CN103981635B - 一种多孔纤维无纺布制备方法 - Google Patents
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Abstract
本发明涉及一种多孔纤维无纺布制备方法。目的是提供的方法应能提升现有无纺布产品性能，使其满足高精度和高性能过滤要求。技术方案是：一种多孔纤维无纺布制备方法，依次按以下步骤进行：(1)将聚合物和稀释剂混合均匀，得到聚合物质量百分比浓度为10～60％的共混物；(2)采用螺杆挤出造粒机将步骤1中的共混物熔融挤出，并在空气中直接冷却造粒；(3)将步骤2中的母粒用熔喷设备生产得到初生无纺布；(4)萃取除去步骤3初生无纺布中的稀释剂，使该无纺布中的纤维成孔，干燥后即得到多孔纤维无纺布；(5)将稀释剂和萃取剂混合废液回收，重复使用。
Description
技术领域
本发明属于产业用纺织品领域，具体涉及一种将热致相分离成孔技术与熔喷技术相结合制备多孔纤维无纺布的方法，制得的无纺布可用于环保、水处理、空气过滤等。
背景技术
熔喷技术是依靠高速、高温气流(常接近聚合物熔点)喷吹聚合物熔体使其得到迅速拉伸而制备超细纤维的一种方法，可一步成形为无纺布。通过熔喷技术生产的由纤维无规堆砌组装成的无纺布，具有非常优良的结构性质，如纤维超细、比表面积大、孔隙率高、孔洞结构相互贯通、溶质扩散阻力小等，特别适合用作吸附和过滤分离材料。熔喷无纺布产品在医卫防护(雾霾、禽流感、空气净化)、保暖隔热、吸音降噪、污水处理(市政废水、原油污染吸附)等领域具有独特的优势。熔喷技术工艺流程短，生产效率高，一条生产线的年生产能力为百吨至千吨级别。由于技术含量高，市场前景大，其发展水平已经成为衡量一个国家纺织工业综合实力的重要标志之一。然而，现有熔喷技术仍存在一些不足之处：纯熔体加工高耗能，模头和热空气温度往往需超过260℃，这又会造成聚合物降解问题；纯熔体粘度大，挤出困难；对母粒熔体流动性要求较高，需用高熔融指数熔喷专用料，如要求使用熔融指数超过800g/10min的聚丙烯母粒，其需通过降解常规聚丙烯或者用茂金属催化生产得到，价格比常规聚丙烯母粒贵50％以上。
现有熔喷无纺布产品仍无法满足高精度和高性能过滤要求，如防雾霾口罩、汽车/坦克发动机防尘等，如若要进一步提高其产品使用效果或性能，需增加其比表面积，这可通过将纤维直径降低至纳米级和引入多孔结构两种途径实现。Nonwoven Technologies公司采用直径为63.5μm的纺丝孔，制备了纤维直径大约为500nm的聚丙烯纤维，但是此方法产量低，同时喷丝板价格异常昂贵，还极易开裂和堵头，生产成本太高。目前国产的熔喷设备和聚丙烯原料均无法满足纳米纤维的生产条件。多孔结构的引入可通过在熔喷聚合物母粒中加入不相容的无机纳米粒子或聚合物，然后通过溶剂溶解或者煅烧的方法来选择性去除成孔，但是此方法会导致纤维机械性能大大下降且存在溶解不完全的问题。
热致相分离技术(thermally induced phase separation，简称TIPS)是近年来发展成熟的一种聚合物成孔方法。在1980年,Castro等第一个提出TIPS制备微孔膜的方法，并申请美国专利US Patent424798。TIPS基本原理如下：对于许多非极性或弱极性热塑性结晶高聚物，在常温下与某些高沸点的小分子液体(稀释剂)互不相溶，但在升高温度下(一般高于结晶高聚物的熔点)可形成均相溶液，降低温度后由于溶解能力下降和聚合物结晶因素诱发产生液-液(L-L)或固-液(S-L)相分离，而后用萃取剂脱除稀释剂，混合物中原稀释剂所占空间变为孔洞，最终形成连贯的微孔结构。TIPS方法只有热交换过程，而不涉及复杂的物质交换过程，因此具有操作简单、影响因素少等优点，同时膜孔隙率高、不易形成缺陷、机械性能好，孔径大小、分布范围、孔隙率可控。
发明内容
本发明的目的是克服上述背景技术中的不足之处，提供一种将热致相分离成孔技术与熔喷技术相结合，实现多孔纤维无纺布大规模制备的方法；以提升现有无纺布产品性能，使其满足高精度和高性能过滤要求。
本发明所采用的技术方案是：一种多孔纤维无纺布制备方法，依次按以下步骤进行：
(1)将聚合物和稀释剂混合均匀，得到聚合物质量百分比浓度为10～60％的共混物；
(2)采用螺杆挤出造粒机将步骤1中的共混物熔融挤出，并在空气中直接冷却造粒；
(3)将步骤2中的母粒用熔喷设备生产得到初生无纺布；
(4)萃取除去步骤3初生无纺布中的稀释剂，使该无纺布中的纤维成孔，干燥后即得到多孔纤维无纺布；
(5)将稀释剂和萃取剂混合废液回收，重复使用。
本发明所使用的聚合物要求成纤性能较优，且具有和稀释剂高温溶解、低温分相的特性。由于稀释剂选择范围十分广泛，因此适合于本发明多孔纤维无纺布制备方法的聚合物也非常多，为聚丙烯、聚偏氟乙烯、聚乙烯、聚酯、聚苯乙烯、聚氨酯、聚酰胺、聚三氟氯乙烯、乙烯-丙烯酸共聚物、聚苯硫醚、聚甲醛、聚(4-甲基-1-戊烯)、聚醚醚酮、聚醚砜、聚丙烯腈、聚砜、聚酰亚胺、聚甲基丙烯酸甲酯、乙烯-乙烯醇共聚物、聚乙烯缩丁醛、聚乳酸、醋酸纤维素、聚氯乙烯、偏氟乙烯-六氟丙烯共聚物中的至少一种。本发明中聚合物在混合物中的质量百分比浓度为10～60％：浓度过高，则发生凝胶化分相过程，无法成孔；浓度过低，则在喷丝过程中纤维断裂，无法形成纤维堆砌无纺布结构，而为珠状纤维或小颗粒堆砌形式。
本发明所使用的稀释剂为沸点在150℃以上并在常温下不能溶解所述聚合物的液体或固体，具体为聚乙二醇(200、400和600)、高级醇类、多元醇类、邻苯二甲酸酯类、甘油酸酯类、苯甲酸酯类、磷酸酯类、有机碳酸酯类、柠檬酸酯类、高级脂肪酯类、丁内酯、二苯甲酮、聚乙烯亚胺、二苯酮、芳香烃、矿物油、液体石蜡、四甲基砜、马来酐、固体石蜡、天然植物油、高级烷烃、高级脂肪酸、高级脂肪胺、硬脂酸钙、异丙胺醇、二甲基砜、二苯砜、二苯醚、苯甲醛中的一种，或者两种以上任意比例的混合。
聚合物和稀释剂的混合使用常规的混合方法，包括使用混合机如Henschel混合器、V型混合机、带状混合机、搅拌式混合机、高速混合机等，可将聚合物/稀释剂初步混合均匀，利于下步造粒。
螺杆挤出造粒机长径比20～60，压缩比3～6，螺杆转速200～600rpm，挤出温度170～250℃，挤出速度50～300kg/h，在空气中直接冷却造粒，根据实际情况选择工艺参数，得到混合均匀的熔喷母粒。
本发明所使用的熔喷设备为常规整体成套生产设备，纺丝工艺参数为狭缝式喷头，喷丝口直径0.2～0.85mm，气槽角度30°～60°，狭缝宽度0.35～0.65mm，模口温度150～230℃，热空气温度180～260℃，气体压力0.05～0.5Mpa,接收距离8～30cm，纺丝速度25～150kg/h，根据实际情况选择工艺参数，得到稀释剂质量百分比浓度为40％～90％的初生无纺布。
用萃取剂去除初生无纺布中的稀释剂从而在该无纺布中的纤维上成孔，萃取过程采用常规浸渍工艺实现，也可按照有关文献(例如中国专利01144479.7；中国专利200410020242.3、中国专利200510086337.X、中国专利200610113814.1)所述方法实现。萃取完成干燥(常规加热干燥工艺)后，即得到多孔纤维无纺布，多孔无纺布幅宽为0.6～3.2m，克重范围为10～75g/m2，纤维平均直径为500nm～15μm，无纺布孔隙率为50％～80％，单根纤维孔隙率为40％～90％，纤维中孔的尺寸分布范围为100nm～1.2μm。
本发明所使用的萃取剂为能溶解稀释剂而不能溶解聚合物的液体，具体为水、乙醇、丙酮、异丙醇、乙二醇、甘油、正己烷、汽油、二氯甲烷、氯仿、丁酮、乙酸乙酯、丁醇、甲醇、石油醚中的一种，或者两种以上任意比例的混合。由于萃取剂沸点低于稀释剂，因而可利用两者沸点相差较大的特性，对稀释剂和萃取剂混合废液采用常规蒸馏或减压蒸馏方式分别回收循环使用，以降低成本。
对于生产过程产生的废气，本发明通过喷淋塔吸收或废气吸附-燃烧方式处理，实现安全、绿色生产。
本发明涉及的多孔纤维无纺布制备方法，也可应用到其它纺丝工艺中去：如先将聚合物/稀释剂母粒熔体挤出纺丝制备多孔纤维，再通过纺粘、针刺等手段制备成多孔纤维无纺布；利用高温静电纺丝技术，可在实验室范围内制备少量多孔纤维无纺布样品。
本发明涉及的多孔纤维无纺布制备方法，也可将熔喷设备中的喷头改为内径为0.1～0.4mm，外径为0.24～0.80mm的同轴喷头，喷头内部亦通高速热空气，转速为1000～2500rpm的高速滚筒作为收集装置，就可制备得到内径为300nm～8μm，外径为500nm～15μm的超细中空纤维膜。和现有直径在100μm以上的中空纤维膜相比，能大大提高污水处理效果。
本发明的有益效果是：
1)稀释剂也是聚合物加工过程中的增塑剂，大量稀释剂的加入可使聚合物熔体粘度大大降低，利于挤出和降低熔喷纤维直径，也可大大降低生产过程中的模头和热空气温度，能耗小且减缓聚合物降解；此外此方法只需用常规聚合物母粒，而不是熔喷专用母粒，能降低原料使用成本。
2)多孔纤维无纺布中单根纤维孔隙率最高可为90％，即无纺布克重仅为原先10％，可大大减小原料消耗量。
3)多孔结构的引入，增加了无纺布比表面积，从而大大提升其在水处理、空气过滤领域中的应用性能。
附图说明
图1中的a图和b图分别是实施例1中所制备的聚丙烯多孔纤维表面和断面的扫描电镜图。
图2中的a图和b图分别是实施例2中所制备的聚丙烯多孔纤维表面和断面的扫描电镜图。
图3中的a图和b图分别是实施例3中所制备的聚丙烯多孔纤维表面和断面的扫描电镜图。
图4中的a图和b图分别是实施例4中所制备的聚偏氟乙烯多孔纤维表面和断面的扫描电镜图。
图5是实施例5中所制备的聚丙烯超细中空纤维断面的扫描电镜图。
具体实施方式
本发明将致相分离成孔技术与熔喷技术相结合制备多孔纤维无纺布，适用此方法的聚合物、稀释剂和萃取剂选择均相当广泛，不同聚合物/稀释剂/萃取剂的排列组合可以得到非常多的工艺条件，但是基本原理不变，可得到不同聚合物种类、幅宽和克重、纤维直径、纤维孔隙率、纤维孔径分布的多孔纤维无纺布。整个生产工艺流程包括混合-挤出造粒-熔喷-萃取-干燥-稀释剂/萃取剂回收，以下结合说明书附图，对本发明作进一步说明，但本发明并不局限于以下实施例。
实施例1聚丙烯/液体石蜡固-液相分离体系
聚合物原料为齐鲁石化产聚丙烯T30S，稀释剂为液体石蜡，萃取剂为正己烷。聚丙烯质量百分比浓度为30％，首先将聚丙烯和液体石蜡在常温下用高速混合机共混均匀。然后用螺杆挤出机造粒，螺杆挤出造粒机长径比42，压缩比3，螺杆转速400rpm，挤出温度180℃，挤出速度150kg/h，在空气中冷却得到聚丙烯/液体石蜡熔喷母粒。将母粒进行熔喷生产，工艺参数为狭缝式喷头，喷丝口直径0.42mm，气槽角度30°，狭缝宽度0.62mm，模口温度185℃，热空气温度200℃，气体压力0.1Mpa,接收距离15cm，纺丝速度100kg/h，初生无纺布克重为100g/m2，幅宽为1.6m，无纺布收集速度为10.4m/min。初生无纺布通过常规浸渍流水线设备，使用正己烷连续浸渍萃取液体石蜡，干燥得到聚丙烯多孔纤维无纺布。将多孔纤维无纺布在液氮下淬断，用扫描电镜分别观察纤维表面和断面形貌，如图1所示。多孔纤维无纺布克重为30g/m2，纤维平均直径为10μm，无纺布孔隙率为60％，单根纤维孔隙率为70％，纤维中孔的尺寸分布范围为300nm～1.2μm。此体系只发生固-液(S-L)相分离，S-L相分离温度为120℃，因此纤维表面形成致密皮层结构，纤维断面为胞腔状孔结构。正己烷和液体石蜡混合废液在80℃常压蒸馏，冷凝收集正己烷蒸汽，液体石蜡留在底部，分别回收循环利用。
实施例2聚丙烯/邻苯二甲酸正丁酯/邻苯二甲酸正辛酯液-液相分离体系
聚合物原料为燕山石化产聚丙烯S1003，稀释剂为邻苯二甲酸正辛酯和邻苯二甲酸正丁酯混合物，萃取剂为异丙醇。聚丙烯质量百分比浓度为20％，邻苯二甲酸正辛酯质量百分比浓度为64％，邻苯二甲酸正丁酯质量百分比浓度为16％。首先将聚丙烯、邻苯二甲酸正辛酯和邻苯二甲酸正丁酯在常温下用高速混合机共混均匀。然后用螺杆挤出机造粒，螺杆挤出造粒机长径比20，压缩比4，螺杆转速600rpm，挤出温度200℃，挤出速度300kg/h，在空气中冷却得到聚丙烯/邻苯二甲酸正辛酯/邻苯二甲酸正丁酯熔喷母粒。将母粒进行熔喷生产，工艺参数为狭缝式喷头，喷丝口直径0.60mm，气槽角度40°，狭缝宽度0.65mm，模口温度200℃，热空气温度220℃，气体压力0.25Mpa,接收距离20cm，纺丝速度200kg/h，初生无纺布克重为200g/m2，幅宽为3.2m，无纺布收集速度为5.2m/min。初生无纺布通过常规浸渍流水线设备，使用异丙醇连续浸渍萃取邻苯二甲酸正辛酯和邻苯二甲酸正丁酯，干燥得到聚丙烯多孔纤维无纺布。将多孔纤维无纺布在液氮下淬断，用扫描电镜分别观察纤维表面和断面形貌，如图2所示。多孔纤维无纺布克重为40g/m2，纤维平均直径为8μm，无纺布孔隙率为75％，单根纤维孔隙率为80％，纤维中孔的尺寸分布范围为300nm～850nm。此体系发生液-液(L-L)相分离，但L-L相分离温度(127℃)和S-L相分离温度(113℃)接近，因此纤维表面形成圆形开孔，纤维断面为双连续孔结构。异丙醇、邻苯二甲酸正辛酯和邻苯二甲酸正丁酯混合废液在120℃常压蒸馏，冷凝收集异丙醇蒸汽，邻苯二甲酸正辛酯和邻苯二甲酸正丁酯留在底部，分别回收循环利用。
实施例3聚丙烯/二苯醚液-液相分离体系
与实施例1基本工艺参数相同，稀释剂选用二苯醚，纤维表面和断面形貌如图3所示，纤维中孔的尺寸分布范围为300nm～650nm。此体系只发生液-液(L-L)相分离，L-L相分离温度为135℃，因此纤维表面形成椭圆形开孔，纤维断面为双连续孔结构。
实施例4聚偏氟乙烯/邻苯二甲酸正丁酯固-液相分离体系
聚合物原料为苏威产聚偏氟乙烯6010，稀释剂为邻苯二甲酸正丁酯，萃取剂为乙醇。聚偏氟乙烯质量百分比浓度为25％，首先将聚偏氟乙烯和邻苯二甲酸正丁酯在常温下用高速混合机共混均匀，然后造粒；螺杆挤出造粒机长径比35，压缩比3.5，螺杆转速300rpm，挤出温度220℃，挤出速度80kg/h，在空气中冷却得到聚偏氟乙烯/邻苯二甲酸正丁酯熔喷母粒。将母粒进行熔喷生产，工艺参数为狭缝式喷头，喷丝口直径0.55mm，气槽角度35°，狭缝宽度0.48mm，模口温度220℃，热空气温度240℃，气体压力0.35Mpa,接收距离30cm，纺丝速度60kg/h，初生无纺布克重为80g/m2，幅宽为1.6m，无纺布收集速度为7.8m/min。收集到的初生无纺布依次在3个乙醇槽中浸渍2h、1h和30min，用于萃取(间歇式浸渍萃取)邻苯二甲酸正丁酯，干燥得到聚偏氟乙烯多孔纤维无纺布。将多孔纤维无纺布在液氮下淬断，用扫描电镜分别观察纤维表面和断面形貌，如图4所示。多孔纤维无纺布克重为20g/m2，纤维平均直径为12μm，无纺布孔隙率为80％，单根纤维孔隙率为75％，纤维中孔的尺寸分布范围为300nm～550nm。此体系只发生固-液(S-L)相分离，S-L相分离温度为138℃，聚偏氟乙烯形成球晶堆积结构，因此纤维表面为圆孔结构，纤维断面为球晶堆积的蜂窝状结构。乙醇和邻苯二甲酸正丁酯混合废液在100℃常压蒸馏，冷凝收集乙醇蒸汽，邻苯二甲酸正丁酯留在底部，分别回收循环利用。
实施例5聚丙烯/液体石蜡固-液相分离体系
基本工艺参数与实施例1同，熔喷设备改用同轴喷头，喷丝口内径为0.25mm，外径为0.42mm，用转速为1600rpm的高速滚筒作为收集装置。在液氮下淬断，用扫描电镜观察中空纤维膜断面形貌，如图5所示，制备得到内径为7.5μm，外径为10μm的超细中空纤维膜，其余性质与实施例1同。
上述实施例只为说明本发明的技术构思及特点，其目的是让熟悉该技术领域的技术人员能够了解本发明的内容并据以实施，并不能以此来限制本发明的保护范围。任何熟悉本专业的技术人员在不脱离本发明技术方案范围内，当可利用上述揭示的技术内容做出些许更动或修饰为等同变化的等效实施例，但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，都应该涵盖在本发明的保护范围之内。
Claims (3)
1.一种多孔纤维无纺布制备方法，依次按以下步骤进行：
(1)将聚合物和稀释剂混合均匀，得到聚合物质量百分比浓度为10～60％的共混物；
(2)采用螺杆挤出造粒机将步骤1中的共混物熔融挤出，并在空气中直接冷却造粒；
(3)将步骤2中的母粒用熔喷设备生产得到初生无纺布；
(4)萃取除去步骤3初生无纺布中的稀释剂，使该无纺布中的纤维成孔，干燥后即得到多孔纤维无纺布；
(5)将稀释剂和萃取剂混合废液回收，重复使用；
所述聚合物为聚丙烯、聚偏氟乙烯、聚乙烯、聚酯、聚苯乙烯、聚氨酯、聚酰胺、聚三氟氯乙烯、乙烯-丙烯酸共聚物、聚苯硫醚、聚甲醛、聚(4-甲基-1-戊烯)、聚醚醚酮、聚醚砜、聚丙烯腈、聚砜、聚酰亚胺、聚甲基丙烯酸甲酯、乙烯-乙烯醇共聚物、聚乙烯缩丁醛、聚乳酸、醋酸纤维素、聚氯乙烯、偏氟乙烯-六氟丙烯共聚物中的至少一种；
所述稀释剂为高级醇类、多元醇类、邻苯二甲酸酯类、甘油酸酯类、苯甲酸酯类、磷酸酯类、有机碳酸酯类、柠檬酸酯类、高级脂肪酯类、丁内酯、二苯甲酮、聚乙烯亚胺、二苯酮、芳香烃、矿物油、液体石蜡、四甲基砜、马来酐、固体石蜡、天然植物油、高级烷烃、高级脂肪酸、高级脂肪胺、硬脂酸钙、异丙胺醇、二甲基砜、二苯砜、二苯醚、苯甲醛中的一种，或者两种以上任意比例的混合；
所述步骤(4)中的萃取采用的萃取剂为水、乙醇、丙酮、异丙醇、乙二醇、甘油、正己烷、汽油、二氯甲烷、氯仿、丁酮、乙酸乙酯、丁醇、甲醇、石油醚中的一种，或者两种以上任意比例的混合；
步骤(1)中的混合所使用的混合机为Henschel混合器、带状混合机、搅拌式混合机中的至少一种；
所述螺杆挤出造粒机的长径比20～60，压缩比3～6，螺杆转速200～600rpm，挤出温度170～250℃，挤出速度50～300kg/h；
熔喷设备采用狭缝式喷头，其喷丝口直径0.2～0.85mm，气槽角度30°～60°，狭缝宽度0.35～0.65mm，模口温度150～230℃，热空气温度180～260℃，气体压力0.05～0.5Mpa,接收距离8～30cm，纺丝速度25～150kg/h。
2.根据权利要求1所述的多孔纤维无纺布的制备方法，其特征在于稀释剂和萃取剂混合废液的回收，采用常规蒸馏或减压蒸馏方式。
3.根据权利要求2所述的多孔纤维无纺布的制备方法，其特征在于熔喷设备采用内径为0.1～0.4mm，外径为0.24～0.80mm的同轴喷头，喷头内部亦通高速热空气；转速为1000～2500rpm的高速滚筒作为收集装置，以制备内径为300nm～8μm，外径为500nm～15μm的超细中空纤维膜。
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