CN117024661A - 一种纺织浆纱用两亲性淀粉/动物胶浆料的制备方法 - Google Patents
一种纺织浆纱用两亲性淀粉/动物胶浆料的制备方法 Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
本发明涉及一种纺织浆纱用两亲性淀粉/动物胶浆料的制备方法，包括：借助酸性试剂处理淀粉和动物胶，得到混合分散体系；加入碱性试剂和环氧氯丙烷，搅拌反应；添加阳离子醚化剂，充分搅拌；引入反应单体和引发剂，实现接枝改性；通过水洗、透析、烘干与粉碎，制得两亲性淀粉/动物胶浆料。本发明具有成本低、反应快、操作简单等优势，获得的浆料可与亲疏水纤维混纺制备的纱线形成良好的结合，改善纱线的可织性。
Description
技术领域
本发明属于纺织浆料领域，特别涉及一种纺织浆纱用两亲性淀粉/动物胶浆料的制备方法。
背景技术
随着生活水平的提高以及经济的快速发展，人们的衣着风格发生了巨大变化。这也对织物的力学性能、热舒适性能等方面提出了更高要求，进而产生了各种类型的亲疏水纤维混纺制备的纱线(如涤/棉混纺纱、锦纶/棉混纺纱等)以满足实际需求。然而，在大规模的工业化织造过程中，需要对这些混纺纱进行上浆处理以提升纱线的力学性能以及伏贴纱线表面毛羽，但上浆难度要明显地高于纯棉纱，这主要是由于纤维间的差异性导致浆液对纱线的贴附效果不稳定，进而影响纱线的上浆均匀效果，使其难以满足实际织造生产要求。为提升混纺纱的可织性，在调制浆液的过程中往往添加大量生物降解性差的浆料组分，如聚乙烯醇、聚丙烯酸和聚酯类等。这种处理方式虽然有利于改善混纺纱的上浆效果，满足实际织造需求，但合成类纺织浆料存在成本过高以及退浆废水处理难度大的问题，也会对自然环境带来严重污染。所以，研究如何借助天然高分子材料制备纺织浆料并取代合成类浆料，已成为当下纺织浆料领域的重要研究方向。
天然高分子材料种类众多，如纤维素类、淀粉类以及动物胶类。其中，淀粉类浆料和动物胶具有绿色安全、可循环再生、易于生物降解等优势，已在纺织浆料领域获得了广泛应用。但由于存在大量羟基以及特殊的空间结构，使得淀粉链的分子间具有极强的氢键作用，导致淀粉液相分散效果差、成膜脆硬，难以满足实际上浆需求，进而严重限制了淀粉基纺织浆料的应用。此外，调制与应用淀粉基浆料的工序均需在高温条件下完成，不仅恶化了工人的工作环境，提高了危险系数，而且也污染了自然环境，浪费了大量的能源，增加了浆料的制备成本。动物胶则主要是从动物的骨头和皮毛中获取丰富的蛋白质，并经过一系列的物理加工获得。动物胶材料具有便于制备并获取、价格低廉、无毒无害且来源广等优势，也可大量应用于纺织浆料领域。然而，由于动物胶的水溶液易于发生团聚凝胶的问题，导致其对纱线的粘附效果不稳定，进而限制其在实际应用过程中受到巨大地限制。因此，如何实现在中低温环境下制备并应用淀粉与动物胶等天然高分子材料在纺织浆纱领域应用成为重要的研究内容。
中国专利号CN111335037A公开了一种环保型纺织浆料及其制备方法，以变性淀粉、丙烯酰胺和助剂为浆料主体，引入天然植物淀粉、纳米粒子、胶类和乙二醇构筑环保型纺织浆料，既可以克服淀粉浆料成膜脆硬的缺点，改善浆料的液相稳定性，降低浆纱的退浆难度，也可以提升纱线的拉伸性和耐磨性，进而增强纱线的可织性。但该发明的制备流程冗长，所需原料种类繁多，不利于大规模制备，进而限制其工业化推广应用。
中国专利号CN101831805B公开了一种高性能、环保型纺织浆料及其制备方法，借助活化聚乙二醇化学修饰动物胶，并与多种高性能变性淀粉、化学助剂进行复配使用，制备出可用于棉、黏胶以及混纺纱经纱上浆的纺织浆料。该方法制备的浆料制备的浆液表现出显著的流动性、良好的成膜性以及上浆效果。然而，在制备过程中存在严重的化学污染，制备过程比较繁琐，对工作人员提出了严格的要求。
发明内容
本发明所要解决的技术问题是提供一种纺织浆纱用两亲性淀粉/动物胶浆料的制备方法，以克服现有合成纺织浆料存在的生产成本高、化学试剂种类繁琐和废水处理难度大等问题。
本发明提供了一种纺织浆纱用两亲性淀粉/动物胶浆料的制备方法，包括如下步骤：
(1)将原淀粉、动物胶、酸性试剂以及分散剂依次添加到水中，充分搅拌并分散均匀，制得淀粉与动物胶的混合分散体系；
(2)加入碱性试剂将上述混合分散体系的pH值调整为9-10，再加入环氧氯丙烷和阳离子醚化剂分别进行反应，制得阳离子醚化淀粉/动物胶分散液；
(3)在上述分散液中加入反应单体和引发剂，反应得到两亲性淀粉/动物胶粗产物；最后通过水洗、透析、烘干与粉碎，得到两亲性淀粉/动物胶浆料。
所述步骤(1)中的原淀粉为玉米淀粉、豌豆淀粉、小麦淀粉、马铃薯淀粉、红薯淀粉、木薯淀粉、绿豆淀粉中的一种或几种；所述原淀粉在混合分散体系中的质量分数为5％-20％。
所述步骤(1)中的动物胶为皮胶、骨胶、血胶、鱼胶、乳酪胶、龟板胶中的一种或几种；所述动物胶在混合分散体系中的质量分数为1％-10％。
所述步骤(1)中的酸性试剂为硫酸、盐酸、硝酸、草酸、柠檬酸、次氯酸中的一种或几种；所述酸性试剂在混合分散体系中的质量分数为0.1％-10％。
所述步骤(1)中的分散剂为乙醚、丙二醇、十二烷基苯磺酸钠、聚乙烯吡咯烷酮中的一种或几种；所述分散剂在混合分散体系中的质量分数为0.1％-8％。
所述步骤(2)中的碱性试剂为NaOH、LiOH、KOH、Ca(OH)2、NaHCO3、Na2CO3中的一种或几种；所述碱性试剂在混合分散体系中的质量分数为0.1％-4％。
所述步骤(2)中的环氧氯丙烷在混合分散体系中的质量分数为0.5-5％。
所述步骤(2)中的阳离子醚化剂为3-氯-2-羟丙基三甲基氯化铵、N-2,3-环氧丙基三甲基氯化铵中的一种或几种；所述阳离子醚化剂在混合分散体系中的质量分数为1-10％。
所述步骤(3)中的反应单体为丙烯酸、丙烯酰胺、乙酸乙烯酯、羟甲基丙烯酰胺、丙烯酸丁酯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸月桂酯中的一种或几种；所述反应单体在分散液中的质量分数为1-10％。
所述步骤(3)中的引发剂为过硫酸铵、过硫酸钾、过硫酸钠中的一种或几种；所述引发剂在分散液中的质量分数为0.1-1％。
所述步骤(1)中的搅拌温度为15-55℃，搅拌时间为0.5-3h。
所述步骤(2)中的反应温度为25-50℃，反应时间为0.5-2h。
所述步骤(3)中的反应温度为30-50℃，反应时间为0.5-1h。
本发明将环氧氯丙烷逐滴添加到混合分散体系中充分反应，以实现淀粉链上的羟基与动物胶中携带的大量活性基团发生有效的化学接枝反应，增强浆料对纤维的粘附效果；将阳离子醚化剂添加到混合分散体系中，充分搅拌，通过阳离子醚化剂修饰淀粉链和动物胶，构筑阳离子醚化淀粉-动物胶分散液，引入阳离子基团可以增强淀粉-动物胶材料的分子间斥力作用，进而提升淀粉-动物胶材料的液相分散稳定性；随后添加反应单体和引发剂对阳离子醚化淀粉-动物胶分散液进行接枝改性，制备两亲性淀粉-动物胶粗产物，淀粉-动物胶接枝单体混合体系以弱化其与疏水性基团的相互作用力，提升浆液与疏水性纤维的结合效果。
有益效果
本发明借助酸水解可以破坏天然淀粉(原淀粉)与动物胶的原有空间结构，弱化材料的结晶区，有效降低高分子的聚合度和分子量，增加反应比表面积，实现降低有效化学反应的难度、提升浆液液相分散效果的目的；通过化学交联的方式，制备淀粉与动物胶的结合产物，以提升混合体系的粘附性能；借助季铵阳离子醚化剂可以赋予淀粉与动物胶大量阳离子基团，增加分子链间的静电斥力，提升其液相分散效果；通过引入反应单体实现分子链的多支化空间结构，增加高分子材料间的空间位阻，同时，借助反应单体中存在的差异性基团，弱化浆料与疏水性纤维的相互作用力，提升浆液对混纺纱的上浆效果。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
(1)淀粉与动物胶的混合分散体系
在20℃的恒温水浴环境中，将10g玉米淀粉、5g鱼胶、2g乙醚、1g盐酸添加到66.5g水中，充分搅拌1h，制备淀粉与动物胶的混合分散体系；
(2)阳离子醚化淀粉-动物胶分散液
在25℃的恒温水浴环境中，利用2g NaOH溶液将淀粉与动物胶的混合分散体系的pH值调节到10，将2g环氧氯丙烷逐滴添加到混合分散体系中，充分搅拌1h；将5g N-2,3-环氧丙基三甲基氯化铵添加到混合分散体系中，充分搅拌2h，制备阳离子醚化淀粉-动物胶分散液；
(3)两亲性淀粉-动物胶粗产物
在30℃的恒温水浴环境中，将5g乙酸乙烯酯逐滴添加到阳离子醚化淀粉-动物胶分散液中，充分搅拌并分散均匀，添加0.5g过硫酸铵，充分反应1h，制备两亲性淀粉-动物胶粗产物；
(4)两亲性淀粉-动物胶浆料
将两亲性淀粉-动物胶粗产物进行多次水洗并抽滤，直至浆料的pH值为7，再通过烘干与粉碎，即可制备两亲性淀粉-动物胶浆料。
实施例2
(1)淀粉与动物胶的混合分散体系
在30℃的恒温水浴环境中，将15g玉米淀粉、8g鱼胶、2g丙二醇、2g盐酸添加到54.5g水中，充分搅拌1h，制备淀粉与动物胶的混合分散体系；
(2)阳离子醚化淀粉-动物胶分散液
在30℃的恒温水浴环境中，利用4g NaOH溶液将淀粉与动物胶的混合分散体系的pH值调节到10，将3g环氧氯丙烷逐滴添加到混合分散体系中，充分搅拌1h；将6g N-2,3-环氧丙基三甲基氯化铵添加到混合分散体系中，充分搅拌2h，制备阳离子醚化淀粉-动物胶分散液；
(3)两亲性淀粉-动物胶粗产物
在30℃的恒温水浴环境中，将2g乙酸乙烯酯和3g丙烯酸丁酯逐滴添加到阳离子醚化淀粉-动物胶分散液中，充分搅拌并分散均匀，添加0.5g过硫酸铵，充分反应1h，制备两亲性淀粉-动物胶粗产物；
(4)两亲性淀粉-动物胶浆料
将两亲性淀粉-动物胶粗产物进行多次水洗并抽滤，直至浆料的pH值为7，再通过烘干与粉碎，即可制备两亲性淀粉-动物胶浆料。
实施例3
(1)淀粉与动物胶的混合分散体系
在30℃的恒温水浴环境中，将12g玉米淀粉、8g鱼胶、2g丙二醇、4g硫酸添加到54.5g水中，充分搅拌1h，制备淀粉与动物胶的混合分散体系；
(2)阳离子醚化淀粉-动物胶分散液
在30℃的恒温水浴环境中，利用4g LiOH溶液将淀粉与动物胶的混合分散体系的pH值调节到10，将5g环氧氯丙烷逐滴添加到混合分散体系中，充分搅拌1h；将6g N-2,3-环氧丙基三甲基氯化铵添加到混合分散体系中，充分搅拌2h，制备阳离子醚化淀粉-动物胶分散液；
(3)两亲性淀粉-动物胶粗产物
在30℃的恒温水浴环境中，将2g乙酸乙烯酯和2g丙烯酸丁酯逐滴添加到阳离子醚化淀粉-动物胶分散液中，充分搅拌并分散均匀，添加0.5g过硫酸铵，充分反应1h，制备两亲性淀粉-动物胶粗产物；
(4)两亲性淀粉-动物胶浆料
将两亲性淀粉-动物胶粗产物进行多次水洗并抽滤，直至浆料的pH值为7，再通过烘干与粉碎，即可制备两亲性淀粉-动物胶浆料。
对比例1
与实施例1的不同之处在于，在25℃的恒温水浴环境中，利用2g NaOH溶液将淀粉与动物胶的混合分散体系的pH值调节到10，将5g N-2,3-环氧丙基三甲基氯化铵添加到混合分散体系中，充分搅拌2h，制备阳离子醚化淀粉-动物胶分散液。
对比例2
与实施例1的不同之处在于，在25℃的恒温水浴环境中，利用2g NaOH溶液将淀粉与动物胶的混合分散体系的pH值调节到10，将2g环氧氯丙烷逐滴添加到混合分散体系中，充分搅拌1h，制备淀粉-动物胶分散液。
对比例3
与实施例1的不同之处在于，在25℃的恒温水浴环境中，利用2g NaOH溶液将淀粉与动物胶的混合分散体系的pH值调节到10，制备淀粉-动物胶分散液。
分别称取实施例1-3中的两亲性淀粉-动物胶浆料与对比例1-3各20g，分别溶于180g去离子水中。在恒温环境中(50℃)，制备含固量为10％的浆液。借助旋转式粘度计(选用4号转子)对构筑的浆液进行粘度测定，每个样品重复测试5次；并借助浆纱机对锦纶/棉混纺纱(18.2tex)进行上浆，并对纱线进行性能测试；测试结果如下表1所示。
表1实施例与对比例制备的浆料的粘度稳定性与成膜性测试
表2实施例与对比例制备的浆料的浆纱效果
通过以上的测试结果可得出，本发明所制备的两亲性淀粉-动物胶浆料具有优良的液相分散效果，良好的成膜性，对亲疏水纤维混纺制备的纱线具有良好的结合效果，通过上浆的方式可显著提升纱线的物理机械性能，有效减少纱线表面有害毛羽，提升纱线上浆质量和可织性。
Claims (10)
1.一种纺织浆纱用两亲性淀粉/动物胶浆料的制备方法，包括如下步骤：
(1)将原淀粉、动物胶、酸性试剂以及分散剂依次添加到水中，充分搅拌并分散均匀，制得淀粉与动物胶的混合分散体系；
(2)加入碱性试剂将上述混合分散体系的pH值调整为9-10，再加入环氧氯丙烷和阳离子醚化剂分别进行反应，制得阳离子醚化淀粉/动物胶分散液；
(3)在上述分散液中加入反应单体和引发剂，反应得到两亲性淀粉/动物胶粗产物；最后通过水洗、透析、烘干与粉碎，得到两亲性淀粉/动物胶浆料。
2.根据权利要求1所述的制备方法，其特征在于：所述步骤(1)中的原淀粉为玉米淀粉、豌豆淀粉、小麦淀粉、马铃薯淀粉、红薯淀粉、木薯淀粉、绿豆淀粉中的一种或几种；所述原淀粉在混合分散体系中的质量分数为5％-20％。
3.根据权利要求1所述的制备方法，其特征在于：所述步骤(1)中的动物胶为皮胶、骨胶、血胶、鱼胶、乳酪胶、龟板胶中的一种或几种；所述动物胶在混合分散体系中的质量分数为1％-10％。
4.根据权利要求1所述的制备方法，其特征在于：所述步骤(1)中的酸性试剂为硫酸、盐酸、硝酸、草酸、柠檬酸、次氯酸中的一种或几种；所述酸性试剂在混合分散体系中的质量分数为0.1％-10％。
5.根据权利要求1所述的制备方法，其特征在于：所述步骤(1)中的分散剂为乙醚、丙二醇、十二烷基苯磺酸钠、聚乙烯吡咯烷酮中的一种或几种；所述分散剂在混合分散体系中的质量分数为0.1％-8％。
6.根据权利要求1所述的制备方法，其特征在于：所述步骤(2)中的碱性试剂为NaOH、LiOH、KOH、Ca(OH)2、NaHCO3、Na2CO3中的一种或几种；所述碱性试剂在混合分散体系中的质量分数为0.1％-4％。
7.根据权利要求1所述的制备方法，其特征在于：所述步骤(2)中的环氧氯丙烷在混合分散体系中的质量分数为0.5-5％。
8.根据权利要求1所述的制备方法，其特征在于：所述步骤(2)中的阳离子醚化剂为3-氯-2-羟丙基三甲基氯化铵、N-2,3-环氧丙基三甲基氯化铵中的一种或几种；所述阳离子醚化剂在混合分散体系中的质量分数为1-10％。
9.根据权利要求1所述的制备方法，其特征在于：所述步骤(3)中的反应单体为丙烯酸、丙烯酰胺、乙酸乙烯酯、羟甲基丙烯酰胺、丙烯酸丁酯、丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸月桂酯中的一种或几种；所述反应单体在分散液中的质量分数为1-10％。
10.根据权利要求1所述的制备方法，其特征在于：所述步骤(3)中的引发剂为过硫酸铵、过硫酸钾、过硫酸钠中的一种或几种；所述引发剂在分散液中的质量分数为0.1-1％。
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