CN110305499B - 一种复合活性黑染料及其应用 - Google Patents

一种复合活性黑染料及其应用 Download PDF

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CN110305499B
CN110305499B CN201910549864.1A CN201910549864A CN110305499B CN 110305499 B CN110305499 B CN 110305499B CN 201910549864 A CN201910549864 A CN 201910549864A CN 110305499 B CN110305499 B CN 110305499B
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崔孟元
朱纯杰
熊建平
张志华
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Hubei Hwalle Dyestuff Industry Co ltd
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Abstract

本发明属于染料技术领域，具体涉及一种复合活性黑染料，包括如式(1)所示的染料、如式(2)所示的染料和如式(3)所示的染料，按重量份数配比如下：式(1)染料50～100份，式(2)染料5～45份，式(3)染料0～5份。本发明还提供一种黑色染料组合物，包括固色碱剂、促染剂以及上述的复合活性黑染料。本发明提供的复合活性黑染料具有较高的染深性、良好的固色率和洗涤性，且原料成本低，通过藏青色的式(1)染料、橙色的式(2)染料、黄色的式(3)染料三种染料复配使得色织物具有更高的匀染性、高的固色率和高牢度性，达到了前所未有的乌黑丰满度及染深性，增加了染料的洗涤性，解决了现有活性黑染料的洗涤性较差、粘色严重等问题，适用于纤维材料的浸染、轧染及防染印花。

Description

一种复合活性黑染料及其应用
技术领域
本发明属于染料技术领域，具体涉及一种复合活性黑染料及其应用。
背景技术
近年来，复合染料技术飞速发展，复合活性染料用途越来越广，不同活性染料相混合，可以起到协同增效的作用。
黑色活性染料是染料中应用较多、产量较大的品种，目前市场上用的大多数是在C.I.活性黑5中加橙色组分复配而成，但其在染色过程中仍存在固色率和染深性低，而且还存在洗涤性较差，粘色严重的问题。
发明内容
为了克服上述现有技术存在的不足，本发明的目的是提供一种复合活性黑染料及其应用，不仅生产成本低、染深性高、固色率好、牢度性高，而且洗涤性好，不沾色。
为实现上述目的，本发明的技术方案为一种复合活性黑染料，包括如式(1)所示的染料、如式(2)所示的染料和如式(3)所示的染料，
Figure BDA0002105172520000021
其中，式(1)染料、式(2)染料、式(3)染料按重量份数配比如下：式(1)染料50～100份，式(2)染料5～45份，式(3)染料0～5份。
上述式(1)染料、式(2)染料、式(3)染料的染料的制备方法如下：
式(1)染料的制备方法：将对位酯(4-硫酸乙酯砜基苯胺)溶于水中打浆50分钟，用冰降温至0-8℃后，加入盐酸，随后加入亚硝酸钠配成30％的溶液，维持T＝5-8℃，pH＝1.0-1.3，反应1.5小时后用氨基磺酸消除多余的亚硝酸钠；将重氮盐加入到H酸溶液中，维持T＝5-8℃，反应4小时后用小苏打干粉调节pH＝6.0-6.5，维持T＝5-8℃，反应4小时后，即可得到上述式(1)所示的染料。
式(2)染料的制备方法：将1份4B酸(3-甲基-6-氨基苯磺酸)加入到水中搅拌，降温0-5℃，向其中滴加盐酸，再在0℃左右加入亚硝酸钠溶液，混合物在该温度下搅拌1小时，得反应物I；
将2份对位酯加到水中配成20％左右浓度混合物，降温0-5℃，加入盐酸，再在0℃左右加入亚硝酸钠溶液，反应物继续在15-20℃下搅拌3小时，反应物II；
把1份3,5-二氨基苯甲酸加入到反应物I中，在4小时过程中用小苏打把反应物的PH值调节到4，反应物在6-7℃搅拌30分钟，把反应物II加入到上述反应物中，在30分钟左右用碳酸钠溶液把PH调节到3.5，再在1小时用碳酸钠调节PH值为6.3，反应2小时，即可得到上述式(2)所示的染料。
式(3)染料的制备方法：将K酸(2-萘胺-3,6,8-三磺酸)在适量水中打浆1小时，加入盐酸搅拌20分钟，用冰降温至0-5℃，滴加30％亚硝酸钠溶液进行重氮化，过程始终保持T＝0-10℃，反应2小时后得K酸重氮盐。将K酸重氮盐加入到经充分打浆的间脲基苯胺中，维持PH＝3-5，T＝10-18℃发生偶合反应，直到检测不出重氮盐为反应终点，得到偶合物；将偶合物加入到经充分冰磨的三聚氯氰，控制T＝0-10℃、PH＝1.5-2发生缩合反应，反应4小时，得到一次缩合物；再向体系中加入对位酯，控制T＝40-50℃，PH＝5-7进行二次缩合反应，即可得到上述式(3)所示的染料。
进一步地，所述复合活性黑染料中，式(1)染料、式(2)染料、式(3)染料按重量份数配比如下：式(1)染料60～80份，式(2)染料20～35份，式(3)染料1～5份。
作为优选的实施方式，所述复合活性黑染料中，式(1)染料、式(2)染料、式(3)染料按重量份数配比如下：式(1)染料70份，式(2)染料25份，式(3)染料5份。
本发明提供的复合活性黑染料用于纤维材料的浸染、轧染及防染印花。
本发明还提供一种黑色染料组合物，包括固色碱剂、促染剂以及上述的复合活性黑染料。
进一步地，所述固色碱剂为氢氧化钠、碳酸钠或碳酸氢钠，所述促染剂为元明粉或氯化钠。
进一步地，还包括防泳移剂、助溶剂、防染盐。
更进一步地，所述防泳移剂为海藻酸钠，助溶剂为尿素，防染盐为间硝基苯磺酸钠。
与现有技术相比，本发明具有以下有益效果：
(1)本发明提供的复合活性黑染料具有较高的染深性、良好的固色率和洗涤性，且原料成本低；
(2)本发明提供的复合活性黑染料由藏青色的式(1)染料、橙色的式(2)染料、黄色的式(3)染料三种染料混合而成，相较单纯的藏青、橙两种染料混合，增强它们染色间的配伍性，使得色织物具有更高的匀染性、高的固色率和高牢度性，达到了前所未有的乌黑丰满度及染深性；
(3)本发明提供的复合活性黑染料是含三偶氮染料复合的黑色染料混合物，染料染色强度高，可以相应减少染色用染料量，降低生产成本；
(4)本发明提供的复合活性黑染料可以在低温下染色，织物上的浮色染料不易上色，其未固定染料更易洗净，增加了染料的洗涤性，解决了现有活性黑染料的洗涤性较差、粘色严重等问题；
(5)本发明提供的复合活性黑染料适用于纤维材料的浸染、轧染及防染印花。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
本发明实施例提供一种复合活性黑染料，包括如式(1)所示的染料、如式(2)所示的染料和如式(3)所示的染料，
Figure BDA0002105172520000051
其中，式(1)染料、式(2)染料、式(3)染料按重量份数配比如下：式(1)染料50～100份，式(2)染料5～45份，式(3)染料0～5份。
优选的，所述复合活性黑染料中，式(1)染料、式(2)染料、式(3)染料按重量份数配比如下：式(1)染料60～80份，式(2)染料20～35份，式(3)染料1～5份。本实施例中通过加入黄色的式(3)染料可以增强染色配伍性和染色强度。
本发明提供的复合活性黑染料用于纤维材料的浸染、轧染及防染印花，尤其是棉质纤维。
本发明还提供一种黑色染料组合物，包括固色碱剂、促染剂以及上述的复合活性黑染料。进一步地，所述固色碱剂为氢氧化钠、碳酸钠或碳酸氢钠，所述促染剂为元明粉或氯化钠。
进一步地，还包括防泳移剂、助溶剂、防染盐。更进一步地，所述防泳移剂为海藻酸钠，助溶剂为尿素，防染盐为间硝基苯磺酸钠。本发明的染液用于印染时加入防泳移剂海藻酸钠，是为了减少染料烘干过程中产生泳移；染液中加入适量助溶剂尿素，尿素能促进染料的溶解、纤维的吸湿和溶胀，有利于染料在纤维中的扩散，提高染料的固色率；由于本发明复合活性黑染料中的染料含有偶氮基，易被汽蒸时的还原蒸汽还原而影响得色，为此加入一定量的间硝基苯磺酸钠(防染盐S)，防染盐S是一种温和的氧化剂，能防止还原气体的影响，间硝基苯磺酸钠还可以起到橙色保护剂的作用，保护橙色的式(2)染料。
实施例1
将80份式(1)染料、20份式(2)染料、1份式(3)染料混合后充分机械混匀即可得到本发明的复合活性黑染料，此染料能将纤维材料纤维通过印染成匀染性高，固色率高，高乌黑丰满度及染深性好的黑色。
浸染：分别将1g按实施例1制得的染料，先用适量的水充分溶解，然后定容于250mI容量瓶中，吸取50mI染液与50mI水混合，然后加入5g棉布、6g硫酸钠。然后以1℃/min的升温速度到60℃，保持30分钟后加入2g碳酸钠，再保持60℃染色30min，随后取出被染棉布用非离子型净洗剂沸腾皂煮15min，再用水洗并在70℃左右烘干。
防染印花：将3份实施例1制得的染料撒入100份含有50份5％海藻酸钠增稠剂、27.8份元明粉、20份尿素、1份间硝基苯磺酸钠及1.2份碳酸氢钠的原浆中，用由此制得的印花色浆对棉织物进行印花并干燥，已印花织物用100-102℃饱和蒸汽汽蒸2分钟，然后漂洗；如果需要可在沸腾下皂煮，再次漂洗并干燥。
实施例2
将70份式(1)染料、25份式(2)染料、5份式(3)染料混合后充分机械混匀即可得到本发明的复合活性黑染料，此染料能将纤维材料纤维通过印染成匀染性高，固色率高，高乌黑丰满度及染深性好的黑色。
浸染：将1g按实施例2制得的染料，先用适量的水充分溶解，然后定容于250mI容量瓶中，吸取50mI染液与50mI水混合，然后加入5g棉布、6g硫酸钠。然后以1℃/min的升温速度到60℃，保持30分钟后加入2g碳酸钠，再保持60℃染色30min，随后取出被染棉布用非离子型净洗剂沸腾皂煮15min，再用水洗并在70℃左右烘干。
防染印花：将2份实施例7制得的染料撒入100份含有50份5％海藻酸钠增稠剂、27.8份元明粉、20份尿素、1份间硝基苯磺酸钠及1.2份碳酸氢钠的原浆中，用由此制得的印花色浆对棉织物进行印花并干燥，已印花织物用100-102℃饱和蒸汽汽蒸2分钟，然后漂洗，如果需要可在沸腾下皂煮，再次漂洗并干燥。
实施例3
将60份式(1)染料、35份式(2)染料、5份式(3)染料混合后充分机械混匀即可得到本发明的复合活性黑染料，此染料能将纤维材料纤维通过印染成匀染性高，固色率高，高乌黑丰满度及染深性好的黑色。
浸染：将1g按实施例3制得的染料，先用适量的水充分溶解，然后定容于250mI容量瓶中，吸取50mI染液与50mI水混合，然后加入5g棉布、6g硫酸钠。然后以1℃/min的升温速度到60℃，保持30分钟后加入2g碳酸钠，再保持60℃染色30min，随后取出被染棉布用非离子型净洗剂沸腾皂煮15min，再用水洗并在70℃左右烘干。
防染印花：将3份实施例7制得的染料撒入100份含有50份5％海藻酸钠增稠剂、27.8份元明粉、20份尿素、1份间硝基苯磺酸钠及1.2份碳酸氢钠的原浆中，用由此制得的印花色浆对棉织物进行印花并干燥，已印花织物用100-102℃饱和蒸汽汽蒸2分钟，然后漂洗，如果需要可在沸腾下皂煮，再次漂洗并干燥。
实施例4
将50份式(1)染料、45份式(2)染料、1份式(3)染料混合后充分机械混匀即可得到本发明的复合活性黑染料，此染料能将纤维材料纤维通过印染成匀染性高，固色率高，高乌黑丰满度及染深性好的黑色。
浸染：将1g按实施例4制得的染料，先用适量的水充分溶解，然后定容于250mI容量瓶中，吸取50mI染液与50mI水混合，然后加入5g棉布、6g硫酸钠。然后以1℃/min的升温速度到60℃，保持30分钟后加入2g碳酸钠，再保持60℃染色30min，随后取出被染棉布用非离子型净洗剂沸腾皂煮15min，再用水洗并在70℃左右烘干。
防染印花：将3份实施例4制得的染料撒入100份含有50份5％海藻酸钠增稠剂、27.8份元明粉、20份尿素、1份间硝基苯磺酸钠及1.2份碳酸氢钠的原浆中，用由此制得的印花色浆对棉织物进行印花并干燥，已印花织物用100-102℃饱和蒸汽汽蒸2分钟，然后漂洗，如果需要可在沸腾下皂煮，再次漂洗并干燥。
实施例5
将100份式(1)染料、5份式(2)染料、3份式(3)染料混合后充分机械混匀即可得到本发明的复合活性黑染料，此染料能将纤维材料纤维通过印染成匀染性高，固色率高，高乌黑丰满度及染深性好的黑色。
浸染：将1g按实施例5制得的染料，先用适量的水充分溶解，然后定容于250mI容量瓶中，吸取50mI染液与50mI水混合，然后加入5g棉布、6g硫酸钠。然后以1℃/min的升温速度到60℃，保持30分钟后加入2g碳酸钠，再保持60℃染色30min，随后取出被染棉布用非离子型净洗剂沸腾皂煮15min，再用水洗并在70℃左右烘干。
防染印花：将3份实施例5制得的染料撒入100份含有50份5％海藻酸钠增稠剂、27.8份元明粉、20份尿素、1份间硝基苯磺酸钠及1.2份碳酸氢钠的原浆中，用由此制得的印花色浆对棉织物进行印花并干燥，已印花织物用100-102℃饱和蒸汽汽蒸2分钟，然后漂洗，如果需要可在沸腾下皂煮，再次漂洗并干燥。
实施例6
将70份式(1)染料、25份式(2)染料混合后充分机械混匀即可得到本发明的复合活性黑染料，此染料能将纤维材料纤维通过印染成匀染性高，固色率高，高乌黑丰满度及染深性好的黑色。
浸染：将1g按实施例6制得的染料，先用适量的水充分溶解，然后定容于250mI容量瓶中，吸取50mI染液与50mI水混合，然后加入5g棉布、6g硫酸钠。然后以1℃/min的升温速度到60℃，保持30分钟后加入2g碳酸钠，再保持60℃染色30min，随后取出被染棉布用非离子型净洗剂沸腾皂煮15min，再用水洗并在70℃左右烘干。
防染印花：将3份实施例6制得的染料撒入100份含有50份5％海藻酸钠增稠剂、27.8份元明粉、20份尿素、1份间硝基苯磺酸钠及1.2份碳酸氢钠的原浆中，用由此制得的印花色浆对棉织物进行印花并干燥，已印花织物用100-102℃饱和蒸汽汽蒸2分钟，然后漂洗，如果需要可在沸腾下皂煮，再次漂洗并干燥。
对采用本发明实施例1-6提供的复合活性黑染料染色后的纤维织物的应用性能进行检测，其检测结果下表所示；
Figure BDA0002105172520000101
由上表可以看出，本发明提供的这种复合活性黑染料具有高固色率、高溶解度，以及良好的日晒牢度和水洗牢度。此外，含有式(3)染料的复合活性黑染料使得色织物具有更高的匀染性、更高的固色率和更高牢度性，达到了前所未有的乌黑丰满度及染深性。另外，将上述实施例制得的复合活性黑染料用于轧染及防染印花，得到染色强度高、匀染性好、固色率高、牢度性高、洗涤性、乌黑丰满的黑色，且洗涤性好，解决了现有活性黑染料的洗涤性较差、粘色严重等问题。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (2)

1.一种复合活性黑染料，其特征在于：包括如式(1)所示的染料、如式(2)所示的染料和如式(3)所示的染料，
Figure FDA0002780418250000011
其中，式(1)染料、式(2)染料、式(3)染料按重量份数配比如下：式(1)染料70份，式(2)染料25份，式(3)染料5份，所述复合活性黑染料用于纤维材料的浸染、轧染及防染印花。
2.一种黑色染料组合物，其特征在于：包括固色碱剂、促染剂以及如权利要求1所述的复合活性黑染料，还包括防泳移剂、助溶剂、防染盐；所述固色碱剂为氢氧化钠、碳酸钠或碳酸氢钠，所述促染剂为元明粉或氯化钠，所述防泳移剂为海藻酸钠，助溶剂为尿素，防染盐为间硝基苯磺酸钠。
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