CN102597343A - 生物可降解的纤维及其制造方法 - Google Patents
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Abstract
本发明涉及包含纤维素和醋酸纤维素复合丝的生物可降解的纤维,和制备这类纤维的方法,所述方法包括在离子型液体或N-甲基吗啉-N-氧化物(NMMO)中提供包含纤维素和醋酸纤维素混合物的溶液粘稠物,并将所述混合物纺入或铸入质子性溶剂中以产生纤维。本发明还涉及由这类纤维制成的材料以及由这类材料制成的服装或软装饰。
Description
本发明涉及生物可降解的复合纤维。
制造纤维最迫切的问题之一就是纤维的生物降解速率。根据环境条件,醋酸纤维素纤维将花费一个月至三年来进行生物降解。
已经提出一系列制备尤其适用于制造卷烟纤维的可生物降解纤维的方法,包括使用醋酸纤维素与其它可生物降解聚合物的复合物、用于提高醋酸纤维素降解速率的添加剂、具有用于提高生物降解性的低取代度(DS)的醋酸纤维素以及生物可降解的聚合物,如PHB/PVB和淀粉,作为纤维或纤维的原材料。
然而,到目前为止,还没有找到能够制造出足够快速地降解的消费者可接受的纤维的令人满意的商业方案。
本发明力图解决这些问题。
本发明提供了生物可降解的纤维,其包含纤维素和醋酸纤维素复合丝。
纤维素和醋酸纤维素通常以纤维或薄膜的形式铸制。一方面,本发明涉及纤维。本发明优选的纤维包含从纤维素和醋酸纤维素凝固溶液纺制出的纤维。
本文所指的纤维素/醋酸纤维素复合丝应被理解为表示从包含纤维素和醋酸纤维素的粘稠物纺制出的细丝。
我们发现,纤维素/醋酸纤维素复合丝的生物降解性显著大于仅包含纤维素或醋酸纤维素的等同丝。不希望受到任何这类理论的束缚,我们认为,复合物中醋酸盐的存在可以破坏纤维素的结晶度,导致该复合物能够比纤维素本身更快地得到降解。
按照常规,纤维素是从纤维胶铸制或纺制成的,并且从同一混合物难以或不可能铸制或纺制出醋酸纤维素,因为醋酸纤维素在这些条件下有水解的可能。相反,按照常规,醋酸纤维素是从丙酮铸制或纺制成的,并且从同一混合物难以或不可能铸制或纺制出纤维素,因为纤维素在丙酮中的溶解度受限。
然而,我们发现通过从离子型液体(IL)或从N-甲基吗啉-N-氧化物(NMMO)铸制或纺制纤维素和醋酸纤维素,可能形成包含这些材料的复合混合物的纺成纤维和铸型薄膜。这类复合物的提高的生物降解性及其在纤维制造中的适用性在之前是没有意识到的。
因此,本发明的纤维优选由从离子型液体(IL)或从N-甲基吗啉-N-氧化物(NMMO)纺制或铸制出的作为混合物的纤维素和醋酸纤维素纤维制成。
IL和NMMO用于溶解纤维素和其它聚合物的用途已被充分证明,例如在阿拉巴马大学的US20050288484和US 20070006774、北卡罗来纳州立大学的US20080188636以及Holbrey等的WO2005098546中。大量的离子型液体,包括前述出版物中公开的那些,适于溶解纤维素和醋酸纤维素,并适于从其铸制成作为混合物的纤维或薄膜。合适的IL的一般类型包括基于咪唑、吡咯、噻唑或吡唑阳离子与卤素、磷酸盐、羧酸盐或金属氯化物阴离子的结合的那些IL。特别优选的IL包括1-丁基-3-甲基咪唑氯化物(BMIM-Cl)、1-丁基-3-甲基咪唑醋酸盐(BMIM-Ac)和1-乙基-3-甲基咪唑醋酸盐(EMIM-Ac)。
从其纺制或铸制纤维的纤维素和醋酸纤维素溶液在本文称为粘稠物。粘稠物还可以包含非质子性溶剂如DMSO、DMF、THF或二噁烷,从而促进纤维素和/或醋酸纤维素的溶解。一种特别优选的非质子性溶剂是DMSO。
粘稠物中醋酸纤维素和纤维素的混合物还可以包含一种或多种其它热塑性材料,例如聚羟基脂肪酸酯如PHB和/或PHVB,这些材料可以为本发明的纤维添加其它功能如防水功能。其它功能性添加剂可以包括用于功能目的的醋精、聚丙烯腈(PAN)、聚-2-羟乙基丙烯酸甲酯(PHEMA)、聚乙烯醇(PVA)、聚苯胺和聚乙二醇,所述功能目的例如吸收谱的改善、降解增强(例如通过水溶性材料)以及成型性能改善,例如湿强度相关。
粘稠物中以及因此本发明的纤维中纤维素与醋酸纤维素的重量比为10∶90至90∶10,例如20∶80至80∶20或30∶70至70∶30。
通常,粘稠物包含高达约50%w/w,优选高达约40%w/w,更优选高达约30%w/w且最优选高达约20%w/w的固体含量。
本发明的纤维还可以包含一种或多种增塑剂如醋精。增塑剂可以包含在粘稠物中,或可以在纺制或铸制之后添加,例如通过喷射在所形成的纤维表面。
本发明的纤维还可以包含促进纤维氧化降解的催化剂。合适的催化剂包括铁和铜的氧化物以及氯化物,可以通过将复合丝浸入水溶性铁盐或铜盐如硫酸盐或氯化物中,并用氢氧化钠或其它合适的沉淀剂处理使氧化物(优选为纳米形式)沉淀于细丝上或细丝中,来将催化剂引入纤维中。
所述纤维还可以包含一种或多种润滑剂以降低静电荷。优选的润滑剂包括矿物油。例如,可以在纺制纤维的过程中将具有乳化剂的1%w/w的矿物油施加到复合丝中。
优选地,本发明的纤维包含以每根细丝1、5或9旦尼尔(细丝厚度(每根细丝的旦尼尔数)定义为9000m单根细丝的质量(克))制造出的纤维素/醋酸纤维素复合丝。
总纤维质量(总旦尼尔)(定义为9000m纤维的总质量,通常包含数千根,例如11,000根单根纤维)将显著随纤维纺制所用的方法和纤维中单根细丝的数量而变化。一根典型的纤维的质量为35,000g。
优选地,本发明的纤维包含具有三叶形细丝横截面的纤维(任选地,用三叶形喷丝孔形成),从而优化表面积。
本发明的纤维含水量优选至少约2%w/w,更优选至少约5%w/w,更优选至少约10%w/w。已发现含水量对防止静电荷至关重要,但优选不要过高(例如,不高于50%w/w),因为纤维具有很高的含水量将难以保持折痕。
本发明的纤维优选包含缠绕的细丝。
本发明还提供了由上文所述的纤维纺织成的或以其它方式制成的材料。
本发明还提供了至少部分地由上文所述的材料制成的服装或软装饰。
本发明还提供了制造纤维的方法,其包括在离子型液体或NMMO中提供包含纤维素和醋酸纤维素混合物的溶液,并将所述混合物纺入或铸入质子性溶剂中以产生纤维。
水是用于混合物再生铸制的优选质子性溶剂。
在本发明的方法中,可以通过在水和/或其它质子性溶剂中再生溶液来产生任何比值的复合纤维素/醋酸纤维素材料。水中的凝固速率已被发现依赖于粘稠物中醋酸纤维素的含量,其中提高的醋酸纤维素水平降低凝固速率。
另一方面,本发明提供了从包含纤维素和醋酸纤维素的凝固粘稠物铸制的生物可降解薄膜,得到的薄膜是纤维素/醋酸纤维素复合材料。
下面结合实施例并参照附图对本发明进行更详细的描述。
图1展示了显示i)醋酸纤维素纤维;ii)纤维素纤维;以及iii)本发明的纤维素和醋酸纤维素混合物纤维的三个载玻片。
图2展示了图1的载玻片在厌氧条件下生物降解2周后。
图3展示了图1的载玻片在厌氧条件下生物降解4周后。
图4展示了图1的载玻片在厌氧条件下生物降解6周后。
实施例1
与等同的纤维素湿纺纤维和等同的醋酸纤维素湿纺纤维相比来评价混合纤维素/醋酸纤维素湿纺纤维的生物降解性。
利用标准的湿纺设备,从EMIM-Ac∶DMSO(20∶80)中i)纤维素(DP~800)和ii)1∶1纤维素∶醋酸纤维素(Eastman,CA-398-30)固体为10%的溶液纺制纤维。使用孔径为70μm的40-孔喷丝头,其浸入含有纯净水的室温凝固池中。湿纤维被卷起,在卷轴上充分洗涤,然后在50℃干燥。
参照图1至4,这些复合材料的惊人特性是在厌氧环境下的生物降解速率超过相同条件下的纤维素,并远远超过醋酸纤维素(参见附录1)。认为(尽管该理论绝对不应被认为是束缚)两种成分形成了最终的混合复合物,以及提高的降解速率来自纤维素结晶度的降低。复合物纤维素成分的降解被认为导致醋酸纤维素成分以分子尺度沉淀。我们还发现,本发明的纤维在有氧条件下的生物降解速率同样被提高。
这些复合材料在制造纤维中的应用提供了获得具有以下特性的纤维性产品的途径:同时具有利用单独的醋酸纤维素所获得的期望的多用性和舒适性,和显著提高的生物降解速率。
实施例2
利用干纺法来制造本发明的纤维。首先将二醋酸纤维素和纤维素(1∶1混合)以10%的固体溶解于EMIM-Ac∶DMSO(20∶80)中来制备粘稠物。添加TiO2以产生增白的外观。然后过滤粘稠物,并纺制进小室中,使得细丝固化并逐渐变细。从一系列纺丝仓纺制出多于10,000根细丝,它们结合形成一股。从所述纤维纺织成材料,并从所述材料制作服装。
发现制得的服装保留了实施例1所示的有利的生物降解性并且具有令人满意的舒适性。
Claims (14)
1.生物可降解的纤维,其包含纤维素和醋酸纤维素复合丝。
2.如权利要求1所述的纤维,其还包含一种或多种其它热塑性材料。
3.如权利要求2所述的纤维,其中所述其它热塑性材料选自以下的一种或多种:PHB、PHVB、聚丙烯腈(PAN)、聚-2-羟乙基丙烯酸甲酯(PHEMA)、聚乙烯醇(PVA)、聚苯胺和聚乙二醇。
4.如权利要求1至3中任一项所述的纤维,其中纤维素与醋酸纤维素的重量比为10∶90至90∶10。
5.如权利要求4所述的纤维,其中纤维素与醋酸纤维素的所述比值为20∶80至80∶20。
6.如权利要求5所述的纤维,其中纤维素与醋酸纤维素的所述比值为30∶70至70∶30。
7.如权利要求1至6中任一项所述的纤维,其还包含一种或多种增塑剂。
8.如权利要求1至7中任一项所述的纤维,其还包含促进所述纤维氧化降解的催化剂。
9.如权利要求1至8中任一项所述的纤维,其还包含一种或多种润滑剂以降低所述纤维上的静电荷。
10.从权利要求1至9中任一项所述的纤维纺织成的或以其它方式产生的材料。
11.至少部分地由权利要求10所述的材料制成的服装或软装饰。
12.制造权利要求1至9中任一项所述的纤维的方法,包括在离子型液体或N-甲基吗啉-N-氧化物(NMMO)中提供包含纤维素和醋酸纤维素混合物的溶液粘稠物,并将所述混合物纺入或铸入质子性溶剂中以产生纤维。
13.如权利要求12所述的方法,其中所述粘稠物还包含非质子性溶剂,以促进所述纤维素和/或醋酸纤维素的溶解。
14.如权利要求13所述的方法,其中所述非质子性溶剂包含DMSO、DMF、THF或二噁烷中的一种或多种。
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