CN1177661A - 光化学稳定的聚酰胺合成物 - Google Patents
光化学稳定的聚酰胺合成物 Download PDFInfo
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- CN1177661A CN1177661A CN97114768A CN97114768A CN1177661A CN 1177661 A CN1177661 A CN 1177661A CN 97114768 A CN97114768 A CN 97114768A CN 97114768 A CN97114768 A CN 97114768A CN 1177661 A CN1177661 A CN 1177661A
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Abstract
一种制备光化学稳定的染色尼龙合成物的工艺,包括提供一种聚(ε－己内酰胺)的成型制品至染浴中,聚合(ε－己内酰胺)是在水、一种羧酸链调节剂和一种受阻哌啶衍生物存在下通过水解聚合制备;并在染浴中用一种或多种金属化或非金属化酸性染料染色成型制品。
Description
本发明涉及具有优良光化学稳定性的染色聚酰胺合成物，特别涉及尼龙6纤维这样一些聚酰胺合成物。
众所周知，某些聚酰胺(尼龙)合成物易于受光热作用而降解。对抗这种降解的尼龙聚合物的稳定化已成为重点开发的主题。尼龙聚合物的改进的光热稳定性来自于在主体聚合物成型前于其中加入添加剂。一种这样的添加的稳定剂是受阻胺光稳定剂类，包括多烷基哌啶衍生的化合物。典型的多烷基哌啶衍生的添加剂对于被稳定的聚合物可为惰性的或为活性的，对此进行描述的文献有：苏联专利申请S.U.670588，1979年6月30日公开；德国专利号DE 3823112A1，1990年1月11日公开；PCT专利申请WO90/09408，1990年8月23日公开；法国专利号2,642,764，1990年8月10日公开；及欧洲专利公开号0516 192 A2，1992年12月2日公开。在德国专利号3,901,717A1中描述了这样的受阻胺添加剂以增强聚酰胺的染色性，此专利于1990年7月26日公开。
与己内酰胺聚合的2，2，6，6-四烷基哌啶〔CAS 768-66-1〕衍生物已用作其它聚合物的热和光的稳定剂。德国专利号2,642,461于1978年3月30日公开，描述了这样的一种稳定剂，优选用于聚氨酯。
尼龙聚合物亦已通过直接将稳定材料结合至聚合物链中而稳定化。例如，ε-己内酰胺可在水、羧酸和受阻哌啶衍生物(多烷基哌啶)存在下聚合，生成改性的抗光热降解的稳定的尼龙6聚合物。这样一种稳定的聚合物在PCT申请WO 95/28443中有描述，该专利于1995年10月26日公开。
多烷基派啶衍生物已用于为各种目的染浴中。英国专利号GB 2 220418A于1990年1月1日公开，描述了受阻胺基的染料盐(包括某些2，2，6，6-四甲基哌啶基)，以及提供聚酰胺染色的阴离子染料基，染色是坚牢的且表现出良好的湿坚牢度(特别是洗涤坚牢度)。公开于1993年6月16日的欧洲专利申请054 699 3A1号描述了用于聚酰胺纤维的受阻胺热和光的稳定剂，这些稳定剂被应用于水浴中，例如染浴。公开于1992年1月15日的欧洲专利申请046 664 7A1描述了用于染色和不染色的聚酰胺纤维材料的受阻胺热和光的稳定剂。这些稳定剂在染色前、染色中或染色后从一水浴中被使用，以提高纤维和染料包括金属化酸性染料的热和光的稳定性。
虽然稳定剂，或作为添加剂或作为聚合物链的组分，对聚合物本身抗热和光的稳定化起了很大作用，但这样的添加剂对通常用以处理这些聚合物的材料的稳定化却不起什么作用。例如，成型的尼龙聚合物通常用染料染色。这些染料在光和热下具有退色或改变颜色的趋势。当染色制品暴露于强光、热和潮湿下，退色特别明显。用于汽车的车顶衬里和地毯的染色纤维在暴露于太阳、热和潮湿中时非常易于退色。
现在人们出乎意料地发现：当由ε-己内酰胺用水作引发剂、在羧酸链调节剂和受阻哌啶衍生物的存在下聚合而制备的尼龙6，用金属化或非金属化的酸性染料将其染色时，这种染色的尼龙6制品对染料和聚合物的耐光化学降解能力大大加强了。
本发明的一个主题是提供光化学稳定的染色尼龙6制品。
在阅读以下详细说明后，有关主题和优点对于本领域普通技术人员是显而易见的。
图1的柱状图表明按照本发明用金属化酸性染料染色的纤维与常规纤维的对比光稳定性。
图2的柱状图表明在染浴中用紫外光稳定剂稳定的金属化酸性染料染色的纤维的光稳定性。
图3的柱状图表明按照本发明，用非金属化酸性染料染色的纤维与常规纤维的对比光稳定性。
图4的柱状图表明在染浴中用含有紫外光稳定剂的非金属化酸性染料染色的纤维的光稳定性。
图5的图描述用按本发明制造的金属化酸性染料染色的纤维与常规纤维暴露于氙光后的对比保留强度。
图6的图描绘在染浴中用含有紫外光稳定剂的金属化酸性染料染色的纤维暴露于氙光后的保留强度。
图7的图描绘用按本发明制造的非金属化酸性染料染色的纤维与常规纤维暴露地氙光后的对比保留强度。
图8的图描绘在染浴中用含有紫外光稳定剂的非金属化酸性染料染色的纤维暴露于氙光后的保留强度。
为了提高对本发明原理的理解，下面给出本发明具体实施方案的说明，并使用了具体的语言进行描述。然而应当理解，使用具体语言并不限制本发明的范围。所讨论的本发明原理的变动、进一步的改进、和进一步应用对于本发明所属领域的技术人员都应被认为是正常的。
本发明是制备光化学稳定的染色尼龙合成物的一种工艺。此工艺包括提供一种成型尼龙制品到一染浴中，并用金属化酸性染料、非金属化酸性染料或其组合使成型制品染色。
用于制造制品的尼龙在水、一种羧酸链调节剂和一种受阻哌啶衍生物存在下通过水解聚合ε-己内酰胺制备。具体说，尼龙可通过在至少有一种受阻胺(哌啶)化合物存在下聚合ε-己内酰胺制备。受阻胺哌啶化合物的化学式为：
式中R表示氢、具有1到20个碳原子的烃基、且优选为具有1到18个碳原子的烷基；或苯。受阻哌啶衍生物优选为一种氨基多烷基哌啶。受阻哌啶衍生物优选为2，2，6，6-四烷基哌啶。示范的受阻哌啶化合物包括：
4-氨基-2，2′，6，6′-四甲基哌啶；
4-(氨烷基)-2，2′，6，6′-四甲基哌啶；
4-(氨芳基)-2，2′，6，6′-四甲基哌啶；
4-(氨芳基/烷基)-2，2′，6，6′-四甲基哌啶；
3-氨基-2，2′，6，6′-四甲基哌啶；
3-(氨烷基)-2，2′，6，6′-四甲基哌啶；
3-(氨芳基/烷基)-2，2′，6，6′-四甲基哌啶；
3-(氨芳基/烷基)-2，2′，6，6′-四甲基哌啶；
2，2′，6，6′-四甲基-4-哌啶羧酸；
2，2′，6，6′-四甲基-4-哌啶烷基羧酸；
2，2′，6，6′-四甲基-4-哌啶芳基羧酸；
2，2′，6，6′-四甲基-4-哌啶烷基/芳基羧酸；
2，2′，6，6′-四甲基-3-哌啶羧酸；
2，2′，6，6′-四甲基-3-哌啶烷基羧酸；
2，2′，6，6′-四甲基-3-哌啶芳基羧酸；和
2，2′，6，6′-四甲基-34-哌啶烷基/芳基羧酸；
受阻胺化合物加至起始单体或聚合反应混合物中。聚合优选按聚合己内酰胺制造尼龙的常规条件进行。受阻胺化合物加至起始单体中的量为0.03至0.8mol％，优选为0.06-0.4mol％，各相对于聚酰胺的1mol胺基。受阻胺化合物可与至少一种常规的链调节剂相结合。适用的链调节剂有，例如，单羧酸如乙酸、丙酸和苯甲酸。二羧酸链调节剂可选择C4-C10烷的二羧酸(例如环己烷-1，4二羧酸)；苯和萘的二羧酸(例如间苯二酸、对苯二酸和萘2，6-二羧酸)；及其组合。二羧酸链调节剂优选为对苯二甲酸。使用的二羧酸的优选用量相对于1mol的酰胺基为0.06-0.6mol％。
按照最终产品所要求的目标端胺基含量和所要求的目标熔融稳定性选择链调节剂的用量。目标端胺基的含量通常基于所希望的纤维对染料的亲合力。目标熔融稳定性基于产品加工的实际需要，例如，熔融纺丝。
水优选用作为聚合引发剂。用作引发剂的水的用量可以变化，但以ε-己内酰胺单体的重量为基础计，典型地约为0.4重量％。
改性的稳定化的尼龙聚合物可按任何常规成型方法成型，例如模压、纤维纺丝等。优选为将尼龙聚合物纺为织物或地毯纤维。本发明的此详细说明的其余部分使用尼龙聚合物的优选的纤维形式，以便有助于向普通技术人员提供具体的实施案例。普通技术人员会理解此讨论所涉及的原理也适用于聚合物的其它成型形式。
成型制品用金属化或非金属化的酸性染料染色。可以纤维形式进行染色，如对长丝、短纤维、纤维束、纤维条、丝条的散纤维染色；或以织物形式染色，如编织无纺或针织制品；或以成衣形式染色。染料优选为非络合酸性染料或1∶2金属络合酸性染料，金属为铬、铁、钴、铜、铝或任何过渡金属。其它类别的染料也可以使用，例如分散、直接或活性染料。可以使用通常的用于尼龙染色的染浴条件。
下列一般条件是典型的而非旨在限制。染浴的容量约相当于所染物品重量的20倍。加入的加工化学品包括一种螯合剂以阻止硬水中金属离子的沉淀或络合、一种均染剂和在金属化酸性染料的情况下的缓慢降低染浴PH的酸供体。加入染料并调节染浴的PH，PH对于酸性染料约为5-7而对于金属化酸性染料约为8-10。将溶液加热至所要求的温度，典型的温度约为95℃至110℃，升温速率为每分钟约0.5至3.0℃并在此温度下保温约30到60分钟。染浴被冷却或排空，而物品用新鲜水彻底清洗。染色的物品在一立式炉中干燥，例如，干毡机、转鼓干燥器，或通过加热罐。染色的物品然后可任意地被热定形，以改进尺寸稳定性。
用于本发明实践的示范性染料包括非金属化染料，例如C.I.酸性黄246；C.I.酸性橙156；C.I.酸性红361；C.I.酸性蓝277；和C.I.酸性蓝324；以及金属化染料，例如C.I.酸性黄59；C.I.酸性橙162；C.I.酸性红51；C.I.酸性蓝171；C.I.酸性棕298；C.I.酸性黑131∶1；和C.I.酸性黑132。
本发明的另一方面是用与己内酰胺共聚的受阻哌啶衍生物所稳定的尼龙制造并用金属化或非金属化的酸性染料染色的尼龙制品。此制品优选为呈纤维形式。制备这种制品的方法和使用优选的组分、染料等已如上述。
本发明将参考下列实施例加以说明。实施例通过图示说明，但并非旨在限制本发明的范围。所有的百分数都是重量百分数，除非另外指出。在下列实施例中，将按照本发明所制造的染色纱与染色的常规纱的光化学稳定性相比较。
在以下的实施例中，除非另外指出，使用下列方法测定所述的性质。
氙光坚牢度
112.8、188.0、225.6和300.8KJ.(SAE方法J1885)加速暴露，水冷却氙弧耐气候仪。
对于氙光的强度稳定性
ASTM方法D2256，夹持长度为5.0英寸，十字头速度10.0英寸/分钟。
臭氧
用AATCC试验方法129-1990测定在高湿度下对大气中臭氧的颜色坚牢度，进行三个循环。
氮的氧化物
用AATCC试验方法164-1992测定在高湿度下对大气中氮的氧化物的颜色坚牢度，进行三个循环。
颜色测量
用应用颜色系统(ACS)的分光光度计产生1976 CIE LAB(D6500发光体，10度观察器)值进行颜色测量。对照未曝光的对照物进行Delta E(AE，总色差)的计算。总色差(Delta E)的CIE LAB测量和计算的细节可在颜色科学文献查到，例如Billmeyer和M.Saltzman，颜色工艺原理，第2版。
实施例1
A.纱的生产
两种不同类型的40/12圆纤维载面半消光纱按照常规的尼龙熔融纺丝技术生产，采用含有0.5％对苯二甲酸(“TPA”)和0.25％三丙酮二胺(“TAD”)的热稳定尼龙6切片(称为“BV403N”)(相对粘度(RV)2.4∶0.3％TiO2)和常规的尼龙6切片(“BS403F”)(相对粘度2.4∶0.3％TiO2)；两者都来自新泽西州奥利夫山BASF公司。纱线在不同速度下生产，且未经强制牵伸。通过调节卷绕速度，使卷绕张力保持在6g。所有样品都针织成管状并染色。表1示出尼龙的性质。表2示出不同工艺速度下的纱的性质。
将纱线针织为管状，按以下所述用金属化酸性染料染成三个色调并用非金属化酸性染料染成三个色调，两者都具有和不具有Cibafast N-2(紫外线稳定剂，商业上来自北卡罗来那州格林斯伯勒Ciba公司)。这些纱在染色后在374°F(190℃)下热定形20秒。
B.用金属化酸性染料染色
20∶1浴比，软化水
0.25g/lVersene(乙二胺四乙酸螯合剂)
按织物重的2.0％UniperolNB-SE
按织物重的2.0％EulysinWP
色调1-云杉绿
0.075％Intralan枣红RLB200 (C.I.号未知)
0.092％Intralan黄2BRL-SM250％ (C.I.号未知)
0.057％Irgalan黄2GL250％ (C.I.酸性黄59)
0.342％Irgalan蓝3GL200 (C.I.酸性蓝171)
1.010％Irgalan灰GL (C.I.酸性黑131∶1)
色调2-浅灰
0.059％Irgalan黄3RL (C.I.酸性橙162)
0.123％Irgalan蓝3GL200
0.062％Intralan枣红RLB200 (C.I.号未知)
0.034％Irgalan灰GL200
0.030％Lanasyn黄LNW (C.I.号未知)
色调3-深酒红
0.520％Irgalan枣红EL200 (C.I.酸性红51)
0.020％Irgalan蓝3GL200
0.200％Irgalan黑RBL200 (C.I.酸性黑132)
0.660％Lanacron棕S-GL (C.I.酸性棕298)
(Intralan和Irgalan染料商业上可由北卡罗来那州夏洛特市Crompton & Knowles Corporation公司获得；Ianacron由北卡罗来那州格林斯伯勒Ciba公司获得；而Lanasyn由北卡罗来那州夏洛特市Sandoz化学品公司获得)。
用苏打灰将浴的PH调节至10.0。样品加热至95℃历时30分钟，并在95℃下保温30分钟。EulysinWP在染色期间使PH值下降至6到7。样品在温水和冷水中漂洗并干燥。其后，管状物在190℃下进行后热定形20秒。
C.用非金属酸性染料染色
20∶1浴比，软化水
1.0％Chemcogen AC(阴离子均染剂，在商业上可由乔治亚州劳伦斯维尔的Phone-Poulenc Inc.以商业名称SupralevTMAC获得)
0.5g/L磷酸三钠
0.25g/L Versene
色调1-灰
0.079％TectilonTM橙3G100％ (C.I.酸性橙156)
0.124％TectilonTM红2B100％ (C.I.酸性红361)
0.114％TelonTM蓝BRL200％ (C.I.酸性蓝324)
色调2-蓝
0.402％TectilonTM黄3GR250％ (C.I.酸性黄246)
0.390％TectilonTM红2B100％
0.1972％TectilonTM蓝4R100％ (C.I.酸性蓝277)
色调3-深酒红
0.829％TectilonTM黄3R250％
2.064％TectilonTM红2B100％
1.025％TectilonTM蓝4R100％
(TectilonTM染料在商业上可由北卡罗来那州格林斯伯勒Ciba公司获得，而TelonTM染料可由宾州匹兹堡Miles Inc.获得)
浴PH用醋酸调节到5.8。样品加热至95℃历时30分钟，并在95℃下保温30分钟。样品在温水和冷水中漂洗并干燥。其后，管状物在190℃下进行后定形20秒。
表I
| 尼龙6 | BS403F(对比的) | BV403N(稳定的) |
| 切片性质：端胺基(meq/kg)相对粘度粉尘(ppm)提取物％H2O，％ | 28.82421900.510.04 | 39.42.452000.300.04 |
表II
纱性质
| 实施例A | 聚合物类型BS403F | 工艺速度(mm)4180 | 旦40 | 延伸率56 | 强度(gpd)4.31 | In.Mod(gpd)16.5 | B.W.S.％8.0 | 乌斯特％CV0.5 |
| B | BS403F | 4980 | 40 | 54 | 4.60 | 16.5 | 7.5 | 0.5 |
| C | BS403F | 5880 | 40 | 51 | 4.73 | 18.0 | 7.4 | 0.5 |
| D | BV403N | 4180 | 40 | 60 | 4.53 | 16.5 | 8.6 | 0.6 |
| E | BV403N | 4980 | 41 | 56 | 4.88 | 16.8 | 8.1 | 0.5 |
| F | BV403N | 5880 | 41 | 51 | 5.18 | 17.7 | 7.4 | 0.5 |
染色并编织过的纱然后以未暴露的相应纱为对照物进行氙光坚牢度、臭氧坚牢度、氮的氧化物坚牢度的试验和总色差(ΔE)的测量。对氮的氧化物、臭氧和光的坚牢度的试验结果示于表III及表IV，并图示于图1至4。
表III
紧牢度性质
金属化酸性染料-无UV稳定剂
CIE LAB，Delta E值
| 1 | 2 | 3 | 1 | 2 | 3 | |||||||||
| 样品云杉绿 | 卷绕速度 | 循环臭氧 | 循环臭氧 | 循环臭氧 | 平均臭氧 | 循环NOx | 循环NOx | 循环NOx | 平均NOx | 112kJ氙 | 188kJ氙 | 225kJ氙 | 300kJ氙 | 平均氙 |
| BS403F | 4180 | 0.6 | 2.0 | 0.8 | 1.1 | 1.5 | 0.2 | 0.6 | 0.8 | 3.8 | 6.9 | 8.5 | 11.3 | 7.6 |
| BS403N | 4180 | 0.3 | 1.5 | 1.8 | 1.2 | 0.2 | 2.1 | 2.0 | 1.4 | 1.6 | 3.3 | 3.7 | 5.1 | 3.4 |
| BS403F | 4980 | 0.5 | 0.5 | 0.6 | 0.5 | 0.3 | 0.5 | 0.4 | 0.4 | 4.3 | 7.2 | 7.9 | 10.9 | 7.6 |
| BS403N | 4980 | 0.5 | 0.4 | 2.4 | 1.1 | 0.1 | 0.1 | 0.2 | 0.1 | 3.3 | 4.7 | 5.0 | 6.4 | 4.9 |
| BS403F | 5880 | 0.4 | 0.4 | 0.5 | 0.4 | 0.3 | 0.5 | 0.3 | 0.4 | 4.3 | 6.2 | 7.9 | 10.4 | 7.2 |
| BS403N | 5880 | 0.1 | 0.2 | 0.2 | 0.2 | 0.4 | 0.6 | 0.2 | 0.4 | 3.1 | 4.7 | 5.2 | 7.0 | 5.0 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 0.9 | 0.8 | 1.3 | 1.0 | 2.5 | 2.4 | 0.6 | 1.8 | 8.8 | 16.3 | 18.7 | 22.0 | 16.5 |
| BS403N | 4180 | 1.3 | 0.6 | 2.0 | 1.3 | 1.4 | 1.5 | 1.5 | 1.5 | 4.0 | 5.7 | 6.6 | 8.4 | 6.2 |
| BS403F | 4980 | 0.6 | 0.7 | 0.7 | 0.7 | 1.1 | 1.0 | 0.6 | 0.9 | 6.3 | 12.3 | 14.4 | 19.9 | 13.2 |
| BS403N | 4980 | 2.4 | 2.1 | 0.8 | 1.8 | 1.9 | 1.8 | 1.6 | 1.8 | 4.5 | 6.1 | 6.9 | 8.0 | 6.4 |
| BS403F | 5880 | 0.3 | 2.4 | 2.4 | 1.7 | 0.4 | 0.2 | 0.3 | 0.3 | 11.0 | 18.0 | 20.8 | 22.7 | 18.1 |
| BS403N | 5880 | 1.3 | 1.1 | 1.3 | 1.2 | 1.7 | 1.6 | 1.4 | 1.6 | 2.2 | 4.3 | 4.8 | 6.4 | 4.4 |
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 1.6 | 1.5 | 1.9 | 1.7 | 0.1 | 1.1 | 1.7 | 1.0 | 2.3 | 2.5 | 4.4 | 5.0 | 3.6 |
| BS403N | 4180 | 0.4 | 1.9 | 1.8 | 1.4 | 0.1 | 0.1 | 0.3 | 0.2 | 2.1 | 3.2 | 3.0 | 4.2 | 3.1 |
| BS403F | 4980 | 0.3 | 1.5 | 1.4 | 1.1 | 1.3 | 0.2 | 0.2 | 0.6 | 3.1 | 3.6 | 4.1 | 5.5 | 4.1 |
| BS403N | 4980 | 0.1 | 0.4 | 0.3 | 0.3 | 0.4 | 0.3 | 0.3 | 0.3 | 2.5 | 3.0 | 3.4 | 4.2 | 3.3 |
| BS403F | 5880 | 0.1 | 0.2 | 0.2 | 0.2 | 0.3 | 0.2 | 0.2 | 0.2 | 2.4 | 3.8 | 4.3 | 5.5 | 4.0 |
| BS403N | 5880 | 0.2 | 0.2 | 0.2 | 0.2 | 0.1 | 0.0 | 0.2 | 0.1 | 1.8 | 3.1 | 3.4 | 3.5 | 3.0 |
表III(续)
坚牢度性质
非金属化酸性染料-无UV稳定剂
CIE LAB，Delta E值
| 1 | 2 | 3 | 1 | 2 | 3 | |||||||||
| 样品云杉绿 | 卷绕速度 | 循环臭氧 | 循环臭氧 | 循环臭氧 | 平均臭氧 | 循环NOx | 循环NOx | 循环NOx | 平均NOx | 112kJ氙 | 188kJ氙 | 225kJ氙 | 300kJ氙 | 平均氙 |
| BS403F | 4180 | 3.9 | 5.7 | 7.2 | 5.6 | 1.4 | 2.0 | 2.3 | 1.9 | 13.0 | 19.5 | 21.2 | 24.4 | 19.5 |
| BS403N | 4180 | 3.9 | 6.2 | 7.8 | 6.0 | 1.5 | 1.9 | 2.2 | 1.9 | 9.1 | 13.3 | 14.6 | 16.7 | 13.4 |
| BS403F | 4980 | 3.9 | 6.2 | 7.8 | 6.0 | 1.2 | 1.7 | 3.1 | 2.0 | 1 3.0 | 19.1 | 21.0 | 23.1 | 19.1 |
| BS403N | 4980 | 3.6 | 5.8 | 7.1 | 5.5 | 1.2 | 1.6 | 2.0 | 1.6 | 9.3 | 13.2 | 14.3 | 16.2 | 13.3 |
| BS403F | 5880 | 4.1 | 6.6 | 8.1 | 6.3 | 1.3 | 2.0 | 2.9 | 2.1 | 12.4 | 18.8 | 22.3 | 23.8 | 19.3 |
| BS403N | 5880 | 3.9 | 6.1 | 7.9 | 6.0 | 1.5 | 1.8 | 2.9 | 2.1 | 9.1 | 12.5 | 14.7 | 16.0 | 13.1 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 1.9 | 3.4 | 4.1 | 3.1 | 1.1 | 1.8 | 2.8 | 1.9 | 7.9 | 12.2 | 13.8 | 17.2 | 12.8 |
| BS403N | 4180 | 1.6 | 2.6 | 3.7 | 2.6 | 1.1 | 1.8 | 1.2 | 1.4 | 5.5 | 8.9 | 10.3 | 12.3 | 9.3 |
| BS403F | 4980 | 2.1 | 3.0 | 4.2 | 3.1 | 0.9 | 1.7 | 2.4 | 1.7 | 7.5 | 12.2 | 13.8 | 17.1 | 12.7 |
| BS403N | 4980 | 1.5 | 2.6 | 3.2 | 2.4 | 0.6 | 0.8 | 2.2 | 1.2 | 5.4 | 9.1 | 10.4 | 12.9 | 9.5 |
| BS403F | 5880 | 1.9 | 3.3 | 3.9 | 3.0 | 0.9 | 2.1 | 1.5 | 1.5 | 7.4 | 11.6 | 13.5 | 16.8 | 12.3 |
| BS403N | 5880 | 1.5 | 2.6 | 3.2 | 2.4 | 0.9 | 1.4 | 1.8 | 1.4 | 5.3 | 9.0 | 10.4 | 12.1 | 9.2 |
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 2.0 | 2.5 | 3.6 | 2.7 | 1.1 | 2.3 | 2.8 | 2.1 | 13.4 | 22.8 | 25.3 | 28.6 | 22.5 |
| BS403N | 4180 | 1.7 | 3.1 | 4.1 | 3.0 | 0.8 | 1.6 | 1.8 | 1.4 | 6.2 | 13.9 | 17.4 | 20.1 | 14.4 |
| BS403F | 4980 | 1.6 | 2.7 | 3.7 | 2.7 | 1.0 | 1.9 | 3.0 | 2.0 | 13.9 | 23.4 | 26.7 | 28.6 | 23.2 |
| BS403N | 4980 | 1.5 | 2.8 | 4.0 | 2.8 | 0.7 | 1.4 | 1.9 | 1.3 | 5.3 | 13.4 | 15.0 | 18.1 | 13.0 |
| BS403F | 5880 | 1.7 | 2.8 | 3.9 | 2.8 | 0.8 | 1.7 | 2.8 | 1.8 | 15.0 | 23.4 | 26.1 | 28.4 | 23.2 |
| BS403N | 5880 | 1.6 | 2.6 | 3.7 | 2.6 | 0.5 | 1.2 | 1.7 | 1.1 | 7.3 | 14.0 | 17.1 | 21.0 | 14.9 |
表III(续)
紧牢度性质
具有1.5％UV稳定剂的金属化酸性染料
CIE LAB，Delta E值
| 1 | 2 | 3 | 1 | 2 | 3 | |||||||||
| 样品云杉绿 | 卷绕速度 | 循环臭氧 | 循环臭氧 | 循环臭氧 | 平均臭氧 | 循环NOx | 循环NOx | 循环NOx | 平均NOx | 112kJ氙 | 188kJ氙 | 225kJ氙 | 300kJ氙 | 平均氙 |
| BS403F | 4180 | 0.1 | 0.3 | 0.4 | 0.3 | 0.1 | 0.2 | 0.3 | 0.2 | 2.2 | 3.0 | 3.7 | 5.5 | 3.6 |
| BS403N | 4180 | 0.1 | 0.1 | 0.1 | 0.1 | 0.5 | 0.5 | 0.3 | 0.4 | 2.9 | 3.6 | 3.9 | 5.4 | 4.0 |
| BS403F | 4980 | 0.2 | 0.1 | 0.1 | 0.1 | 0.2 | 0.4 | 0.3 | 0.3 | 2.4 | 2.9 | 3.6 | 4.5 | 3.4 |
| BS403N | 4980 | 0.3 | 0.5 | 0.3 | 0.4 | 1.0 | 0.1 | 0.1 | 0.4 | 2.7 | 3.1 | 4.0 | 5.3 | 3.8 |
| BS403F | 5880 | 0.1 | 0.1 | 0.4 | 0.2 | 0.1 | 0.2 | 0.3 | 0.2 | 2.3 | 3.1 | 4.0 | 4.7 | 3.5 |
| BS403N | 5880 | 0.3 | 0.4 | 0.5 | 0.4 | 0.1 | 0.3 | 0.2 | 0.2 | 2.9 | 3.8 | 5.4 | 2.0 | 3.5 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 0.8 | 0.8 | 0.9 | 0.8 | 0.6 | 0.4 | 0.5 | 0.5 | 3.0 | 4.7 | 5.3 | 7.0 | 5.0 |
| BS403N | 4180 | 0.5 | 0.7 | 0.8 | 0.7 | 0.4 | 0.3 | 0.5 | 0.4 | 3.0 | 4.9 | 5.9 | 7.9 | 5.4 |
| BS403F | 4980 | 0.6 | 0.7 | 0.6 | 0.6 | 0.3 | 0.3 | 0.3 | 0.3 | 2.9 | 4.7 | 5.2 | 7.0 | 5.0 |
| BS403N | 4980 | 0.6 | 0.6 | 0.7 | 0.6 | 0.4 | 0.4 | 0.4 | 0.4 | 5.6 | 4.4 | 6.0 | 7.6 | 5.9 |
| BS403F | 5880 | 0.4 | 0.6 | 0.6 | 0.5 | 0.3 | 0.2 | 0.5 | 0.3 | 3.2 | 4.5 | 6.0 | 7.6 | 5.3 |
| BS403N | 5880 | 0.6 | 0.4 | 0.8 | 0.6 | 0.3 | 0.2 | 1.2 | 0.6 | 2.9 | 4.8 | 6.1 | 7.8 | 5.4 |
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 0.4 | 0.2 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 1.7 | 2.4 | 2.8 | 2.9 | 2.5 |
| BS403N | 4180 | 0.1 | 0.1 | 0.2 | 0.1 | 0.2 | 0.3 | 0.2 | 0.2 | 1.7 | 2.2 | 2.4 | 3.5 | 2.5 |
| BS403F | 4980 | 0.1 | 0.1 | 0.2 | 0.1 | 0.2 | 0.4 | 0.2 | 0.3 | 1.9 | 2.1 | 2.6 | 3.2 | 2.5 |
| BS403N | 4980 | 0.2 | 0.4 | 0.2 | 0.3 | 0.4 | 0.1 | 0.1 | 0.2 | 2.0 | 2.5 | 2.9 | 3.6 | 2.7 |
| BS403F | 5880 | 0.1 | 0.2 | 0.1 | 0.1 | 0.4 | 0.1 | 0.1 | 0.2 | 2.0 | 2.3 | 2.6 | 3.4 | 2.6 |
| BS403N | 5880 | 0.1 | 0.2 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 2.4 | 3.0 | 3.2 | 3.8 | 3.1 |
表III(续)
紧牢度性质
具有1.5％UV稳定剂的非金属化酸性染料
CIE LAB，Delta E值
| 1 | 2 | 3 | 1 | 2 | 3 | |||||||||
| 样品 | 卷绕速度 | 循环臭氧 | 循环臭氧 | 循环臭氧 | 平均臭氧 | 循环Nox | 循环Nox | 循环Nox | 平均Nox | 112kJ氙 | 188kJ氙 | 225kJ氙 | 300kJ氙 | 平均氙 |
| 云杉绿 | ||||||||||||||
| BS403F | 4180 | 2.8 | 4.8 | 5.5 | 4.4 | 0.8 | 1.4 | 2.1 | 1.4 | 10.3 | 13.6 | 14.6 | 15.9 | 13.6 |
| BS403N | 4180 | 3.2 | 4.7 | 6.0 | 4.6 | 0.8 | 1.3 | 1.9 | 1.3 | 10.9 | 13.8 | 15.3 | 17.5 | 14.4 |
| BS403F | 4980 | 3.3 | 2.0 | 6.7 | 4.0 | 0.8 | 1.4 | 2.1 | 1.4 | 10.2 | 13.8 | 15.2 | 17.1 | 14.1 |
| BS403N | 4980 | 3.0 | 4.8 | 6.3 | 4.7 | 0.7 | 1.2 | 1.9 | 1.3 | 9.9 | 15.1 | 15.2 | 16.6 | 14.2 |
| BS403F | 5880 | 3.2 | 5.0 | 7.1 | 5.1 | 0.9 | 1.6 | 1.8 | 1.4 | 10.8 | 14.3 | 15.6 | 16.9 | 14.4 |
| BS403N | 5880 | 3.0 | 5.2 | 6.3 | 4.8 | 0.8 | 1.4 | 1.7 | 1.3 | 10.6 | 14.2 | 15.3 | 17.8 | 14.5 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 2.0 | 3.1 | 3.6 | 2.9 | 1.0 | 2.4 | 2.1 | 1.8 | 5.4 | 8.5 | 10.1 | 12.5 | 9.1 |
| BS403N | 4180 | 1.6 | 2.9 | 3.7 | 2.7 | 0.7 | 0.8 | 2.5 | 1.3 | 5.3 | 8.6 | 10.6 | 12.5 | 9.3 |
| BS403F | 4980 | 1.7 | 2.9 | 4.3 | 3.0 | 0.9 | 1.7 | 1.4 | 1.3 | 5.8 | 8.7 | 9.7 | 12.2 | 9.1 |
| BS403N | 4980 | 1.6 | 2.5 | 3.3 | 2.5 | 1.1 | 0.8 | 1.9 | 1.3 | 5.6 | 8.7 | 10.5 | 13.4 | 9.6 |
| BS403F | 5880 | 1.8 | 2.9 | 4.1 | 2.9 | 1.1 | 1.3 | 2.9 | 1.8 | 6.2 | 9.2 | 10.5 | 13.2 | 9.8 |
| BS403N | 5880 | 1.5 | 2.7 | 3.6 | 2.6 | 0.5 | 0.9 | 1.6 | 1.0 | 5.5 | 8.7 | 10.7 | 13.1 | 9.5 |
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 1.6 | 2.5 | 3.5 | 2.5 | 1.4 | 1.4 | 1.7 | 1.5 | 7.8 | 17.5 | 19.9 | 24.3 | 17.4 |
| BS403N | 4180 | 1.8 | 3.0 | 4.1 | 3.0 | 0.5 | 1.4 | 2.0 | 1.3 | 6.4 | 12.9 | 16.1 | 19.6 | 13.8 |
| BS403F | 4980 | 1.4 | 2.6 | 3.6 | 2.5 | 0.8 | 1.2 | 1.8 | 1.3 | 9.0 | 18.9 | 21.3 | 24.9 | 18.5 |
| BS403N | 4980 | 1.9 | 2.7 | 3.6 | 2.7 | 0.6 | 1.3 | 1.9 | 1.3 | 4.8 | 11.9 | 14.2 | 19.6 | 12.6 |
| BS403F | 5880 | 1.7 | 3.0 | 4.1 | 2.9 | 0.6 | 1.4 | 1.9 | 1.3 | 9.4 | 19.1 | 21.9 | 24.0 | 18.6 |
| BS403N | 5880 | 1.9 | 3.0 | 3.9 | 2.9 | 0.8 | 1.4 | 2.6 | 1.6 | 4.9 | 12.3 | 16.0 | 20.0 | 13.3 |
19
表IV
坚牢度性质
三色平均值
| 样品(卷绕速度) | 臭氧 | NOx | 氙 |
| 金属化酸性染料无UV稳定剂 | |||
| BS403F(4180) | 1.3 | 1.2 | 9.2 |
| BV403N(4180) | 1.3 | 1.0 | 4.2 |
| BS403F(4980) | 0.8 | 0.6 | 8.3 |
| BV403N(4980) | 1.0 | 0.7 | 4.8 |
| BS403F(5880) | 0.8 | 0.3 | 9.8 |
| BV403N(5880) | 0.5 | 0.7 | 4.1 |
| 1.5％UV稳定剂 | |||
| BS403F(4180) | 0.5 | 0.3 | 3.7 |
| BV403N(4180) | 0.3 | 0.4 | 3.9 |
| BS403F(4980) | 0.3 | 0.3 | 3.6 |
| BV403N(4980) | 0.4 | 0.3 | 4.1 |
| BS403F(5880) | 0.3 | 0.2 | 3.8 |
| BV403N(5880) | 0.4 | 0.3 | 4.0 |
| 非金属化酸性染料无UV稳定剂 | |||
| BS403F(4180) | 3.8 | 2.0 | 18.3 |
| BV403N(4180) | 3.9 | 1.5 | 12.4 |
| BS403F(4980) | 3.9 | 1.9 | 18.3 |
| BV403N(4980) | 3.6 | 1.4 | 11.9 |
| BS403F(5880) | 4.0 | 1.8 | 18.3 |
| BV403N(5880) | 3.7 | 1.5 | 12.4 |
| 1.5％UV稳定剂 | |||
| BS403F(4180) | 3.3 | 1.6 | 13.4 |
| BV403N(4180) | 3.4 | 1.3 | 12.5 |
| BS403F(4980) | 3.2 | 1.3 | 13.9 |
| BV403N(4980) | 3.3 | 1.3 | 12.1 |
| BS403F(5880) | 3.7 | 1.5 | 14.3 |
| BV403N(5880) | 3.4 | 1.3 | 12.4 |
本发明在染色的光坚牢度方面，即使忽略掉稳定剂，相对于常规的染色纤维仍显示出显著的改进。
经氙光照射后保留强度的结果示于表V。经氙光照射后保留强度的图表结果示于图5-8。本发明显示出，无论使用金属化酸或酸性染料，相对于常规纤维在强度上(不使用稳定剂)都有显著的改进。
表V
氙暴露后的保留强度
金属化酸染料-无UV稳定剂
| 112kJ | 188kJ | 225kJ | 300kJ | |||||||||||
| 样品云杉绿 | 卷绕速度 | 初始强度 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 |
| BS403F | 4180 | 3.9 | 2.7 | 69.2 | 62.3 | 2.2 | 56.4 | 46.2 | 1.8 | 46.2 | 40.0 | 1.1 | 28.2 | 26.9 |
| BS403N | 4180 | 3.5 | 3.5 | 100.0 | 93.3 | 2.7 | 77.1 | 79.6 | 2.1 | 60.0 | 67.8 | 2.1 | 60.0 | 62.7 |
| BS403F | 4980 | 3.8 | 3.0 | 78.2 | 73.2 | 2.2 | 57.9 | 47.8 | 1.8 | 47.4 | 36.6 | 1.0 | 26.3 | 27.1 |
| BS403N | 4980 | 4.1 | 3.1 | 75.6 | 82.9 | 2.7 | 65.6 | 71.4 | 2.5 | 61.0 | 65.7 | 2.1 | 51.2 | 58.3 |
| BS403F | 5880 | 3.3 | 2.9 | 87.9 | 71.9 | 2.2 | 66.7 | 49.2 | 1.9 | 57.6 | 41.7 | 1.3 | 39.4 | 33.9 |
| BS403N | 5880 | 4.1 | 3.1 | 75.6 | 83.0 | 2.5 | 61.0 | 69.3 | 2.3 | 56.1 | 62.9 | 2.1 | 51.2 | 57.2 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 3.6 | 1.2 | 33.3 | 0.4 | 11.1 | 0.2 | 5.6 | 0.0 | 0.0 | ||||
| BS403N | 4180 | 4.0 | 3.2 | 80.0 | 2.9 | 72.5 | 2.6 | 65.0 | 2.2 | 55.0 | ||||
| BS403F | 4980 | 3.9 | 2.2 | 56.4 | 0.6 | 15.4 | 0.0 | 0.0 | 0.0 | 0.0 | ||||
| BS403N | 4980 | 4.2 | 3.5 | 83.3 | 2.8 | 66.7 | 2.6 | 61.9 | 2.4 | 57.1 | ||||
| BS403F | 5880 | 3.9 | 1.4 | 35.9 | 0.2 | 5.1 | 0.0 | 0.0 | 0.0 | 0.0 | ||||
| BS403N | 5880 | 4.1 | 3.5 | 85.4 | 2.9 | 70.7 | 2.6 | 63.4 | 2.4 | 58.5 | ||||
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 3.8 | 3.2 | 84.2 | 2.7 | 71.1 | 2.6 | 68.4 | 2.0 | 52.6 | ||||
| BS403N | 4180 | 3.7 | 3.7 | 100.0 | 3.3 | 89.2 | 2.9 | 78.4 | 2.7 | 73.0 | ||||
| BS403F | 4980 | 4.0 | 3.4 | 85.0 | 2.8 | 70.0 | 2.5 | 62.5 | 2.2 | 55.0 | ||||
| BS403N | 4980 | 3.9 | 3.5 | 89.7 | 3.2 | 82.1 | 2.9 | 74.4 | 2.6 | 66.7 | ||||
| BS403F | 5880 | 3.7 | 3.4 | 91.9 | 2.8 | 75.7 | 2.5 | 67.6 | 2.3 | 62.2 | ||||
| BS403N | 5880 | 4.2 | 3.7 | 88.1 | 3.2 | 76.2 | 2.9 | 69.0 | 2.6 | 61.9 | ||||
表V(续)
氙暴露后的保留强度
非金属化酸性染料-无UV稳定剂
| 112kJ | 188kJ | 225kJ | 300kJ | |||||||||||
| 样品云杉绿 | 卷绕速度 | 初始强度 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 |
| BS403F | 4180 | 3.9 | 1.5 | 38.5 | 49.2 | 0.4 | 10.3 | 25.5 | 0.2 | 5.1 | 16.7 | 0.0 | 0.0 | 6.1 |
| BS403N | 4180 | 4.2 | 2.7 | 64.3 | 70.1 | 1.9 | 45.2 | 50.8 | 1.6 | 38.1 | 39.0 | 1.1 | 26.2 | 26.5 |
| BS403F | 4980 | 3.9 | 1.3 | 33.3 | 46.0 | 0.4 | 10.3 | 24.6 | 0.2 | 5.1 | 17.8 | 0.0 | 0.0 | 5.8 |
| BS403N | 4980 | 3.8 | 2.8 | 73.7 | 77.1 | 2.0 | 51.8 | 55.8 | 1.7 | 44.7 | 45.5 | 1.4 | 36.8 | 34.1 |
| BS403F | 5880 | 4.0 | 1.2 | 30.0 | 47.2 | 0.4 | 10.0 | 25.6 | 0.2 | 5.0 | 17.8 | 0.0 | 0.0 | 7.6 |
| BS403N | 5880 | 4.1 | 2.8 | 68.3 | 71.5 | 2.2 | 53.7 | 56.1 | 1.6 | 39.0 | 43.1 | 1.3 | 31.7 | 30.9 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 3.8 | 2.5 | 65.8 | 1.7 | 44.7 | 1.2 | 31.6 | 0.7 | 18.4 | ||||
| BS403N | 4180 | 4.1 | 3.1 | 75.6 | 2.4 | 58.5 | 1.8 | 43.9 | 1.3 | 31.7 | ||||
| BS403F | 4980 | 4.0 | 2.5 | 62.5 | 1.7 | 42.5 | 1.3 | 32.5 | 0.7 | 17.5 | ||||
| BS403N | 4980 | 3.9 | 3.3 | 84.6 | 2.4 | 61.5 | 2.0 | 51.3 | 1.5 | 38.5 | ||||
| BS403F | 5880 | 4.1 | 2.7 | 65.9 | 1.8 | 43.9 | 1.4 | 34.1 | 0.7 | 17.1 | ||||
| BS403N | 5880 | 4.1 | 3.3 | 80.5 | 2.7 | 65.9 | 2.2 | 53.7 | 1.7 | 41.5 | ||||
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 3.7 | 1.6 | 43.2 | 0.8 | 21.6 | 0.5 | 13.5 | 0.0 | 0.0 | ||||
| BS403N | 4180 | 3.7 | 2.6 | 70.3 | 1.8 | 48.6 | 1.3 | 35.1 | 0.8 | 21.6 | ||||
| BS403F | 4980 | 3.8 | 1.6 | 42.1 | 0.8 | 21.1 | 0.6 | 15.8 | 0.0 | 0.0 | ||||
| BS403N | 4980 | 3.7 | 2.7 | 73.0 | 2.0 | 54.1 | 1.5 | 40.5 | 1.0 | 27.0 | ||||
| BS403F | 5880 | 3.5 | 1.6 | 45.7 | 0.8 | 22.9 | 0.5 | 1 4.3 | 0.2 | 5.7 | ||||
| BS403N | 5880 | 4.1 | 2.7 | 65.9 | 2.0 | 48.8 | 1.5 | 36.6 | 0.8 | 19.5 | ||||
表V(续)
暴光后的保留强度
具有1.5％UV稳定剂的金属化酸性染料
| 112kJ | 188kJ | 225kJ | 300kJ | |||||||||||
| 样品云杉绿 | 卷绕速度 | 初始强度 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 |
| BS403F | 4180 | 4.0 | 3.6 | 90.0 | 95.7 | 3.1 | 77.5 | 82.7 | 2.7 | 67.5 | 77.6 | 2.4 | 60.0 | 67.3 |
| BS403N | 4180 | 3.6 | 3.3 | 91.7 | 92.1 | 2.7 | 75.0 | 76.0 | 2.5 | 69.4 | 68.9 | 2.1 | 58.3 | 59.1 |
| BS403F | 4980 | 3.6 | 3.5 | 97.2 | 99.0 | 2.9 | 80.6 | 83.7 | 2.7 | 75.0 | 77.4 | 2.4 | 66.7 | 68.5 |
| BS403N | 4980 | 3.5 | 3.3 | 94.3 | 90.9 | 2.8 | 80.0 | 74.8 | 2.1 | 60.0 | 61.6 | 2.1 | 60.0 | 56.0 |
| BS403F | 5880 | 3.5 | 3.3 | 94.3 | 93.0 | 2.7 | 77.1 | 74.4 | 2.4 | 68.6 | 71.1 | 2.2 | 62.9 | 65.8 |
| BS403N | 5880 | 4.1 | 3.4 | 82.9 | 86.9 | 2.6 | 63.4 | 68.8 | 2.4 | 58.5 | 63.8 | 2.2 | 53.7 | 56.3 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 3.7 | 3.4 | 91.9 | 2.9 | 78.4 | 2.8 | 75.7 | 2.4 | 64.9 | ||||
| BS403N | 4180 | 3.9 | 3.2 | 82.1 | 2.7 | 69.2 | 2.4 | 61.5 | 1.9 | 48.7 | ||||
| BS403F | 4980 | 3.7 | 3.6 | 97.3 | 2.7 | 73.0 | 2.5 | 67.6 | 2.1 | 56.8 | ||||
| BS403N | 4980 | 4.2 | 3.4 | 81.0 | 2.5 | 59.5 | 2.2 | 52.4 | 1.8 | 42.9 | ||||
| BS403F | 5880 | 3.9 | 3.4 | 87.2 | 2.3 | 58.2 | 2.6 | 66.7 | 2.3 | 59.0 | ||||
| BS403N | 5880 | 3.9 | 3.4 | 87.2 | 2.6 | 66.7 | 2.4 | 61.5 | 1.9 | 48.7 | ||||
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 3.9 | 4.1 | 105.1 | 3.6 | 92.3 | 3.5 | 89.7 | 3.0 | 76.9 | ||||
| BS403N | 4180 | 3.7 | 3.8 | 102.7 | 3.1 | 83.8 | 2.8 | 75.7 | 2.6 | 70.3 | ||||
| BS403F | 4980 | 3.9 | 4.0 | 102.6 | 3.8 | 97.4 | 3.5 | 89.7 | 3.2 | 82.1 | ||||
| BS403N | 4980 | 4.0 | 3.9 | 97.5 | 3.4 | 85.0 | 2.9 | 72.5 | 2.6 | 65.0 | ||||
| BS403F | 5880 | 4.1 | 4.0 | 97.6 | 3.6 | 87.8 | 3.2 | 78.0 | 3.1 | 75.6 | ||||
| BS403N | 5880 | 4.2 | 3.8 | 90.5 | 3.2 | 76.2 | 3.0 | 71.4 | 2.8 | 66.7 | ||||
表V(续)
暴光后的保留强度
具有1.5％UV稳定剂的非金属化酸性染料
| 112kJ | 188kJ | 225kJ | 300kJ | |||||||||||
| 样品云杉绿 | 卷绕速度 | 初始强度 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 | 强度 | ％保留强度 | 3平均色 |
| BS403F | 4180 | 4.0 | 3.0 | 75.0 | 73.8 | 2.5 | 62.5 | 52.9 | 2.1 | 52.5 | 44.1 | 1.6 | 40.0 | 33.0 |
| BS403N | 4180 | 3.8 | 2.9 | 76.3 | 74.1 | 2.2 | 57.9 | 55.6 | 1.4 | 36.8 | 39.5 | 0.9 | 23.7 | 26.0 |
| BS403F | 4980 | 3.8 | 2.9 | 76.3 | 73.2 | 2.4 | 63.2 | 55.5 | 1.9 | 50.0 | 44.9 | 1.5 | 39.5 | 30.8 |
| BS403N | 4980 | 3.5 | 2.8 | 80.0 | 77.9 | 2.0 | 57.1 | 56.7 | 1.7 | 48.6 | 46.1 | 1.0 | 28.6 | 27.5 |
| BS403F | 5880 | 4.1 | 2.9 | 70.7 | 71.9 | 2.3 | 56.1 | 54.7 | 2.0 | 48.8 | 42.3 | 1.3 | 31.7 | 28.7 |
| BS403N | 5880 | 4.2 | 2.9 | 69.0 | 72.7 | 2.2 | 52.4 | 54.5 | 1.8 | 42.9 | 44.6 | 1.1 | 26.2 | 28.1 |
| 灰 | ||||||||||||||
| BS403F | 4180 | 4.0 | 3.3 | 82.5 | 2.4 | 60.0 | 2.3 | 57.5 | 1.8 | 45.0 | ||||
| BS403N | 4180 | 4.0 | 3.2 | 80.0 | 2.6 | 65.0 | 2.0 | 50.0 | 1.3 | 32.5 | ||||
| BS403F | 4980 | 4.1 | 3.3 | 80.5 | 2.6 | 63.4 | 2.3 | 56.1 | 1.7 | 41.5 | ||||
| BS403N | 4980 | 3.9 | 3.4 | 87.2 | 2.5 | 64.1 | 2.1 | 53.8 | 1.3 | 33.3 | ||||
| BS403F | 5880 | 4.0 | 3.4 | 85.0 | 2.6 | 65.0 | 2.1 | 52.5 | 1.6 | 40.0 | ||||
| BS403N | 5880 | 4.0 | 3.3 | 82.5 | 2.6 | 65.0 | 2.2 | 55.0 | 1.5 | 37.5 | ||||
| 深酒红 | ||||||||||||||
| BS403F | 4180 | 3.6 | 2.3 | 63.9 | 1.3 | 36.1 | 0.8 | 22.2 | 0.5 | 13.9 | ||||
| BS403N | 4180 | 4.1 | 2.7 | 65.9 | 1.8 | 43.9 | 1.3 | 31.7 | 0.9 | 22.0 | ||||
| BS403F | 4980 | 3.5 | 2.2 | 62.9 | 1.4 | 40.0 | 1.0 | 28.6 | 0.4 | 11.4 | ||||
| BS403N | 4980 | 3.9 | 2.6 | 66.7 | 1.9 | 48.7 | 1.4 | 35.9 | 0.8 | 20.5 | ||||
| BS403F | 5880 | 3.5 | 2.1 | 60.0 | 1.5 | 42.9 | 0.9 | 25.7 | 0.5 | 14.3 | ||||
| BS403N | 5880 | 3.9 | 2.6 | 66.7 | 1.8 | 46.2 | 1.4 | 35.9 | 0.8 | 20.5 | ||||
实施例2
用常规的聚酰胺熔融纺丝技术制备四种1100/68有光的三叶截面的聚酰胺纱。此纱由尼龙6聚合物制备，聚合物用0.095重量％的苯甲酸(样品2BA)、0.15重量％的丙酸(样品2PA)、0.13重量％的对苯二甲酸(样品2TPA)和0.30重量％的对苯二甲酸加上0.15重量％的三丙酮二胺〔4-氨基-2，2，6，6-四甲基哌啶〕(样品2TPA/TAB)进行了调节(封端)。将纱针织为管状，并用下列添加剂在75℃下洗涤20分钟。
20∶1的浴比，软化水
0.5g/l KieralonNB-OL(阴离子和非离子表面活性剂，商业上来自新泽西州奥利夫山BASF公司)
0.5g/l TSPP(焦磷酸四钠)
然后每一管状物在一由主染浴分出的染浴中染色，主染浴中含有下列化合物：
30∶1的浴比，软化水
按织物重量的2.0％UniperolNB-SE(一种氧乙烯均染剂，商业上来自新泽西州奥利夫山BASF公司)
按织物重量的2.0％EulysinWP(一种低挥发性的有机酯，用于调节PH，商业上来自BASF公司)
0.005％Irgalan红B-K200％ (C.I.酸性红182)
0.125％Irgalan黑BGL200％ (C.I.酸性黑107)
0.030％Irgalan黄3RL250％ (C.I.酸性橙162)
(Lanasyn和Irgalan染料商业上分别来自北卡罗来纳州夏洛特的Sandoz化学公司和北卡罗来纳州学格林斯伯勒的Ciba公司。)
用苏打灰将浴的初始PH调节至10.0。在染浴中，样品加热至95℃历时30分钟，并在95℃下保温30分钟。将染浴冷却。EulysinWP在染色期间使PH值下降至6到7。随后将样品从染浴中移出，先用温水再用冷水漂洗并干燥。每一染色管状物的各段用SAE试验方法J1885暴露于112.8KJ的氙光下。相对于染色面未曝光的样品，每种纱的ΔE(总色差)值示于表VI。
表IV
| 样品 | ΔE |
| 2BA | 18.2 |
| 2PA | 16.0 |
| 2TPA | 17.5 |
| 2TPA/TAD | 3.5 |
实施例3
如实施例2所述，制备四种聚酰胺纱。每一种纱通过使用于地毯纱的常规装置进行蒸汽热定形。每一种纱如同实施例2那样洗涤和染色，但在染色中用以下的蓝色调：
0.013％Irgalan枣红EL200％ (C.I.酸性红251)
0.049％Irgalan蓝3GL (C.I.酸性蓝171)
0.026％Irgalan灰GL200％ (C.I.酸性黑131∶1)
0.002％Lanacron棕S-GL (C.I.酸性棕298)
每一染色管状物的各段用SAE试验方法J1885暴露于112.8KJ的氙光下。ΔE值示于表VII。
表VII
| 样品 | ΔE |
| 3BA | 23.3 |
| 3PA | 21.0 |
| 3TPA | 21.7 |
| 3TPA/TAD | 11.5 |
Claims (14)
1.一种制备光化学稳定的染色尼龙合成物的工艺，包括：提供至染浴中一种在水和一种羧酸链调节剂及一种受阻哌啶衍生物存在下水解聚合制成的聚(ε-己内酰胺)的成型制品，调节剂选择如下：
乙酸；
丙酸；
苯甲酸；
环己烷-1，4-二羧酸；
萘-2，6-二羧酸；
对苯二甲酸；
间苯二甲酸；及
它们的组合；
在染浴中用一种或多种金属化或非金属化酸性染料染色成型制品。
2.权利要求1的工艺，其特征为上述提供的制品为一种成型为纤维、膜、或模压品的制品。
3.权利要求1和2的工艺，其特征为上述提供的制品为地毯面纱或编织物形式的纤维。
4.权利要求1至3的工艺，其特征为上述受阻哌啶衍生物是一种氨基多烷基哌啶。
5.权利要求1至4的工艺，其特征为上述非金属化酸性染料由以下类中选出：
C.I.酸性黄246；
C.I.酸性橙156；
C.I.酸性红361；
C.I.酸性蓝277；及
C.I.酸性蓝324；
6.权利要求1至5的工艺，其特征为上述金属化酸性染料由以下类别中选出：
C.I.酸性黄59；
C.I.酸性橙162；
C.I.酸性红51；
C.I.酸性蓝171；
C.I.酸性棕298；
C.I.酸性黑131：1；及
C.I.酸性黑132；
7.一种光化学稳定尼龙制品，包括一种由聚合物成型并用金属或非金属化染料染色的制品，聚合物为在水、一种羧酸链调节剂和一种受阻哌啶衍生物存在下通过水解聚合ε-己内酰胺生成的。
8.权利要求7的制品，其特征为上述制品具有纤维、膜或模压件的形状。
9.权利要求7和8的制品，其特征为上述羧酸链调节剂选自下列类别：
乙酸；
丙酸；
苯甲酸；
环己烷-1，4-二羧酸；
萘-2，6-二羧酸；
对苯二甲酸；
间苯二甲酸；及
它们的组合；
及一种受阻哌啶衍生物。
10.权利要求7至9的制品，其特征为上述受阻哌啶衍生物是一种氨基多烷基胺。
11.权利要求7至9的制品，其特征为上述受阻哌啶衍生物选自以下类别：
4-氨基-2，2′，6，6′-四甲基哌啶；
4-(氨烷基)-2，2′，6，6′-四甲基哌啶；
4-(氨芳基)-2，2′，6，6′-四甲基哌啶；
4-(氨芳基/烷基)-2，2′，6，6′-四甲基哌啶；
3-氨基-2，2′，6，6′-四甲基哌啶；
3-(氨烷基)-2，2′，6，6′-四甲基哌啶；
3-(氨芳基)-2，2′，6，6′-四甲基哌啶；
3-(氨芳基/烷基)-2，2′，6，6′-四甲基哌啶；
2，2′，6，6′-四甲基-4-哌啶羧酸；
2，2′，6，6′-四甲基-4-哌啶烷基羧酸；
2，2′，6，6′-四甲基-4-哌啶芳基羧酸；
2，2′，6，6′-四甲基-4-哌啶烷基/芳基羧酸；
2，2′，6，6′-四甲基-3-哌啶羧酸；
2，2′，6，6′-四甲基-3-哌啶烷基羧酸；
2，2′，6，6′-四甲基-3-哌啶芳基羧酸；和
2，2′，6，6′-四甲基-34-哌啶烷基/芳基羧酸；
12.权利要求7至11的制品，其特征为上述非金属化酸性染料由以下类别中选出；
C.I.酸性黄246；
C.I.酸性橙156；
C.I.酸性红361；
C.I.酸性蓝277；及
C.I.酸性蓝324；
13.权利要求7至12的制品，其特征为上述金属化酸性染料由以下类别中选出：
C.I.酸性黄59；
C.I.酸性橙162；
C.I.酸性红51；
C.I.酸性蓝171；
C.I.酸性棕298；
C.I.酸性黑131∶1；及
C.I.酸性黑132；
14.权利要求7至13的制品，其特征为上述制品为纤维。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US690,692 | 1996-07-31 | ||
| US08/690,692 US5851238A (en) | 1996-07-31 | 1996-07-31 | Photochemically stabilized polyamide compositions |
| US690692 | 1996-07-31 |
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| CN1137306C CN1137306C (zh) | 2004-02-04 |
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| US (2) | US5851238A (zh) |
| EP (1) | EP0822275B1 (zh) |
| JP (1) | JPH10183480A (zh) |
| CN (1) | CN1137306C (zh) |
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| EP0546993A1 (de) * | 1991-12-09 | 1993-06-16 | Ciba-Geigy Ag | Wasserlöschliche Triazinderivate zur photochemischen und thermischen Stabilisierung von Polyamidfasermaterialien |
| EP0601439B1 (de) * | 1992-12-07 | 1999-07-07 | BASF Aktiengesellschaft | Farbstoffmischungen, enthaltend Azofarbstoffe mit einer Kupplungskomponente aus der Diaminopyridinreihe |
| JP3260517B2 (ja) * | 1993-10-06 | 2002-02-25 | ダイスタージャパン株式会社 | 分散染料組成物及びこれを用いる疎水性繊維の染色方法 |
| CA2122210C (en) * | 1993-08-16 | 2000-02-15 | Anil W. Saraf | Process for the manufacture of a post-heat set dyed fabric consisting essentially of polyamide fibers with improved dye washfastness and heat stability |
| US5380828A (en) * | 1993-10-05 | 1995-01-10 | Ciba-Geigy Corporation | Azodicarboxylic acid derivatives containing hindered amine moieties as polymer stabilizers |
| US5466761A (en) * | 1993-10-29 | 1995-11-14 | Dsm N.V. | Nylon alloys |
| CA2187821C (en) * | 1994-04-15 | 2001-10-23 | Klaus Weinerth | Inherently light- and heat-stabilized polyamides |
| TW287181B (zh) * | 1994-05-10 | 1996-10-01 | Taishl Kagaku Kogyo Kk | |
| US5489639A (en) * | 1994-08-18 | 1996-02-06 | General Electric Company | Copper salts for laser marking of thermoplastic compositions |
| US5595701A (en) * | 1995-05-12 | 1997-01-21 | The Goodyear Tire & Rubber Company | Process for making a polyurea backed product with a polyurethane skin |
| US5618909A (en) * | 1995-07-27 | 1997-04-08 | Alliedsignal Inc. | Light stabilized polyamide substrate and process for making |
| JPH0941217A (ja) * | 1995-07-31 | 1997-02-10 | Teijin Ltd | 粗面化ポリアミド繊維の製造方法 |
| JPH0941218A (ja) * | 1995-07-31 | 1997-02-10 | Teijin Ltd | 粗面化ポリアミド繊維の製造方法 |
| DE19537614C3 (de) * | 1995-10-09 | 2003-10-02 | Inventa Ag | Polycaprolactam mit neuartiger Kettenregelung |
-
1996
- 1996-07-31 US US08/690,692 patent/US5851238A/en not_active Expired - Fee Related
-
1997
- 1997-02-21 US US08/804,312 patent/US5814107A/en not_active Expired - Fee Related
- 1997-03-10 CA CA002199639A patent/CA2199639C/en not_active Expired - Fee Related
- 1997-07-17 EP EP97112189A patent/EP0822275B1/en not_active Revoked
- 1997-07-17 DE DE69719629T patent/DE69719629T2/de not_active Expired - Lifetime
- 1997-07-30 CN CNB97114768XA patent/CN1137306C/zh not_active Expired - Fee Related
- 1997-07-31 JP JP9219950A patent/JPH10183480A/ja not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012776A (zh) * | 2012-12-07 | 2013-04-03 | 四川大学 | 一种原位稳定化尼龙6及其制备方法 |
| CN103012776B (zh) * | 2012-12-07 | 2014-12-10 | 四川大学 | 一种原位稳定化尼龙6及其制备方法 |
| CN109415538A (zh) * | 2016-06-27 | 2019-03-01 | 科莱恩塑料和涂料有限公司 | 添加剂组合物用于制备缩聚聚合物的用途 |
| CN109415538B (zh) * | 2016-06-27 | 2022-03-01 | 科莱恩塑料和涂料有限公司 | 添加剂组合物用于制备缩聚聚合物的用途 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0822275A2 (en) | 1998-02-04 |
| CA2199639A1 (en) | 1998-02-01 |
| US5814107A (en) | 1998-09-29 |
| JPH10183480A (ja) | 1998-07-14 |
| DE69719629D1 (de) | 2003-04-17 |
| US5851238A (en) | 1998-12-22 |
| EP0822275A3 (en) | 1998-10-07 |
| CA2199639C (en) | 2001-06-26 |
| CN1137306C (zh) | 2004-02-04 |
| EP0822275B1 (en) | 2003-03-12 |
| DE69719629T2 (de) | 2003-09-11 |
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