CN117026653A - 一种耐水洗的活性黑染料及其生产方法 - Google Patents

一种耐水洗的活性黑染料及其生产方法 Download PDF

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CN117026653A
CN117026653A CN202311005016.7A CN202311005016A CN117026653A CN 117026653 A CN117026653 A CN 117026653A CN 202311005016 A CN202311005016 A CN 202311005016A CN 117026653 A CN117026653 A CN 117026653A
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dye
reactive black
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谢宏斌
赵学东
曾莹
贺瑾铃
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Foshan Xingyuan Dyeing And Chemical Co ltd
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Abstract

本发明公开了一种耐水洗的活性黑染料及其生产方法。本发明中，染料的内部添加了季铵盐‑52，含有多个羟基能够参与聚氨酯的聚合反应，含有季铵盐结构，能够与可交联颜料之间形成静电吸附作用，提高染料在棉纤维上的上染率、颜色深度和耐磨擦牢固，从而使得制得的染料耐水洗牢固度为5级，具有优异的耐水洗特性，从而提高了制得的布料的耐水洗度，增加了布料的耐用性。染料的内部添加了防紫外线剂和阻燃剂，从而使得染料得到的布料在之后的使用过程中，当处于光线较强的室外环境使用时，布料的抗紫外线能力得到了增强，从而提高了对于人体的保护性，同时当处于火灾意外情况下，也会尽量使得布料不会轻易燃烧，从而增加了对于人体的保护性。

Description

一种耐水洗的活性黑染料及其生产方法
技术领域
本发明属于活性黑染料技术领域，具体为一种耐水洗的活性黑染料及其生产方法。
背景技术
活性染料以色泽鲜艳、色谱齐全，应用简便、价格较廉、适应性强、牢度优良而著称，现已发展成为棉用染料中最重要的染料类别，成为世界重点发展和关注的一类染料。这类染料分子中含有能与纤维素纤维发生化学反应的基团，染色时染料与纤维素纤维反应，二者之间形成共价键而固着在织物上，使耐洗和耐摩擦牢度优于其他染料；传统法活性黑为几种染料单独合成，喷雾干燥后再进拼混设备混拼均匀，或通过湿拼技术的直接从染料溶液复配，色光调整好再进行喷雾干燥。
但是常见的染料在使用过程中，染料的阻燃效果不够好，从而使得制得的布料在使用过程中，安全性不够高。
发明内容
本发明的目的在于：为了解决上述提出的问题，提供一种耐水洗的活性黑染料及其生产方法。
本发明采用的技术方案如下：一种耐水洗的活性黑染料及其生产方法，所述耐水洗的活性黑染料及其生产方法包括以下步骤：
S1:将磺甲基J酸加入到三聚氯氰打浆液中，打浆后加入混合碱溶液，调节并维持pH3.5～4，进行缩合反应，得到浓缩染料液A；
S2:将亚硫酸钠溶液缓慢加入至预制重氮液中重氮化反应2-3h，得到重氮盐溶液B；
S3:将H酸加入水中搅拌打浆1-2h，然后将除亚硝酸钠后的重氮盐分批加入，恒温反应得到酸性偶合液C；
S4:将氢氧化钠溶液加入至酸性偶合液中直至pH为6，然后加入缓释苏打恒温恒pH搅拌反应，得到碱性耦合液D；
S5:进行复合配方制剂的称取，称取消泡剂10～12重量份、防紫外线剂10～15重量份、阻燃剂13～17重量份、润湿剂11～15重量份、媒染剂11～15重量份、季铵盐无醛固色剂11～15重量份和植物基抗菌剂12～18重量份；
S6:将步骤S5中称量好的消泡剂、防紫外线剂、抗菌剂、润湿剂、媒染剂、季铵盐无醛固色剂和植物基抗菌剂充分混合，之后再称量碱性耦合液D200～280重量份，将其置于搅拌反应容器内部进行搅拌混合，得到活性黑染料预制液E；
S7:将步骤S6制得的活性黑染料预制液E快速降温，并过滤得到浓缩液，然后将滤液喷雾干燥得到耐水洗的活性黑染料；
S8:对步骤S7制得的耐水洗的活性黑染料进行保存包装，即可结束整个耐水洗的活性黑染料的制备。
在一优选的实施方式中，所述步骤S1中，三聚氯氰打浆液由三聚氯氰与分散剂加入到冰水混合物中打浆得到。
在一优选的实施方式中，所述分散剂为木质素磺酸钠、分散剂NNO或分散剂MF。
在一优选的实施方式中，所述步骤S1中，混合碱溶液的浓度为12wt％；所述混合碱为纯碱与小苏打，纯碱与小苏打的质量比为11:19。
在一优选的实施方式中，所述步骤S2中，亚硝酸钠溶液的浓度为26-28％，温度为5-10℃，所述重氮化反应采用刚果红试纸监控。
在一优选的实施方式中，所述步骤S4中，氢氧化钠溶液的质量浓度为10-12％。
在一优选的实施方式中，所述步骤S5中，所述媒染剂包括：十二水合硫酸铝钾0.4-0.9份、钾明矾0.9-1.2份、丹宁0.2-0.5份、硫酸铝钾0.8-1.3份、硫酸铜0.2-0.7份、硫酸钴0.3-0.7份。
在一优选的实施方式中，所述步骤S5中，阻燃剂为红磷微胶囊、季戊四醇双磷酸酯、三苯基磷酸酯、二苯基磷酸酯、聚磷酸铵、磷酸氢二铵、磷酸二胍、氰尿酸三聚氰胺中的至少两种的复配混合物。
在一优选的实施方式中，所述步骤S5中，植物基抗菌剂包括：桧柏6重量份、艾蒿5重量份、五味子7重量份、艾叶粉8重量份和纳米抗菌银离子15重量份。
在一优选的实施方式中，所述步骤S5中，防紫外线剂包括二氧化硅50％～70％；硼砂3％～7％；2，4-二羟基二苯甲酮10％～15％；N，N-二正丁基二硫代氨基甲酸镍5％～10％；胍类抗菌剂1％～3％；双酚A二缩水甘油醚3％～8％；烷基季铵盐0.2％～1％；铝锆酸酯偶联剂0.5％～1.2％；对氯邻硝基苯胺0.3％～0.7％。
综上所述，由于采用了上述技术方案，本发明的有益效果是：
1、本发明中，染料的内部添加了季铵盐-52，含有多个羟基能够参与聚氨酯的聚合反应，含有季铵盐结构，能够与可交联颜料之间形成静电吸附作用，提高染料在棉纤维上的上染率、颜色深度和耐磨擦牢固，从而使得制得的染料耐水洗牢固度为5级，具有优异的耐水洗特性，从而提高了制得的布料的耐水洗度，增加了布料的耐用性。
2、本发明中，染料的内部添加了防紫外线剂和阻燃剂，从而使得染料得到的布料在之后的使用过程中，当处于光线较强的室外环境使用时，布料的抗紫外线能力得到了增强，从而提高了对于人体的保护性，同时当处于火灾意外情况下，也会尽量使得布料不会轻易燃烧，从而增加了对于人体的保护性。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例，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作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例一：
一种耐水洗的活性黑染料及其生产方法，所述耐水洗的活性黑染料及其生产方法包括以下步骤：
S1:将磺甲基J酸加入到三聚氯氰打浆液中，打浆后加入混合碱溶液，调节并维持pH3.5～4，进行缩合反应，得到浓缩染料液A；
S2:将亚硫酸钠溶液缓慢加入至预制重氮液中重氮化反应2-3h，得到重氮盐溶液B；
S3:将H酸加入水中搅拌打浆1-2h，然后将除亚硝酸钠后的重氮盐分批加入，恒温反应得到酸性偶合液C；
S4:将氢氧化钠溶液加入至酸性偶合液中直至pH为6，然后加入缓释苏打恒温恒pH搅拌反应，得到碱性耦合液D；
S5:进行复合配方制剂的称取，称取消泡剂10重量份、防紫外线剂10重量份、阻燃剂13重量份、润湿剂11重量份、媒染剂11重量份、季铵盐无醛固色剂11重量份和植物基抗菌剂12重量份；
S6:将步骤S5中称量好的消泡剂、防紫外线剂、抗菌剂、润湿剂、媒染剂、季铵盐无醛固色剂和植物基抗菌剂充分混合，之后再称量碱性耦合液D200～280重量份，将其置于搅拌反应容器内部进行搅拌混合，得到活性黑染料预制液E；
S7:将步骤S6制得的活性黑染料预制液E快速降温，并过滤得到浓缩液，然后将滤液喷雾干燥得到耐水洗的活性黑染料；
S8:对步骤S7制得的耐水洗的活性黑染料进行保存包装，即可结束整个耐水洗的活性黑染料的制备。
所述步骤S1中，三聚氯氰打浆液由三聚氯氰与分散剂加入到冰水混合物中打浆得到。
所述分散剂为木质素磺酸钠、分散剂NNO或分散剂MF。
所述步骤S1中，混合碱溶液的浓度为12wt％；所述混合碱为纯碱与小苏打，纯碱与小苏打的质量比为11:19。
所述步骤S2中，亚硝酸钠溶液的浓度为26-28％，温度为5-10℃，所述重氮化反应采用刚果红试纸监控。
所述步骤S4中，氢氧化钠溶液的质量浓度为10-12％。
所述步骤S5中，所述媒染剂包括：十二水合硫酸铝钾0.4-0.9份、钾明矾0.9-1.2份、丹宁0.2-0.5份、硫酸铝钾0.8-1.3份、硫酸铜0.2-0.7份、硫酸钴0.3-0.7份。
所述步骤S5中，阻燃剂为红磷微胶囊、季戊四醇双磷酸酯、三苯基磷酸酯、二苯基磷酸酯、聚磷酸铵、磷酸氢二铵、磷酸二胍、氰尿酸三聚氰胺中的至少两种的复配混合物。
所述步骤S5中，植物基抗菌剂包括：桧柏6重量份、艾蒿5重量份、五味子7重量份、艾叶粉8重量份和纳米抗菌银离子15重量份。
所述步骤S5中，防紫外线剂包括二氧化硅50％～70％；硼砂3％～7％；2，4-二羟基二苯甲酮10％～15％；N，N-二正丁基二硫代氨基甲酸镍5％～10％；胍类抗菌剂1％～3％；双酚A二缩水甘油醚3％～8％；烷基季铵盐0.2％～1％；铝锆酸酯偶联剂0.5％～1.2％；对氯邻硝基苯胺0.3％～0.7％。
本发明中，染料的内部添加了季铵盐-52，含有多个羟基能够参与聚氨酯的聚合反应，含有季铵盐结构，能够与可交联颜料之间形成静电吸附作用，提高染料在棉纤维上的上染率、颜色深度和耐磨擦牢固，从而使得制得的染料耐水洗牢固度为5级，具有优异的耐水洗特性，从而提高了制得的布料的耐水洗度，增加了布料的耐用性。
本发明中，染料的内部添加了防紫外线剂和阻燃剂，从而使得染料得到的布料在之后的使用过程中，当处于光线较强的室外环境使用时，布料的抗紫外线能力得到了增强，从而提高了对于人体的保护性，同时当处于火灾意外情况下，也会尽量使得布料不会轻易燃烧，从而增加了对于人体的保护性。
实施例二：
一种耐水洗的活性黑染料及其生产方法，所述耐水洗的活性黑染料及其生产方法包括以下步骤：
S1:将磺甲基J酸加入到三聚氯氰打浆液中，打浆后加入混合碱溶液，调节并维持pH3.5～4，进行缩合反应，得到浓缩染料液A；
S2:将亚硫酸钠溶液缓慢加入至预制重氮液中重氮化反应2-3h，得到重氮盐溶液B；
S3:将H酸加入水中搅拌打浆1-2h，然后将除亚硝酸钠后的重氮盐分批加入，恒温反应得到酸性偶合液C；
S4:将氢氧化钠溶液加入至酸性偶合液中直至pH为6，然后加入缓释苏打恒温恒pH搅拌反应，得到碱性耦合液D；
S5:进行复合配方制剂的称取，称取消泡剂12重量份、防紫外线剂15重量份、阻燃剂17重量份、润湿剂15重量份、媒染剂15重量份、季铵盐无醛固色剂15重量份和植物基抗菌剂18重量份；
S6:将步骤S5中称量好的消泡剂、防紫外线剂、抗菌剂、润湿剂、媒染剂、季铵盐无醛固色剂和植物基抗菌剂充分混合，之后再称量碱性耦合液D200～280重量份，将其置于搅拌反应容器内部进行搅拌混合，得到活性黑染料预制液E；
S7:将步骤S6制得的活性黑染料预制液E快速降温，并过滤得到浓缩液，然后将滤液喷雾干燥得到耐水洗的活性黑染料；
S8:对步骤S7制得的耐水洗的活性黑染料进行保存包装，即可结束整个耐水洗的活性黑染料的制备。
所述步骤S1中，三聚氯氰打浆液由三聚氯氰与分散剂加入到冰水混合物中打浆得到。
所述分散剂为木质素磺酸钠、分散剂NNO或分散剂MF。
所述步骤S1中，混合碱溶液的浓度为12wt％；所述混合碱为纯碱与小苏打，纯碱与小苏打的质量比为11:19。
所述步骤S2中，亚硝酸钠溶液的浓度为26-28％，温度为5-10℃，所述重氮化反应采用刚果红试纸监控。
所述步骤S4中，氢氧化钠溶液的质量浓度为10-12％。
所述步骤S5中，所述媒染剂包括：十二水合硫酸铝钾0.4-0.9份、钾明矾0.9-1.2份、丹宁0.2-0.5份、硫酸铝钾0.8-1.3份、硫酸铜0.2-0.7份、硫酸钴0.3-0.7份。
所述步骤S5中，阻燃剂为红磷微胶囊、季戊四醇双磷酸酯、三苯基磷酸酯、二苯基磷酸酯、聚磷酸铵、磷酸氢二铵、磷酸二胍、氰尿酸三聚氰胺中的至少两种的复配混合物。
所述步骤S5中，植物基抗菌剂包括：桧柏6重量份、艾蒿5重量份、五味子7重量份、艾叶粉8重量份和纳米抗菌银离子15重量份。
所述步骤S5中，防紫外线剂包括二氧化硅50％～70％；硼砂3％～7％；2，4-二羟基二苯甲酮10％～15％；N，N-二正丁基二硫代氨基甲酸镍5％～10％；胍类抗菌剂1％～3％；双酚A二缩水甘油醚3％～8％；烷基季铵盐0.2％～1％；铝锆酸酯偶联剂0.5％～1.2％；对氯邻硝基苯胺0.3％～0.7％。
本发明中，染料的内部添加了季铵盐-52，含有多个羟基能够参与聚氨酯的聚合反应，含有季铵盐结构，能够与可交联颜料之间形成静电吸附作用，提高染料在棉纤维上的上染率、颜色深度和耐磨擦牢固，从而使得制得的染料耐水洗牢固度为5级，具有优异的耐水洗特性，从而提高了制得的布料的耐水洗度，增加了布料的耐用性。
本发明中，染料的内部添加了防紫外线剂和阻燃剂，从而使得染料得到的布料在之后的使用过程中，当处于光线较强的室外环境使用时，布料的抗紫外线能力得到了增强，从而提高了对于人体的保护性，同时当处于火灾意外情况下，也会尽量使得布料不会轻易燃烧，从而增加了对于人体的保护性。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。

Claims (10)

1.一种耐水洗的活性黑染料及其生产方法，其特征在于：所述耐水洗的活性黑染料及其生产方法包括以下步骤：
S1:将磺甲基J酸加入到三聚氯氰打浆液中，打浆后加入混合碱溶液，调节并维持pH3.5～4，进行缩合反应，得到浓缩染料液A；
S2:将亚硫酸钠溶液缓慢加入至预制重氮液中重氮化反应2-3h，得到重氮盐溶液B；
S3:将H酸加入水中搅拌打浆1-2h，然后将除亚硝酸钠后的重氮盐分批加入，恒温反应得到酸性偶合液C；
S4:将氢氧化钠溶液加入至酸性偶合液中直至pH为6，然后加入缓释苏打恒温恒pH搅拌反应，得到碱性耦合液D；
S5:进行复合配方制剂的称取，称取消泡剂10～12重量份、防紫外线剂10～15重量份、阻燃剂13～17重量份、润湿剂11～15重量份、媒染剂11～15重量份、季铵盐无醛固色剂11～15重量份和植物基抗菌剂12～18重量份；
S6:将步骤S5中称量好的消泡剂、防紫外线剂、抗菌剂、润湿剂、媒染剂、季铵盐无醛固色剂和植物基抗菌剂充分混合，之后再称量碱性耦合液D200～280重量份，将其置于搅拌反应容器内部进行搅拌混合，得到活性黑染料预制液E；
S7:将步骤S6制得的活性黑染料预制液E快速降温，并过滤得到浓缩液，然后将滤液喷雾干燥得到耐水洗的活性黑染料；
S8:对步骤S7制得的耐水洗的活性黑染料进行保存包装，即可结束整个耐水洗的活性黑染料的制备。
2.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S1中，三聚氯氰打浆液由三聚氯氰与分散剂加入到冰水混合物中打浆得到。
3.如权利要求2所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述分散剂为木质素磺酸钠、分散剂NNO或分散剂MF。
4.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S1中，混合碱溶液的浓度为12wt％；所述混合碱为纯碱与小苏打，纯碱与小苏打的质量比为11:19。
5.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S2中，亚硝酸钠溶液的浓度为26-28％，温度为5-10℃，所述重氮化反应采用刚果红试纸监控。
6.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S4中，氢氧化钠溶液的质量浓度为10-12％。
7.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S5中，所述媒染剂包括：十二水合硫酸铝钾0.4-0.9份、钾明矾0.9-1.2份、丹宁0.2-0.5份、硫酸铝钾0.8-1.3份、硫酸铜0.2-0.7份、硫酸钴0.3-0.7份。
8.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S5中，阻燃剂为红磷微胶囊、季戊四醇双磷酸酯、三苯基磷酸酯、二苯基磷酸酯、聚磷酸铵、磷酸氢二铵、磷酸二胍、氰尿酸三聚氰胺中的至少两种的复配混合物。
9.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S5中，植物基抗菌剂包括：桧柏6重量份、艾蒿5重量份、五味子7重量份、艾叶粉8重量份和纳米抗菌银离子15重量份。
10.如权利要求1所述的一种耐水洗的活性黑染料及其生产方法，其特征在于：所述步骤S5中，防紫外线剂包括二氧化硅50％～70％；硼砂3％～7％；2，4-二羟基二苯甲酮10％～15％；N，N-二正丁基二硫代氨基甲酸镍5％～10％；胍类抗菌剂1％～3％；双酚A二缩水甘油醚3％～8％；烷基季铵盐0.2％～1％；铝锆酸酯偶联剂0.5％～1.2％；对氯邻硝基苯胺0.3％～0.7％。
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