CN114214783A - 一种可降解的去油污湿巾及其制备方法 - Google Patents

一种可降解的去油污湿巾及其制备方法 Download PDF

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CN114214783A
CN114214783A CN202111560146.8A CN202111560146A CN114214783A CN 114214783 A CN114214783 A CN 114214783A CN 202111560146 A CN202111560146 A CN 202111560146A CN 114214783 A CN114214783 A CN 114214783A
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polylactic acid
degradable
degreasing
maleic anhydride
wet tissue
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CN114214783B (zh
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田晓辉
周守权
彭志云
徐桂平
唐圣明
徐敏
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去油污湿巾，包括湿巾基材和湿巾浸液，所述湿巾载体是三明治结构的复合无纺布结构，依次是改性聚乳酸纤维层，粘胶纤维和木浆纤维复合层，改性聚乳酸纤维层，所述改性聚乳酸是马来酸酐接枝聚乳酸和侧链含羟基聚合物通过熔融共挤出得到。本发明制备得到的去油污湿巾，引入了改性聚乳酸纤维层，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，对不同材质的油污清除效果好。

Description

一种可降解的去油污湿巾及其制备方法
技术领域
本申请涉无纺布领域，具体涉及一种可降解的去油污湿巾及其制备方法。
背景技术
厨房油渍污垢难以清除，传统的清理方法采用厨房清洁剂和抹布擦试进行清洁，但抹布长时间使用容易滋生霉菌，易使手部肌肤受到伤害，变得粗糙难看；而厨房清洁剂属于强碱性清洁剂或者含有有机溶剂，异味大，对皮肤会造成损伤，使用时往往需要带上手套进行，并不方便；而且挥发性的物质容易在空气中飘散，对呼吸道产生一定的危害和影响，不宜长期使用。
复合水刺无纺布是近年来新型的一种材料，是利用高压微细水流喷射到一层或多层纤维网，使纤维发生运动和位移，重新排列并且互相缠绕，得到具有一定机械强力的复合织物材料。水刺加固可以将多种纤维复合在一起，发挥各种纤维的作用，是目前复合无纺布的主要加工技术。目前去油污湿巾为了增加吸湿性，一般采用木浆纤维，但是其保水性较差，在清理厨房，特别是面积较大的厨房器具，比如抽油烟机，灶台等，需要反复的蘸取清洁剂，操作不方便而且容易清洁不干净。所以目前擦拭材料需要加入高吸水树脂和粘合剂，增加湿巾的保液能力和湿态下的强度，但是所得材料往往可降解性较差，不利于环保。非织造擦拭布作为一次性的使用产品，在城市生活中大量的被使用和丢弃，特别和残余垃圾一起掩埋地下，会对土壤土质造成一些不利影响。因此，可降解的擦拭材料是目前发展的趋势。
现有技术多用聚乳酸和其他纤维一起复合得到可降解的擦拭非织造材料，比如CN108221177A公开了一种三层复合非织造材料，是两个作为外层的聚乳酸纤维和作为里层木浆纤维基材得到的复合材料；该专利只是简单将聚乳酸纤维和木浆纤维通过水刺加固工艺制成的三明治复合结构，在吸水、保水和力学性能都还有待进一步提升。
CN111058303A公开了一种可降解高摩擦无纺布，是聚乳酸母粒熔融喷出滴落在木浆无纺布表面形成，但是该专利得到的材料只是从提高摩擦系数入手，没有考虑去油污湿巾的其他性能，比如吸水性、保水性和力学性能，实际上，单纯提高摩擦系数，而忽视其他性能，不能满足擦拭湿巾的要求。
专利CN110682635A公开了一种可降解材料清洁巾，是相互链接的吸尘曾和擦拭层，都是可生物降解的纤维材料无纺布，通过聚乳酸的点胶体连接。其多种材料都是采用可生物降解的材料制备而成。但是该专利制得湿巾，在湿态下力学强度不够打标，容易发生撕裂，掉毛等现象，还不能满足实际需求。
CN112813580A公开了一种壳生物降解的擦拭用非制造部，包括木浆纤维，聚乳酸。其实将聚乳酸熔融挤出，喷丝，拉伸得到聚乳酸纤维，梳理成网作为面层和底层，与中间层木浆纤维热粘和固定。
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，却忽视了擦拭材料所需要的吸水性、保水性，力学性能以及柔软的手感。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，作为擦拭材料不利于吸水性和保水性的提高。
开发一种可降解的去油污湿巾具有重要的实际意义，其在满足去油污湿巾需要的吸水性、保水性、力学强度，特别是在湿态下的力学强度，去油污能力等多方面综合性能的同时，具有一定的生物可降解性。
发明内容
为了解决现有技术中去油污的湿巾无法，或者很难生物降解，早场严重的环境问题，随意丢弃或者进行垃圾掩埋会对土壤造成污染，影响土质。本发明提供了一种厨房去污湿巾采用“三明治”结构的复合水刺无纺布，外层的上层和下层采用改性聚乳酸纤维层，中间层采用粘胶纤维和木浆纤维进行水刺复合制成复合无纺布，改善了传统无纺布强力差的问题，提高了断裂强力。本发明的复合水刺无纺布吸水性好，保水性强，力学性能，特别是在湿态下的力学性能好，并且可生物降解，不会对环境造成污染。本发明采用了自主研发的以去离子水、天然椰油精华、苯氧乙醇、香精为主要成份的厨房清洁乳液，产品去除油渍污能力强，好擦免洗，避免抹布隐患。天然椰精华，温和不伤手。使用方便，擦试过后留余芳香气息。产品去除油渍污垢能力强，便于携带使用方便。
本发明第一个目的是提供一种可降解的去油污湿巾，包括湿巾基材和湿巾浸液，所述湿巾载体是三明治结构的复合无纺布结构，依次是改性聚乳酸纤维层，粘胶纤维和木浆纤维复合层，改性聚乳酸纤维层，所述改性聚乳酸是马来酸酐接枝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20-30g/m2，粘胶纤维和木浆纤维复合层克重为35-50g/m2。
进一步地，马来酸酐接枝聚乳酸和侧链含羟基聚合物的质量比为3-10：1，优选5-8：1。
进一步地，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；优选地，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；更优选地，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马来酸酐接枝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，以特定比例的聚乙醇和含羟基烷基丙烯酸酯的聚合物的复配一起和马来酸酐接枝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。
马来酸酐接枝聚乳酸的接枝率为2-6％，优选2.3-3.6％。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。
马来酸酐接枝聚乳酸的制备方法为本领域所熟知，具体是聚乳酸与马来酸酐在引发剂存在下反应得到马来酸酐接枝聚乳酸；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，马来酸酐，引发剂的质量比为100：3-7：0.1-0.5，优选100：2.5-4：0.1-0.3。
在本发明一个优选技术方案中，采用熔融挤出法制备马来酸酐接枝聚乳酸，具体是按照比例称量聚乳酸，马来酸酐和引发剂，马来酸酐和引发剂，与聚乳酸混合均匀，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。进一步度，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：将马来酸酐接枝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20-30g/m2改性聚乳酸纤维层，马来酸酐接枝聚乳酸和含羟基聚合物的质量比为3-10：1，优选5-8：1；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。
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，并且卷曲度较高，在保持了较好的柔软细腻的手感同时，对油污的去除能力更加强劲。
粘胶纤维和木浆纤维复合层中，粘胶纤维和木浆纤维的质量比为1:2-3.5，优选1:2.5-2.8。
粘胶纤维和木浆纤维复合层是将粘胶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。
进一步地，所述湿巾浸液包括以下原料：去离子水、天然椰油精华、苯氧乙醇、香精。
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、1-3份天然椰油精华、0.1-0.4份苯氧乙醇、0.05-0.2份香精。
本发明第二个目的是提供上述可降解的去油污湿巾的制备方法，包括以下步骤：按照次序分别铺设改性聚乳酸纤维层，粘胶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，得到所述可降解的去油污湿巾。
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)。粘胶纤维和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2.5份马来酸酐，0.2份过氧化二苯甲酰溶于7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，切粒，干燥得到马来酸酐接枝聚乳酸，测试接枝率为2.3％。
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4份，丙酮用量为11份，最终测试，所得马来酸酐接枝聚乳酸的接枝率为3.6％。
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2份，丙酮用量为11份，最终测试，所得马来酸酐接枝聚乳酸的接枝率为1.8％。
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7份，丙酮用量为11份，最终测试，所得马来酸酐接枝聚乳酸的接枝率为6.1％。
实施例1
(1)取50份制备例1得到的马来酸酐接枝聚乳酸和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25g/m2。
(2)将粘胶纤维和木浆纤维通过水刺复合，水刺压力40bar，其中粘胶纤维和木浆纤维的质量比为1:2.5，得到粘胶纤维和木浆纤维的复合无纺布，克重40g/m2。
(3)将步骤(1)的改性聚乳酸纤维层，步骤(2)的粘胶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，2.2份天然椰油精华，0.3份苯氧乙醇，0.1份香精混合均匀制得，待湿巾载体吸液饱和后取出，封装即得去油污湿巾。
实施例2
其他条件和操作与实施例1相同，区别在于，马来酸酐接枝聚乳酸用量改为80份。
实施例3
其他条件和操作与实施例1相同，区别在于，马来酸酐接枝聚乳酸用量改为30份。
实施例4
其他条件和操作与实施例1相同，区别在于，马来酸酐接枝聚乳酸用量改为100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)中马来酸酐接枝聚乳酸为制备例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)中马来酸酐接枝聚乳酸为制备例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)中马来酸酐接枝聚乳酸为制备例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得到的马来酸酐接枝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25g/m2。
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。
去油污效果按照以下等级进行评定，手持湿巾对模拟的厨房油污(分别在陶瓷和PE材质上进行，模拟油污是植物油，动物油体积比例2:1的混合物，油污大致为圆形，直径3cm左右)进行擦拭，反复擦拭3次，按照以下标准进行去油污效果进行评价：等级A：擦拭后无油污残留，表面不挂水珠；等级B，肉眼观察无明显油污，挂水珠；等级C：肉眼观察有少量油污残留，挂水珠；等级D：肉眼可见，有明显的油污残留。
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 BDA0003420263860000071
Figure BDA0003420263860000081
从表1数据可知，本发明制备得到的去油污湿巾，引入了改性聚乳酸纤维层，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，对不同材质的油污清除效果好。

Claims (10)

1.一种可降解的去油污湿巾，包括湿巾基材和湿巾浸液，所述湿巾载体是三明治结构的复合无纺布结构，依次是改性聚乳酸纤维层，粘胶纤维和木浆纤维复合层，改性聚乳酸纤维层，所述改性聚乳酸是马来酸酐接枝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所述的可降解的去油污湿巾，其特征在于，所述改性聚乳酸纤维层克重为20-30g/m2，粘胶纤维和木浆纤维复合层克重为35-50g/m2。
3.根据权利要求1所述的可降解的去油污湿巾，其特征在于，马来酸酐接枝聚乳酸和侧链含羟基聚合物的质量比为3-10：1，优选5-8：1。
4.根据权利要求1所述的可降解的去油污湿巾，其特征在于，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；优选地，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；更优选地，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。
5.根据权利要求1所述的可降解的去油污湿巾，其特征在于，马来酸酐接枝聚乳酸的接枝率为2-6％，优选2.3-3.6％。
6.根据权利要求5所述的可降解的去油污湿巾，其特征在于，以聚乳酸，马来酸酐和引发剂为原料制备得到马来酸酐接枝聚乳酸，聚乳酸的重均分子量为15-30万，聚乳酸，马来酸酐，引发剂的质量比为100：3-7：0.1-0.5，优选100：2.5-4：0.1-0.3。
7.根据权利要求1所述的可降解的去油污湿巾，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：将马来酸酐接枝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，铺网得到克重的20-30g/m2改性聚乳酸纤维层，马来酸酐接枝聚乳酸和含羟基聚合物的质量比为3-10：1，优选5-8：1。
8.根据权利要求1所述的可降解的去油污湿巾，其特征在于，粘胶纤维和木浆纤维复合层中，粘胶纤维和木浆纤维的质量比为1:2-3.5，优选1:2.5-2.8。
9.根据权利要求1所述的可降解的去油污湿巾，其特征在于，所述湿巾浸液包括以下原料：去离子水、天然椰油精华、苯氧乙醇、香精；
优选地，所述湿巾浸液包括以下质量份的原料：100份去离子水、1-3份天然椰油精华、0.1-0.4份苯氧乙醇、0.05-0.2份香精。
10.权利要求1-9任一项所述的可降解的去油污湿巾的制备方法，包括以下步骤：按照次序分别铺设改性聚乳酸纤维层，粘胶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，得到所述可降解的去油污湿巾。
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CN115110204B (zh) * 2022-06-23 2024-02-09 星固科技(陕西)有限公司 一种聚乳酸复合熔喷过滤材料及其制备方法
CN115569083A (zh) * 2022-10-21 2023-01-06 浙江凯燕护理用品科技有限公司 一种高含水量抗菌卫生湿巾及其制备方法
CN115569083B (zh) * 2022-10-21 2024-01-30 浙江凯燕护理用品科技有限公司 一种高含水量抗菌湿巾及其制备方法
CN116043363A (zh) * 2022-12-19 2023-05-02 龙帛生物科技有限公司 一种生物基缓释洗涤纤维以及含有上述纤维的洗碗巾

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