲基-4-羟基哌啶的缩聚产物
3,9-二(1,1-二甲基-2-羟乙基)-2,4,8,10-四氧杂螺[5.5]十一烷、1,2,3,4-丁烷四羧酸四甲酯和1,2,2,6,6-五甲基-4-羟基哌啶的缩聚产物;
1,4-二(2,2,6,6-四甲基哌啶-4-基)-2,2-二甲基-1,4-二氮杂-4-氧丙烷;
4-氨基-2,2,6,6-四甲基哌啶和四羟甲基乙炔二脲的反应产物;
1,6-六甲撑二[N-甲酰基-(2,2,6,6-四甲基哌啶-4-基)胺];
N-(2,2,6,6-四甲基哌啶-4-基)马来酰亚胺和C20-C24α-烯烃的共聚物;
聚[3-(2,2,6,6-四甲基哌啶-4-基氧基)丙基甲基硅氧烷];
2,4-二氯-6-[N-丁基-N-(2,2,6,6-四甲基哌啶-4-基)氨基]-s-三嗪和1,10-二氨基-4,7-二氮杂癸烷的缩聚产物;
3-(2,2,4,4-四甲基-7-氧杂-3,20-二氮杂-21-氧-二螺[5,1,11,2]二十一烷-20-基)丙酸十二烷基酯;
其中R′=R″或H
例如,在本发明中有用的位阻胺包括下列:
低聚化合物,其是4,4′-六甲撑二(氨基(1-丙氧基-2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(1-丙氧基-2,2,6,6-四甲基哌啶-4-基)丁基氨基]-s-三嗪的缩合产物(CAS#247243-62-5);
其中R′是
低聚化合物,其是4,4′-六甲撑二(氨基(2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(2,2,6,6-四甲基哌啶-4-基)丁基氨基]-s-三嗪的缩合产物;
二(2,2,6,6-四甲基哌啶-4-基)癸二酸酯;
2,4-二氯-6-叔辛基氨基-s-三嗪和4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物;
1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶和琥珀酸的缩聚产物;
二(2,2,6,6-四甲基哌啶-4-基)癸二酸酯和2,4-二氯-6-叔辛基氨基-s-三嗪与4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物的混合物;
1-(2-羟乙基)-2,2,6,6-四甲基-4-羟基哌啶与琥珀酸的缩聚产物和2,4-二氯-6-叔辛基氨基-s-三嗪与4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物的混合物;
二(1,2,2,6,6-五甲基哌啶-4-基)癸二酸酯;
二(1,2,2,6,6-五甲基哌啶-4-基)(3,5-二叔丁基-4-羟基苄基)丁基丙二酸酯;
2,4-二氯-6-吗啉代-s-三嗪和4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物;
2,4-二氯-6-吗啉代-s-三嗪和4,4′-六甲撑二(氨基-(1-甲基-2,2,6,6-四甲基哌啶)的缩聚产物;
N,N′,N″,N-四[(4,6-二(丁基-1,2,2,6,6-五甲基哌啶-4-基)氨基-s-三嗪-2-基]-1,10-二氨基-4,7-二氮杂癸烷;
其中R′=R″或H
本发明的低聚位阻胺和“缩聚”产物位阻胺的分子量大于约1000g/mol。某些非低聚位阻胺也具有大于约1000g/mol的分子量。这些高分子量位阻胺特别有利。
例如,本发明的位阻胺选自:
其中R′=R″或H
和其中
其中n是使得低聚空间位阻胺的总分子量超过约1000g/mol的整数。
特别值得注意的是选自以下的位阻光稳定剂:
N,N′,N″,N-四[(4,6-二(丁基-1,2,2,6,6-五甲基哌啶-4-基)氨基-s-三嗪-2-基]-1,10-二氨基-4,7-二氮杂癸烷;和
其中n是使得低聚空间位阻胺的总分子量超过约1000g/mol的整数。
这些化合物中的许多相应于以上的说明书,其中位阻胺被称作低聚或缩聚产物。
本发明的UVA和位阻胺稳定剂总计的存在量基于聚烯烃的重量为例如约0.05-5重量%,例如约0.1-1重量%,特别是约0.2-0.5重量%。
UVA与位阻胺的重量比为约1∶9-9∶1,例如约1∶7-7∶1,约1∶5-5∶1或约1∶3-3∶1。
在提及可染性添加剂或提及稳定添加剂时用的术语“有效量”是指分别导致预期的染色和光稳定性效果的量。
本文所用的术语“纤维”或“丝”是指具有高长宽比和小横截面的柔韧的、合成的、宏观上均匀的物体。这些纤维可以通过任何本领域已知的工艺制备,包括但不限于直接轮廓挤出(direct profileextrusion)和切割或纤化条带。因此,可以预见本发明的组合物可用于制备可染色的纤维,包括可染色的织造和非织造聚烯烃纤维。
本发明组合物通过熔体挤出工艺制备,以形成纤维或丝。根据已知的技术,如用于纱线或人造短纤维的连续丝纺丝工艺和非织造工艺如纺粘生产工艺和熔喷生产工艺,通过将熔融聚合物挤出通过小孔口而形成纤维或丝。通常,然后将由此形成的纤维或丝拉伸或拉长,引起分子取向并影响结晶度,导致直径减少和物理性能改善。在非织造工艺如纺粘和熔喷中,纤维或丝直接置于多孔表面如运动着的平传送带上,并通过各种方法的任何一种来至少部分固化,所述方法包括但不限于热粘合、机械粘合或化学粘合方法。本领域技术人员公知的是可以结合各种工艺或结合不同工艺获得的织物,以制备具有某些希望特性的复合材料织物。其例子是结合纺粘和熔喷来制备层压织物,其称为SMS,意思是有两个纺粘织物外层和一个熔喷织物内层。另外,这两种工艺中的一种或两者可以以任何配置与人造短纤维梳理工艺或由非织造人造短纤维梳理工艺产生的粘合织物相结合。在这种层压织物中,通常通过以上所列举的方法之一将各层至少部分固化。
本发明也适用于熔体挤出双组分纤维,其中组分之一是本发明的聚烯烃。
聚烯烃的非织造织物可以具有梳理的纤维结构或包含纤维或丝无规排列的垫。织物可以由众多已知工艺中的任何一个形成,包括水力缠结(hydroentanglement)或射流喷网技术,或通过气流成网或熔喷成丝、绵胎拉伸、缝编等,这取决于由该织物制成的制品的最终用途。
纺粘丝的尺寸为约1.0-3.2旦尼尔。熔喷的纤维一般具有小于15微米的纤维直径,一般小于5微米,范围可以低至亚微米水平。复合材料结构的网可以加工成多种基重。该纤维的尺寸取决于最终用途。例如,更沉重的纤维常常用于毛毯背衬,与之相反的纤维常用于制备服装面料等。本发明的纤维例如可以为约1-1500旦尼尔。
热塑性聚丙烯纤维一般在约210-240℃的温度下挤出,其固有地是疏水性的,因为它们是基本上无孔的,并由不能吸引或结合染色的连续分子链组成。结果,未经处理的聚丙烯织物即使具有开孔结构,也往往阻碍染色的施用。
按照本发明,可染性添加剂和光稳定剂添加剂被结合进热塑性聚烯烃如聚丙烯的熔体中,并且与该聚烯烃一起挤出成为纤维和丝的形式,然后在随后的工艺步骤或伴随的工艺步骤中被骤冷、减薄并形成织物。
可染性添加剂和光稳定剂添加剂可以与将要被熔体挤出的聚合物小丸复合。为改善加工,添加剂可以预配制或复合到低MFR聚丙烯中,该低MFR聚丙烯也包含少量无机物粉末如滑石、及其它传统的稳定剂。
将添加剂混合到聚烯烃中是通过通常使用的技术如辊碾磨、在班伯里型混合机中混合、或在挤出机料筒中混合等将其混合到熔融聚合物而进行的。通过将添加剂与未加热的聚合物颗粒混合以便使添加剂基本上均匀分布在聚合物主体中,可以缩短加热过程(即其处于高温下的时间),由此降低在熔融温度充分混合所需的时间。
便利地是,添加剂还可以与在某些情况中可能希望加入的任何其它添加剂基本上同时或顺序地加入。添加剂也可以与其它添加剂预混合,然后将共混物加入聚合物中。可以预见,在有些情况下该添加剂可能具有有助于其它添加剂更容易或更均匀地分散或溶于聚烯烃中的额外好处。为了更容易地进行逐批次质量控制,优选使用聚合物/添加剂共混物的浓缩母炼胶,其随后逐份被共混到额外量的聚合物中,完成最终希望的制剂。母炼胶或纯添加剂可在聚合物仍然是熔体并离开聚合容器或设备组(train)之后注入到新制备的聚合物中,并在该熔融聚合物冷却成固体或被用于进一步加工以前与其共混。
将可染性添加剂结合到本发明的聚烯烃纤维或丝中使得这些天然疏水性材料的可染性发生可察觉的改善。这种改变是持久的,使得纤维或丝和由其制备的织物不会因老化或处理而丧失它们的可染性。改善的可染性对于反复洗涤是稳定的,不会丧失性能,甚至长时间洗涤也是如此。
本发明的目的在于非织造织物,例如聚丙烯织物。目的还在于在常规纺织品工艺中用于织造或编织的线或纱。
本发明的组合物开用于人造短纤维、长丝纱、质地化的长丝纱、条带状材料、纤化的条带、膜、非织造织物、织造织物和针织织物、针刺植绒毛毯、织造和立毛毛毯、织造衣物、家具和汽车蒙皮材料、织造工业织物、用于一次性尿布的非织造吸附剂、包括一次性医疗衣物的非织造衣物、过滤介质、合成纸张等等。
不考虑影响非织造织物性能的其它因素,例如基重、纤维直径、粘合纤维的程度和种类,以及复合结构如以上已经描述的SMS结构的协同效应和影响,本发明的添加剂都有效。
本发明不限于单组分纤维。预计可以证明聚烯烃双组分纤维,特别是聚丙烯和聚乙烯的并排型或包-芯型纤维具有与聚丙烯或聚乙烯的单组分纤维相同的实际好处。
由本发明的纤维和丝制备的可染色织物包括织造衣物(外衣和内衣);毛毯;家具和汽车蒙皮材料、织造工业织物;非织造吸附剂,用于尿布、卫生垫、失禁垫、干湿揩布、绷带、减少溢出物的装置和医疗用的吸收垫;非织造衣物,包括一次性的医疗衣物;毡;压制的板材;土工布;过滤器(双极的);包装材料,包括信封和合成纸张。
本发明的织物可通过暴露于约0.5-10兆拉德的γ辐照而灭菌。利用γ辐照灭菌被用于医院衣物等。
本发明的聚烯烃纤维、丝和织物也可以结合或施加合适的其它添加剂,如抗氧化剂、加工助剂及其它添加剂。
例如,本发明的组合物也可任选包含约0.01-10重量%,优选约0.025-5重量%,特别是约0.1-3重量%的其它添加剂,例如各种常规稳定剂辅助添加剂,如下列的材料或其混合物。
抗氧化剂
1.烷基化的一元酚,例如2,6-二叔丁基-4-甲基苯酚,2-叔丁基-4,6-二甲基苯酚,2,6-二叔丁基-4-乙基苯酚,2,6-二叔丁基-4-正丁基苯酚,2,6-二叔丁基-4-异丁基苯酚,2,6-二环戊基-4-甲基苯酚,2-(α-甲基环己基)-4,6-二甲基苯酚,2,6-二-十八烷基-4-甲基苯酚,2,4,6-三-环己基苯酚,2,6-二叔丁基-4-甲氧基甲基苯酚,侧链为直链或带支链的壬基酚诸如2,6-二-壬基-4-甲基苯酚,2,4-二甲基-6-(1-甲基十一烷-1-基)苯酚,2,4-二甲基-6-(1-甲基十七烷-1-基)苯酚,2,4-二甲基-6-(1-甲基十三烷-1-基)苯酚以及它们的混合物。
2.烷硫基甲基酚,例如2,4-二辛硫基甲基-6-叔丁基苯酚,2,4-二辛硫基甲基-6-甲基苯酚,2,4-二辛硫基甲基-6-乙基苯酚,2,6-二-十二烷硫基甲基-4-壬基苯酚。
3.氢醌和烷基化的氢醌,例如2,6-二-叔丁基-4-甲氧基苯酚,2,5-二-叔丁基氢醌,2,5-二-叔戊基氢醌,2,6-二苯基-4-十八烷氧基苯酚,2,6-二叔丁基氢醌,2,5-二叔丁基-4-羟基苯甲醚,3,5-二叔丁基-4-羟基苯甲醚,硬脂酸3,5-二叔丁基-4-羟基苯基酯,己二酸双(3,5-二叔丁基-4-羟基苯基)酯。
4.生育酚,例如α-生育酚,β-生育酚,γ-生育酚,δ-生育酚和它们的混合物(维生素E)。
5.羟基化的硫代二苯醚,例如2,2′-硫代双(6-叔丁基-4-甲基苯酚),2,2′-硫代双(4-辛基苯酚),4,4′-硫代双(6-叔丁基-3-甲基苯酚),4,4′-硫代双(6-叔丁基-2-甲基苯酚),4,4′-硫代双(3,6-二-仲戊基苯酚),4,4′-双(2,6-二甲基-4-羟基苯基)-二硫化物。
6.亚烷基双酚,例如2,2′亚甲基双(6-叔丁基-4-甲基苯酚),2,2′-亚甲基双(6-叔丁基-4-乙基苯酚),2,2′-亚甲基双[4-甲基-6-(α-甲基环己基)苯酚],2,2′-亚甲基双(4-甲基-6-环己基苯酚),2,2′-亚甲基双(6-壬基-4-甲基苯酚),2,2′-亚甲基双(4,6-二叔丁基苯酚),2,2′-亚乙基双(4,6-二叔丁基苯酚),2,2-亚乙基双(6-叔丁基-4-异丁基苯酚),2,2′-亚甲基双[6-(α-甲基苄基)-4-壬基苯酚],2,2′-亚甲基双[6-(α,α-二甲基苄基)-4-壬基苯酚],4,4′-亚甲基双(2,6-二叔丁基苯酚),4,4′-亚甲基双(6-叔丁基-2-甲基苯酚),1,1-双(5-叔丁基-4-羟基-2-甲基苯基)丁烷,2,6-双(3-叔丁基-5-甲基-2-羟基苄基)-4-甲基苯酚,1,1,3-三(5-叔丁基-4-羟基-2-甲基苯基)丁烷,1,1-双(5-叔丁基-4-羟基-2-甲基苯基)-3-正十二烷基巯基丁烷,乙二醇双[3,3-双(3-叔丁基-4-羟基苯基)丁酸酯],双(3-叔丁基-4-羟基-5-甲基-苯基)二环戊二烯,对苯二甲酸双[2-(3′-叔丁基-2-羟基-5-甲基苄基)-6-叔丁基-4-甲基苯基]酯,1,1-双(3,5-二甲基-2-羟基苯基)丁烷,2,2-双-(3,5-二叔丁基-4-羟基苯基)丙烷,2,2-双-(5-叔丁基-4-羟基-2-甲基苯基)-4-正十二烷基巯基丁烷,1,1,5,5-四(5-叔丁基-4-羟基-2-甲基苯基)戊烷。
7.苄基化合物,例如3,5,3′,5′-四叔丁基-4,4′-二羟基二苄基醚,十八烷基-4-羟基-3,5-二甲基苄基巯基乙酸酯,十三烷基-4-羟基-3,5-二-叔丁基苄基巯基乙酸酯,三(3,5-二叔丁基-4-羟基苄基)胺,1,3,5-三(3,5-二叔丁基-4-羟基苄基)-2,4,6-三甲基苯、双(3,5-二叔丁基-4-羟基苄基)硫化物、3,5-二叔丁基-4-羟基苄基-巯基乙酸异辛酯、双(4-叔丁基-3-羟基-2,6-二甲基苄基)二硫代对苯二甲酸酯,1,3,5-三(3,5-二叔丁基-4-羟基苄基)异氰脲酸酯、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)异氰脲酸酯、3,5-二叔丁基-4-羟基苄基-磷酸双十八烷基酯和3,5-二叔丁基-4-羟基苄基-磷酸单乙酯钙盐。
8.羟苄基化的丙二酸酯,例如2,2-双(3,5-二叔丁基-2-羟苄基)丙二酸双十八烷基酯,2-(3-叔丁基-4-羟基-5-甲基苄基)丙二酸双十八烷基酯,2,2-双(3,5-二叔丁基-4-羟基苄基)丙二酸双十二烷基巯基乙基酯,2,2-双(3,5-二叔丁基-4-羟基苄基)丙二酸双[4-(1,1,3,3-四甲基丁基)苯基]酯。
9.芳族羟苄基化合物,例如1,3,5-三(3,5-二叔丁基-4-羟基苄基)-2,4,6-三甲基苯,1,4-双(3,5-二叔丁基-4-羟基苄基)-2,3,5,6-四甲基苯,2,4,6-三(3,5-二叔丁基-4-羟基苄基)苯酚。
10.三嗪化合物,例如2,4-双(辛基巯基)-6-(3,5-二叔丁基-4-羟基苯胺基)-1,3,5-三嗪,2-辛基巯基-4,6-双(3,5-二叔丁基-4-羟基苯胺基)-1,3,5-三嗪,2-辛基巯基-4,6-双(3,5-二叔丁基-4-羟基苯氧基)-1,3,5-三嗪,2,4,6-三-(3,5-二叔丁基-4-羟基苯氧基)-1,2,3-三嗪,1,3,5-三(3,5-二叔丁基-4-羟基苄基)异氰脲酸酯,1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)异氰脲酸酯,2,4,6-三(3,5-二叔丁基-4-羟基苯乙基)-1,3,5-三嗪,1,3,5-三(3,5-二叔丁基-4-羟基苯丙酰基)-六氢-1,3,5-三嗪,1,3,5-三(3,5-二环己基-4-羟基苄基)异氰脲酸酯。
11.苄基膦酸酯,例如2,5-二叔丁基-4-羟基苄基膦酸二甲酯,3,5-二叔丁基-4-羟基苄基膦酸二乙酯,3,5-二叔丁基-4-羟基苄基膦酸双十八烷基酯,5-叔丁基-4-羟基-3-甲基苄基膦酸双十八烷基酯,3,5-二叔丁基-4-羟基苄基膦酸的单乙酯的钙盐。
12.酰基氨基酚,例如,4-羟基月桂酰苯胺,4-羟基硬脂酰苯胺,2,4-二辛基巯基-6-(3,5-叔丁基-4-羟基苯胺基)-s-三嗪和N-(3,5-二叔丁基-4-羟基苯基)氨基甲酸辛酯。
13.β-(3,5-二叔丁基-4-羟基苯基)丙酸与-元或多元醇形成的酯,例如其与甲醇、乙醇、正辛醇、异辛醇、十八碳醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊基二醇、硫代二甘醇、二甘醇、三甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N′-双(羟乙基)草酰胺、3-硫杂十一碳醇、3-硫杂十五碳醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷所形成的酯。
14.β-(5-叔丁基-4-羟基-3-甲基苯基)丙酸与一元或多元醇所形成的酯,例如,其与甲醇、乙醇、正辛醇、异辛醇、十八碳醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊基二醇、硫代二甘醇、二甘醇、三甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N-双(羟乙基)草酰胺、3-硫杂十一碳醇、3-硫杂十五碳醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷所形成的酯。
15.β-(3,5-二环己基-4-羟基苯基)丙酸与一元或多元醇形成的酯,例如,其与甲醇、乙醇、辛醇、十八碳醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊基二醇、硫代二甘醇、二甘醇、三甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N′-双(羟乙基)草酰胺、3-硫杂十一碳醇、3-硫杂十五碳醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷所形成的酯。
16.3,5-二叔丁基-4-羟基苯乙酸与一元或多元醇形成的酯,例如其与甲醇、乙醇、辛醇、十八碳醇、1,6-己二醇、1,9-壬二醇、乙二醇、1,2-丙二醇、新戊基二醇、硫代二甘醇、二甘醇、三甘醇、季戊四醇、三(羟乙基)异氰脲酸酯、N,N′-双(羟乙基)草酰胺、3-硫杂十一碳醇、3-硫杂十五碳醇、三甲基己二醇、三羟甲基丙烷、4-羟甲基-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷所形成的酯。
17.β-(3,5-二叔丁基-4-羟基苯基)丙酸的酰胺,例如,N,N′-双(3,5-二叔丁基-4-羟基苯丙酰基)六亚甲基二酰胺、N,N′-双(3,5-二叔丁基-4-羟基苯丙酰基)三亚甲基二酰胺、N,N′双-(3,5-二叔丁基-4-羟基苯丙酰基)肼、N,N′-双-[2-(3-[3,5-二叔丁基-4-羟基苯基]丙酰氧基)乙基]草酰胺(NaugardXL-1,由Uniroyal公司提供)。
18.抗坏血酸(维生素C)
19.胺抗氧化剂,例如N,N′-二异丙基-对苯二胺、N,N′-二仲丁基-对苯二胺、N,N′-双(1,4-二甲基戊基)-对苯二胺、N,N′-双(1-乙基-3-甲基戊基)对苯二胺、N,N′-双(1-甲基庚基)-对苯二胺、N,N′-二环己基对苯二胺、N,N′-二苯基-对苯二胺、N,N′-双(2-萘基)对苯二胺、N-异丙基-N′-苯基-对苯二胺、N-(1,3-二甲基丁基)-N′-苯基对苯二胺、N-(1-甲基庚基)-N′-苯基-对苯二胺、N-环己基-N′-苯基-对苯二胺、4-(对甲苯氨磺酰基)二苯基胺、N,N′-二甲基-N,N′-二仲丁基-对苯二胺、二苯胺、N-烯丙基二苯基胺、4-异丙氧基二苯基胺、N-苯基-1-萘胺、N-(4-叔辛基苯基)-1-萘胺、N-苯基-2-萘胺、辛基化的二苯基胺,例如p,p′-二叔辛基二苯胺、4-正丁基氨基苯酚、4-丁酰基氨基苯酚、4-壬酰基氨基苯酚、4-十二碳酰基氨基苯酚、4-十八碳酰基-氨基苯酚、双(4-甲氧基苯基)胺、2,6-二叔丁基-4-二甲基氨基甲基苯酚、2,4′-二氨基二苯基甲烷、4,4′-二氨基-二苯基甲烷、N,N,N′,N′-四甲基-4,4′-二氨基二苯基甲烷、1,2-双[(2-甲基苯基)氨基]乙烷、1,2-双(苯基氨基)丙烷、(邻甲苯基)双胍、双[4-(1′,3′-二甲基丁基)苯基]胺、叔辛基化的N-苯基-1-萘胺,一和二烷基化的叔丁基/叔辛基二苯胺的混合物,一和二烷基化的壬基二苯胺的混合物,一和二烷基化的十二烷基二苯胺的混合物,一和二烷基化的异丙基/异己基二苯胺的混合物,一和二烷基化的叔丁基二苯胺的混合物,2,3-二氢-3,3-二甲基-4H-1,4-苯并噻嗪,吩噻嗪,一和二烷基化的叔丁基/叔辛基吩噻嗪的混合物,一和二烷基化的叔辛基吩噻嗪的混合物,N-烯丙基吩噻嗪,N,N,N′,N′-四苯基-1,4-二氨基丁-2-烯。
金属钝化剂,例如N,N′-二苯基草酰胺、N-水杨醛-N′-水杨酰基肼、N,N′-双(水杨酰基)肼、N,N′-双(3,5-二叔丁基-4-羟基苯基丙酰基)肼、3-水杨酰氨基-1,2,4-***、双(亚苄基)草酰基二酰肼、草酰苯胺、间苯二甲酰基二酰肼、癸二酰基双苯基酰肼、N,N′-二乙酰基己二酰基二酰肼、N,N′-双(水杨酰基)草酰基二酰肼、N,N′-双(水杨酰基)硫代丙酰基二酰肼。
亚磷酸酯和亚膦酸酯,例如亚磷酸三苯酯、亚磷酸二苯基烷基酯、亚磷酸苯基二烷基酯、亚磷酸三(壬基苯基)酯、亚磷酸三月桂基酯、亚磷酸三(十八烷基)酯、二亚磷酸二硬脂基季戊四醇酯、亚磷酸三(2,4-二叔丁基苯基)酯、二亚磷酸二异癸基季戊四醇酯、二亚磷酸双(2,4-二叔丁基苯基)季戊四醇酯、二亚磷酸双(2,6-二叔丁基-4-甲基苯基)季戊四醇酯、二亚磷酸二异癸氧基季戊四醇酯、二亚磷酸双(2,4-二叔丁基-6-甲基苯基)季戊四醇酯、二亚磷酸双(2,4,6-三(叔丁基苯基)季戊四醇酯、三亚磷酸三硬脂基山梨糖醇酯、二亚膦酸四(2,4-二叔丁基苯基)4,4′-亚联苯基酯、6-异辛氧基-2,4,8,10-四叔丁基-12H-二苯并[d,f]-[1,3,2]-二氧杂磷杂环庚二烯(dioxaphosphepin)、6-氟-2,4,8,10-四叔丁基-12-甲基-二苯并[d,g]-[1,3,2]-二氧杂磷杂环辛三烯、亚磷酸双(2,4-二叔丁基-6-甲基苯基)甲基酯、亚磷酸双(2,4-二叔丁基-6-甲基苯基)乙基酯、2,2′,2″-次氮[三乙基三(3,3′,5,5′-四叔丁基-1,1′-联苯-2,2′-二基)亚磷酸酯]、亚磷酸2-乙基己基(3,3′,5,5′-四叔丁基-1,1′-联苯-2,2′-二基)酯。
特别优选下列亚磷酸酯:
亚磷酸三(2,4-二叔丁基苯基)酯(Irgafos168,Ciba SpecialtyChemicals Corp.)、亚磷酸三(壬基苯基)酯。
羟胺,例如N,N-二苄基羟胺,N,N-二乙基羟胺,N,N-二辛基羟胺,N,N-二月桂基羟胺,N,N-双(十四烷基)羟胺,N,N-双(十六烷基)羟胺,N,N-双(十八烷基)羟胺,N-十六烷基-N-十八烷基羟胺,N-十七烷基-N-十八烷基羟胺,N-甲基-N-十八烷基羟胺,由氢化牛脂胺衍生得到的N,N-二烷基羟胺。
硝酮,例如N-苄基-α-苯基硝酮,N-乙基-α-甲基硝酮,N-辛基-α-庚基硝酮,N-月桂基-α-十一烷基硝酮,N-十四烷基-α-十三烷基硝酮,N-十六烷基-α-十五烷基硝酮,N-十八烷基-α-十七烷基硝酮,N-十六烷基-α-十七烷基硝酮,N-十八烷基-α-十五烷基硝酮,N-十七烷基-α-十七烷基硝酮,N-十八烷基-α-十六烷基硝酮,N-甲基-α-十七烷基硝酮,由衍生自氢化牛脂胺的N,N-二烷基羟基胺得到的硝酮。
氧化胺,例如美国专利5,844,029和5,880,191中公开的氧化胺衍生物、二癸基甲基氧化胺、三癸基氧化胺、三(十二烷基)氧化胺和三(十六烷基氧化胺)。
苯并呋喃酮和二氢吲哚酮,例如公开在U.S.4,325,863、U.S.4,338,244、U.S.5,175,312、U.S.5,216,052、U.S.5,252,643、DE-A-4316611、DE-A-4316622、DE-A-4316876、EP-A-0589839、EP-A-0591102、EP-A-1291384中的那些或3-[4-(2-乙酰氧基乙氧基)苯基]-5,7-二叔丁基苯并呋喃-2-酮、5,7-二叔丁基-3-[4-(2-硬脂酰氧基乙氧基)苯基]苯并呋喃-2-酮、3,3′二[5,7-二叔丁基-3-(4-[2-羟基乙氧基]苯基)苯并呋喃-2-酮、5,7-二叔丁基-3-(4-乙氧基苯基)苯并呋喃-2-酮、3-(4-乙酰氧基-3,5-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(3,5-二甲基-4-新戊酰氧基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(3,4-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(2,3-二甲基苯基)-5,7-二叔丁基苯并呋喃-2-酮、3-(2-乙酰基-5-异辛基苯基)-5-异辛基苯并呋喃-2-酮。
硫代增效剂,例如硫代二丙酸二月桂基酯或硫代二丙酸二硬脂基酯。
过氧化物清除剂,例如β-硫代二丙酸的酯,例如月桂基、硬脂基、肉豆蔻基或十三烷基酯、巯基苯并咪唑或2-巯基苯并咪唑的锌盐,二丁基二硫代氨基甲酸锌,双(十八烷基)二硫化物,四(β-十二烷基巯基)丙酸季戊四醇酯。
聚酰胺稳定剂,例如与碘化物和/或磷化合物结合的铜盐以及二价锰盐。
碱性辅助稳定剂,例如蜜胺、聚乙烯基吡咯烷酮、二氰二酰胺、氰尿酸三烯丙基酯、脲衍生物、肼衍生物、胺、聚酰胺、聚氨酯、高级脂肪酸的碱金属盐和碱土金属盐,例如硬脂酸钙、硬脂酸锌、山萮酸镁、硬脂酸镁、蓖麻醇酸钠、软脂酸钾、邻苯二酚锑或邻苯二酚锌。
成核剂,例如一些无机物质,诸如滑石,金属氧化物,诸如二氧化钛或氧化镁、优选碱土金属的磷酸盐、碳酸盐或硫酸盐;有机化合物,诸如单或多羧酸及其盐,例如4-叔丁基苯甲酸、己二酸、二苯基乙酸、丁二酸钠或苯甲酸钠;聚合物诸如离子共聚物(离聚物)。
填充剂和增强剂,例如碳酸钙、硅酸盐、玻璃纤维、玻璃球、石棉、滑石、高岭土、云母、硫酸钡、金属氧化物和氢氧化物、碳黑、石墨、木粉、面粉或其它天然产物的纤维、合成纤维。
分散剂,如聚环氧乙烷蜡或矿物油。
其它添加剂,例如增塑剂、润滑剂、乳化剂、颜料、染料、荧光增白剂、流变添加剂、催化剂、流动控制剂、滑爽剂、交联剂、交联促进剂、卤素清除剂、烟雾抑制剂、防火试剂、抗静电剂、澄清剂如取代和未取代的二亚苄基山梨糖醇、苯并嗪酮紫外线吸收剂如2,2′-对亚苯基-二(3,1-苯并嗪-4-酮)、Cyasorb3638(CAS#18600-59-4)和起泡剂。
特别值得注意的其它添加剂是酚类抗氧剂(以上列表第1-17项)和/或加工稳定剂例如亚磷酸酯、亚膦酸酯和/或苯并呋喃酮。
例如,常用于本领域中的添加剂可任选结合进本发明的可染色纤维中。这种材料的典型例子包括亲水性改性剂如单酸甘油酯如单硬脂酸甘油酯,带有亲水性侧链基团的长链烃,如线型磷酸烷基酯的钾或钠盐,或其组合。亲水性基团可以是羧酸酯、硫酸酯、磺酸酯、磷酸酯、膦酸酯、以及季铵盐和聚醚基团。另外,在染色期间可以使用膨胀剂、润湿剂、染料相容剂和增稠剂如各种树胶。因为聚烯烃纤维常常用于户外应用如户外毛毯,所以加入紫外稳定剂是有利的。还可以向组合物中加入抗氧化剂。
另外可以预见,本发明的组合物会显示出改善了聚烯烃基织物或非织造垫的可洗性。非极性聚烯烃倾向于束缚住污垢,因为它们都是疏水性的。可以预料本发明的可染性添加剂有助于洗涤剂穿透织物或基质,从而洗涤剂可以使污垢和油疏松并将其冲走。
还可以预见,将本发明可染性添加剂结合到聚烯烃中会增大聚烯烃纺织物和非织造织物的吸收性和芯吸性。一个例子是婴儿尿布中的熔喷非织造吸收体。可以预料,通过将极性可染性添加剂结合到聚烯烃中来使得非织造丝的表面更亲水会大大地提高尿布的吸湿特性。
还可以预见,结合可染性添加剂会提高纤维、织物及其它制品的耐磨性。耐磨性在形成的纤维的拉伸中是很重要的。一般,通过施胶来降低纤维和拉伸***金属表面之间的摩擦。
按照本发明制备的聚烯烃织造和非织造纤维还显示出优越可印刷性。作为其固有疏水性的结果,聚烯烃纤维和织物可能在可印刷性(即标准印刷技术)方面存在问题。本发明的组合物克服了这些问题。
常规方法可用于染色本发明的纤维。例如,纤维可以使用常规染料和分散染料技术在染色浴中染色。通常,染料以染料溶液的形式施加,使得其可以通过将纤维通过槽(例如包含染料溶液的槽)浸渍,或通过将染料溶液喷在纤维上,或通过使用级联辊技术而容易地施加。通常染料溶液可以是印刷膏剂的形式,一般用其通过辊筒印刷或丝网印刷来进行染色。纤维可以使用一种或多种染色技术多次染色。
对于酸性染料,含水染色浴的pH值一般为约2-11,通常为约2-6。可以使用各种化合物而根据需要调节pH值,如使用甲酸、乙酸、氨基磺酸、柠檬酸、磷酸、硝酸、硫酸、磷酸单钠、磷酸四钠、磷酸三钠、氢氧化铵、氢氧化钠及其组合。可使用表面活性剂来帮助节约地将水溶性分散染料分散在染色浴中。一般,将非离子表面活性剂用于该目的。在染色步骤期间,可以搅拌染色浴以提高上色率。染色步骤可以在各种温度进行,而较高温度通常会促进上色率。
本领域已知的另一技术是喷射染色,其通过使用文丘里型喷射***使染料高温染色和冲击在运动着的织物上。载体容许在大气压和低于100℃的条件下更快的染色。载体一般是可以在水中乳化并且对纤维具有亲合力的有机化合物。这种载体的代表性例子包括芳族烃如联苯和甲基萘、酚如苯基苯酚、氯代烃如二氯和三氯苯、芳香酯如水杨酸甲酯、苯甲酸丁酯、邻苯二甲酸二乙酯和苯甲醛。通常在染色后除去载体。
在使用与上述添加剂的染料混合物染色之后,可以在宽范围的高温下把干热施加到纤维上,使染料穿透纤维,并固定在纤维中。染料固定步骤包括将纤维暴露于干热,例如在烘箱中。温度可以高述复合纤维的熔化温度或玻璃化温度。通常,越高的干燥温度使干燥时间越短。一般,加热时间为约1-10分钟。然后可将残留的染料从纤维中除去。
分散染料混合物因此可以以多种方式施用于聚丙烯纤维。染料混合物可以使用各种众所周知的技术,沿着由纤维形成的纱的长度周期性地施加,以产生预期效果。一种染色纤维的适合方法称为“编织拆散”染色技术。依据这种方法,使纤维形成纱,一般又将纱编织成管状构造。然后将染料混合物周期性地施加到编织的管状物上。染色之后,将管状物拆散,纱因此具有周期性的图案。根据备选的印刷方法纤维首先形成纱,然后将纱织造或编织成织物,是簇绒成毛毯。常规平板筛网印花机可用来将染料混合物施加到织物或毛毯上。
在染色范围进行连续染色,其中织物或毛毯连续通过染料溶液,其时间足够长以完成最初的染料渗透。通过本领域已知的方法,一些分散染料可以在加热和部分真空下升华到聚合物纤维中。对根据本发明制备的聚烯烃组合物的印刷可以如下实现:用分散染料通过在压力下用足够的热量进行热转移印刷,以使染料扩散或分散到聚烯烃中。可以使用块料切片、平板筛网和热转移间歇法、压花辊子和旋转筛网印刷连续法。不同染料溶液可以在由本发明组合物制成的织物或毛毯通过射流之下时以预编程序列喷射织物或毛毯上形成图案。可以计量染料溶液并将其断开或切断成点滴图案,其滴落在从其下通过的染色毛毯上,在毛毯上形成扩散的过染色图案。当染色由若干不同纤维例如尼龙、聚酯等和聚烯烃组成的风格毛毯时,聚烯烃的竞争性染色是有用的。不同的风格化效果可以通过控制所存在的每种纤维上的色调深度而制成。取决于所存在的纤维,可以使用酸染料、分散染料和金属络合染料及其组合来获得风格化效果。通过控制可染色的组合物中的反应产物和/或可染性添加剂的量可能制出粗花呢效应。可以对由这种纱制成的织物进行印刷染色、间隔染色和连续染色。
有许多市售的分散染料。染料基于使用方法分类,在更小尺度上基于化学组成由Society of Dyers and Colorists分类。各种分散染料列在Textile Chemist and Colorist的“Dyes and Pigments by Color Indexand Generic Names”,1992年7月,卷24,No.7,这是the AmericanAssociation of Textile Chemists and Colorists的出版物。
染料是用来着色各种基材如纸张、塑料或纺织材料的有浓烈颜色的物质。据信染料通过物理吸收,通过形成盐或金属络合物或通过形成共价化学键而被保留在这些基材中。用来将染料施用于基材的方法大不一样,取决于基材和染料的类别。通过施用方法而不是通过化学组成使染料与颜料区别开。在施用期间,染料通过溶解或汽化而失去其晶体结构。有时晶体结构在染色工艺的较后阶段期间恢复。相反,颜料在整个施用步骤中保留其晶体或颗粒形式。
因此,必需有性能大不相同的大量染料,因为待染色的材料数量很大。在全世界范围内,人们相信数万种不同染料都实现了工业重要性。通常,染料以2种方式分类。一种分类方法是通过化学组成分类其中染料根据生色团或分子的发色单元分类。第二种分类方法基于染料的最终用途的类别。国际上在整个染料制造和染料应用行业都接受用于颜色索引(CI)的这种双重分类***。在这些***中,染料进行分类,根据化学类别给每种化合物一个CI数,并且根据用法或施用类别给每种染料一个CI名称。分散染料通常是水不溶性的非离子染料,一般被用来从含水分散体染色亲水性纤维。分散染料已被用于聚酯、尼龙和乙酸酯纤维。
优选本发明的染料是蒽醌蓝色染料、蒽醌红色染料、重氮红色染料或硝基黄色染料。例如本发明的染料是蒽醌蓝色染料、蒽醌红色染料、重氮红色染料或硝基黄色染料。
例如,本发明的染料是蒽醌染料。
例如,本发明的染料是蓝BLF(CI 60766,CI分散蓝120、CI分散蓝77)、蓝GLF(CI 60767、CI分散蓝27)、蓝BGE-01-200(CI 61104、CI 668210、CI分散蓝60、CI分散蓝99)、蓝R200(CI 63265)、蓝3RL-02(CI 63285)、红FBN(CI分散红60)、红CB(CI 26765)、黄GWL(CI10338、CI分散黄37、CI分散黄42)、黄CR(CI 40001、CI直接黄6)或黄HLG(CI 58840)。
在拉伸前可将许多纺丝油剂用于纤维。这种油剂可以是水基的。纺丝油剂可以是阴离子的或非离子的,如本领域众所周知的。而且,如本领域众所周知的,在染色前可将纤维整理(finish),通过机械卷曲或成形进行质地化(texturizing)。
可以预见,本发明的稳定剂体系对于其它的已知聚烯烃可染性添加剂也是有效的。例如,本发明的可染性添加剂混合物可以用以下物质来代替:美国专利6,679,754的聚醚酯酰胺、聚酯、聚醚胺、马来酸酐接枝的聚丙烯、这些聚合物的高度支化或枝状物、和具有极性侧链的聚丙烯。
下列实施例更详细地举例说明本发明。它们不应被认为是以任何方式限定本发明。所有份和百分数按重量计算,除非另有说明。
本发明实施例中使用的添加剂是:
UVAs:
HPT:2,4-二苯基-6-(2-羟基-4-己氧基苯基)-s-三嗪
BZT:5-氯-2-(2-羟基-3,5-二叔丁基苯基)-2H-苯并***
HALS:
NH:低聚化合物,其是2,4-二氯-6-叔辛基氨基-s-三嗪和4,4′-六甲撑二(氨基-2,2,6,6-四甲基哌啶)的缩聚产物
NMe:N,N′,N″,N-四[(4,6-二(丁基-1,2,2,6,6-五甲基哌啶-4-基)氨基-s-三嗪-2-基]-1,10-二氨基-4,7-二氮杂癸烷
NORP:低聚化合物,其是4,4′-六甲撑二(氨基(1-丙氧基-2,2,6,6-四甲基哌啶))与2-氯-4,6-二(二丁基氨基)-s-三嗪封端的2,4-二氯-6-[(1-丙氧基-2,2,6,6-四甲基哌啶-4-基)丁基氨基]-s-三嗪的缩合产物
可染性添加剂:
共聚酰胺和乙烯-乙酸乙烯酯共聚物的混合物
实施例1:聚丙烯纤维可染性和光稳定性
聚丙烯纤维的制备:基于一个批次总计为1,000克来称重纤维级聚丙烯、Montell PROFAX 6301(RTM)、稳定剂添加剂和可染性添加剂。将各成分置于塑料袋中,并进行转筒混合。混合物装进带有41孔圆形喷丝头的HILLS LAB FIBER EXTRUDER中。挤出机的温度分布为190、204、218、232和232℃。750psi的恒压经由一个反馈回路控制着螺杆速率。进料、拉伸和松驰辊处于65、86和86℃,并以120、600和575米/分旋转。拉伸比是5∶1(600米/分钟/120米/分钟)。在紧临进料辊之处纤维接触6%的含水纤维整理油剂溶液。该纤维整理油剂溶液是来自Goulston Industries的LUROL PP-4521。在线路末端的LEESONA绕线器将纤维收集在线轴上。最终的单丝纤度为10。纱的总纤度为410(41根丝×10旦尼尔)。收集的纤维从线轴处移走,并用LAWSON HEMPHILL FAK样品编织机编织成短袜。从短袜剪下十克样品。
染色工艺:
a)染料溶液的制备:通过将1.000g染料溶于1,000g蒸馏水中,制备分散染料的溶液。这些溶液用作染料母液。对于分散染料,将水加热到49-71℃,然后向水中加入染料。
b)染料助剂溶液的制备:制成的染料助剂溶液包含:缓冲剂(硫酸铵,1.25g/L)、匀染剂(Ciba TinegalALS,0.625g/L)、润滑剂(CibafluidLA,1.875g/L)和消泡剂(CibaflowSF,0.125g/L)。用浓度为10%(w/w)的乙酸调节pH值为4.5-5.5。这些是染料助剂母液。
c)聚丙烯纤维的染色:将ROACHES可编程染色浴设置成下列条件:以2℃/分钟从30℃升温到125℃,在125℃下保持60分钟,然后以5.5℃/分钟的最大冷却速率冷却。为获得0.4%的基于纤维重量(OWF)的染料,将40克染料母液、160g助剂母液、10g如前述制备的聚丙烯短袜全部加到ROACHES的钢制250cc圆筒中。因此浴比是20-1。密封圆筒、将其放入染色浴中,启动循环并使圆筒旋转。在染色循环完成之后,从圆筒中取出短袜。然后用自来水漂洗短袜。借助于离心分离抽提器从短袜中除去过量水,并在强制通风烘箱中在100℃干燥15分钟。
d)还原清除:然后短袜进行还原清除,以除去没有固定到纤维上的疏松染料。这通过在30℃下用200cc下列溶液处理10g染色的聚丙烯短袜10分钟来进行:3cc/L 40%NaOH w/v,1g/L亚硫酸氢钠。还原清除后,如上所述地漂洗和干燥短袜。
e)用来评价耐光牢度的设备和步骤;测量颜色变化、K/S、耐摩擦掉色牢度和耐洗牢度的细节
完成染色的短袜折叠两次,并在Datacolor分光光度计SF600上以最小反射率的波长测量K/S值。仪器条件是:CIE lab,D65光源,10度观测角,包括的光谱分量(SCI),小区域视图(SAV),扫描波长=400-700纳米。K/S值越高表明色调深度越大。K/S值通过仪器计算,其中K=吸收,S=散射,R=在最小反射率下的反射率值:
K/S=(1-R)2/2R
样品根据ASTM G26在Atlas Ci65A氙弧人工老化试验仪中进行人工老化试验。人工老化试验仪(干燥的)条件是:黑色板温度=63℃,照度=0.35W/m2,湿球温度差=14℃,调节水=38℃,循环=连续光照,过滤器=硼硅酸盐。
颜色变化(人工老化前后对比)是ΔE(DE)值。DE通过仪器由L、a和b值,使用如下公式计算,其中L、a和b值来自CIE体系,来自反射率值:
[(ΔL)2+(Δa)2+(Δb)2]1/2=ΔE (DE)
制备下列样品。所有样品包含8重量%的可染性添加剂混合物。对照蓝色A:
染料:0.4OWF蓝R200
没有稳定剂
对照红色A:
染料:0.4OWF红FBN
没有稳定剂
对照黄色A:
染料:0.4WOF黄CR
没有稳定剂
对照蓝色B:
染料:1.0OWF蓝R200
没有稳定剂
对照红色B:
染料:1.0OWF红FBN
没有稳定剂
对照黄色B:
染料:1.0OWF黄CR
没有稳定剂
A)染料:0.4OWF蓝R200
稳定剂添加剂:0.12%HPT、0.17%NORP
B)染料:0.4OWF蓝R200
稳定剂添加剂:0.12%HPT、0.18%NH、0.12%BZT
C)染料:0.4OWF红FBN
稳定剂添加剂:0.12%HPT、0.17%NORP
D)染料:0.4OWF红FBN
稳定剂添加剂:0.12%HPT、0.18%NH、0.12%BZT
E)染料:0.4OWF黄CR
稳定剂添加剂:0.12%HPT、0.17%NORP
F)染料:0.4OWF黄CR
稳定剂添加剂:0.12%HPT、0.17%NMe
G)染料:1.0OWF蓝R200
稳定剂添加剂:0.12%HPT、0.17%NORP
H)染料:1.0OWF蓝R200
稳定剂添加剂:0.12%HPT、0.17%NMe
J)染料:1.0OWF红FBN
稳定剂添加剂:0.12%HPT、0.17%NORP
K)染料:1.0OWF红FBN
稳定剂添加剂:0.12%HPT、0.12%BZT
L)染料:1.0OWF黄CR
稳定剂添加剂:0.12%HPT、0.17%NORP
M)染料:1.0OWF黄CR
稳定剂添加剂:0.12%HPT、0.17%NMe
结果列在下表中。蓝色染料样品的K/S在630纳米测量,红色染料样品在520纳米测量,黄色染料样品在450纳米测量。
样品 | K/S | 240小时时的DE |
对照蓝色AAB对照红色ACD对照黄色AEF对照蓝色BGH对照红色BJK对照黄色BLM | 10.110.911.610.810.110.714.715.014.515.415.517.517.819.219.515.518.416.5 | 35.011.513.238.68.77.424.615.117.025.59.99.121.913.115.031.117.816.9 |
本发明的制剂显示出优良的可染性和耐光牢度。
耐光牢度例如测量为具有小于约20的240小时时的DE,根据ASTM G26测量,例如本发明的DE为在240小时时小于约15,根据ASTM G26测量。
Claims (12)
1.一种包含熔体共混物的可染色、光稳定的聚烯烃纤维或丝,该共混物包含
i)聚烯烃基材,
ii)有效量的选自聚酰胺、共聚酰胺和聚醚聚酰胺的至少一种可染性添加剂和选自乙烯-乙酸乙烯酯共聚物的至少一种可染性添加剂的组合,
iii)有效量的选自紫外线吸收剂的至少一种添加剂和选自位阻胺光稳定剂的至少一种添加剂的组合,和
该纤维或丝进一步包含至少一种分散染料。
2.包含权利要求1的聚烯烃纤维或丝的织造或非织造织物。
3.权利要求1的纤维或丝,其包含至少一种选自共聚酰胺的可染性添加剂。
4.权利要求1的纤维或丝,其中基于聚烯烃的重量,存在的可染性添加剂为约0.1-15重量%。
5.权利要求1的纤维或丝,其中选自聚酰胺、共聚酰胺和聚醚聚酰胺的添加剂与乙烯-乙酸乙烯酯共聚物的重量比为约1∶9-9∶1。
6.权利要求1的纤维或丝,其中紫外线吸收剂选自羟基苯基苯并***和三芳基s-三嗪。
7.权利要求1的纤维或丝,其中基于聚烯烃的重量,存在的紫外线吸收剂和位阻胺光稳定剂总计为约0.05-5重量%。
8.权利要求1的纤维或丝,其中紫外线吸收剂与位阻胺光稳定剂的重量比为约1∶9-9∶1。
9.权利要求1的纤维或丝,其中所述染料选自蒽醌蓝染料、蒽醌红染料、重氮红染料和硝基黄染料。
10.权利要求1的纤维或丝,其包含进一步的添加剂。
11.权利要求10的纤维或丝,其含有酚类抗氧剂和/或加工稳定剂作为所述进一步的添加剂。
12.一种制备可染色、光稳定的聚烯烃纤维或丝的方法,该方法包括熔体共混一种组合物,该组合物包含
i)聚烯烃基材,
ii)有效量的选自聚酰胺、共聚酰胺和聚醚聚酰胺的至少一种可染性添加剂和选自乙烯-乙酸乙烯酯共聚物的至少一种可染性添加剂的组合,
iii)有效量的选自紫外线吸收剂的至少一种添加剂和选自位阻胺光稳定剂的至少一种添加剂的组合,
该方法进一步包括用至少一种分散染料处理所述熔体共混物。
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- 2005-04-13 KR KR1020067022050A patent/KR20070004054A/ko not_active Application Discontinuation
- 2005-04-13 CA CA002561275A patent/CA2561275A1/en not_active Abandoned
- 2005-04-13 EP EP05738020A patent/EP1738002A1/en not_active Withdrawn
- 2005-04-13 CN CNA200580011757XA patent/CN1942613A/zh active Pending
- 2005-04-13 WO PCT/EP2005/051612 patent/WO2005103345A1/en not_active Application Discontinuation
- 2005-04-13 JP JP2007508898A patent/JP2007533867A/ja not_active Withdrawn
- 2005-04-15 US US11/107,613 patent/US20050239927A1/en not_active Abandoned
- 2005-04-21 TW TW094112697A patent/TW200602523A/zh unknown
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