CN116926971A - 一种抗原纤化组合物及在莱赛尔织物上的应用 - Google Patents

一种抗原纤化组合物及在莱赛尔织物上的应用 Download PDF

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CN116926971A
CN116926971A CN202310797214.5A CN202310797214A CN116926971A CN 116926971 A CN116926971 A CN 116926971A CN 202310797214 A CN202310797214 A CN 202310797214A CN 116926971 A CN116926971 A CN 116926971A
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陈卓越
王景
张金波
梁永标
赵发宝
黄尚东
郭炳昌
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DYMATIC CHEMICALS Inc
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Abstract

本发明公开了一种抗原纤化组合物及在莱赛尔织物上的应用，包括交联剂60～90、分散剂20～50、缓冲剂1～5，交联剂为一种或多种复配使用的多官能团型三嗪类化合物，其分子结构通式为：

Description

一种抗原纤化组合物及在莱赛尔织物上的应用
技术领域
本发明涉及染整技术领域，特别是涉及一种抗原纤化组合物及在莱赛尔织物上的应用。
背景技术
目前，降低Lyocell纤维原纤化倾向主要是通过抗原纤化交联剂来实现的。公开号为WO 95/28516A的专利公布了具有多个丙烯酰胺基的交联剂，优选为1,3,5-三丙烯酰-六氢三嗪，有效地减少了溶纺纤维素纤维的原纤化倾向，但该交联剂合成繁琐，价格昂贵，水溶性差且交联后对碱不稳定；公开号为WO 99/19555A的专利报道了取代的二氯三嗪交联剂，优选为2,4-二氯-6-羟基三嗪钠盐，抗原纤化性能良好，此类交联剂含液率较高，用量大，不易长期存储，易发生水解且对酸不稳定。专利CN103306136A是以低聚多元酸和C2-C6多元酸的组合物作为交联剂，通过高温加热提高纤维抗原纤化性能，但因使用工艺复杂，整理后织物泛黄和强力损伤较大，工业化难度较大。此外，这些交联剂均在纤维制成阶段添加，而莱赛尔织物在染整加工过程中的原纤化是目前染整段最严重的问题，也是迫切需要解决的行业难题。因此，研制与应用一款通用性强、高效、色光色变小的水溶性交联剂用于染整交联乃是当务之急。
发明内容
本发明的目的在于提供一种抗原纤化组合物及在莱赛尔织物上的应用，通过选择合适的交联剂与助剂组合，提供一种合成工艺简单、水溶性和稳定性好的组合物及莱赛尔针织物/机织物的抗原纤化处理方法，且该组合物不会在碱性和元明粉促染的条件下析出，可直接用于染色同浴交联，无需改变原来染色工艺，使用方便，大大缩短了工艺流程，对染色深度影响小。采用该组合物整理的莱赛尔织物，具有抗原纤化性能优异、透染和均匀性优异、织物色光色变小、安全无甲醛等特点。
为解决上述技术问题，本发明是通过以下技术方案实现的：
一种抗原纤化组合物，包括交联剂、分散剂、缓冲剂，其特征在于，其重量份组分是，交联剂：60～90，分散剂：20～50，缓冲剂：1～5，由上述组分混合后喷雾干燥制得固态的抗原纤化组合物；
交联剂为一种或多种复配使用的多官能团型三嗪类化合物，其分子结构通式为：
其中，活性基X和Y是相同或是不同的，选自F、Cl、烟酸、异烟酸、三乙烯二胺、4-β-羟乙砜基硫酸酯苯胺-2-磺酸、对氨基苯基-β-羟乙基砜硫酸酯、间氨基苯基-β-羟乙基砜硫酸酯、2-(2-氨基乙基)砜基乙醇硫酸酯、2-[(氯乙基)砜基]乙醇盐酸盐的一种或多种；
R为改性基或活性基，选自F、Cl、OH、对氨基苯磺酸、间氨基苯磺酸、对氨基苯甲酸、2,5-二磺酸苯胺的一种或多种，用来调节交联剂的直接性和水溶性，对反应也有一定改善；
A为连接基或架桥基，选自对苯二胺、间苯二胺、邻苯二胺、2,4-二氨基苯磺酸、2,5-二氨基苯磺酸、间苯二胺双磺酸、乙二胺、丙二胺、己二胺、聚乙二醇、聚醚胺的一种或多种。
上述的抗原纤化组合物，所述分散剂是烷基酚聚氧乙烯醚、脂肪胺聚氧乙烯醚、脂肪醇聚氧乙烯醚、脂肪醇聚氧乙烯醚硫酸钠、脂肪醇聚氧乙烯醚羧酸钠、异构醇聚氧乙烯醚、仲烷基磺酸钠、十二烷基苯磺酸钠、十二烷基硫酸钠、甲基萘磺酸甲醛缩合物、亚甲基二萘磺酸钠、苄基萘磺酸甲醛缩合物、烷基苯磺酸甲醛缩合物、木质素磺酸钠中的一种或多种。能够提高交联剂的溶解性、耐盐碱稳定性和纤维的渗透性。
上述的抗原纤化组合物，所述缓冲剂选自三(羟甲基)氨基甲烷+乙二胺四乙酸、三(羟甲基)氨基甲烷+乙二胺四乙酸二钠、三乙醇胺+乙二胺四乙酸二钠、丁二酸+己内酰胺、磷酸氢二钠+磷酸二氢钠、磷酸氢二钠+磷酸二氢钾组合中的一种。通过采用上述技术方案，交联剂为多活性基，反应性和交联率高，组合物中存在两种耐酸碱不同的活性基，使交联后纤维-交联剂键稳定性好，且该商品化组合物可以直接用于染色同浴交联，不会从染液中析出影响染色，透染和均匀性优异。
上述的抗原纤化组合物在莱赛尔织物上的应用：采用染色同浴交联，浴比1：4-10，前处理后织物，加入抗原纤化组合物2-5g/L，运转均匀，加入染料运转均匀，加入元明粉，继续运转20min，升温至60-80℃，分三次加入纯碱，继续运转40-60min，出缸、水洗、中和、烘干，即可制得抗原纤化的莱赛尔织物。
本发明具有以下有益效果：
(1)本发明采用多活性基交联剂的混合物为主体，具备交联后耐碱的一氯/二氯均三嗪/季铵阳离子和耐酸的乙烯砜官能团，其结构在中性条件下具有较好的稳定性，一个活性基团被水解，另一个活性基团仍与织物发生反应，反应性较高，且耐酸型和耐碱型的活性基使交联后织物-交联剂键稳定性好。
(2)本申请通过交联剂与分散剂组合，增加了交联剂结构亲水性和扩散性，使交联剂与织物内部充分接触反应，从而提高了交联率。且分散剂提供的空间位阻和静电斥力有利于交联剂分子的耐盐碱稳定性，工作液可以在一小时内保持澄清透明，防止交联剂水溶性不足或因遇到染液的盐碱后缔合度增加从而析出，导致不均匀的处理效果的情况。
(3)本发明组合物适用于莱赛尔针织物的先交联后染色工艺或染色同浴交联，以及莱赛尔机织物的轧染汽蒸工艺，染色和抗原纤化的同浴进行，大大缩短了工艺流程，节约时间和能源。交联设备为常规染整设备，工厂现有设备不需要改装，染色工艺流程不需要做出更改，客户使用方便，容易操作。
(4)本发明使用的交联剂合成工艺简单，价格便宜，通过对刚制备出的交联剂溶液进行加分散剂、缓冲剂打浆处理，标准化喷雾干燥后进行存储，交联剂的存放保质期变长，可以存放一年甚至更长时间，产品的强度基本没有变化。
(5)抗原纤化效果好，耐洗性好，对染色深度影响小，无甲醛释放，避免了对人体和环境的危害。
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作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。
实施例1：
1、抗原纤化组合物：
(1)按下述各组分重量百分比选取原料：
其中交联剂A的结构式见表8。
(2)所述抗原纤化组合物配制方法，具体为：先用碳酸钠调节反应到终点的交联剂A浆液的pH为5-6，然后在22％含量的交联剂A的反应液中加入十二烷基苯磺酸钠，亚甲基二萘磺酸钠NNO，丁二酸，己内酰胺，在15-20℃充分搅拌1小时，然后将浆液转入喷塔储槽，喷雾干燥后包装，即得抗原纤化组合物I-1。
2、抗原纤化交联整理：
浴比1：8，前处理后织物，加入抗原纤化组合物3g/L，运转均匀，加入活性黄3RS3.5g/L、活性黑KN-B 2g/L，运转均匀，加入元明粉40g/L，继续运转20min，升温至60℃，分三次加入纯碱20g/L，继续运转40min，出缸、水洗、中和、烘干，即可制得抗原纤化的莱赛尔织物。
实施例2～6:
按照上述实施例1所述的方法，不同的是，采用下表1中等质量分数的原料组分交联剂、分散剂、缓冲剂分别代替实施例1中的组分进行组合，可制得本发明所述的抗原纤化组合物：
表1实施例2～6的抗原纤化组合物
交联剂的结构见表8。
实施例7
1、抗原纤化组合物：
(1)按下述各组分重量百分比选取原料：
其中交联剂A和交联剂G的结构式见表8。
(2)所述抗原纤化组合物配制方法，具体为：先用碳酸钠调节反应到终点的交联剂A浆液的pH为5-6，然后在15％含量的交联剂A的反应液中加入交联剂G固体，十二烷基苯磺酸钠，亚甲基二萘磺酸钠NNO，丁二酸，己内酰胺，在15-20℃充分搅拌1小时，然后将浆液转入喷塔储槽，喷雾干燥后包装，即得抗原纤化组合物I-7。
2、抗原纤化交联整理：
浴比1：8，前处理后织物，加入抗原纤化组合物3g/L，运转均匀，加入活性黄3RS3.5g/L、活性黑KN-B 2g/L，运转均匀，加入元明粉40g/L，继续运转20min，升温至60℃，分三次加入纯碱20g/L，继续运转40min，出缸、水洗、中和、烘干，即可制得抗原纤化的莱赛尔织物。
实施例8～12:
按照上述实施例7所述的方法，不同的是，采用下表2中等质量分数的原料组分交联剂、分散剂、缓冲剂分别代替实施例7中的组分进行组合，可制得本发明所述的抗原纤化组合物：
表2实施例8～12的抗原纤化组合物
交联剂结构见表8。
对比例1
本对比例与本实施例7的不同之处在于，本对比例的组合物，由以下重量份数的原料制成：
1、抗原纤化组合物：
(1)按下述各组分重量百分比选取原料：
(2)所述抗原纤化组合物配制方法，具体为：先用碳酸钠调节反应到终点的交联剂A浆液的pH为5-6，然后在15％含量的交联剂A反应液中加入交联剂G固体，丁二酸，己内酰胺，在15-20℃充分搅拌1小时，然后将浆液转入喷塔储槽，喷雾干燥后包装，即得抗原纤化组合物I-13。
2、抗原纤化交联整理：
浴比1：8，前处理后织物，加入抗原纤化组合物2.4g/L(交联剂含量与实施例一致)，运转均匀，加入活性黄3RS 3.5g/L、活性黑KN-B 2g/L，运转均匀，加入元明粉40g/L，继续运转20min，升温至60℃，分三次加入纯碱20g/L，继续运转40min，出缸、水洗、中和、烘干，即可制得抗原纤化的莱赛尔织物。
对比例2～6:
按照上述对比例1所述的方法，不同的是，采用下表3中等质量分数的原料组分交联剂、分散剂、缓冲剂分别代替比例1中的组分进行组合，可制得本发明所述的抗原纤化组合物：
表3对比例2～6的抗原纤化组合物
性能检测试验
1.耐盐碱测试：100ml去离子水中，分别加入2g上述实施例1-12和对比例1-6得到的抗原纤化组合物，升温至60℃，保温搅拌10min。保温取样，搅拌下加入盐碱(使溶液中含有20g/L碳酸钠和40g/L硫酸钠)，使用30％烧碱溶液调pH＝12。在60℃下，每隔5min取样，用斑点法观察其溶解情况，至组合物在滤纸上有明显晕圈为止，计算耐盐碱时间，结果如表4所示：
表4抗原纤化组合物的耐盐碱测试结果
由上表4得出，按本发明所述方法制得的抗原纤化组合物可以明显延长交联剂的耐盐碱时间，提高交联剂的溶解度，可以防止交联剂在同浴染色时从染液中析出。
2.织物交联染色后性能效果检测：大量的洗涤实验发现，中深色的莱赛尔织物洗后会产生白霜外观甚至布面结白球，令布面外观效果产生变化。因此，本发明针对织物原纤化程度的判定方法，是测试织物的抗起毛起球等级、色变、染色深度K/S值差，空白样为未经交联处理的织物，结果如表5所示。此外，表6为莱赛尔织物同浴染色后的扫描电子显微镜图像。
表5织物交联染色后性能效果检测结果
表6莱赛尔织物交联染色后电镜测试结果列表
由表5和表6可以看出，交联组合物整理后Lyocell织物的抗起毛起球效果得到改善，可以达到4级，且交联洗后色变也减小，布面效果明显无发白、发旧、色变、毛羽等情况，电镜下抗原纤化效果明显；交联剂与分散剂相互配合，增加了交联剂结构亲水性和扩散性，使纤维与交联剂反应和交联更加充分，透染和均匀性优异，从而使得整理后的织物抗原纤化效果相对于未加入分散剂的对比例(工作液肉眼可见浑浊，布面出现部分原纤化)来说，增加较为明显。
3.交联后耐酸碱测试：130/100/60℃下测试方法：浴比1：10，室温加入原纤化整理后织物，工作液调不同pH值：pH＝2、3、4、5、6、7、8、9、10、11、12、13；加热至130/100/60℃，保温40min，水洗，烘干，测试抗起球起毛等级和色变。室温(25℃)下耐碱测试方法：将织物加入不同浓度的烧碱溶液中浸泡1min，稀碱中冲洗，水洗，烘干，测试抗起球起毛等级和色变。抗起球起毛等级为3-4级和色变为4级以上，表示耐受此条件下酸碱值，结果如表7所示。
表7抗原纤化相关性能的测试结果
由表7可以看出，两种耐酸碱不同的活性基组合使交联后织物-交联剂键稳定性好，具有优良的酸碱耐受性，可以满足染整各个应用场景需求。
表8：Key Substances in Patent
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以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为所述的具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。

Claims (4)

1.一种抗原纤化组合物，包括交联剂、分散剂、缓冲剂，其特征在于，其重量份组分是，交联剂：60～90，分散剂：20～50，缓冲剂：1～5，由上述组分混合后喷雾干燥制得固态的抗原纤化组合物；
交联剂为一种或多种复配使用的多官能团型三嗪类化合物，其分子结构通式为：
其中，活性基X和Y是相同或是不同的，选自F、Cl、烟酸、异烟酸、三乙烯二胺、4-β-羟乙砜基硫酸酯苯胺-2-磺酸、对氨基苯基-β-羟乙基砜硫酸酯、间氨基苯基-β-羟乙基砜硫酸酯、2-(2-氨基乙基)砜基乙醇硫酸酯、2-[(氯乙基)砜基]乙醇盐酸盐的一种或多种；
R为改性基或活性基，选自F、Cl、OH、对氨基苯磺酸、间氨基苯磺酸、对氨基苯甲酸、2,5-二磺酸苯胺的一种或多种；
A为连接基或架桥基，选自对苯二胺、间苯二胺、邻苯二胺、2,4-二氨基苯磺酸、2,5-二氨基苯磺酸、间苯二胺双磺酸、乙二胺、丙二胺、己二胺、聚乙二醇、聚醚胺的一种或多种。
2.根据权利要求1所述的抗原纤化组合物，其特征在于：所述分散剂是烷基酚聚氧乙烯醚、脂肪胺聚氧乙烯醚、脂肪醇聚氧乙烯醚、脂肪醇聚氧乙烯醚硫酸钠、脂肪醇聚氧乙烯醚羧酸钠、异构醇聚氧乙烯醚、仲烷基磺酸钠、十二烷基苯磺酸钠、十二烷基硫酸钠、甲基萘磺酸甲醛缩合物、亚甲基二萘磺酸钠、苄基萘磺酸甲醛缩合物、烷基苯磺酸甲醛缩合物、木质素磺酸钠中的一种或多种。
3.根据权利要求1所述的抗原纤化组合物，其特征在于：所述缓冲剂选自三(羟甲基)氨基甲烷+乙二胺四乙酸、三(羟甲基)氨基甲烷+乙二胺四乙酸二钠、三乙醇胺+乙二胺四乙酸二钠、丁二酸+己内酰胺、磷酸氢二钠+磷酸二氢钠、磷酸氢二钠+磷酸二氢钾组合中的一种。
4.根据权利要求1所述的抗原纤化组合物在莱赛尔织物上的应用，其特征在于：采用染色同浴交联，浴比1：4-10，前处理后织物，加入抗原纤化组合物2-5g/L，运转均匀，加入染料运转均匀，加入元明粉，继续运转20min，升温至60-80℃，分三次加入纯碱，继续运转40-60min，出缸、水洗、中和、烘干，即可制得抗原纤化的莱赛尔织物。
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