CN1882739B - 提高色泽深度的方法 - Google Patents

提高色泽深度的方法 Download PDF

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CN1882739B
CN1882739B CN2004800337861A CN200480033786A CN1882739B CN 1882739 B CN1882739 B CN 1882739B CN 2004800337861 A CN2004800337861 A CN 2004800337861A CN 200480033786 A CN200480033786 A CN 200480033786A CN 1882739 B CN1882739 B CN 1882739B
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P·乌兹尔
U·施特拉姆
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Abstract

本发明涉及提高染色天然或合成聚酰胺纤维材料的色泽深度的方法,所述方法包括在染色之前、当中或之后采用包含式(1)的化合物的液体处理纤维材料,其中R为卤素、C1-C12烷基、C5-C24芳基、C6-C36芳烷基、-OR1或-NR1R2,R1和R2各自独立为氢、C1-C12烷基(未取代或用一个或多个羟基、氨基、巯基、羧基、磺基、C1-C12烷基磺酰基、C5-C24芳基磺酰基或C6-C36芳烷基磺酰基取代)、C5-C24芳基(未取代或用一个或多个羟基、氨基、羧基、磺基、C1-C12烷基磺酰基、C5-C24芳基磺酰基或C6-C36芳烷基磺酰基取代)或C6-C36芳烷基(未取代或用一个或多个羟基、氨基、羧基、磺基、C1-C12烷基磺酰基、C5-C24芳基磺酰基或C6-C36芳烷基磺酰基取代),X和Y各自独立为巯基、-NR3R4或-N+R3R4R5A-,其中R3、R4和R5各自独立为氢或C1-C12烷基,A-为氯离子、溴离子、碘离子、硫酸根离子或甲基硫酸根离子,R6和R7各自独立为氢或C1-C12烷基,x和y各自独立为2至12的数。

Description

提高色泽深度的方法
本发明涉及通过染色之前、当中或之后采用氨基取代的三嗪衍生物进行处理来提高染色天然或合成聚酰胺纤维材料色泽深度的方法。
在聚酰胺纤维,特别是聚酰胺微纤维染色过程中,可采用酸性染料获得深色泽,尽管以良好的洗牢度性能为代价。
相反地,当用活性染料进行染色时可获得良好的洗牢度性能,尽管这种情况下不容易获得深色泽。
已经发现:如果染色之前、当中或之后采用包含特定氨基取代的三嗪的液体处理聚酰胺纤维材料可获得洗牢度高的深色泽。
本发明涉及提高染色天然或合成聚酰胺纤维材料的色泽深度的方法,所述方法包括在染色之前、当中或之后采用包含式(1)的化合物的液体处理纤维材料:
其中R为卤素、C1-C12烷基、C5-C24芳基、C6-C36芳烷基、-OR1或-NR1R2,R1和R2各自独立为氢、C1-C12烷基(未取代的或用一个或多个羟基、氨基、巯基、羧基、磺基、C1-C12烷基磺酰基、C5-C24芳基磺酰基或C6-C36芳烷基磺酰基取代的)、C5-C24芳基(未取代的或用一个或多个羟基、氨基、羧基、磺基、C1-C12烷基磺酰基、C5-C24芳基磺酰基或C6-C36芳烷基磺酰基取代的)或C6-C36芳烷基(未取代的或用一个或多个羟基、氨基、羧基、磺基、C1-C12烷基磺酰基、C5-C24芳基磺酰基或C6-C36芳烷基磺酰基取代的),
X和Y各自独立为巯基、-NR3R4或-N+R3R4R5A-,其中R3、R4和R5各自独立为氢或C1-C12烷基,A-为氯离子、溴离子、碘离子、硫酸根离子或甲基硫酸根离子,
R6和R7各自独立为氢或C1-C12烷基,
x和y各自独立为2至12的数。
作为R或R1-R5之一的C1-C12烷基可为例如甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基、新戊基、正己基、正辛基、正癸基或正十二烷基。
作为R或R1-R5之一的C6-C24芳基为例如苯基、3-氨基-4-磺苯基、甲苯基、基、2,4,6-三异丙基苯基(isityl)、萘基和蒽基。
合适的C6-C24芳烷基为例如苄基和2-苯乙基。
在本发明的方法中,优选使用其中x和y相同的式(1)的化合物。
优选的式(1)的化合物中,x和y为3、4或6。
还优选其中X和Y相同的式(1)的化合物。
特别优选使用其中R为式-NH-(CHR8)z-Z的基团的式(1)的化合物,其中R8为氢或C1-C12烷基,Z为羟基、巯基或氨基,z为2至12的数。
合适的通式(1)的化合物的实例为式(101)-(112)的化合物:
Figure S04833786120060529D000041
特别优选的通式(1)的化合物为式(101)、(102)、(103)、(105)和(112)的化合物。
式(1)的化合物为已知的或可通过已知方法制备,如通过氰尿酰氯连续地和式X-(CHR6)x-NH2的化合物、式Y-(CHR7)y-NH2的化合物和式R1-NH2的化合物反应,其中X、Y、x、y、R1、R6和R7如上文中所定义的。
用于本发明的方法中的式(1)的化合物可方便地使用,不考虑浴比,其量为0.01-15%重量,优选0.1-10%重量,特别是0.5-7%重量,以聚酰胺纤维材料的重量计。
采用式(1)的化合物对聚酰胺纤维材料的处理可在染色之后、当中或优选之前进行。
当采用氨基取代的三嗪衍生物对聚酰胺纤维材料的处理在染色过程中进行时,本发明的方法可通过将上述量的式(1)的化合物加入染液中并采用常规方式对纤维材料进行染色而方便地进行。
然而,优选采用氨基取代的三嗪衍生物对聚酰胺纤维材料的处理在染色之前进行。预处理后,纺织材料可方便地在室温或稍高温度下用水清洗。
合适的聚酰胺纤维材料包括天然聚酰胺纤维材料(如毛或丝)和合成聚酰胺纤维材料(如聚酰胺-6或聚酰胺-6.6)及纤维混合物(如毛/纤维素或聚酰胺/纤维素纤维混合物或聚酰胺/毛纤维混合物)。纤维材料优选合成聚酰胺纤维材料,特别是微纤维。
可使用任何形式的纺织材料,如纤维、纱线、机织物或针织物。
采用氨基取代的三嗪衍生物对聚酰胺纤维材料的处理优选按照浸染法进行,这种情况下浴比选择范围较宽,如为1∶4-1∶100,优选1∶5-1∶70,特别是1∶10-1∶40。
不需要特殊的装置。例如可使用常规染色装置,如开口浴槽、绞盘染槽、卷染机、或者桨式装置、喷射装置或循环装置。
所述方法方便地在如20-130℃,优选50-120℃,特别是60-100℃的温度下进行。处理时间可为如10-60分钟,优选15-40分钟。所述液体的pH通常为7-13,优选8-12.5,特别是10-12。
除了本发明的助剂外,所述液体还可包含常规添加剂,如电解质(如氯化钠或硫酸钠)、分散剂和润湿剂、pH调节剂和消泡剂。
采用如阴离子染料或活性染料进行染色。任何常规阴离子染料或活性染料(如Colour Index,第三版(1971)中所述)都是合适的。
阴离子染料的实例包括含磺基的单偶氮、多偶氮、金属络合偶氮、蒽醌、酞菁染料和甲染料。
用于聚酰胺纤维材料染色的阴离子染料为其游离磺酸或优选其盐形式。
用于聚酰胺纤维材料染色的染料可包含其它添加剂,如氯化钠或糊精。
聚酰胺纤维材料的染色可按照常规染色或印染方法,如按照轧染或浸染法进行。除了水和染料外,染色液或印染浆可包含其它添加剂,如润湿剂、消泡剂、匀染剂或影响纺织材料特性的试剂,如柔软剂、阻燃剂或抗污剂、抗水剂和抗油剂和软水剂及天然或合成增稠剂,如藻酸盐和纤维素醚。
根据所需色泽深度,染色浴中染料的量可在大范围内变化;已证实:通常为待染色材料的0.01-15%重量,特别是0.01-10%重量的量是有利的。
采用阴离子染料或活性染料的染色优选在pH为1-8,特别是2-7的条件下进行。浴比可在大范围内选择,如1∶3-1∶50,优选1∶5-1∶30。染色优选在50-130℃,特别是80-120℃下进行。
按照本发明的方法获得了染料(如阴离子染料或活性染料)在聚酰胺纤维材料上的染色,所述染色显示实质上提高的色泽深度,而洗牢度或耐日光牢度性能没有受到负面影响。
本发明还涉及纺织助剂,所述助剂包含式(1)的化合物的水溶液。
本发明的纺织助剂可包含其它添加剂,如润湿剂、分散剂或pH调节剂。
如下实施例用于举例说明本发明。除非另有说明,温度为摄氏度,份为重量份,百分比是指重量百分比。重量份与体积份之比表示为千克比升。
I.制备实施例
I.1.式(101)的化合物
Figure S04833786120060529D000061
将9.22克氰尿酰氯、35克冷水、50克冰、0.5克磷酸氢二钠和1滴Irgapadol FFU(分散剂,Ciba Specialty Chemicals)引入750毫升磺化烧瓶中并在0-2℃下搅拌30分钟。随后加入17.6克1,6-二氨基己烷和35克水的溶液(已在2-5℃下用4N HCl中和至pH 7.5)。在2℃下搅拌混合物3小时,通过加入1N NaOH使得pH保持恒定为7.0。然后将温度缓慢升至25℃;pH仍保持恒定为7.0。在25℃下搅拌3小时后,在pH 7.0下非常缓慢地将温度分步升至95℃。在95℃下搅拌2小时后,反应完成。冷却物料并将副产物过滤掉。
得到405克活性含量为4.5%的澄清无色溶液。
I.2.式(102)的化合物
Figure S04833786120060529D000071
类似于实施例I.1,9.22克氰尿酰氯与13.4克1,4-二氨基丁烷反应。得到505克活性含量为4.1%的澄清无色溶液。
I.3.式(103)的化合物
将4.61克氰尿酰氯、25克冷水、30克冰和1滴Irgapadol FFU(分散剂,Ciba Specialty Chemicals)引入350毫升磺化烧瓶中并在0-2℃下搅拌30分钟。40分钟内将1.53克乙醇胺和5.0克水的溶液逐滴加入。加入过程中,pH保持恒定为7.0-7.5。加入后,在2℃下搅拌混合物90分钟,通过加入1N NaOH使得pH保持恒定为7.0。随后加入5.8克1,6-二氨基己烷和10克水的溶液(已在2-5℃下用4N HCl中和至pH 7.5)。然后将温度非常缓慢升至50℃,pH保持恒定为7.0。50℃下搅拌混合物2小时。pH为7.0下,非常缓慢地将温度分步升至95℃。在95℃下保持4小时后,反应完成。冷却物料并将副产物过滤掉。
得到182克活性含量为2.9%的澄清无色溶液。
I.4.式(112)的化合物
Figure S04833786120060529D000081
将18.4克氰尿酰氯、30克冷水、30克冰和1滴Irgapadol FFU引入350毫升磺化烧瓶中并在0-2℃下搅拌30分钟。随后加入7.45克1,2-二氨基丙烷和20克水的溶液(已在2-5℃下用37%HCl中和至pH 7.5)。在2℃下搅拌混合物,通过加入7.45克1,2-二氨基丙烷和8.0克水的溶液使得pH保持恒定为6.5。加入完成后,在2℃下再搅拌1小时,通过加入4N NaOH保持pH为6.5。然后将温度缓慢升至25℃,pH仍保持恒定为6.5。在25℃下保持2小时后,反应完成。将副产物过滤掉。
得到195克活性含量为16%的澄清无色溶液。
II.应用实施例
II.1.微纤维的预处理和染色
(a)预处理
在室温下将5克聚酰胺微纤维织物(PA-Meryl microfibre 5-3101)浸入含5.55克制备实施例I.1的产物(5%活性产物,以纤维重量计)和45克水的液体(已用NaOH调整至pH 11)中。随后以2℃/分钟的加热速率将液体加热至98℃。在98℃保持30分钟后,以3℃/分钟将液体冷却到60℃。
预处理后,用水清洗织物,首先在25℃,然后在50-60℃,随后在25℃用稀醋酸(pH 6.0)清洗。
(b)染色
室温下,将已预处理的织物浸入已用80%醋酸调整至pH 3的含8%Eriofast Red 2B(Ciba Specialty Chemicals)和1克/升TinovetinJUN(润湿剂,Ciba Specialty Chemicals)的液体中。随后以2℃/分钟的加热速率将液体加热至98℃。98℃下保持60分钟后,以3℃/分钟将液体冷却到60℃。
染色后,首先在50℃下用水清洗织物,然后在70℃下用Na2CO3水溶液清洗20分钟,在30-40℃用水清洗,最后在室温下用稀醋酸(0.5ml 80%醋酸/每升)清洗,再用水清洗。
II.2.用3.4克制备实施例I.1的产物重复实施例II.1.。
II.3.用6.1克制备实施例I.2的产物重复实施例II.1.。
II.4.用8.7克制备实施例I.3的产物重复实施例II.1。
II.5.用1.6克制备实施例I.4的产物重复实施例II.1.。
得到具有暗色泽的染色,而洗牢度和耐日光牢度没有受到负面影响。

Claims (8)

1.一种提高染色天然或合成聚酰胺纤维材料的色泽深度的方法,所述方法包括在染色之前、当中或之后采用包含式(101)、(102)、(103)或(112)的化合物的液体处理纤维材料:
2.权利要求中1的方法,其中所述液体中式(101)、(102)、(103)或(112)的化合物的量为聚酰胺纤维材料重量的0.01-15%重量。
3.权利要求1或2的方法,其中所述纤维材料已在染色前经过处理。
4.权利要求1或2的方法,其中所述采用包含式(101)、(102)、(103)或(112)的化合物的液体进行的处理在20-130℃的温度下进行。
5.权利要求3的方法,其中所述处理在pH为7-13的条件下进行。
6.权利要求1或2的方法,其中所述采用包含式(101)、(102)、(103)或(112)的化合物的液体进行的处理按照浸染法进行。
7.权利要求1或2的方法,其中所述聚酰胺纤维材料为微纤维形式。
8.一种纺织助剂,所述纺织助剂包含权利要求1的式(101)、(102)、(103)或(112)的化合物的水溶液。
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