CN105008611A - 化学改性的纤维素纤维的处理 - Google Patents

化学改性的纤维素纤维的处理 Download PDF

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CN105008611A
CN105008611A CN201380073403.2A CN201380073403A CN105008611A CN 105008611 A CN105008611 A CN 105008611A CN 201380073403 A CN201380073403 A CN 201380073403A CN 105008611 A CN105008611 A CN 105008611A
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W.L.邦内芬
L.L.巴拉米
S.弗雷
D.帕森斯
G.斯托里
J.汤普森
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Convatec Technologies Inc
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Abstract

一种具有至少7wt%的含湿量的化学改性的纤维素纤维或长丝，所述纤维素纤维或长丝通过包括以下步骤的方法获得：(i)获得纤维素纤维或长丝和通过取代化学改性纤维素，以增加其吸收性；(ii)在步骤(i)之后在含有水和最多至99wt%的水混溶性有机溶剂的混合物中洗涤所述纤维；(iii)将所述纤维干燥至按重量计至少7%的含湿量，以此为摘要。

Description

化学改性的纤维素纤维的处理
本发明涉及化学改性的纤维素纤维和用于由它们制备非织造纤维网的方法。尤其是，它涉及可以梳理机上被梳理以产生网的化学改性的纤维素纤维。所述纤维可例如通过针刺或缠结该网而被最终加工成非织造织物，所述织物适于用在吸收性个人产品或吸收性医疗产品如伤口敷料中。还描述了适合形成化学改性的纤维素纤维的网或化学改性的纤维与其他非凝胶纤维，例如粘胶或天丝（Tencel）或其他纤维素纤维的共混物的网的梳理方法。
吸收性纤维素纤维是为人熟知的。例如GB-A-2220881和GB-A-2094802描述了由再生纤维素纤维(粘胶丝)纤维或由棉生产羧甲基纤维素纤维。还已知具有较大吸收性和强度的羧甲基纤维素纤维可以由溶纺纤维素纤维制造。此类纤维被描述在EP 0616650中，并且通过使溶纺纤维素纤维与强碱和一氯乙酸试剂反应制造。还已知替代的对纤维素纤维的化学改性是可能的，并且也具有增加纤维素纤维的吸收性的效果。可以例如通过磺化改性纤维素纤维，例如通过在形成醚键构成纤维素骨架的葡糖酐单体上的一个或多个羟基基团处用烷基磺酸酯基（alkyl sulphonate）取代。这种类型的改性纤维素被称为纤维素磺酸酯或纤维素烷基磺酸酯，其一些不溶性形式被描述在WO2012 / 061225中。
纤维素纤维的改性需要将所述纤维暴露于一种或多种通过取代来改性纤维素的试剂，取代度决定了所述纤维的吸收性和溶解性。随着取代度增加，改性的纤维素变得越来越可溶。随着溶解性增加，吸收性也增加。
对于一些应用而言，例如对于吸收性凝胶伤口敷料，需要化学改性的纤维是不溶性的，并且当暴露于伤口流体时保留一些它们的纤维形式，并因此需要在溶解性和吸收性之间找到平衡。所述化学改性的纤维可以是丝束、长丝、丝条、纱线或短纤维、织造织物、非织造织物或针织织物的形式。
一旦在酸中已经发生了改性与中和，则需要洗涤纤维以除去任何未反应的碱、氯乙酸盐、烷基磺酸盐、其他改性剂或任何副产物如氯化钠或乙醇酸钠。一般在最初使用水洗，优选使用水与水混溶性有机溶剂的混合物，例如水和IMS的混合物，所述洗液的主要部分是有机溶剂。所述洗液可以含有有机羟基化合物、表面活性剂和/或酸。所述有机羟基化合物是含有至少一个醇式羟基的化合物，例如乙醇、甲醇或其他低分子量的醇，和/或化合物诸如乙二醇或丙二醇。
最终的洗液或油剂(finish)通常含有大百分比的醇，例如，99%的工业乙醇和1%的乳化剂或100%的醇。在洗涤之后，如EP 0680344中所述，通过强制空气干燥或辐射热干燥在低温下干燥纤维。
作为在改性之后纤维所经历的一个或多个洗涤步骤，其涉及使用相对高百分比的有机溶剂，如工业乙醇，所述纤维的干燥需要从环境和安全性的角度来进行管理所释放的溶剂。减少在洗涤过程中使用的有机溶剂的百分比，从而可容易​​地满足环境和安全标准将是所需要的。由于材料和责任的成本降低，因此使用较低百分比的有机溶剂还存在潜在的成本和效率的优势。
我们已经发现，减少例如用于洗涤改性的纤维素纤维的洗涤液中的有机溶剂的百分比产生了具有较低的拉伸强度的纤维，使得它们较不适合于在纺织机械如梳理机上进行加工。较低的拉伸强度可导致在梳理时纤维断裂的问题，这产生了较高水平的空气传播的棉绒或灰尘(飞毛)(fly))和断裂纤维从成品织物的较大脱落。较高水平的飞毛使增加对织物生产过程中的清洁和环境管理成为必要，这进而增加了成本。由于在制造过程中纤维趋向于从织物掉落，在该过程中还存在更多的废物。
纤维断裂还可不利地影响短纤维长度(staple length)，这具有降低由纤维制成的梳理网和非织造织物的强度的影响。可能的是纤维断裂导致了其中没有制备出非织造垫的失效的梳理过程。当敷料的完整性可能受到损害时，较弱的产品可能更难以从伤口去除。
现在我们已经发现可以通过对纤维中的含湿量进行受控管理来以减轻改性纤维中的低拉伸强度的问题。
因此，本发明提供了通过处理具有至少7wt%的含湿量的纤维制备的化学改性的纤维素纤维网，其具有至少3 N每cm(N/cm)的横向上的拉伸强度。
通过控制在作为化学改性方法的一部分的对改性纤维的洗涤之后的干燥过程或者在干燥之后通过调理纤维以将它们的含湿量增加到至少7%来控制所述纤维的含湿量，将纤维的拉伸强度增加到其中可以例如在梳理机上处理所述纤维以产生非织造纤维网而不产生过度的飞毛或不从由所述网制成的织物脱落的程度。优选地，通过控制在作为化学改性方法的一部分的对改性纤维的洗涤之后的干燥过程来使所述纤维的含湿量保持在11-20%。
优选地，在具有80-120gsm的定量的针刺网上于横向上测量拉伸强度。
因此，本发明在另一方面中提供了用于制备化学改性的纤维素纤维的非织造网的方法，所述方法包括以下步骤：
(i) 获得具有至少7%的含湿量的化学改性的纤维素纤维；
(ii) 梳理所述纤维以制成纤维的非织造网。
所述纤维通常是由使用在洗涤液中包含小于99wt%如95wt%的有机溶剂的洗液或最终冲洗液（rinse）的改性方法产生的那些。通过控制含湿量，可以将所述纤维加工成固结的形式（consolidated form），其允许通过常规的梳理手段生产织物同时减轻了在织物生产设施环境中的纤维断裂和飞毛的问题。固结的形式可以例如是纱线、丝条、织造织物、非织造织物或针织织物。
当纤维是用织造机械进行加工时，如果发现所述纤维的含湿量太低，则通过将所述纤维暴露于水分丰富的环境至少24小时来增加改性纤维素纤维的含湿量。可选地，可控制在化学改性方法结束时的对纤维的干燥，以将所述纤维的含湿量保持在高于7%，直到所述纤维经受进一步的处理，如用织造机械例如通过梳理和针刺。
优选地，经梳理、针刺的纤维网具有3N/cm-25N/cm、更优选7N/cm-25N/cm、且最优选10N/cm-25N/cm的拉伸强度。
通过切割出五个25mm×75mm的尺寸的样本测量经梳理、针刺网的拉伸强度，其中长尺寸在待测试的方向上。拉伸测试是以50mm标距长度(有效的测试织物长度)进行。将样品的一端固定在拉伸测试机的上部夹具并使其悬垂入下部夹具中。然后在不拉伸样品或使其为松弛的情况下通过闭合所述夹具将样品固定。将十字头速度设定至100mm/min并将样品拉至断裂。通过断裂时的力除以以cm表示的样品宽度来计算拉伸强度。
优选地，在用织造机械进行处理之前纤维的含湿量是7wt%-20wt%，且更优选11%-18%。更优选地，含湿量是11.5wt%-15wt%，且最优选其为12wt%-15wt%。12.5%-15%的含湿量是特别优选的，且15%是最优选的。
术语含湿量表示纤维样品中含有的水分的量(按重量测量)，其以其经调理过的重量的百分数的形式并通过干燥时的损失来测量。
纤维的含湿量是通过使用按照仪器手册操作的水分天平（moisture balance）计算干燥时的损失来测量的。为方便起见，在制造所述纤维的过程期间，对含湿量的比较测量可使用水分测定仪（moisture meter）例如Aquaboy(TEMI)进行。
本发明中的术语梳理是指解开、清洁和混杂纤维的机械过程，以产生适于进一步处理的连续的网或丝条。
在本发明的进一步方面中，本发明提供了具有至少7wt%的含湿量的化学改性的纤维素纤维。
现在将通过以下实施例来举例说明本发明。
实施例 1
一旦经梳理和针刺便通过测量使用具有不同的醇含量的洗液制备的干燥过的改性纤维素纤维的初始含湿量来进行纤维的含湿量相对于其拉伸强度的比较。然后通过在潮湿氛围中于55-60%的相对湿度下将所述纤维调理24小时来增加该初始含湿量，并再次测量该经针刺的织物的拉伸强度。图1显示了在水分调理以增加含湿量之前和之后的纤维含湿量与经梳理、针刺的织物在横向上的拉伸强度的相对关系。
结果表明，纤维的含湿量影响所得经梳理和针刺的网的拉伸强度。在图1的表中的开头为IDA的列是指在作为改性方法的一部分的洗涤液中使用的IDA(工业变性乙醇)的百分比。开头为%的列是指纤维中的%水分并且开头为N/cm的列是指所得的经梳理、针刺的网在横向上的拉伸强度。从图1中可以看出，降低洗涤液中的IDA%对由未经调理的纤维制成的经梳理和针刺的网的拉伸强度具有负面影响。还可以看出，一旦那些纤维的含湿量提高到大于11%，如12.5-14%的水分，则那些经梳理、针刺的网的拉伸强度值增加。
实施例 2
含湿量对含银的伤口敷料的拉伸强度的影响。
通过将溶纺纤维素丝束改性至0.3的取代度以形成羧甲基纤维素，用有机酸中和到5.5的pH来制备敷料。通过在主要为有机的溶剂中的离子交换方法如通过在Ep1343510中描述的方法添加1.2%的阳离子银，在含有氯化钠和EDTA二钠的含水有机溶液中洗涤以用于光稳定并携带约0.4%的EDTA。接着在含有纤维整理剂(包含吐温20和苄索氯铵)的有机溶剂洗液中洗涤(以在经整理的产物上得到0.135%wt/wt BeCl)，然后用暖空气干燥，切割成切断纤维（staple）并通过梳理和针刺法（needle punching process）加工成非织造毡。从网中切割适当尺寸的敷料并将其包装在不能渗透光、水分的和蒸气的热密封的箔袋中。
从包装中取出所述敷料，然后使其经受各种受控的环境。
受控的环境
如包装时的氛围，在无任何预调理的情况下进行测试
零湿度：储存在具有在一层硅胶干燥剂上方的3个穿孔有机玻璃架的正方形的干燥器中，调理最少5天
25℃/ 60%RH，调理至少6天
30℃/ 65%RH，调理至少6天
40℃/ 75%RH，调理至少6天
在打开包装后立即测试样品(如包装时的氛围)。将从其他环境取出的样品在取出期间密封在塑料袋中，然后立即测试。塑料袋(也在相应的受控环境下进行预调理)用于保持样品的环境湿度直到测试时间点。
干燥时的损失 (LOD)
使用按照仪器手册操作的Ohaus水份天平MB23来确定样品的LOD。使用大于1克的样品质量。将样品切割以适合在秤盘内，确保与加热元件存在足够间隙。使用具有110℃的最高温度极限的标准化方法。当样品质量停止减少并稳定时自动确定终结点。在这些条件下所述织物没有烧焦。通常，样品将经受10分钟的循环。
织物厚度 ( 蓬松度 (loft))
使用Hampden Soft Materials Thickness Gauge, Model FMTml-4D, S/N 14082来测试样品。针对每批次6个敷料来确定织物厚度(有时称为蓬松度)。
织物干拉伸强度
使用带条切割模具和压机（press）沿长度(纵向)和跨宽度(横向)切割出2.5cm×7.5cm矩形条。如表1所述调理样品。当以每分钟100mm的恒定分开速率下拉伸50mm测试长度时，记录峰值力以及在产生该力的时延伸率。
结果
表1
干燥时的损失是所有可以通过在110℃下加热被除去的挥发性物质的总和。这些包括乙醇、水和一定程度的乙酸。
对于此特定的纤维，对于此实施例而言，纺织试验表明用于根据本发明的伤口敷料的纤维可以在42%-50%RH于约18-20℃下成功地被纺织。试验表明可以有效地梳理具有10.5%-11.5%w/w的含湿量的纤维。
结果表明，拉伸强度、蓬松度和LOD全部都是平衡含湿量的函数。结果表明，将能够纺织具有大于9%的含湿量的纤维以制备适用于本发明中的敷料。
实施例 3
材料
在该研究中使用两种凝胶纤维类型；纤维素乙基磺酸酯(CES)和羧甲基纤维素(CMC)。
表1对使用的凝胶纤维的总结
凝胶纤维
CES纤维丝束
CMC纤维丝束
方法
如BS EN 5079：1996所述将单纤维安装到梳理窗口。
另外，制备丝束捆用于评估含湿量。
在所选的相对湿度下调理最少16小时之前，在105℃下用烘箱干燥纤维1小时。称取烘箱干燥的丝束捆的质量(W1)和经调理的丝束捆的质量(W2)以使用等式1来评估所述纤维的含湿量。
等式1：
使用在BS EN 5079：1996中描述的方法测试经调理的样品的单纤维拉伸强度。
在45%RH、65%RH和85%RH下测试纤维。
结果
结果发现，如表2中所示，在65%RH下调理的样品中看到显著高于(P≤0.05)在45%RH和85%RH下调理的那些样品的拉伸强度。
表2 结果的总结

Claims (43)

1.通过处理具有至少7wt%的含湿量的纤维获得的化学改性的纤维素针刺纤维网，其具有在横向上测得的至少3N/cm的拉伸强度。
2.具有至少7wt%的含湿量的化学改性的纤维素纤维。
3.如权利要求1或权利要求2所述的化学改性的纤维网或化学改性的纤维，其具有11wt%-18wt%的含湿量。
4.如权利要求1或权利要求2所述的化学改性的纤维网或化学改性的纤维，其具有12wt%-15wt%的含湿量。
5.如权利要求1或权利要求2所述的化学改性的纤维网或化学改性的纤维，其具有15wt%的含湿量。
6.如前述权利要求中任一项所述的化学改性的纤维网或化学改性的纤维，其中所述纤维通过包括使用含有小于99wt%的水混溶性有机溶剂的洗涤组合物的洗涤步骤的化学改性方法获得。
7.如权利要求1或权利要求3-6中任一项所述的化学改性的纤维网，通过梳理和针刺对其进行处理，其具有3N/cm-25N/cm的拉伸强度。
8.如权利要求7所述的化学改性的纤维网，其具有80-120gsm的定量。
9.如权利要求7或8所述的化学改性的纤维网，其具有7N/cm-25N/cm的拉伸强度。
10.如权利要求7、8或9所述的化学改性的纤维网，其具有10N/cm -25N/cm的拉伸强度。
11.用于生产化学改性的纤维素纤维的非织造网的方法，所述方法包括以下步骤：
(i) 获得具有至少7%的含湿量的化学改性的纤维素纤维；
(ii) 梳理和针刺所述纤维，以制成纤维的非织造网。
12.如权利要求11所述的方法，其中所述纤维通过包括其中用含有小于99wt%的有机溶剂的组合物洗涤所述纤维的步骤的化学改性方法获得。
13.如权利要求12所述的方法，其中洗涤组合物包含小于95wt%的水混溶性有机溶剂。
14.如权利要求12-13中任一项所述的方法，其中在所述洗涤步骤之后，将所述纤维干燥至至少7%的含湿量。
15.如权利要求12所述的方法，其中所述纤维通过在具有至少40%的相对湿度的空气中调理所述纤维以将所述纤维的含湿量增加到至少7%获得。
16.如权利要求18所述的方法，其中所述相对湿度为45%-85%。
17.如权利要求18或19所述的方法，其中所述相对湿度为50%-65%。
18.如权利要求11-17中任一项所述的方法，其中所述纤维具有11wt%-18wt%的含湿量。
19.如权利要求11-18中任一项所述的方法，其中所述纤维具有12wt%-15wt%的含湿量。
20.如权利要求11-19中任一项所述的方法，其中所述纤维具有14wt%-15wt%的含湿量。
21.用于生产化学改性的纤维素纤维的非织造网的方法， 所述方法包括以下步骤：
(i) 获得纤维素纤维或长丝并通过取代化学改性纤维素，以增加其吸收性，然后；
(ii) 用含有水和最多至99wt%的水混溶性有机溶剂的组合物洗涤所述纤维；并然后
(iii) 在受控的气氛中将所述纤维干燥至至少7wt%的含湿量。
22.如权利要求21所述的方法，其中洗涤组合物含有小于95wt%的有机溶剂。
23.如权利要求21或22所述的方法，其中所述方法包括针刺所述网以形成伤口敷料的附加步骤。
24.如权利要求23所述的方法，其中所述方法包括在使所述敷料保持在无菌和受控的环境中的囊袋中将所述敷料密封和灭菌的附加步骤。
25.如权利要求21-24中任一项所述的方法，其中所述纤维具有11wt%-18wt%的含湿量。
26.如权利要求21-25中任一项所述的方法，其中所述纤维具有12wt%-15wt%的含湿量。
27.如权利要求21-26中任一项所述的方法，其中所述纤维具有14wt%-15wt%的含湿量。
28.具有至少7wt%的含湿量的化学改性的纤维素纤维或长丝，其通过包括以下步骤的方法获得：
(i) 获得纤维素纤维或长丝并通过取代化学改性纤维素，以增加其吸收性；
(ii) 在步骤(i)之后在含有水和最多至99wt%的水混溶性有机溶剂的混合物中洗涤所述纤维；
(iii) 将所述纤维干燥至至少7wt%的含湿量。
29.如权利要求28所述的方法，其中所述洗涤组合物含有小于95wt%的有机溶剂。
30.如权利要求28或29所述的方法，其中所述方法包括梳理和针刺所述纤维以形成伤口敷料的附加步骤。
31.如权利要求30所述的方法，其中所述方法包括在无菌环境中保持所述敷料的含湿量的囊袋中将所述敷料密封和灭菌的附加步骤。
32.如权利要求28-31中任一项所述的方法，其中所述纤维或长丝具有11wt%-18wt%的含湿量。
33.如权利要求28-32中任一项所述的方法，其中所述纤维或长丝具有12wt%-15wt%的含湿量。
34.如权利要求28-33中任一项所述的方法，其中所述纤维或长丝具有14wt%-15wt%的含湿量。
35.用于生产化学改性的纤维素纤维的非织造网的方法，所述方法包括以下步骤：
(i) 获得纤维素纤维或长丝并通过取代化学改性纤维素，以增加其吸收性，然后；
(ii) 用含有最多至99wt%的有机溶剂的组合物洗涤所述纤维；并然后
(iii) 在具有至少40%的相对湿度的气氛中调理所述纤维，以将所述纤维的含湿量增加到至少7%。
36.如权利要求35所述的方法，其中洗涤组合物含有小于95wt%的有机溶剂。
37.如权利要求35或36所述的方法，其中所述调理是在具有45%-85%的相对湿度的空气中。
38.如权利要求35-37中任一项所述的方法，其中所述相对湿度为50%-65%。
39.如权利要求35-38中任一项所述的方法，其中所述纤维具有11wt%-18wt%的含湿量。
40.如权利要求35-39中任一项所述的方法，其中所述纤维具有12wt%-15wt%的含湿量。
41.如权利要求35-40中任一项所述的方法，其中所述纤维具有14wt%-15wt%的含湿量。
42.如权利要求35-41中任一项所述的方法，其中所述方法包括梳理和针刺所述纤维以形成伤口敷料的附加步骤。
43.如权利要求42所述的方法，其中所述方法包括在无菌环境中保持所述敷料的含湿量的囊袋中将所述敷料密封和灭菌的附加步骤。
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US20150354096A1 (en) 2015-12-10
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