CN114404304A - 一种可降解的消毒护肤湿巾及其制备方法 - Google Patents

一种可降解的消毒护肤湿巾及其制备方法 Download PDF

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CN114404304A
CN114404304A CN202210110240.1A CN202210110240A CN114404304A CN 114404304 A CN114404304 A CN 114404304A CN 202210110240 A CN202210110240 A CN 202210110240A CN 114404304 A CN114404304 A CN 114404304A
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polylactic acid
modified
degradable
wet tissue
maleic anhydride
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CN114404304B (zh
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董二莹
梁怀玉
田晓辉
周敏东
彭志云
叶挺
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Zhejiang Youquan Nursing Products Co ltd
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Abstract

本发明涉及一种可降解的消毒湿护肤湿巾，包括湿巾浸液和可降解的复合无纺布作为湿巾浸液的载体，所述复合无纺为三明治结构，依次是改性聚乳酸纤维层，莱赛尔纤维和木浆纤维复合层，改性聚乳酸纤维层，所述改性聚乳酸是季铵盐和马来酸酐共同接枝改性的聚乳酸和侧链含羟基聚合物通过熔融共挤出得到。本发明制备得到的消毒湿护肤湿巾，手感、强度、吸水性、保水性、抗菌性的综合性能方面达到优异，并且可降解，不会造成环境污染。

Description

一种可降解的消毒护肤湿巾及其制备方法
技术领域
本申请涉湿巾领域，具体涉及一种可降解的消毒护肤湿巾及其制备方法。
背景技术
新冠病毒疫情期间，大部分人因为条件限制，不能经常对手部或接触的物体进行消毒，从而增加了被传染的几率。而酒精、消毒液、洗手液不方便随身携带，现有市面上的湿巾又多以清洁、护肤为主要功效，在消毒、杀菌方面效果比较弱。因此，加强湿巾的消毒、抗菌性能是目前市场受欢迎的一类产品。
但是通常由于此类湿巾是在湿态下进行保存，对材料在湿态下的强度有一定要求，往往提高湿巾强度的方法，比如提高分子量，提高交联程度等方法，都会使湿巾的降解性能下降甚至失去降解性能。而此类湿巾都是一次性使用产品，使用一次后就会被丢弃，这样会对环境造成不利的影响，如果掩埋至土中而长期不能降解，会对土壤环境造成污染和破坏。因此，研发一种可降解的消毒湿巾对环保具有重要意义，也满足了市场的需求。
现有技术往往以植物纤维、甲壳素纤维作为可降解的纤维材料制备可降解湿巾，但是上述材料对人体皮肤的擦拭感不好，不够舒适，影响了其在市场上的销售。
CN112006584A公开了一种多功能湿巾，该专利公开的湿巾具有可降解性的原因是加入碱性纤维素酶，其可以对湿巾基体材料的棉纤维、大豆纤维、椰子纤维的蛋白质酶解，促使湿巾降解。但是一方面是加大湿巾的制造成本，另一方面加入的碱性纤维素酶可能也对人体皮肤有一定的刺激性。
聚乳酸是一种新发展的可降解材料，其生物亲和性好，已经广泛已用于各种可降解的一次性制品的生产，比如餐盒、塑料袋、一次性注射液用具、手术缝合线、低分子量的聚乳酸还可以用于药物的缓释包装剂型。
CN112006968A公开了一种消毒湿巾，其实采用聚乳酸纤维和菠萝叶纤维开松，梳理、铺网、收卷后作为湿巾基布和湿巾液一起浸渍得到。
CN101745137A公开了一种可降解的消毒湿巾，其湿巾载体是的原料包括聚乳酸，壳聚糖，甲壳素。
以上现有技术直接使用聚乳酸，目的是获得可降解的擦拭材料，但是在获得生物可降解性的同时，却忽视了消毒用湿巾所需要的吸水性、保水性，力学性能以及对皮肤的触感问题。聚乳酸由于制备工艺，分子量一般较低，力学性能，特别是湿态下力学性能不好；此外，聚乳酸亲脂性比较强，作为消毒湿巾材料不利于吸水性和保水性的提高。
发明内容
为了解决现有技术中消毒抗菌的护肤湿巾无法降解，随意丢弃或者进行垃圾掩埋会对土壤造成污染，影响土质，造成严重的环境问题。本发明提供一种基于改性聚乳酸纤维的可降解的消毒护肤湿巾，本发明湿巾基布为三明治的复合结构，依次是改性聚乳酸纤维层，莱赛尔纤维和木浆纤维复合层，改性聚乳酸纤维层，改善了传统采用植物纤维制成的湿巾基布吸水性、保水性、力学性能、手感等综合性能不能满足日益增长的消毒护肤湿巾的市场需要的问题，解决了传统湿巾无法降解，造成环境污染的问题。
为解决上述问题，本发明提供了以下技术方案：
本发明第一个目的是提供一种可降解的消毒护肤湿巾，包括湿巾浸液和可降解的复合无纺布作为湿巾浸液的载体，所述复合无纺为三明治结构，依次是改性聚乳酸纤维层，莱赛尔纤维和木浆纤维复合层，改性聚乳酸纤维层，所述改性聚乳酸是季铵盐和马来酸酐共同接枝改性的聚乳酸和侧链含羟基聚合物通过熔融共挤出得到。
进一步地，所述改性聚乳酸纤维层克重为15-20g/m2，莱赛尔纤维和木浆纤维复合层克重为20-30g/m2。
进一步地，所述改性聚乳酸中，季铵盐和马来酸酐共同接枝改性的聚乳酸和含羟基聚合物的质量比为4-6：1。
进一步地，所述季铵盐和马来酸酐共同接枝改性的聚乳酸是聚乳酸和季铵盐单体，马来酸酐接枝改性得到，聚乳酸，季铵盐单体，马来酸酐的质量比为100：0.6-1：1.8-3；优选地，所述季铵盐单体选自十二烷基二甲基烯丙基氯化铵，双十二烷基甲基烯丙基氯化铵，十四烷基二甲基烯丙基氯化铵，十六烷基二甲基烯丙基氯化铵中的至少一种。
本发明采用长链烷基季铵盐单体，在聚乳酸表面引发聚合接枝改性，使接枝改性的聚乳酸纤维层具有一定的抗菌性能，并且由于抗菌活性物质季铵盐是通过化学键合在聚乳酸表面的，这种抗菌性能稳定性好，相比于共混改性更能够发挥抗菌活性。
进一步地，所述季铵盐和马来酸酐共同接枝改性的聚乳酸的接枝率为1.9-4.2％，优选 2.1-3.5％。接枝率不易过高，否则侧链的马来酸酐和侧链含羟基的聚合物反应程度太大，交联密度大，影响所得改性聚乳酸纤维层的吸水性和保水性；接枝率不易过低，否则不能充分和侧链含羟基的聚合物有效复合，所得聚乳酸纤维层的力学强度不足。接枝率按照以下公式进行：A＝(m1-m0)/m0×100％，其中m1是接枝改性聚乳酸的质量，m0是聚乳酸质量。
接枝改性聚乳酸的制备方法为本领域所熟知，具体是聚乳酸与单体(季铵盐和马来酸酐) 在引发剂存在下反应得到接枝改性聚乳酸；其中，聚乳酸的重均分子量为15-30万，引发剂没有特别限定，本领域常用引发剂即可，比如过氧化二苯甲酰，过氧化二异丙苯。进一步地，聚乳酸，季铵盐单体，马来酸酐，引发剂的质量比为100：0.6-1：1.8-3：0.2-0.4。
在本发明一个优选技术方案中，采用熔融挤出法制备季铵盐和马来酸酐共同接枝改性的聚乳酸，具体是按照比例称量聚乳酸，季铵盐单体，马来酸酐和引发剂，将物料混合均匀，蒸除低沸点有机溶剂，加入双螺杆挤出机中熔融挤出进行接枝反应，双螺杆挤出机的温度为170-200℃，挤出物经过冷却，切粒，干燥得到马来酸酐接枝聚乳酸。所述低沸点有机溶剂选自丙酮，乙醇中的至少一种。
进一步地，所述改性聚乳酸纤维层是通过包括以下步骤的制备方法制得：将季铵盐和马来酸酐共同接枝改性的聚乳酸和含羟基聚合物一起通过双螺杆挤出机加热熔融，计量泵计量，纺丝，牵伸，冷却得到克重的15-20g/m2改性聚乳酸纤维层，接枝改性的聚乳酸和含羟基聚合物的质量比为4-6：1；双螺杆挤出各区温度在190-220℃，纺丝温度在200-220℃，冷却温度在5-15℃，牵伸时牵伸机的牵伸拉力控制为0.3-0.6bar。
优选地，所述侧链含羟基聚合物选自聚乙烯醇，含羟基烷基丙烯酸酯的聚合物中至少一种；所述含羟基烷基丙烯酸酯选自甲基丙烯酸羟乙酯、丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯、丙烯酸羟丁酯、甲基丙烯酸羟丁酯、聚乙二醇单甲基丙烯酸酯、聚乙二醇单丙烯酸酯中的至少一种；进一步优选地，所述侧链含羟基聚合物为聚乙烯醇和含羟基烷基丙烯酸酯的聚合物按照质量比1：1-1.7的混合物。
侧链含羟基的聚合物会和接枝改性聚乳酸上的酸酐在熔融条件下发生一定程度的酯化反应，使得改性聚乳酸的亲水性得到改善，增加了改性聚乳酸纤维的亲水性和保水性，并且改性聚乳酸的降解性能并没有受到显著的不利影响，在适当条件下仍保持了合适的降解率。发明人预料不到地发现，以特定比例的聚乙烯醇和含羟基烷基丙烯酸酯的聚合物的复配一起和季铵盐和马来酸酐共同接枝改性的聚乳酸一起熔融挤出，所得聚乳酸纤维的力学强度也同时得到了改善。
按照本发明上述工艺得到的改性聚乳酸纤维长度、纤度适中，具有很好的的柔软细腻的手感，使用时对皮肤亲和性好，不会有扎手和粗糙的感觉，同时表面的季铵盐发挥本体的抗菌作用，可以少使用甚至不使用乙醇作为消毒浸液也具有很好的抗菌活性。
莱赛尔纤维和木浆纤维复合层中，莱赛尔纤维和木浆纤维的质量比为1：2-3。莱赛尔纤维和木浆纤维复合层是将莱赛尔纤维和木浆纤维通过水刺复合制成复合无纺布。水刺压力为30-50bar。
更进一步地，所述湿巾浸液包括以下质量份的原料：100份去离子水、0-200份乙醇、 0.1-0.5份天然提取物、0-0.5份护肤剂、0-2份保湿剂。所述香精选自芦荟提取物、薰衣草提取物、桂花提取物、绿茶提取物中的至少一种；所述保湿剂选自甘油、丁二醇、山梨醇、木糖醇、聚乙二醇、透明质酸中的至少一种；所述护肤剂选自维生素A、维生素C、橄榄油中的至少一种。
本发明第二个目的是提供上述可降解的消毒护肤湿巾的制备方法，包括以下步骤：按照次序分别铺设改性聚乳酸纤维层，莱赛尔纤维和木浆纤维复合层，改性聚乳酸纤维层，经过水刺加固得到水刺布，轧液机轧液，干燥，卷成布卷，分切，添加湿巾浸液，包装，得到可降解的消毒湿护肤湿巾。
进一步地，所述水刺加固是经过5-7次水刺工艺，使各纤维层的纤维网相互缠结，加固成网；优选地，水刺压力为30-50bar。优选地，水刺工艺中水刺的压力是逐渐升高，再逐渐降低，比如，在本发明一个具体实施例，采用7次水刺工艺，1号水刺头的压力为30bar， 2号水刺头的压力为35bar，3号水刺头的压力为40bar，14号水刺头的压力为45bar，5号水刺头的压力为50bar，6号水刺头的压力为45bar，7号水刺头的压力为45bar。
具体实施方式
下面通过实施例对本申请进行进一步的阐述。本发明实施例所用原料均可来自于商业采购。本发明实施例中所述“份”，若无特别指明，均为质量份，所述“％”若无特别指明，均为质量百分比。
本发明聚乳酸采购自弹普乐橡塑优先公司，分子量约26万，为半透明颗粒，表面有光泽，熔体流动速率5.3g/min(190℃，2.16kg)。莱赛尔纤维采购自杭州兴都纺织品有限公司，100％天丝，70D；木浆纤维采购自山东富辉纺织科技有限公司，其中粘胶纤维长度38mm，纤度1.4旦；木浆纤维长度17mm，比重11.2g/cm3。聚甲基丙烯酸羟乙酯采购自菏泽昌盛源科技股份有限公司，分子量约5万。聚乙烯醇采购自郑州奥瑞金化工产品有限公司，牌号PVA2699，聚合物2600。
制备例1
将1.8份马来酸酐，0.6份十二烷基二甲基烯丙基氯化铵，0.2份过氧化二苯甲酰溶于 6份丙酮中，加入100份聚乳酸混合均匀，加热蒸除丙酮，从双螺杆挤出机中进料口进料，双螺杆挤出机各区温度是第一区170℃，第二区180℃，第三区185℃，第四区190℃，第五区190℃，熔融挤出后，经过冷却，洗涤除去未反应的单体和未接枝在聚乳酸上的聚合物，切粒，干燥得到季铵盐和马来酸酐共同接枝改性的聚乳酸，测试接枝率为2.1％。
制备例2
其他条件和操作与制备例1相同，区别在于马来酸酐用量为3份，十二烷基二甲基烯丙基氯化铵用量为1份，丙酮用量为9份，最终测试，所得接枝改性聚乳酸的接枝率为3.5％。
制备例3
其他条件和操作与制备例1相同，区别在于马来酸酐用量为1.5份，最终测试，所得接枝改性聚乳酸的接枝率为1.9％。
制备例4
其他条件和操作与制备例1相同，区别在于马来酸酐用量为4份，丙酮用量为10份，最终测试，所得接枝改性聚乳酸的接枝率为4.2％。
对比制备例
其他条件和操作与制备例1相同，区别在于不加入十二烷基二甲基烯丙基氯化铵。最终测试，所得接枝改性聚乳酸的接枝率为1.6％。
实施例1
(1)取40份制备例1得到的季铵盐和马来酸酐共同接枝改性的聚乳酸和10份侧链含羟基聚合物(聚乙烯醇和聚甲基丙烯酸羟乙酯按照质量比1:1的混合物)加入到双螺杆挤出机中加热熔融，双螺杆挤出机各区温度是第一区190℃，第二区200℃，第三区210℃，第四区210℃，第五区205℃，第六区205℃，经过计量泵剂量(温度205℃)，纺丝(温度205℃)，牵伸(牵伸拉力0.6bar)，冷却(12℃)，控制计量泵，使最终所得改性聚乳酸纤维层的克重为20g/m2。
(2)将莱赛尔纤维和木浆纤维通过水刺复合，水刺压力40bar，其中莱赛尔纤维和木浆纤维的质量比为1:2，得到莱赛尔纤维和木浆纤维的复合无纺布，克重30g/m2。
(3)将步骤(1)的改性聚乳酸纤维层，步骤(2)的莱赛尔纤维和木浆纤维的复合层，步骤(1) 的改性聚乳酸纤维层依次叠加进行水刺加固，水刺加固工艺为7道水刺，1号水刺头的压力为30bar，2号水刺头的压力为35bar，3号水刺头的压力为40bar，14号水刺头的压力为 45bar，5号水刺头的压力为50bar，6号水刺头的压力为45bar，7号水刺头的压力为45bar，水刺加固得水刺布，进行轧液，真空干燥(-0.2MPa，100℃)，卷帘(60m/s)，分切为10cm×7cm 尺寸得到湿巾载体，湿巾载体浸渍于湿巾浸液中，湿巾浸液是100份去离子水，0.1份芦荟提取物、0.1份绿茶提取物、0.3份苯氧乙醇，0.8份山梨醇、0.3份透明质酸、0.2份维生素A混合均匀制得，待湿巾载体吸液饱和后取出，封装即得消毒湿护肤湿巾。
实施例2
其他条件和操作与实施例1相同，区别在于，季铵盐和马来酸酐共同接枝改性的聚乳酸用量改为60份。
实施例3
其他条件和操作与实施例1相同，区别在于，季铵盐和马来酸酐共同接枝改性的聚乳酸用量改为30份。
实施例4
其他条件和操作与实施例1相同，区别在于，季铵盐和马来酸酐共同接枝改性的聚乳酸用量改为80份。
实施例5
其他条件和操作与实施例1相同，区别在于，10份侧链含羟基聚合物为聚乙烯醇和聚甲基丙烯酸羟乙酯按照质量比1:1.7的混合物。
实施例6
其他条件和操作与实施例1相同，区别在于，10份侧链含羟基聚合物为聚乙烯醇和聚甲基丙烯酸羟乙酯按照质量比1:0.8的混合物。
实施例7
其他条件和操作与实施例1相同，区别在于，10份侧链含羟基聚合物为聚乙烯醇和聚甲基丙烯酸羟乙酯按照质量比1:2的混合物。
实施例8
其他条件和操作与实施例1相同，区别在于，10份侧链含羟基聚合物为聚乙烯醇。
实施例9
其他条件和操作与实施例1相同，区别在于，10份侧链含羟基聚合物为聚甲基丙烯酸羟乙酯。
实施例10
其他条件和操作与实施例1相同，区别在于，步骤(1)中接枝改性聚乳酸为制备例2制得。
实施例11
其他条件和操作与实施例1相同，区别在于，步骤(1)中接枝改性聚乳酸为制备例3制得。
实施例12
其他条件和操作与实施例1相同，区别在于，步骤(1)中接枝改性聚乳酸为制备例4制得。
对比例1
其他条件和操作与实施例1相同，区别在于，直接以取50份制备例1得到的接枝改性聚乳酸在双螺杆挤出机中加热熔融，最终所得聚乳酸纤维层的克重为20g/m2。
对比例2
其他条件和操作与实施例1相同，区别在于，步骤(1)中接枝改性聚乳酸为对比制备例制得。
应用例
对上述实施例和对比例得到的复合无纺布擦拭材料进行以下性能测试，结果如下表1 所示。
吸水率按照GB/T 24218-2017进行测试。保水性是在25±1℃，65±5RH％条件下，30min后测试水分流失率。
断裂强力按照GB/T 24218-2017进行测试
生物可降解性，在25±5℃自然条件下，将擦拭材料埋藏在深度20cm的普通花池土壤中，从试验开始，每隔10天加入少量水，保持土壤湿润，60天后取出，测试降解率，降解率按照B＝(m0-mt)/m0×100％计算，其中m0是样品初始质量，mt是样品存放30天后的质量，测试先洗去表面泥土，干燥至恒重再进行测试。
抗菌性：以日常生活中代表性的大肠杆菌作为测试菌种。参照GB15979-2002方法对本发明湿巾的杀菌率进行测试，作用时间5min，杀菌率按照如下标准晶型等级评价：A级，杀菌率≥95％；B级：95％＞杀菌率≥90％；C级：杀菌率＜90％。
手感测试是挑选10名受试者使用本发明湿巾，按照1，2，3，4，5，5个分级进行评价打分，其中5份为满分，表示手感最为舒适，1份为最低分，表示手感最差，取平均值。
表1
Figure BDA0003494873330000081
从表1数据可知，本发明制备得到的抗菌护肤湿巾，可生物降解，对环境友好；同时综合性能优异，具有很好的吸水性，保水性，力学强度，手感柔和，是一种复合现在市场需求和环保要求的新型消毒抗菌湿巾。

Claims (10)

1.一种可降解的消毒湿护肤湿巾，包括湿巾浸液和可降解的复合无纺布作为湿巾浸液的载体，所述复合无纺为三明治结构，依次是改性聚乳酸纤维层，莱赛尔纤维和木浆纤维复合层，改性聚乳酸纤维层，所述改性聚乳酸是季铵盐和马来酸酐共同接枝改性的聚乳酸和侧链含羟基聚合物通过熔融共挤出得到。
2.根据权利要求1所述的可降解的消毒湿护肤湿巾，其特征在于，所述改性聚乳酸纤维层克重为15-20g/m2，莱赛尔纤维和木浆纤维复合层克重为20-30g/m2；优选地，莱赛尔纤维和木浆纤维复合层中，莱赛尔纤维和木浆纤维的质量比为1：2-3。
3.根据权利要求1所述的可降解的消毒湿护肤湿巾，其特征在于，所述改性聚乳酸中，季铵盐和马来酸酐共同接枝改性的聚乳酸和含羟基聚合物的质量比为4-6：1。
4.根据权利要求1所述的可降解的消毒湿护肤湿巾，其特征在于，所述季铵盐和马来酸酐共同接枝改性的聚乳酸是聚乳酸和季铵盐单体，马来酸酐接枝改性得到，聚乳酸，季铵盐单体，马来酸酐的质量比为100：0.6-1：1.8-3；优选地，所述季铵盐单体选自十二烷基二甲基烯丙基氯化铵，双十二烷基甲基烯丙基氯化铵，十四烷基二甲基烯丙基氯化铵，十六烷基二甲基烯丙基氯化铵中的至少一种。
5.根据权利要求1所述的可降解的消毒湿护肤湿巾，其特征在于，所述季铵盐和马来酸酐共同接枝改性的聚乳酸的接枝率为1.9-4.2％，优选2.1-3.5％。
6.根据权利要求1所述的可降解的消毒湿护肤湿巾，其特征在于，接枝改性聚乳酸的制备方法是聚乳酸与单体(季铵盐和马来酸酐)在引发剂存在下反应得到接枝改性聚乳酸；其中，聚乳酸的重均分子量为15-30万；优选地，聚乳酸，季铵盐单体，马来酸酐，引发剂的质量比为100：0.6-1：1.8-3：0.2-0.4；
更优选地，采用熔融挤出法制备季铵盐和马来酸酐共同接枝改性的聚乳酸，包括以下步骤：按照比例称量聚乳酸，季铵盐单体，马来酸酐和引发剂，将物料混合均匀，蒸除低沸点有机溶剂，加入双螺杆挤出机中熔融挤出进行接枝反应，双螺杆挤出机的温度为170-200℃，挤出物经过冷却，切粒，干燥得到马来酸酐接枝聚乳酸。
7.根据权利要求1所述的可降解的消毒湿护肤湿巾，其特征在于，所述改性聚乳酸纤维层是通过包括以下步骤的制备方法制得：将季铵盐和马来酸酐共同接枝改性的聚乳酸和含羟基聚合物一起通过双螺杆挤出机加热熔融，计量泵计量，纺丝，牵伸，冷却得到克重的15-20g/m2改性聚乳酸纤维层，接枝改性的聚乳酸和含羟基聚合物的质量比为4-6：1；双螺杆挤出各区温度在190-220℃，纺丝温度在200-220℃，冷却温度在5-15℃，牵伸时牵伸机的牵伸拉力控制为0.3-0.6bar；
优选地，所述侧链含羟基聚合物选自聚乙烯醇，含羟基烷基丙烯酸酯的聚合物中至少一种；所述含羟基烷基丙烯酸酯选自甲基丙烯酸羟乙酯、丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯、丙烯酸羟丁酯、甲基丙烯酸羟丁酯、聚乙二醇单甲基丙烯酸酯、聚乙二醇单丙烯酸酯中的至少一种。
8.根据权利要求7所述的可降解的消毒湿护肤湿巾，其特征在于，所述侧链含羟基聚合物为聚乙烯醇和含羟基烷基丙烯酸酯的聚合物按照质量比1：1-1.7的混合物。
9.根据权利要求1所述的可降解的消毒湿护肤湿巾，其特征在于，所述湿巾浸液包括以下质量份的原料：100份去离子水、0-200份乙醇、0.1-0.5份天然提取物、0-0.5份护肤剂、0-2份保湿剂；
优选地，所述香精选自芦荟提取物、薰衣草提取物、桂花提取物、绿茶提取物中的至少一种；所述保湿剂选自甘油、丁二醇、山梨醇、木糖醇、聚乙二醇、透明质酸中的至少一种；所述护肤剂选自维生素A、维生素C、橄榄油中的至少一种。
10.权利要求1-9任一项所述可降解的消毒湿护肤湿巾的制备方法，其特征在于，包括以下步骤：按照次序分别铺设改性聚乳酸纤维层，莱赛尔纤维和木浆纤维复合层，改性聚乳酸纤维层，经过水刺加固得到水刺布，轧液机轧液，干燥，卷成布卷，分切，添加湿巾浸液，包装，得到可降解的消毒湿护肤湿巾。
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