CN105714549A - 无杀菌剂的预润湿海绵布 - Google Patents

无杀菌剂的预润湿海绵布 Download PDF

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CN105714549A
CN105714549A CN201511036077.5A CN201511036077A CN105714549A CN 105714549 A CN105714549 A CN 105714549A CN 201511036077 A CN201511036077 A CN 201511036077A CN 105714549 A CN105714549 A CN 105714549A
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CN105714549B (zh
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L·曼斯
N·蒂申
M·P·斯克洛茨
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Abstract

本发明描述了一种用吸湿作用的无机盐预润湿的基于再生纤维素的无杀菌剂的海绵布，其用纤维和/或网机械增强，并且包含吸湿活性盐，特征在于所述海绵布具有少于0.80的aw值.由于低aw值，该海绵布具有杀菌作用、抑菌作用、杀真菌作用和/或抑制真菌作用.该吸湿活性盐优选为氯化镁.其可以与其它的无机盐组合，与低分子量单-或多羟基醇组合，与糖，糖酯，单-或多元羧酸，单-或多元羧酸酯组合和/或与亲水聚合物组合。该海绵布优选通过粘胶法制备。

Description

无杀菌剂的预润湿海绵布
本发明涉及预润湿的、无杀真菌剂和/或杀细菌剂处理的基于再生纤维素的海绵布，其用内置纤维和/或网机械增强。
基于再生纤维素的用纤维和/或网机械增强的海绵布是已知的(参见EP2368936A2)。这种类型的干燥海绵布是相对硬的，用网增强的那些甚至由于弯曲而破碎。相对于干硬的海绵布，消费者更喜欢相对柔软的、预润湿的海绵布。而且，它们具有相对更多的体积和柔软的手感。因此，海绵布通常用吸湿活性盐的水溶液来处理，特别是用氯化镁溶液。然而，这种预润湿的海绵布的缺点是存在霉菌污染的趋势，特别是当它们在密封的薄膜包装中时。迄今为止，为了克服该缺点，预润湿的海绵布用杀菌剂处理。该物质通常添加进氯化镁溶液中。该氯化镁和某些杀菌剂在首次使用海绵布时清洗出来。然而，这种活性成分的存在，或通常更多地为杀菌剂，在未来将标注在该海绵布的销售包装上。这可能妨碍销售。进而，在海绵布中使用杀菌剂将经过审批，而且存在审批相当严格的趋势。
DE29618058U1公开了一种海绵布，其通过粘胶法制备，并且其提供杀菌剂。用γ-射线或过氧化物进行干海绵布的消毒也是已知的。
因此，本申请的目的是提供预润湿的海绵布，其用与杀菌剂不同的方法防止霉菌和其他微生物的污染。此处的“防止”指的是微生物被消灭或至少阻止它们繁殖。
微生物繁殖的先决条件是在该海绵布中存在活性的游离水。在材料中游离的有效水分的测度为aw值。其被定义为在相同温度下在每种情况下测量的材料的水蒸气压除以水的水蒸气压的商值。
该aw值在0-1之间，纯水的aw值为1。绝对无水的材料的aw值为0。细菌要求至少0.91的aw值，以能够进行繁殖。金黄色葡萄球菌也可以在0.86-0.90的aw值下存活。为了繁殖，酵母要求至少0.88-0.94的aw值，而霉菌甚至能够在0.80-0.85的aw值下繁殖。因此，对于具有高于0.80的aw值的预润湿海绵布来说，存在所述微生物传播的风险。特别是当该海绵布在水蒸气密封包装中和储存温度增加的时候更是这样。
因此，如果在海绵布中游离的可利用水的份数降低至aw值低于0.80时，上述目的可以在全范围内完成。通过这种方法，该海绵布的其他性能，特别是润湿厚度和机械稳定性，不应受到不良的影响。
因此，本申请提供用吸湿作用的无机盐预润湿并基于再生纤维素的无杀菌剂的海绵布，其用纤维和/或网机械增强，特征在于无菌海绵布包含至少一种物质，所述物质选自由无机盐、单-或多羟基低分子量脂肪醇、糖、糖酯、单-或多元羧酸，单一或多元羧酸的酯和亲水聚合物组成的组，其用量为足以使海绵布中的aw值小于0.8的量。
根据本发明的海绵布不包含杀真菌剂、杀细菌剂或其他杀菌剂，这种杀菌是应申报的，根据用于储存期间产品保护剂和用于纤维、皮革、树胶和聚合材料的保护剂所涉及Regulation(EU)No.528/2012的杀生剂产品中包含的所有现存的活性物质的***检验的工作计划，在2014年8月4日提交的CommissionDelegatedRegulation(EU)No.1062/2104的部分1的附件II，即用于本申请的申请资料中有效的6和9类型版本的产品。这个法规的部分1的附件II后附在本申请中。关于本申请，这种海绵布指的是“无杀菌剂”。
根据本发明的海绵布通常通过粘胶法生产。例如该方法描述在德国专利807439中。在该方法中，纤维胶与芒硝晶体混合以得到海绵布粗品。相对短的纤维(约2mm-30mm的纤维长度，优选3-6mm)也可以添加至该粗品中。该纤维通常为棉纤维(优选精梳落棉)，也可以使用由其他天然纤维和/或合成纤维制成的纤维。该纤维不必用强碱性纤维胶过度处理。该海绵布粗品以平面层的形式施用至旋转的穿孔传送带上，并且在传送带上传送至加热的沉淀和再生浴中，其中纤维自纤维胶中再生。该芒硝具有32-33℃的相对低的熔点。因此其在加热的沉淀和再生浴中熔化并且析出。相应的孔或腔则留在该海绵布中。然后该粗品海绵布传送通过各种清洗浴和(用于预润湿)通过具有吸湿盐溶液的浴，特别是氯化镁水溶液。然后多余的液体用一对轧辊的辅助而从该海绵布中除去。
根据本发明的海绵布中的水分通常为75-200wt％，优选100-150wt％，在每种情况下基于该海绵布的干重量。因此，它具有非常柔软和良好的“感觉”，这对消费者来说特别重要。
该海绵布粗品——具有或没有纤维——也可以以薄层的形式施用至网的一边或两边上。该网通常由聚酯或棉花组成。然后用该粗品覆盖的网传送通过沉淀、再生和清洗浴。
已发现，该aw值可以通过不同的方法降低。在本发明的一个实施方式中，除了添加作为柔软剂的吸湿盐之外，通过进一步添加至少一种无机盐，海绵布中的aw值降低到0.80以下。例如该进一步加入的盐为氯化锂、氯化钠(食盐)，氯化钾，硫酸钠，硫酸镁或硫酸钙。该进一步的无机盐通常不具有吸湿作用。该进一步的无机盐的用量方便地为10-30wt％，优选15-25wt％，在每种情况下基于该海绵布的干重量。
通常，该进一步的盐以溶液的形式与氯化镁溶液一起施用，例如传送该海绵布通过具有不同盐溶液的浸渍罐。该盐的浓度选择为使aw值降低至0.80以下的浓度。
下表汇总了不同盐的饱和溶液的aw值：
盐 LiCl MgCl2 K2CO3 Mg(NO3)2 NaBr SrCl2 NaCl KCl
aw值 0.112 0.327 0.438 0.529 0.577 0.708 0.753 0.843
在各种盐溶液中使用的溶剂可以为水，但是特别有利的是水与单-或多羟基低分子量醇的混合物。
本发明中的低分子量醇为至多具有6个碳原子的醇，其除了碳原子之外，仅包含氧和氢原子，并且仅仅具有羟基作为官能团。该单-或多羟基醇特别地为乙醇、正丙醇、异丙醇、亚乙基二醇(乙二醇)、二乙二醇、1，2一丙二醇或1，3一丙二醇或其混合物。具体到本发明，多羟基醇应理解为至多具有8个羟基，优选至多具有6个羟基的醇。
在进一步的实施方式中，该吸湿作用的无机盐、优选氯化镁的份数提高到超过目前已知份数，直至aw值达到少于0.8的份数。例如，这可通过用20-22％(强度重量)的水性氯化镁溶液浸渍该海绵布来完成。氯化镁的份数不能显著地增加到22wt％以上，否则该溶液太黏并且海绵布的吸收也不好。
单-或多羟基低分子量醇同样也降低海绵布的aw值。如果使用这种醇，那么海绵布中的盐份数可以减少。所述进一步的无机盐则可以完全分散。
最后，aw值降低至小于0.80也可以通过添加糖、糖酯、单-或多元羧酸、单-或多元羧酸酯或其混合物来完成。该糖通常是单-或二糖。糖或糖酯的份数为使得该海绵布不发粘并且使该海绵布的孔保持开放。该特定添加剂可以与盐和/或单-或多羟基醇结合。
最后，本发明所述的海绵布也可以包含亲水聚合物。它们也对降低aw值有贡献。合适的亲水聚合物为低聚糖和多糖及其衍生物，例如果聚糖和左聚糖，壳聚糖，卡拉胶，果胶和海藻酸盐及其衍生物，例如海藻酸丙二醇酯。合适的也可以是纤维素醚，例如羧基烷基纤维素(例如羧甲基纤维素)，羟基烷基纤维素(例如羟乙基-和羟丙基纤维素)和烷基羟基烷基纤维素(例如甲基羟乙基纤维素和乙基羟丙基纤维素)。合适的也可以为合成亲水聚合物，例如聚乙烯吡咯烷酮和具有乙烯吡咯烷酮单元的共聚物，具有下述单元的聚合物和共聚物：二甲基氨基乙基(甲基)丙烯酸酯，聚(甲基)丙烯酸和聚丙交酯。如果需要，该亲水聚合物在水中的溶解性可以用低分子量交联剂来调节，例如水合乙醛酸(在这里“低分子量”指的是少于300g/mol的分子量)。该亲水聚合物的份数可以为至多15wt％，优选5-10wt％，在每种情况下基于海绵布的干重量。
在根据本发明的海绵布中，可以组合来自上面描述的两个或多个基团的aw值降低剂。在每种情况下其具有少于0.80的aw值并且因此不再需要应申报的杀菌剂。
下面的实施例用于解释本发明。其中百份数应理解指的是重量百分比，除非特别指出或文中有直接证据。
为了确定aw值，使用来自G.LufftMess-undRegeltechnikGmbH，D-70736Fellbach的型号为5803.056的aw值测量计。仪器的校准使用特定纸来进行，其在20℃下，用饱和的水性氯化钡溶液润湿，直到有液滴低落。在测量期间，在常温下约2.5-3小时之后可以确定明确的aw值。对于变动的测量温度，通过带有校准表的设备来确保20℃有效的aw值。对于±1℃的偏差，可以考虑±0.002的aw值的校准。该校准表在15-25℃的范围内有效。下面实施例中规定的和在本申请其他部分的所有aw值都指的是20℃的温度。
实施例1(用改变浓度的氯化镁溶液浸渍的海绵布，没有杀菌剂)
将胶粘法生产的用棉纤维增强的海绵布放置在不同浓度的水性氯化镁溶液中，然后被挤压以除去过量的溶液。用增加浓度的氯化镁溶液浸渍的海绵布涉及下述样品1-5。包含大于22wt％的MgCl2的水性溶液不再被该海绵布充分吸收。
样品号 溶液中MgCl2的用量[wt％] aw值
1 16.1 0.85
2 18.1 0.825
3 20.0 0.78
4 22.0 0.75
按照方法AATCC100审查每个样品的抗菌性能。
对此，在每种情况下，0.5ml的在0.9％重量的水性NaCl溶液中的大肠杆菌(DSM1576)的悬浮液施用到每个海绵布试样中(边缘长度2cm)，并且该样品分别在36℃下在无菌的培养皿中储存24小时。然后，用10ml的BDD/E中和溶液从试样中除去细菌，并且通过平板倾注法确定细菌数量。所有的研究进行三次。上述样品不另外灭菌。
营养培养基：CASO-琼脂
培养时间：2天
细菌数量的减少计算如下：
基于初始的细菌数量：
减少％＝(T0-Tx)/T0×100
其中T0为刚接种后每个试样的细菌数量，和
Tx为接种24小时后每个试样的细菌数量。
结果汇总在下表中：
*CFU＝菌落形成单位
数据显示，仅在海绵布用20-22wt％的水性MgCl2溶液浸渍时达到最大抗菌效率。
实施例2(用不含额外杀菌剂的氯化镁溶液浸渍的海绵布和用包含氯化镁和杀菌剂的柔软剂溶液浸渍的海绵布)
对下述预润湿的海绵布样品进行研究：
测试了样品对霉菌黑曲霉(DSM1957)的抗性。根据DIN53931实施该测试。
“Demin.水”指的是去离子水。
对此，霉菌的孢子悬液施用至促繁殖营养培养基中，并且培养24小时，以使孢子发芽。然后，具有4cm直径的样品圆形试样放在培养的营养培养基中。在29±1℃下在潮湿条件中储存14天后，视觉和肉眼可见地评估在试样上和营养培养基周围的霉菌生长。
所有试样都表现出抑制区的形成(在样品附近的无繁殖区)。在营养培养基周围的表面发现显著的霉菌繁殖和形成显著的孢子。
该实验显示，如果软化剂溶液中的氯化镁浓度足够高的话，添加杀菌剂没有提高该海绵布对霉菌的抗性。将去离子水(demin.water)替换为工业用水没有导致杀霉菌性能上的任何变化。
实施例3(用MgCl2与其他盐的混合物浸渍的海绵布)
如在实施例2中描述的，根据DIN53931实施样品对霉菌黑曲霉(DSM1957)的抗性测试。然而，这种类型的装载是极限，因此在实际条件下没有上升。
在样品6的情况下，储存一周后，从边缘到中心出现具有显著孢子形成的显著繁殖(少于样品表面的25％被繁殖覆盖)；在储存两周后，样品表面完全(100％)被繁殖覆盖。
在样品7的情况下，储存一周后，从边缘到中心覆盖具有显著孢子形成的显著繁殖(少于样品表面的25％被繁殖覆盖)；在储存两周后，样品表面被各自的菌落覆盖(样品表面的25-75％被繁殖覆盖)。结果显示，根据盐的类型，抗菌效果是不同的。
此外，如实施例1中所描述的，还检测了样品对金黄色葡萄球菌(DSM799)和大肠杆菌(DSM1576)的抗菌效果。该检测结果汇总在下表中。
测试细菌金黄色葡萄球菌：
测试细菌大肠杆菌：
为了对比，在目前通常的海绵布上测定aw值，其用与本申请不同浓度的氯化镁溶液预润湿，海绵布均通过胶粘法制备并且都包含棉纤维作为机械增强剂，但是不含有网。该值汇总在下表中。也包含只用水润湿的海绵布的数据。
最后，也测定了来源于竞争对手的预润湿纤维素海绵布的aw值。在这些海绵布中的氯化镁含量没有标注并且没有进行测定。
)1：SpontexAquaPur，苹果绿
)2：SpontexAquaPur，红
)3：WettexViledaOriginal，黄
)4：WettexViledaOriginal，蓝
2014年8月4日提交的Regulation(EU)No.1062/2104的附件II的部分1的摘录

Claims (6)

1.用吸湿作用的无机盐预润湿并基于再生纤维素的无杀菌剂的海绵布，其用纤维和/或网机械增强，其特征在于海绵布包含至少一种物质，所述物质选自由无机盐、单-或多羟基低分子量脂肪醇、糖、糖酯、单-或多元羧酸、单-或多元羧酸的酯和亲水聚合物组成的组，其用量为足以使海绵布中的aw值小于0.8的量。
2.根据权利要求1的海绵布，其特征在于：该无机盐为氯化锂、氯化钠，氯化钾，硫酸钠，氯化镁，硫酸镁和/或硫酸钙。
3.根据权利要求1或2的海绵布，其特征在于：该多羟基低分子量脂肪醇为乙醇、正丙醇、异丙醇、乙二醇、二乙二醇、1，2-丙二醇或1，3-丙二醇或其混合物。
4.根据权利要求1-3中一项或多项的海绵布，其特征在于：亲水聚合物为低聚糖或多糖或其衍生物，优选果聚糖或左聚糖，壳聚糖，卡拉胶，果胶，海藻酸盐或其衍生物，特别是海藻酸丙二醇酯，纤维素醚，优选羧基烷基纤维素，羟基烷基纤维素或烷基羟基烷基纤维素，聚乙烯吡咯烷酮或具有乙烯吡咯烷酮单元的共聚物，具有下述单元的聚合物或共聚物：(甲基)丙烯酸二甲氨基乙酯，聚(甲基)丙烯酸或聚丙交酯.
5.根据权利要求1-4中一项或多项的海绵布，其特征在于：海绵布中的水分通常为75-200wt％，优选100-150wt％，在每种情况下基于该海绵布的干重量.
6.根据权利要求1-5中一项或多项的海绵布，其特征在于：其通过粘胶法制备。
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