CN114753142B - 一种可持久抗菌的人造革用水刺非织造布及其制备方法 - Google Patents

一种可持久抗菌的人造革用水刺非织造布及其制备方法 Download PDF

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CN114753142B
CN114753142B CN202210569035.1A CN202210569035A CN114753142B CN 114753142 B CN114753142 B CN 114753142B CN 202210569035 A CN202210569035 A CN 202210569035A CN 114753142 B CN114753142 B CN 114753142B
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fiber
coupling agent
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王玉萍
朱宏伟
乔国华
许国良
李萌
钱军
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Zhejiang Wangjin Nonwovens Co ltd
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Abstract

本发明提供了一种可持久抗菌的人造革用水刺非织造布及其制备方法，所述水刺非织造布的纤维原料包括：尼龙6纤维，改性PET纤维、粘胶纤维，所述改性PET纤维的制备方法包括以下步骤：通过用低温等离子体先对PET纤维处理使其表面产生羟基，再浸泡于巯基偶联剂溶液中与巯基偶联剂的水解产物反应，然后在紫外照射条件下，再与不饱和胍类化合物溶液反应获得。由包括这种改性PET纤维、尼龙6纤维、粘胶纤维制作的非织造布洗涤多次后抗菌性损失小，具有持久、高效的抗菌性。同时还发现粘胶纤维具有协同N‑氰基‑N'‑[2‑羟基‑3‑(烯丙基氧基)丙基]胍接枝改性PET纤维提高水刺非织造布抗撕裂性能的作用。

Description

一种可持久抗菌的人造革用水刺非织造布及其制备方法
技术领域
本发明属于水刺非织造布技术领域，具体涉及一种可持久抗菌的人造革用水刺非织造布及其制备方法。
背景技术
天然皮革产品具有透水汽性能好、吸湿性能强等优点，深受人们的喜爱，但随着人口数量的增大，天然皮革的市场需求、价格也日渐增长，这样的现状促使人造革日新月异的发展。人造革是以纤维织物做底基，由合成树脂和各种助剂制成的混合涂料做面层，所制成的外观类似皮革的符合材料，合成树脂包括聚氯乙烯、聚酰胺、聚氨酯、聚烯烃等，底基包括机织布、针织布、非织造布。在众多底基材料中，水刺非织造布是一种起步较晚，但却因具有强力高、吸湿性好、透气性好、不易起毛、手感柔软、悬垂性好、无化学粘合剂、不污染、使用舒适等优点而快速进入这一领域，且迅速取代传统材料在人造革市场份额。
以水刺非织造布为底基制成的人造革多用于制鞋面、鞋衬里、制球、汽车内外饰等，它们是以涤纶、锦纶、丙纶等化学纤维为原料，特点是革品尺寸稳定性好，裁边或打孔处整齐光滑不掉纱，整体效果更加近似于真皮。近些年，随着人们物质生活水平的提高和卫生保健意识的增强，人们对生活和环境中的卫生要求也在迅速提高，毫无疑问，开发一种既具有上述水刺非织造布皮革基布众多优点，又具有高效抑菌功能的水刺非织造皮革基布，除有利于进一步提高人民的健康卫生水平外，还将大大拓宽非织造布的市场空间。
目前，增强水刺非织造布抗菌性的方法主要分为后处理法与纤维改良法两大类。后处理法指在纤维或织物制织的后整理阶段通过涂层等整理方法将抗菌剂添加到织物上使其具有抗菌性；纤维改良法指在纺织纤维纺丝过程中通过添加抗菌剂进行接枝、混炼等方法制成抗菌纤维的方法。目前，相对于复杂的纤维改良法，后处理法是一种更为简便、流行的加工处理方法，公开的现有技术如专利CN201811393483.0公开了一种抗静电、抗菌涤纶过滤基布的制备方法，选择铯离子和银离子混合，并与贝壳粉混合后焙烧的方式，加明胶制成微胶囊，然后加入到涤纶纤维中，可以显著提高涤纶过滤基布的抗菌性能；专利CN200810244145.0公开了纳米竹炭消臭鞋底革，采用纳米竹炭的表面细孔结构和它的化学成分以及湿放湿平衡作用来消除鞋的臭味，把含纳米竹炭的聚氨酯树脂浆料涂覆于离型纸上形成表皮层与由锦纶或涤纶纤维通过梳理成网，针刺或高速水刺使纤维间相互缠合成非织造布或机织布、编织布或非织造布与机织布、编织布复合成复合基布，通过粘合层使表层与这些基布贴合，除去离型纸，获得具有高效的消臭鞋底革，其中竹炭除富含微量元素外还含有天然竹醋成分，可以杀菌。专利CN201810850750.6公开了吸湿、透气、抗菌的聚氨酯合成革用水刺无纺布的制备方法，该发明利用椰糠的良好保水性能，将采用椰糠改性产物来提高材料的吸湿性，4-乙酰氧基苯乙烯和四烷基氟化铵提高其吸水效果，三氟乙酸酐提高抗菌剂的固定效果，保持抗菌效果的持久，二异丙基氨基锂和2-羟基丙三羧酸提高抗菌剂的抗菌效果，物质A提高聚氨酯粘合剂的分散性，使该聚氨酯具有吸湿、透气、抗菌性。
以上技术均为利用后处理法提高水刺非织造布抗菌性的方法，但抗菌效果不理想，经数十次洗涤后，抗菌剂从纤维表面溶出，织物抗菌效果下降，因此研发一种可持久抗菌的水刺非织造布人造革基布，对提高人民的健康卫生水平，进一步拓宽非织造布的市场空间具有重要意义。
发明内容
为解决上述技术问题，本发明提供了一种可持久抗菌的人造革用水刺非织造布及其制备方法，非织造布采用PET纤维、改性PET纤维、粘胶纤维为纤维原料，其中改性PET纤维的表面接枝有不饱和胍类化合物，其首先通过低温等离子体对PET纤维处理使其表面产生羟基，然后纤维表面的羟基与巯基偶联剂上的烷氧基发生水解缩合反应，最后在紫外照射下再与不饱和胍类化合物发生巯基-烯基点击反应获得，这种改性PET纤维洗涤后抗菌性不下降，具有持久、高效的抗菌性。
为实现上述目的，采取以下具体技术方案：
一种可持久抗菌的人造革用水刺非织造布，所述水刺非织造布的纤维原料包括：尼龙6纤维，改性PET纤维、粘胶纤维，所述改性PET纤维的制备方法包括以下步骤：通过用低温等离子体先对PET纤维处理使其表面产生羟基，再浸泡于巯基偶联剂溶液中与巯基偶联剂的水解产物反应，然后在紫外照射条件下，再与不饱和胍类化合物溶液反应获得。
胍基化合物中的胍基团是一种有效的活性基团，可以与生物体中的基团或元素相互作用，破坏其正常的物质和能量代谢，通过对PET纤维低温等离子体处理使其表面产生羟基，利用巯基偶联剂对产生羟基的PET纤维进行表面处理，得到表面有巯基的PET纤维，最后在紫外照射下通过PET纤维表面的纤维与不饱和胍类化合物发生巯基-烯基点击反应，成功地在PET表面化学接枝上具有抗菌活性的胍基。
进一步地，所述水刺非织造布包括如下重量份的纤维原料：10-20份尼龙6纤维、80-100份改性PET纤维、10-18份粘胶纤维，所述巯基偶联剂的用量为PET纤维的10-15wt％，所述巯基偶联剂溶液包括巯基偶联剂、水、低碳醇三者体积比为1-5:5-10:25-34，所述不饱和胍类化合物与巯基偶联剂的摩尔比为1.12-1.24:1，所述不饱和胍类化合物溶液的浓度为15-25wt％。
所述PET纤维的直径为14-28μm。
所述改性PET纤维的接枝率为18.4-26.3wt％。
所述巯基偶联剂包括(3-巯丙基)三乙氧基硅烷、(3-巯基丙基)三甲氧基硅烷、2-巯基乙基三乙氧基硅烷、3-巯丙基(二甲氧基)甲硅烷中的一种或两种及以上的组合。
所述不饱和胍类化合物包括1-[3-烯丙基氧基-2-羟基丙基]双胍、1-氨基-2-[(E)-2-己基十二碳-2-烯基]胍、1-[(E)-2-(3,4-二羟基苯基)乙烯基]胍、[3-(烯丙基氧基)-2-羟基丙基]胍、3-甲基-2-丁烯基胍、N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍中的一种或两种及以上的组合。
优选的，所述不饱和胍类化合物为N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍。发明人预料不到地发现，粘胶纤维具有协同以N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍接枝改性的PET纤维提高水刺非织造布抗撕裂性能的作用。
所述改性PET纤维通过包括如下步骤的方法制得：
1)以氧气为放电介质，用低温等离子体对PET纤维表面进行处理，备用；
2)将步骤1)所得纤维浸泡于巯基偶联剂溶液中，调节pH，浸泡，过滤，加热并恒温反应，反应结束后真空干燥至恒重，备用；
3)将步骤2)所得纤维浸泡于接枝溶液中，紫外照射，反应结束后过滤，洗涤，真空干燥即得改性PET纤维。
步骤3)所述接枝溶液包括有机溶剂、不饱和胍类化合物、光引发剂，所述接枝溶液中不饱和胍类化合物的浓度为15-25wt％，所述有机溶剂包括苯、甲苯、二甲苯、乙醇、丙酮中的一种或两种及以上的组合；所述光引发剂选自2-羟基-2-甲基-1-苯基-1-丙酮、2-羟基-2-甲基-1-[4-(2-羟基乙氧基)苯基]-1-丙酮中的一种，所述光引发剂的用量为不饱和胍类化合物的1-3wt％；所述紫外光强为10-30mW/cm2，所述紫外照射时间为10-60min；
步骤2)所述巯基偶联剂溶液包括巯基偶联剂、水、低碳醇，所述巯基偶联剂、水、有机醇的体积比为1-5:5-10:25-34，所述低碳醇选自甲醇、乙醇、异丙醇中的一种或两种的组合；所述调节pH为调节至3-5，所述调节剂为0.05-0.1mol/L的盐酸溶液，所述加热为50-80℃加热0.5-2h，所述真空干燥温度为50-80℃；
步骤1)所述氧气流量为30-50mL/min，等离子体中空管气压为30-100Pa，PET纤维经过低温等离子体发射装置的速度为50-100m/h，所述碳纤维距离低温等离子体发射装置20-50mm，等离子体发射功率为30-100W，处理温度为10-20℃。
所述粘胶纤维为普通粘胶纤维，断裂强度为1.6-2.7cN/dtex，直径为10-30μm。
所述尼龙6纤维的线密度为0.8-3dtex。
本发明还提供了上述可持久抗菌的人造革用水刺非织造布的制备方法，包括如下步骤：
将尼龙6纤维、改性PET纤维、粘胶纤维分别开松，然后混合，梳理成网，水刺加固，烘干，卷绕即得上述人造革用水刺非织造布。
所述开松为分别将PET纤维、改性PET纤维、粘胶纤维用开松机开松；
所述混合为将开松后的PET纤维、改性PET纤维、粘胶纤维混合均匀，得混合纤维；
所述梳理成网为将混合纤维使用梳理机梳理，并使用铺网机形成交叉混合均匀的纤维网；
所述水刺加固的水刺速度为3-10m/min，水刺压力为200-400bar；
所述烘干为将水刺加固后的纤维网110℃-130℃烘箱烘干。
所述水刺非织造布的面密度为80-100g/m2。
与现有技术相比，本发明的有益效果是：
本发明制备了一种表面接枝有不饱和胍类化合物的改性PET纤维，其首先通过低温等离子体对PET纤维处理使其表面产生羟基，然后纤维表面的羟基与巯基偶联剂上的烷氧基发生水解缩合反应，最后在紫外照射下再与不饱和胍类化合物发生巯基-烯点击反应获得，这种改性PET纤维洗涤后抗菌性不下降，具有持久、高效的抗菌性。
具体实施方式
下面结合具体实施例对本发明作进一步的说明，但并不局限于说明书上的内容。若无特殊说明，本发明实施例中所述“份”均为重量份。所用试剂均为本领域可商购的试剂。
粘胶纤维购自泉州海天轻纺有限公司，断裂强度为2.1cN/dtex，直径为25μm。
制备改性PET纤维
制备例1
1)以氧气为放电介质，用低温等离子体对直径为25μm的PET纤维表面进行处理，处理条件为：氧气流量为50mL/min，等离子体中空管气压为50Pa，PET纤维经过低温等离子体发射装置的速度为80m/h，所述碳纤维距离低温等离子体发射装置50mm，等离子体发射功率为100W，处理温度为20℃。
2)将100份步骤1)所制纤维浸泡于由(3-巯丙基)三乙氧基硅烷、水、乙醇按照体积比5:5:30为组成的120份混合物中，用0.05mol/L的盐酸溶液调节pH至3，浸泡，过滤，加热至60℃并恒温反应2h，去离子去水和无水乙醇交替洗涤3次，50℃真空干燥至恒重，备用；
3)将步骤2)所制纤维浸泡于由125份由106份甲苯、18.6份N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍、0.4份2-羟基-2-甲基-1-苯基-1-丙酮的混合物中，光强为30mW/cm2的紫外照射30min，反应结束后过滤，用DMF洗涤3次，100℃真空干燥即得改性PET纤维。
制备例2
其余与制备例1相同，不同之处在于，步骤3)125份不饱和胍类化合物溶液由16.8份N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍，0.4份2-羟基-2-甲基-1-苯基-1-丙酮，94.8份甲苯混合而成。
制备例3
其余与制备例1相同，不同之处在于，由(3-巯丙基)三乙氧基硅烷、水、乙醇按照体积比为5:5:30组成的混合物的用量为80份。
制备例4
其余与制备例1相同，不同之处在于，用等量的[3-(烯丙基氧基)-2-羟基丙基]胍替换N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍。
制备水刺非织造布
实施例1-4
将10份线密度为1.5dtex的尼龙6纤维、100份改性PET纤维分别对应制备例1-4所制备的、18份粘胶纤维用开松机分别开松，然后将三种纤维混合均匀，梳理铺成交叉、混合均匀0.4mm厚的纤维网，三道水刺加固：第一道100-200bar、第二道300-400bar、第三道200-300bar、水刺速度为7.6m/min，最后120℃烘干，卷绕得面密度为87.3g/m2的人造革用水刺非织造布。
实施例5
其余与实施例1相同，不同之处在于粘胶纤维的用量为10份。
将上述制备例及对比制备例中的改性PET纤维参照下式进行接枝率的计算
G＝m1-m0/m0
式中m0、m1分别为PET纤维的重量、改性PET纤维的重量。
表1
项目 接枝率％
制备例1 26.3
制备例2 24.1
制备例3 18.4
制备例4 25.7
将上述实施例及对比实施例制备的水刺非织造布进行以下性能测试：
抑菌性：根据GB/T 20944.3-2008《纺织品抗菌性能的评价第3部分：振荡法》对实施例及对比实施例制备的水刺非织造布进行抗菌性测试。试验用菌：金黄色葡萄球菌试验用培养基：营养琼脂培养基，蛋白胨5g，牛肉浸膏3g，琼脂15g，蒸馏水1000mL混合，灭菌后，pH值6.8±0.2。
抑菌耐洗性测试：室温下，水刺非织造布用天然皂粉(浓度为2g/L)浸泡5min，漂洗3次，然后晾干，为一次洗涤过程，对洗涤50次的水刺非织造布进行上述抑菌性能测试。
拉伸断裂性能：参照标准GB/T24218.3《纺织品非织造布试验方法断裂强力和断裂伸长率的测定》测试非织造材料的拉伸断裂性能，尺寸20cm×5cm，夹持隔离为10cm，拉伸速度为100m/min。
表2
由上表2可以看出本发明制备的水刺非织造布洗涤多次后抑菌性损失小，具有持久、高效的抗菌性，此外还发现粘胶纤维具有协同N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍接枝改性的PET纤维提高水刺非织造布抗撕裂性能的作用。
上述详细说明是针对本发明其中之一可行实施例的具体说明，该实施例并非用以限制本发明的专利范围，凡未脱离本发明所为的等效实施或变更，均应包含于本发明技术方案的范围内。

Claims (8)

1.一种可持久抗菌的人造革用水刺非织造布，其特征在于，所述水刺非织造布包括以下质量份的纤维原料：10-20份尼龙6纤维，80-100份改性PET纤维、10-18份粘胶纤维，所述改性PET纤维的制备方法包括以下步骤：通过用低温等离子体先对PET纤维处理使其表面产生羟基，再浸泡于巯基偶联剂溶液中与巯基偶联剂的水解产物反应，然后在紫外照射条件下，再与不饱和胍类化合物溶液反应获得；所述巯基偶联剂的用量为PET纤维的10-15wt%，所述巯基偶联剂溶液包括巯基偶联剂、水、低碳醇三者体积比为1-5:5-10:25-34，所述不饱和胍类化合物与巯基偶联剂的摩尔比为1.12-1.24:1，所述不饱和胍类化合物溶液的浓度为15-25wt%；所述改性PET纤维的接枝率为18.4-26.3wt%；所述不饱和胍类化合物为N-氰基-N'-[2-羟基-3-(烯丙基氧基)丙基]胍。
2.权利要求1所述可持久抗菌的人造革用水刺非织造布，其特征在于，所述PET纤维的直径为14-28μm。
3.权利要求1所述可持久抗菌的人造革用水刺非织造布，其特征在于，所述巯基偶联剂选自(3-巯丙基)三乙氧基硅烷、(3-巯基丙基)三甲氧基硅烷、2-巯基乙基三乙氧基硅烷、3-巯丙基(二甲氧基)甲硅烷中的一种或多种的组合。
4.权利要求1所述可持久抗菌的人造革用水刺非织造布，其特征在于，所述改性PET纤维通过包括如下步骤的方法制得：
1）以氧气为放电介质，用低温等离子体对PET纤维表面进行处理，备用；
2）将步骤1）所得纤维浸泡于巯基偶联剂溶液中，调节pH，浸泡，过滤，加热并恒温反应，反应结束后真空干燥至恒重，备用；
3）将步骤2）所得纤维浸泡于接枝溶液中，紫外照射，反应结束后过滤，洗涤，真空干燥即得改性PET纤维。
5.权利要求4所述可持久抗菌的人造革用水刺非织造布，其特征在于，
步骤2）所述巯基偶联剂溶液包括巯基偶联剂、水、低碳醇，所述调节pH为调节至3-5，调节剂为0.05-0.1mol/L的盐酸溶液，所述加热为50-80℃加热0.5-2h；
步骤3）所述接枝溶液包括有机溶剂、不饱和胍类化合物、光引发剂，所述光引发剂的用量为不饱和胍类化合物的1-3wt%；所述紫外照射光强为10-30mW/cm2，所述紫外照射时间为10-60min。
6.权利要求1所述可持久抗菌的人造革用水刺非织造布，其特征在于，所述粘胶纤维为普通粘胶纤维，断裂强度为1.6-2.7cN/dtex，直径为10-30μm；所述尼龙6纤维的线密度为0.8-3dtex。
7.权利要求1-6任一项所述可持久抗菌的人造革用水刺非织造布的制备方法，其特征在于，包括如下步骤：
将尼龙6纤维、改性PET纤维、粘胶纤维分别开松，然后混合，梳理成网，水刺加固，烘干，卷绕即得上述人造革用水刺非织造布。
8.权利要求7所述可持久抗菌的人造革用水刺非织造布的制备方法，其特征在于，
所述水刺加固的水刺速度为3-10m/min，水刺压力为200-400bar；所述烘干为将水刺加固后的纤维网110℃-130℃烘箱烘干；所得人造革用水刺非织造布的面密度为80-100g/m2。
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