CN1503635A - 由聚合物溶液制造的高表面积微孔纤维 - Google Patents
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Abstract
一种乙酸纤维素纤维及其制备方法(图2),该纤维具有多个微孔腔或孔隙(图3)的外表面积。
Description
发明背景
本发明涉及由聚合物溶液制造的高表面积微孔纤维,和尤其涉及用于过滤应用的高表面积纤维,其中使用表面微孔保留固体和/或液体试剂,用于选择性过滤,以降低某些烟尘组分。
在香烟过滤中使用的目前的乙酸纤维素(CA)纤维是通过干纺法制造的,该方法允许20-25%CA的丙酮溶液牵引或挤压通过喷丝板的底部细孔或喷嘴,和在约5-10米长的纺丝柱中,通过除去丙酮溶剂,缓慢收缩成最终的纤维形状。在柱子中用加压的热空气流干燥,由于所包含的热量导致由此形成的具有诸如“R”、“I”、“Y”和“X”截面的纤维具有连续的芯截面和相对有限的外表面积,其中所述截面取决于牵引或挤压纤维所通过的细孔的形状。
发明概述
因此,本发明的一个目的是通过形成保留固体和/或液体试剂用的微孔,增加由聚合物溶液制造的某些纤维的外表面积,在降低烟产品如香烟内的某些烟尘组分中,用于选择性过滤。
本发明另一目的是生产高表面积纤维的方法,在烟产品如香烟内用于过滤应用。
本发明再一目的是由聚合物溶液制造的高表面积纤维的生产方法,其中使用在该纤维表面上的微孔保留固体和/或液体试剂,在降低烟产品内的某些烟尘组分中,用于选择性过滤。
根据本发明,使聚合物溶液通过干纺法的喷丝板。在气流纺柱中一定程度的干燥之后,对纤维的最初形式施用减压快速蒸发法,在此,在纤维表面上形成聚合物的干燥表皮。在减压下,在该表皮内的残留量的溶剂或发泡剂爆裂或破裂,并通过不同的微孔路径快速离开纤维,从而留下具有微孔腔和内部空隙体积的高表面积纤维。对于乙酸纤维素来说,为了保护在纤维表面内如此形成的微孔,在蒸发法中,低于60℃的蒸发温度很必要的。
可将该方法拓展到除乙酸纤维素之外的聚合物溶液以及除丙酮之外的溶剂和所谓破裂剂。还有,合适的纤维是由熔体聚合物纺丝原液制造的纤维,它含有在冷硬外表皮内俘获的空气。可在线上或以分批方式使用低温蒸发法。
附图的简要说明
连同附图,根据下述详细说明的阅读,除了以上所述的那些特征和优点之外,本发明的新特征和优点对本领域的技术人员来说是显而易见的,在附图中类似的参考符号是指类似的部分,和其中
图1A是根据本发明实施例1生产的纤维的微观表面图象;
图1B是根据本发明实施例1生产的纤维的微观截面视图;
图2是根据本发明实施例2生产的纤维的微观表面图象;
图3是根据本发明实施例3生产的纤维的微观表面图象;
图4是根据本发明实施例4生产的部分干燥的纤维的微观表面图象;
图5是根据本发明实施例4生产的在约65℃下干燥的纤维的微观表面图象;
图6A是根据本发明实施例4生产的在约45-55℃下干燥的纤维的微观表面图象;
图6B是图6A所示的纤维的微观截面视图。
发明详述
以下是本发明的详细说明和实施例。
A.CA/丙酮溶液的制备。向配有机械搅拌和玻璃塞的100ml三颈圆底烧瓶中加入50ml丙酮(Fisher Scientific,99.6%),接着在中速搅拌下加入11.88g CA丝束纤维。在添加完之后,塞住烧瓶,和所添加的纤维缓慢溶解在溶剂内,过夜形成均匀的白色粘稠溶液。
B.干纺法形成纤维。将约10ml上述溶液通过配有塑料管的塑料注射器缓慢转移到10ml的挤出套筒内。然后将套筒安装在DACA9mm Piston Extruder Model 40000(它带有0.75mm的圆形单一细孔模头)上,并以20mm/min的活塞速度,在室温下挤出。在垂直滴落到21-cm溶剂的通风孔(venting)间隙内之后,在铝盘内收集挤出的纤维,所述通风孔间隙由两个鼓风喷嘴和排气罩的组合而产生。通过真空烘箱或在罩内的高气流进一步快速蒸发残余的溶剂。
实施例-1在60℃真空干燥之后获得的纤维
在该实施例中,在金属板上收集纤维,然后将它放入60℃的真空烘箱中。通过干冰阱,机械泵在该烘箱内产生高真空。捕获的溶剂快速蒸发并在纤维表面上形成微孔。图1A和1B示出了在真空和60℃下干燥20分钟之后所形成的纤维的微观表面和截面视图。显然,形成直径约1微米的孔。这些孔如此小,以致于仅可以在1000×图象(1微米/刻度)下,而不是在400×图象(2.5微米/刻度)下观察到它们。经实测,在储存超过3个月孔结构是稳定的。
由于在水平位置上收集并干燥在该实施例中的纤维样品,所以它们并不维持图1A和1B所示的它们的圆形截面。它们各向异性地收缩成截面尺寸为25-150微米的扁平狗骨头形状。在该工艺中,在没有接触的情况下,通过垂直地处理纤维,可能将它收缩成圆形截面。仅使用该实施例和下述实施例证明改良乙酸纤维素纤维的表面孔隙率的精神,和不使用它们限制本发明的范围。所得多孔纤维可具有任何截面形状。
实施例-2由较低温度蒸发工艺获得的多孔纤维
在该实施例中,进一步以不加热的工艺干燥上述纺丝纤维样品。通过在没有加热情况下,在真空烘箱中快速抽气,或在室温下在高度排气的罩内除去残留溶剂25分钟。图2示出了所得样品的典型表面图象。甚至在400×图象下,直径达3微米的较大孔清晰可见。显然,温度和压力对纤维表面上的孔隙率的最终形成扮演着重要的角色。
实施例-3使用固体碳酸氢铵(AHC)试剂的实验
在多孔塑料的制造中,碳酸氢铵(NH4HCO3,AHC)是已知的发泡剂。它在约60℃下分解放出CO2、NH3和H2O。在该实施例中,使用这一试剂的固体形式,在纤维内形成大孔。纤维的制备和纺丝方案与实施例1相同。如实施例1所述,混合2.0g固体AHC粉末(Aldrich,99%)与40ml乙酸纤维素的丙酮溶液,从而启动实验。在机械搅拌过夜之后,所以固体颗粒被混合到溶液内。然后在DACA活塞式挤出机中对10ml该混合物纺丝。当使用1.25mm的模头时,不可能拉出连续的单丝。在以30.4mm/分的速率使用0.5mm圆横截面模头时,在130cm长的滴落距离之后,通过人工缠绕在80-mm的筒管上,收集所形成的邻接纤维单丝。然而,在流过模头之前,在套筒底部上发现沉积着大的固体颗粒。可能是,在此情况下,仅仅小量的该试剂实际上通过模头掺入到纤维内。在该试剂分解和在约60℃的温度和真空下除去残留溶剂25分钟之后,观察到在纤维表面上直径达2.5微米的孔,如图3所示。在该实施例中形成的孔比实施例1中的那些大得多,这是因为存在小量的发泡剂所致。为了具有甚至更大的效果,可在不使纤维破裂的情况下,使额外的发泡剂必须流过模头。在下述实施例中,通过使用亚微米的固体粒子形式或溶解形式的发泡剂可实现它。
实施例-4使用溶解的碳酸氢铵(AHC)试剂的实验
A.NH4HCO3/H2O溶液的制备。在室温下,在磁搅拌下,将2.0g上述AHC固体缓慢加入到含10.0g蒸馏水的烧杯中。在固体颗粒溶解之后,在室温下,在密闭的小瓶内储存所形成的溶液。
B.含NH4HCO3/H2O的CA/丙酮溶液的制备。向配有机械搅拌和玻橘塞的100ml三颈圆底烧瓶中加入50ml丙酮(FisherScientific,99.6%),接着在中速搅拌下加入12.5g CA丝束纤维。在添加完之后,塞住烧瓶,和所添加的纤维缓慢溶解在溶剂内,过夜形成均匀的白色粘稠溶液。然后,在剧烈的机械搅拌下,将1ml以上制备的AHC溶液加入到该溶液中。在添加之后,在使用前,持续缓和地搅拌混合物至少1小时。
C.干纺法形成大孔纤维。将约10ml上述溶液通过塑料注射器经塑料管转移到10ml的挤出套筒内.然后将套筒安装在DACA 9mmPiston Extruder Model 40000(它带有1.5mm的圆形单一细孔模头)上,并以20mm/min的活塞速度,在室温下挤出。在垂直滴落到130-cm预干燥的间隙内之后,在铝盘内收集挤出的纤维,所述间隙由两个鼓风喷嘴和排气罩的组合而产生。由于混合物内的AHC分解,在这一部分干燥样品的表面上观察到直径达5-10微米的大孔,如图4所示。然而,由于存在残留的溶剂,所以该结构体不稳定。在大气压下,在室温下储存之后,它弛豫(relax)回具有图2所示的孔径较小的更稳定的结构。
为了充分除去残留溶剂,在60-65℃的温度下,在真空烘箱内进一步处理105.6mg以上收集的纤维30分钟,在除去约6%的残留溶剂之后,获得99.6mg干纤维。图5示出了纤维的表面。由于加热,所以因聚合物链的运动导致最初的大孔部分被破坏,并与实施例1相类似,弛豫回直径约1微米的较小孔。饶有兴趣的是,一些直径为10-15微米的超大孔在该工艺中保存了下来。
为了保持所形成的孔结构,应当在低温高真空短时间内处理纤维。可在约50℃的温度下,在5分钟的高真空烘箱处理下有效地除去残留溶剂(约5-7%)。例如,在45-55℃下,在真空烘箱中仅处理5分钟1.7580g上述部分干燥的纤维,结果得到1.6333g干纤维。如图6A和6B所示,在干纤维表面内形成直径为3-5微米的大孔。也发现该孔结构在室温下长时间地储存时是稳定的。
总之,上述实施例证明通过快速蒸发残留溶剂,或在干纺法之中或之后通过纤维表面的表皮吹气,可形成直径为1-15微米的孔。这些孔提供较高的可接近接触表面积,用于纤维接触气相吸附物,和也提供内纤维空间,容纳过滤领域用的额外吸收剂/试剂。为了保护所形成的直径大于1微米的孔,优选减压下的低温蒸发工艺。
Claims (3)
1.一种乙酸纤维素纤维,它具有带多个从表面延伸到纤维内的微孔腔的外表面积,和该纤维具有部分内空隙体积。
2.一种香烟过滤元件,它包括多根乙酸纤维素纤维,其中各纤维具有带多个从表面延伸到纤维内的微孔腔的外表面积,和固体和/或液体试剂保留在微孔腔内用于选择性过滤香烟。
3.一种制备乙酸纤维素纤维的方法,它包括下述步骤:使乙酸纤维素的丙酮溶液通过喷丝板形成纤维,部分干燥所形成的纤维以便在该纤维的外部上产生表皮,和在预定程度的干燥之后,向所形成的纤维施加真空,从而引起所形成的纤维内部的丙酮爆裂或破裂,并沿微孔路径经表皮离开纤维,从而在纤维的外表面上形成延伸到纤维内部的微孔腔。
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Cited By (4)
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CN103720042A (zh) * | 2013-12-20 | 2014-04-16 | 苏州鑫帛泰纺织科研有限公司 | 多孔中空纤维香烟滤嘴 |
CN104872810A (zh) * | 2015-04-01 | 2015-09-02 | 湖南中烟工业有限责任公司 | 一种改性烟梗纤维的制备方法及应用 |
CN105887228A (zh) * | 2016-05-06 | 2016-08-24 | 南通醋酸纤维有限公司 | 利用紫外光辅助干法纺丝产多孔二醋酸纤维丝束的制备方法 |
CN112030254A (zh) * | 2020-08-28 | 2020-12-04 | 平湖爱之馨环保科技有限公司 | 一种微孔纤维及其制造方法 |
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AU2002357720A1 (en) * | 2001-11-30 | 2003-06-17 | Philip Morris Products S.A. | Continuous process for impregnating solid adsorbent particles into shaped micro-cavity fibers and fiber filters |
US7935298B2 (en) | 2003-12-23 | 2011-05-03 | Virginia Commonwealth University | Method of producing fibers by electrospinning at high pressures |
US10285431B2 (en) * | 2004-12-30 | 2019-05-14 | Philip Morris Usa Inc. | Encapsulated flavorant designed for thermal release and cigarette bearing the same |
US10188140B2 (en) | 2005-08-01 | 2019-01-29 | R.J. Reynolds Tobacco Company | Smoking article |
US20070215167A1 (en) | 2006-03-16 | 2007-09-20 | Evon Llewellyn Crooks | Smoking article |
US8157918B2 (en) | 2005-09-30 | 2012-04-17 | Philip Morris Usa Inc. | Menthol cigarette |
KR100738106B1 (ko) * | 2006-02-09 | 2007-07-12 | 삼성전자주식회사 | 컬러 필터의 제조장치 |
US9220301B2 (en) | 2006-03-16 | 2015-12-29 | R.J. Reynolds Tobacco Company | Smoking article |
US8282739B2 (en) | 2006-08-03 | 2012-10-09 | Philip Morris Usa Inc. | Preformed cigarette having a specifically defined immobilized flavorant additive insert positioned therein |
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GB2009667B (en) * | 1977-12-09 | 1982-05-12 | Mitsubishi Acetate Co Ltd | Surface-modified cellulose acetate filaments and a process for producing the same |
US4821750A (en) * | 1985-05-31 | 1989-04-18 | Celanese Corporation | Cigarette filters |
JP3982589B2 (ja) * | 1995-03-03 | 2007-09-26 | テイジン トワロン ビー. ブイ. | 紡糸可能溶液のための遠心紡糸法 |
US6209547B1 (en) * | 1998-10-29 | 2001-04-03 | Philip Morris Incorporated | Cigarette filter |
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CN103720042A (zh) * | 2013-12-20 | 2014-04-16 | 苏州鑫帛泰纺织科研有限公司 | 多孔中空纤维香烟滤嘴 |
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