CN105603719A - 化学还原法易染聚酰亚胺面料的制备方法 - Google Patents
化学还原法易染聚酰亚胺面料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种化学还原法易染聚酰亚胺面料的制备方法，包括以下步骤：（1）聚酰亚胺面料碱性还原性溶液处理：将聚酰亚胺面料放入盛有碱性还原性溶液的抗压容器罐中，压力为0.1-0.2Mpa，温度为100-110℃，处理时间为10-60min；（2）聚酰亚胺面料洗涤：将经过碱性还原性溶液处理的聚酰亚胺面料取出水洗6-10次并进行烘干，烘干在70-100℃烘箱中进行，烘干时间为1-2h。所述碱性还原性溶液为氢氧化钠或碳酸钠与还原剂的混合溶液，其中氢氧化钠或碳酸钠与还原剂的摩尔比为2:1，氢氧化钠或碳酸钠的摩尔百分浓度为0.1-10%，还原剂的摩尔百分浓度为0.05-5%。本发明在不损害聚酰亚胺面料物理和化学性能的基础上使聚酰亚胺面料由不可染色变为可染色面料，解决了聚酰亚胺难以染色的问题。
Description
技术领域
本发明涉及一种化学还原法易染聚酰亚胺面料的制备方法，属于功能纺织材料技术领域。
背景技术
聚酰亚胺机械性能良好，而且既可以承受高达400℃的温度，又能在-200℃以下的超低温保持正常性能，还拥有很好的绝缘性能，可以说整体性能十分良好。由于这些良好的性能，聚酰亚胺的发展前景也是十分可观。
根据组成聚酰亚胺的单体的不同，聚酰亚胺可以分为不含苯环的脂肪族聚酰亚胺、一种单体含有苯环的半芳香族聚酰亚胺和两种单体均含苯环的芳香族聚酰亚胺三种。而根据热性质，则可分为热塑性和热固性聚酰亚胺。
聚酰亚胺是一类分子主链上含有酰亚胺环结构(式1)的聚合物。芳香族聚酰亚胺可以由多种多样的单体组成，这使其结构呈现多样化。而聚酰亚胺同时又拥有优秀的综合性能，这是许多高分子材料望尘莫及的。而多种多样的合成方法和加工手段，使得聚酰亚胺可以大量生产而不受条件限制。以上多种优点使聚酰亚胺材料有着宽阔的应用面，而在一些高科技领域如航空航天、电子工业、纳米、激光等，聚酰亚胺面料更是大展光彩。
芳香族聚酰亚胺由于其独特的化学结构而具有优异的综合性能，主要包括：良好的热稳定性，由3,3′,4,4′-联苯四甲酸二酐(BPDA)与对苯二胺(PDA)所制备的聚酰亚胺的热分解温度高达600℃[3]；优异的耐低温性能，即使在液氦中也不会脆裂；良好的尺寸稳定性和力学性能；优异的抗辐射性；良好的绝缘性和介电性；优异的阻燃性以及低毒和良好的生物相容性。聚酰亚胺所具有的优异性能使其得到了人们的广泛关注，开发出多种形式的聚酰亚胺产品；目前已成功商业化生产的聚酰亚胺产品有：薄膜、纤维和工程塑料等。
在纺织领域，聚酰亚胺纤维拥有良好好前景，因其有较佳可纺性能，结合其自身的优良性能，可以应用于特殊服装领域。聚酰亚胺的良好的隔热性能使得由它制作的隔热防护服穿在身上十分舒适，且皮肤与其适应性能较佳。由于聚酰亚胺的稳定性能，有聚酰亚胺面料制成的衣物使用时间也长，不易变形，又很安全。同时，聚酰亚胺面料在劳动防护服方面的应用量、需求量都很大，我国许多特殊的工作岗位，在工作时都需要劳动防护服，这方面的需求量每年超过35万套。制作这么多的劳动防护服，每年需要的有着耐高温阻燃性能的服装用纤维高达300吨左右。可以说聚酰亚胺在服装方面的应用有着很大的优势。
在无纺布制造方面，聚酰亚胺纤维也大有作为。装甲部队兵、赛车手、飞行员等特殊行业在工作中需要大量的防火阻燃纤维制作的衣服，有聚酰亚胺面料纺制的无纺布是应用于这一块的最佳材料。聚酰亚胺纤维制造的无纺布往往结合纳米技术，形成高科技纳米产品，具有保暖性能，又很舒服，可以用在军用服装、防生化武器特种服装、高效烟雾防护面罩等国防领域，也可以走进人民群众的生活，制成一些可以消除异常体味的休闲式服装。
但是聚酰亚胺面料要得到很好的应用还需要解决难以染色，纺织品应用受限制的难题。
发明内容
本发明的目的是克服现有技术中存在的不足，提供一种化学还原法易染聚酰亚胺面料的制备方法，采用碱性还原性溶液对聚酰亚胺面料进行化学改性和处理，经处理后聚酰亚胺纤维表面产生大量的活性基团，并获得复杂表面，增加了与染料分子的结合力和上染率，获得可染聚酰亚胺面料。
按照本发明提供的技术方案，一种化学还原法易染聚酰亚胺面料的制备方法，其特征是，包括以下步骤：
(1)聚酰亚胺面料碱性还原性溶液处理：将聚酰亚胺面料放入盛有碱性还原性溶液的抗压容器罐中，压力为0.1-0.2Mpa，温度为100-110℃，处理时间为10-60min；
(2)聚酰亚胺面料洗涤：将经过碱性还原性溶液处理的聚酰亚胺面料取出水洗6-10次并进行烘干，烘干在70-100℃烘箱中进行，烘干时间为1-2h。
进一步的，还包括聚酰亚胺面料染色处理：将烘干后的聚酰亚胺面料采用分散染料进行染色，染色条件为130-135℃水浴，0.3-0.5MPa，染色时间为1-2h。
进一步的，所述碱性还原性溶液为氢氧化钠或碳酸钠与还原剂的混合溶液，其中氢氧化钠或碳酸钠与还原剂的摩尔比为2:1，氢氧化钠或碳酸钠的摩尔百分浓度为0.1-10％，还原剂的摩尔百分浓度为0.05-5％。
进一步的，所述还原剂为连二亚硫酸钠、连二硫酸钠或硫化钠。
本发明在不损害聚酰亚胺面料物理和化学性能的基础上使聚酰亚胺面料由不可染色变为可染色面料，解决了聚酰亚胺难以染色的问题，并且由于碱性还原性溶液的作用使得面料表面形成大量的活性基团，其中的氨基不仅可以染料分子结合，更具有很强的杀菌功能，可以提高聚酰亚胺面料的抗菌和杀菌功能，增加了面料附加值的同时也扩展了其在纺织范围内的应用领域。
附图说明
图1为对比例的电镜扫描图。
图2为实施例1的电镜扫描图。
图3为实施例2的电镜扫描图。
图4为实施例3的电镜扫描图。
图5为实施例4的电镜扫描图。
图6为实施例5的电镜扫描图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1-5：一种化学还原法易染聚酰亚胺面料的制备方法，包括以下步骤：
(1)聚酰亚胺面料碱性还原性溶液处理：将聚酰亚胺面料放入含有如表1所示的碱性还原性溶液的抗压容器罐中，压力为0.1-0.2MPa，温度为100-110℃，时间为10-60min；
(2)聚酰亚胺面料洗涤：将经过碱性还原性溶液处理的聚酰亚胺面料取出水洗6-10次并进行烘干，烘干在70-100摄氏度烘箱中进行，烘干时间为1-2h。
表1
测试例1：扫描电镜测试
分别对实施例1-5及对比例的样品进行扫描电镜测试，结果分别如图1-图6所示。从图1中可以看到，未经碱性还原性溶液处理的聚酰亚胺面料中的纤维表面光滑，从图2-6中可以看到，经过碱性还原性溶液处理后的纤维表面呈现复杂化。复杂的表面更容易使得染料分子上载，提高了面料的上染率；而经过碱性还原性溶液处理后的纤维表面由于大分子链的断裂而产生的活性基团如氨基和被还原的羟基等，具有很强的活性，可以与染料分子结合，增加了面料的色牢度。
测试例2：水洗色牢度检验
将实施例1-5及对比例的聚酰亚胺面料进行染色，以判定碱处理效果。采用分散染料，染色条件为130-135℃水浴，0.3-0.5MPa，染色时间为1-2h。具体染料及助剂、染色升温工艺如表2、3所示：
表2染料助剂
| 染料及助剂 | 比例/质量百分浓度(％) |
| 100％S_4RL | 0.08 |
| 100％_5BL | 0.08 |
| HGL深蓝 | 0.2 |
| 98％冰醋酸 | 0.78 |
| TF-212匀染剂 | 0.19 |
| DM_1364除油剂 | 0.51 |
表3染色升温工艺
对聚酰亚胺面料染色后的水洗色牢度检验结果如表4所示。
表4
由表4可以看出，经过碱性还原性溶液处理的聚酰亚胺面料水洗色牢度较未经处理的聚酰亚胺面料的有提高，即经过碱性还原性溶液处理后，聚酰亚胺面料的染色性能得到提高。
Claims (4)
1.一种化学还原法易染聚酰亚胺面料的制备方法，其特征是，包括以下步骤：
（1）聚酰亚胺面料碱性还原性溶液处理：将聚酰亚胺面料放入盛有碱性还原性溶液的抗压容器罐中，压力为0.1-0.2Mpa，温度为100-110℃，处理时间为10-60min；
（2）聚酰亚胺面料洗涤：将经过碱性还原性溶液处理的聚酰亚胺面料取出水洗6-10次并进行烘干，烘干在70-100℃烘箱中进行，烘干时间为1-2h。
2.如权利要求1所述的化学还原法易染聚酰亚胺面料的制备方法，其特征是：还包括聚酰亚胺面料染色处理：将烘干后的聚酰亚胺面料采用分散染料进行染色，染色条件为130-135℃水浴，0.3-0.5MPa，染色时间为1-2h。
3.如权利要求1所述的化学还原法易染聚酰亚胺面料的制备方法，其特征是：所述碱性还原性溶液为氢氧化钠或碳酸钠与还原剂的混合溶液，其中氢氧化钠或碳酸钠与还原剂的摩尔比为2:1，氢氧化钠或碳酸钠的摩尔百分浓度为0.1-10%，还原剂的摩尔百分浓度为0.05-5%。
4.如权利要求3所述的化学还原法易染聚酰亚胺面料的制备方法，其特征是：所述还原剂为连二亚硫酸钠、连二硫酸钠或硫化钠。
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