CN110936683B - 一种防水透湿功能纤维素基多孔复合材料及其制备及应用 - Google Patents
一种防水透湿功能纤维素基多孔复合材料及其制备及应用 Download PDFInfo
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Abstract
本发明涉及一种防水透湿功能纤维素基多孔复合材料及其制备及应用,复合材料由下到上依次包括,疏水纤维素多孔材料底层,具有两亲性的纤维素多孔材料中层,超亲水纤维素多孔材料上层。本发明所得复合材料在服装领域应用时,在发挥防水透湿功能的同时,还有着极佳的保温隔热效果。
Description
技术领域
本发明属于功能性多孔复合材料及其制备和应用领域,特别涉及一种防水透湿功能纤维素基多孔复合材料及其制备及应用。
背景技术
防水透湿功能材料是一种同时具有良好防水性和透湿性的新型功能材料。这类材料可以应用在许多恶劣环境条件下,其作为服装面料使用时可保护人体不受到狂风暴雨的影响并能够及时的向外部环境传输水蒸气,从而极大的提高服装的穿着舒适性;同时在医疗化工行业中,防水透湿功能材料还可以有效阻隔有毒液体试剂与人体的直接接触,从而避免试剂可能对人体造成的感染或伤害。近年来,市场上对防水透湿材料的需求与日俱增,它的应用领域也不单是在军需用品和专业化的医疗防护用品领域发展,也正迅速扩张到户外休闲运动服装及装备领域。目前市场上防水透湿材料主要存在以下两种情况:一种是材料本身有着优异的阻水性但是透湿性较差,另一种是材料的透湿性良好但防水性能不能达到市场要求,因此急需开发一类同时兼具良好防水性和透湿性的功能材料。
纤维素作为自然界中储量最为丰富的天然高分子,相比于传统经有机合成制备的有机高分子相比,纤维素来源丰富且有着较好的生物相容性及可降解性能,同时表面带有的大量的羟基使其具有良好的吸湿性。以纤维素为原料经化学改性后制备的多孔材料可广泛应用于催化剂载体、高效吸附材料、隔热保温材料、超级电容器等领域。但由于传统纤维素多孔材料的机械性能较差,需要用硅烷偶联剂对其进行改性,以此增强纤维素多孔材料的机械性能,进而扩展其应用领域。
CN103660464A公开了一种防水透湿复合膜和具有防水透湿性的防水透湿布,其主要原料由聚四氟乙烯和聚氨酯构成。尽管该方法制备的防水透湿膜和透湿布具有良好的防水透湿性能,但是由于聚四氟乙烯和聚氨酯均为不可降解的高分子材料,其成本较高且不利于当前可持续发展的主题。
CN103963393公开了一种防水透湿复合膜及其制备方法,该方法选用静电纺丝的技术制备具有纳米级/亚微米级的多孔膜,由于利用静电纺丝技术制备防水透湿复合膜成本高且效率低,不利于大规模工业化推广。
发明内容
本发明所要解决的技术问题是提供一种防水透湿功能纤维素基多孔复合材料的制备及应用,克服现有技术生产成本高、产品后期不易回收、不可降解的缺陷,本发明的多孔材料内部分为上层、中层、底层三层多孔结构,每一层都有着不同的孔径以及水接触角,最后经不同工艺制备而成。其中最底层多孔材料有着较好的疏水性并且内部有着较大的孔径,中间层多孔材料具有两亲性,而最上层多孔材料则表现为超亲水性且内部孔径最小。经过不同的制备方法,最后可将这三层多孔材料复合为一种具有多重孔结构的纤维素基多孔复合材料。该材料在接触水滴后,在水的拉普拉斯压力作用下,可将水滴从底层自下而上传输到材料的上层,从而达到透湿的效果。此外,由于底层多孔材料疏水设计,使得该纤维素基多孔复合材料能够有效的防止水滴反渗,进而达到防水的效果。
本发明的一种多层纤维素基多孔复合材料,所述复合材料由下到上依次包括,疏水纤维素多孔材料底层,具有两亲性的纤维素多孔材料中层,超亲水纤维素多孔材料上层。
所述疏水纤维素多孔材料的孔径大小为30-50微米;具有两亲性的纤维素多孔材料的孔径大小为1-10微米;超亲水纤维素多孔材料孔径大小200-300纳米。
所述疏水纤维素多孔材料为包括纤维素多孔材料和聚氨酯的复合材料;具有两亲性的纤维素多孔材料为硅烷偶联剂改性的纤维素纳米线和改性的细菌纤维素复合多孔材料;上层超亲水纤维素多孔材料为超亲水细菌纤维素多孔材料。
所述疏水纤维多孔材料底层的水接触角为128-140°,超亲水纤维素多孔材料上层水接触角为0-3°。
所述疏水纤维素多孔材料中还含有三防整理剂;所述改性的纤维素纳米线采用的硅烷偶联剂为甲基三甲氧基硅烷,甲基二乙氧基硅烷,二甲基二乙烯基硅烷,二甲基二甲氧基硅烷中的一种或几种;改性的细菌纤维素为采用硅烷偶联剂为KH560和聚乙烯亚胺进行改性处理;超亲水细菌纤维素为KH560和聚乙烯亚胺处理的细菌纤维素。
本发明的一种多层纤维素基多孔复合材料的制备方法,包括:
(1)将纤维素多孔材料浸入聚氨酯溶液中,同时加入三防整理剂,常温下真空浸渍10~20min,取出后放入凝固浴中,凝固浴温度为30~40℃,10~20min后取出,洗涤,干燥,得到疏水纤维素多孔材料;
(2)将上述疏水纤维素多孔材料固定在模具底部,再将改性的纤维素纳米线和改性的细菌纤维素的混合溶液倒入模具中,干燥,得到双层纤维素多孔复合材料;
(3)将上述双层纤维素多孔材料固定在模具底部,再将含有KH560和聚乙烯亚胺的细菌纤维素混合溶液倒入模具中,干燥,即得多层纤维素基多孔复合材料。
所述步骤(1)中纤维素多孔材料具体为:纤维素纳米线悬浮液中加入硅烷偶联剂,常温下搅拌2~4h后,用液氮冷冻10min后转移至冷冻干燥机中,其中冻干温度为-50℃,冻干时间为30~40h,之后将冻干后的纤维素多孔材料转移至110℃烘箱中放置1~2h。
进一步,所述纤维素纳米线悬浮液的固含量为1~2wt%;所述纤维素纳米线和硅烷偶联剂的质量比为1:0.5~1。
进一步,所述纤维素纳米线的长度为1~20μm,直径为20-40nm;硅烷偶联剂为甲基三甲氧基硅烷,甲基二乙氧基硅烷,二甲基二乙烯基硅烷,二甲基二甲氧基硅烷中的一种或几种。
所述步骤(1)中聚氨酯溶液的固含量为4~8wt%;所述纤维素多孔材料浸入聚氨酯溶液中,其中纤维素多孔材料的质量占比为10~20wt%,聚氨酯含浸液的质量占比为78~86wt%,三三防整理剂的质量分数为2~4wt%;防整理剂为杜邦Teflon;凝固浴为水和N,N-二甲基甲酰胺凝固浴,其中水的质量占比为70~90wt%,N,N-二甲基甲酰胺的质量占比为10~30wt%。
所述步骤(1)中干燥为60~80℃下干燥10~20h。
所述步骤(2)中改性的纤维素纳米线和改性的细菌纤维素的混合溶液具体为:细菌纤维素悬浮液中加入硅烷偶联剂KH560和聚乙烯亚胺,搅拌2~4h,得到细菌纤维素混合液;纤维素纳米线悬浮液中加入硅烷偶联剂,搅拌2~4h,得到纤维素纳米线混合液,然后按纤维素纳米线混合溶液和细菌纤维素混合溶液的质量比为1:0.4~0.8混合,搅拌10~20min。
所述细菌纤维素悬浮液的固含量为1~2wt%;纤维素纳米线悬浮液的固含量为1~2wt%;所述细菌纤维素的长度为1~50μm,直径为10~20nm;纤维素纳米线的长度为1~20μm,直径为20-40nm;纤维素纳米线和硅烷偶联剂的质量比为1:0.5~1;细菌纤维素与KH560、聚乙烯亚胺的质量比为1:0.5~1:0.4~0.8。
所述细菌纤维素悬浮液由下列方法制备:将细菌纤维素浸入NaOH溶液中,80~100℃下加热4~8h后将细菌纤维素取出,并用去离子水洗至中性,之后将细菌纤维素剪碎,利用均质机搅拌1~2h,从而得到细菌纤维素悬浮液。
进一步,上述NaOH溶液的浓度为0.5~1mol/L;均质机的转速为15000~20000r/min。
所述步骤(2)中干燥为80℃干燥20-30h。
所述步骤(3)中细菌纤维素悬浮液的固含量为1~2wt%;所述细菌纤维素、KH560和聚乙烯亚胺的质量比为1:0.5~1:0.5~1。
所述步骤(3)中干燥为80℃干燥20-30h。
本发明的一种所述方法制备的多层纤维素基多孔复合材料。
本发明提供一种所述多层纤维素基多孔复合材料的应用。
有益效果
(1)本发明制备的多层纤维素基多孔复合材料,主要由上、中、下三层不同孔径大小的纤维素多孔材料组成。其底层纤维素多孔材料由于与聚氨酯复合,因此表现出了极佳的柔性和机械性能,同时,该多孔材料还有着较好的疏水性能。中层纤维素多孔材料是由经不同硅烷偶联剂改性的纤维素纳米线和细菌纤维素混合溶液制备而成,该材料表现出了较好的双亲性和有着较小的孔径。该复合材料的上层是由细菌纤维素经亲水处理后制备而成,由于细菌纤维素尺寸较小,其孔径相比于底层和中层纤维素多孔材料孔径最小,同时还有着超亲水性能。
(2)本发明的多层纤维素基多孔复合材料的底层纤维素多孔材料在与聚氨酯复合后,其机械性能明显增加。因此该纤维素多孔材料在作为多层纤维素多孔复合材料的基底时,可使得整个复合材料表现出较好的柔性,从而极大的提高了材料的可加工性能和应用范围。
(2)本发明制备的多层纤维素多孔复合材料从下至上三层纤维素多孔材料,分别采用不同的纤维素原料经不同成型工艺制备而成,这使得制备的纤维素多孔材料从底层至上层孔径越来越小,从而使多层纤维素多孔材料的毛细力从下至上越来越大,极大的增强了材料的水气运输能力(透湿量>8000g/m)。
(3)本发明制备的多层纤维素多孔复合材料从下至上三层纤维素多孔材料依次表现出超疏水、既不亲水也不疏水、超亲水三种性能,从而使得该复合材料在水气运输时,其底层可有效的避免水气的反渗,中间层的双亲性能可加速水气的运输,而上层的超亲水性能有利于水气的快速蒸发。因此,本发明制备的多层纤维素多孔复合材料在实际应用过程中能够发挥出防水透湿效果(耐水压>30kPa)。
(4)由于纤维素多孔材料本身有着较好的隔热性能,本发明制备的多层纤维素多孔复合材料由三种不同孔径大小的纤维素多孔材料复合而成,因此其在服装领域应用时,在发挥防水透湿功能的同时,还有着极佳的保温隔热效果(导热系数<40Wm-1K-1)。
(5)本发明制备的多层纤维素多孔复合材料均采用纤维素作为原料,从而使得该产品在后期可以生物降解,符合当前环保可持续发展的主题。
附图说明
图1是本发明制备的多层纤维素多孔复合材料的示意图。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
首先制备单层疏水纤维素多孔材料,具体制备过程为:取1wt%固含量的纤维素纳米线悬浮液(天津木精灵有限公司),纤维素纳米线长度为1μm,直径为20nm,之后加入甲基三甲氧基硅烷(上海国药集团化学试剂有限公司,CAS:1185-55-3),其中纤维素纳米线和甲基三甲氧基硅烷的质量比为1:0.5。常温下搅拌2h后,将混合溶液用液氮冷冻10min后转移至冷冻干燥机中,其中冻干温度为-50℃,冻干时间为30h,之后将冻干后的纤维素多孔材料转移至110℃烘箱中放置1h。将制备的纤维素多孔材料浸入4wt%固含量的聚氨酯溶液中(济宁佰一化工有限公司,HK3100),其中纤维素多孔材料的质量占比为10wt%,聚氨酯含浸液的质量占比为86wt%,同时加入4wt%质量分数的三防整理剂杜邦Teflon,常温下真空浸渍10min。之后将浸渍聚氨酯后的纤维素多孔材料取出,放入水/N,N-二甲基甲酰胺凝固浴中,其中水的质量占比为70wt%,N,N-二甲基甲酰胺的质量占比为30wt%,凝固浴温度为30℃,10min后取出水洗3次,60℃下干燥10h后可得疏水纤维素多孔材料。
之后制备双层纤维素多孔复合材料,其底层为疏水纤维素多孔材料,上层为具有两亲性的纤维素多孔材料,具体制备过程为:首先制备细菌纤维素悬浮液,将细菌纤维素(海南椰果股份有限公司)浸入0.5mol/L浓度的NaOH溶液中,80℃下加热4h后将细菌纤维素取出,并用去离子水洗至中性。之后将细菌纤维素剪碎,利用均质机在15000r/min转速下搅拌1h,从而得到细菌纤维素悬浮液。取上述制备的含有甲基三甲氧基硅烷的纤维素纳米线混合溶液,搅拌2h。再取1wt%固含量的细菌纤维素悬浮液,其中细菌纤维素的长度为1μm,直径为10nm,之后加入硅烷偶联剂KH560和聚乙烯亚胺(上海国药集团化学试剂有限公司,CAS:9002-98-6,分子量2000),其中细菌纤维素与KH560、聚乙烯亚胺的质量比为1:0.5:0.4,搅拌2h。之后取搅拌好的纤维素纳米线混合溶液和细菌纤维素混合溶液,其中纤维素纳米线混合溶液和细菌纤维素混合溶液的质量比为1:0.4,搅拌10min。将上述制备的疏水纤维素多孔材料固定在模具底部,再将制备的纳米纤维素和细菌纤维素的混合溶液倒入模具中。最后将模具转移至80℃烘箱对纳米纤维素和细菌纤维素的混合溶液进行干燥,20小时后取出,可得双层纤维素多孔复合材料。
将上述制备的双层纤维素多孔复合材料固定在模具底部,再将上述制备的含有KH560和聚乙烯亚胺的细菌纤维素混合溶液倒入模具中,其中细菌纤维素、KH560和聚乙烯亚胺的质量比为1:0.5:0.5。将模具转移至80℃烘箱,对细菌纤维素的混合溶液进行干燥,20h后取出,最后可得具有疏水透气功能的多层纤维素基多孔复合材料,其中疏水纤维素多孔材料的孔径大小为30微米;具有两亲性的纤维素多孔材料的孔径大小为1微米;超亲水纤维素多孔材料孔径大小200纳米。其耐水压(GBT 4744-1997)、透湿量(按照ASTM E96干燥剂法测试)、导热系数(参考标准GB/T10294-2008)、底层以及上层水接触角(参考标准GBT30693-2014)见表1。
实施例2
首先制备单层疏水纤维素多孔材料,具体制备过程为:取2wt%固含量的纤维素纳米线悬浮液(天津木精灵有限公司),纤维素纳米线长度为20μm,直径为40nm,之后加入甲基二乙氧基硅烷,其中纤维素纳米线和甲基二乙氧基硅烷的质量比为1:1。常温下搅拌4h后,将混合溶液用液氮冷冻10min后转移至冷冻干燥机中,其中冻干温度为-50℃,冻干时间为40h,之后将冻干后的纤维素多孔材料转移至110℃烘箱中放置2h。将制备的纤维素多孔材料浸入8wt%固含量的聚氨酯溶液中(济宁佰一化工有限公司,HK3100),其中纤维素多孔材料的质量占比为20wt%,聚氨酯含浸液的质量占比为78wt%,同时加入2wt%质量分数的三防整理剂杜邦Teflon,常温下真空浸渍20min。之后将浸渍聚氨酯后的纤维素多孔材料取出,放入水/N,N-二甲基甲酰胺凝固浴中,其中水的质量占比为90wt%,N,N-二甲基甲酰胺的质量占比为10wt%,凝固浴温度为40℃,20min后取出水洗3次,80℃下干燥20h后可得疏水纤维素多孔材料。
之后制备双层纤维素多孔复合材料,其底层为疏水纤维素多孔材料,上层为具有两亲性的纤维素多孔材料,具体制备过程为:首先制备细菌纤维素悬浮液,将细菌纤维素(海南椰果股份有限公司)浸入1mol/L浓度的NaOH溶液中,100℃下加热8h后将细菌纤维素取出,并用去离子水洗至中性。之后将细菌纤维素剪碎,利用均质机在20000r/min转速下搅拌2h,从而得到细菌纤维素悬浮液。取步骤1制备的含有甲基二乙氧基硅烷的纤维素纳米线混合溶液,搅拌4h。再取2wt%固含量的细菌纤维素悬浮液,其中细菌纤维素的长度为25μm,直径为20nm,之后加入硅烷偶联剂KH560和聚乙烯亚胺(上海国药集团化学试剂有限公司,CAS:9002-98-6,分子量2000),其中细菌纤维素与KH560、聚乙烯亚胺的质量比为1:1:0.8,搅拌4h。之后取搅拌好的纤维素纳米线混合溶液和细菌纤维素混合溶液,其中纤维素纳米线混合溶液和细菌纤维素混合溶液的质量比为1:0.8,搅拌20min。将上述制备的疏水纤维素多孔材料固定在模具底部,再将制备的纳米纤维素和细菌纤维素的混合溶液倒入模具中。最后将模具转移至80℃烘箱对纳米纤维素和细菌纤维素的混合溶液进行干燥,30小时后取出,可得双层纤维素多孔复合材料。
最后制备多层纤维素多孔复合材料,其底层为疏水纤维素多孔材料,中层为具有两亲性的纤维素多孔材料,上层为超亲水纤维素多孔材料,具体制备过程为:将上述制备的双层纤维素多孔复合材料固定在模具底部,再将上述制备的含有KH560和聚乙烯亚胺的细菌纤维素混合溶液倒入模具中,其中细菌纤维素、KH560和聚乙烯亚胺的质量比为1:1:1。将模具转移至80℃烘箱对细菌纤维素的混合溶液进行干燥,30h后取出,最后可得具有疏水透气功能的多层纤维素基多孔复合材料,其中疏水纤维素多孔材料的孔径大小为50微米;具有两亲性的纤维素多孔材料的孔径大小为10微米;超亲水纤维素多孔材料孔径大小300纳米。其耐水压(GBT 4744-1997)、透湿量(按照ASTM E96干燥剂法测试)、导热系数(参考标准GB/T10294-2008)、底层以及上层水接触角(参考标准GBT 30693-2014)见表1。
实施例3
首先制备单层疏水纤维素多孔材料,具体制备过程为:取1.2wt%固含量的纤维素纳米线悬浮液(天津木精灵有限公司),纤维素纳米线长度为10μm,直径为30nm,之后加入二甲基二乙烯基硅烷,其中纤维素纳米线和二甲基二乙烯基硅烷的质量比为1:0.6。常温下搅拌2h后,将混合溶液用液氮冷冻10min后转移至冷冻干燥机中,其中冻干温度为-50℃,冻干时间为35h,之后将冻干后的纤维素多孔材料转移至110℃烘箱中放置1h。将制备的纤维素多孔材料浸入5wt%固含量的聚氨酯溶液中(济宁佰一化工有限公司,HK3100),其中纤维素多孔材料的质量占比为15wt%,聚氨酯含浸液的质量占比为81wt%,同时加入4wt%质量分数的三防整理剂杜邦Teflon,常温下真空浸渍12min。之后将浸渍聚氨酯后的纤维素多孔材料取出,放入水/N,N-二甲基甲酰胺凝固浴中,其中水的质量占比为80wt%,N,N-二甲基甲酰胺的质量占比为20wt%,凝固浴温度为35℃,14min后取出水洗3次,70℃下干燥15h后可得疏水纤维素多孔材料。
之后制备双层纤维素多孔复合材料,其底层为疏水纤维素多孔材料,上层为具有两亲性的纤维素多孔材料,具体制备过程为:首先制备细菌纤维素悬浮液,将细菌纤维素(海南椰果股份有限公司)浸入0.8mol/L浓度的NaOH溶液中,90℃下加热5h后将细菌纤维素取出,并用去离子水洗至中性。之后将细菌纤维素剪碎,利用均质机在18000r/min转速下搅拌1.5h,从而得到细菌纤维素悬浮液。取上述制备的含有二甲基二乙烯基硅烷的纤维素纳米线混合溶液,搅拌3h。再取1.2wt%固含量的细菌纤维素悬浮液,其中细菌纤维素的长度为40μm,直径为20nm,之后加入硅烷偶联剂KH560和聚乙烯亚胺(上海国药集团化学试剂有限公司,CAS:9002-98-6,分子量2000),其中细菌纤维素与KH560、聚乙烯亚胺的质量比为1:0.7:0.6,搅拌3h。之后取搅拌好的纤维素纳米线混合溶液和细菌纤维素混合溶液,其中纤维素纳米线混合溶液和细菌纤维素混合溶液的质量比为1:0.5,搅拌15min。将上述制备的疏水纤维素多孔材料固定在模具底部,再将制备的纳米纤维素和细菌纤维素的混合溶液倒入模具中。最后将模具转移至80℃烘箱对纳米纤维素和细菌纤维素的混合溶液进行干燥,25小时后取出,可得双层纤维素多孔复合材料。
最后制备多层纤维素多孔复合材料,其底层为疏水纤维素多孔材料,中层为具有两亲性的纤维素多孔材料,上层为超亲水纤维素多孔材料,具体制备过程为:将上述制备的双层纤维素多孔复合材料固定在模具底部,再将上述制备的含有KH560和聚乙烯亚胺的细菌纤维素混合溶液倒入模具中,其中细菌纤维素、KH560和聚乙烯亚胺的质量比为1:0.8:0.8。。将模具转移至80℃烘箱对对细菌纤维素的混合溶液进行干燥,25h后取出,最后可得具有疏水透气功能的多层纤维素基多孔复合材料,其中疏水纤维素多孔材料的孔径大小为40微米;具有两亲性的纤维素多孔材料的孔径大小为5微米;超亲水纤维素多孔材料孔径大小250纳米。其耐水压(GBT 4744-1997)、透湿量(按照ASTM E96干燥剂法测试)、导热系数(参考标准GB/T10294-2008)、底层以及上层水接触角(参考标准GBT 30693-2014)见表1。
实施例4
首先制备单层疏水纤维素多孔材料,具体制备过程为:取1.2wt%固含量的纤维素纳米线悬浮液(天津木精灵有限公司),纤维素纳米线长度为10μm,直径为30nm,之后加入二甲基二甲氧基硅烷,其中纤维素纳米线和二甲基二甲氧基硅烷的质量比为1:0.7。常温下搅拌3h后,将混合溶液用液氮冷冻10min后转移至冷冻干燥机中,其中冻干温度为-50℃,冻干时间为38h,之后将冻干后的纤维素多孔材料转移至110℃烘箱中放置2h。将制备的纤维素多孔材料浸入6wt%固含量的聚氨酯溶液中(济宁佰一化工有限公司,HK3100),其中纤维素多孔材料的质量占比为18wt%,聚氨酯含浸液的质量占比为79wt%,同时加入3wt%质量分数的三防整理剂杜邦Teflon,常温下真空浸渍15min。之后将浸渍聚氨酯后的纤维素多孔材料取出,放入水/N,N-二甲基甲酰胺凝固浴中,其中水的质量占比为85wt%,N,N-二甲基甲酰胺的质量占比为15wt%,凝固浴温度为34℃,20min后取出水洗3次,80℃下干燥18h后可得疏水纤维素多孔材料。
之后制备双层纤维素多孔复合材料,其底层为疏水纤维素多孔材料,上层为具有两亲性的纤维素多孔材料,具体制备过程为:首先制备细菌纤维素悬浮液,将细菌纤维素(海南椰果股份有限公司)浸入0.7mol/L浓度的NaOH溶液中,100℃下加热6h后将细菌纤维素取出,并用去离子水洗至中性。之后将细菌纤维素剪碎,利用均质机在16000r/min转速下搅拌2h,从而得到细菌纤维素悬浮液。取上述制备的含有二甲基二甲氧基硅烷的纤维素纳米线混合溶液,搅拌4h。再取1.2wt%固含量的细菌纤维素悬浮液,其中细菌纤维素的长度为30μm,直径为15nm,之后加入硅烷偶联剂KH560和聚乙烯亚胺(上海国药集团化学试剂有限公司,CAS:9002-98-6,分子量2000),其中细菌纤维素与KH560、聚乙烯亚胺的质量比为1:0.6:0.4,搅拌4h。之后取搅拌好的纤维素纳米线混合溶液和细菌纤维素混合溶液,其中纤维素纳米线混合溶液和细菌纤维素混合溶液的质量比为1:0.6,搅拌15min。将上述制备的疏水纤维素多孔材料固定在模具底部,再将制备的纳米纤维素和细菌纤维素的混合溶液倒入模具中。最后将模具转移至80℃烘箱对纳米纤维素和细菌纤维素的混合溶液进行干燥,27h后取出,可得双层纤维素多孔复合材料。
最后制备多层纤维素多孔复合材料,其底层为疏水纤维素多孔材料,中层为具有两亲性的纤维素多孔材料,上层为超亲水纤维素多孔材料,具体制备过程为:将上述制备的双层纤维素多孔复合材料固定在模具底部,再将上述制备的含有KH560和聚乙烯亚胺的细菌纤维素混合溶液倒入模具中,其中细菌纤维素、KH560和聚乙烯亚胺的质量比为1:0.8:0.7。将模具转移至80℃烘箱对细菌纤维素的混合溶液进行干燥,28h后取出,最后可得具有疏水透气功能的多层纤维素基多孔复合材料,其中疏水纤维素多孔材料的孔径大小为40微米;具有两亲性的纤维素多孔材料的孔径大小为6微米;超亲水纤维素多孔材料孔径大小280纳米。其耐水压(GBT 4744-1997)、透湿量(按照ASTM E96干燥剂法测试)、导热系数(参考标准GB/T10294-2008)、底层以及上层水接触角(参考标准GBT 30693-2014)见表1。
表1多层纤维素基多孔复合材料的耐水压、透湿量、底层以及上层水接触角
由表1可以看出,与对比例CN103963393中公开的耐水压和透湿量数据相比,本发明制备的多层纤维素基多孔复合材料具有较高的耐水压和透湿量。同时,该复合材料的底层显示了疏水性能,上层展现出了超亲水性能,从而说明该材料有着良好的疏水透气性能。
Claims (7)
1.一种多层纤维素基多孔复合材料的制备方法,包括:
(1)将纤维素多孔材料浸入聚氨酯溶液中,同时加入三防整理剂,常温下真空浸渍10~20min,取出后放入凝固浴中,凝固浴温度为30~40℃,10~20min后取出,洗涤,干燥,得到疏水纤维素多孔材料;其中纤维素多孔材料具体为:纤维素纳米线悬浮液中加入硅烷偶联剂,常温下搅拌2~4h后,用液氮冷冻,冻干,其中冻干温度为-50℃,冻干时间为30~40h,再在110℃放置1~2h;
(2)将上述疏水纤维素多孔材料固定在模具底部,再将改性的纤维素纳米线和改性的细菌纤维素的混合溶液倒入模具中,干燥,得到双层纤维素多孔复合材料;其中改性的纤维素纳米线和改性的细菌纤维素的混合溶液具体为:细菌纤维素悬浮液中加入硅烷偶联剂KH560和聚乙烯亚胺,搅拌2~4h,得到细菌纤维素混合液;纤维素纳米线悬浮液中加入硅烷偶联剂,搅拌2~4h,得到纤维素纳米线混合液,然后按纤维素纳米线混合溶液和细菌纤维素混合溶液的质量比为1:0.4~0.8混合,搅拌10~20min;
(3)将上述双层纤维素多孔材料固定在模具底部,再将含有KH560和聚乙烯亚胺的细菌纤维素混合溶液倒入模具中,干燥,即得多层纤维素基多孔复合材料。
2.根据权利要求1所述制备方法,其特征在于,所述步骤(1)中聚氨酯溶液的固含量为4~8wt%;所述纤维素多孔材料浸入聚氨酯溶液中,其中纤维素多孔材料的质量占比为10~20wt%,聚氨酯含浸液的质量占比为78~86wt%,三防整理剂的质量分数为2~4wt%;三防整理剂为杜邦Teflon;凝固浴为水和N,N-二甲基甲酰胺凝固浴,其中水的质量占比为70~90wt%,N,N-二甲基甲酰胺的质量占比为10~30wt%。
3.根据权利要求1所述制备方法,其特征在于,所述步骤(2)中细菌纤维素悬浮液的固含量为1~2wt%;纤维素纳米线悬浮液的固含量为1~2wt%;所述细菌纤维素的长度为1~50μm,直径为10~20nm;纤维素纳米线的长度为1~20μm,直径为20-40nm;纤维素纳米线和硅烷偶联剂的质量比为1:0.5~1;细菌纤维素与KH560、聚乙烯亚胺的质量比为1:0.5~1:0.4~0.8。
4.一种权利要求1所述方法制备的多层纤维素基多孔复合材料,其特征在于,所述复合材料由下到上依次包括,疏水纤维素多孔材料底层,具有两亲性的纤维素多孔材料中层,超亲水纤维素多孔材料上层;
所述疏水纤维素多孔材料为包括纤维素多孔材料和聚氨酯的复合材料,疏水纤维素多孔材料中还含有三防整理剂;具有两亲性的纤维素多孔材料为硅烷偶联剂改性的纤维素纳米线和改性的细菌纤维素复合多孔材料;上层超亲水纤维素多孔材料为超亲水细菌纤维素多孔材料;
其中改性的细菌纤维素为采用硅烷偶联剂为KH560和聚乙烯亚胺进行改性处理;超亲水细菌纤维素为KH560和聚乙烯亚胺处理的细菌纤维素。
5.根据权利要求4所述复合材料,其特征在于,所述疏水纤维素多孔材料的孔径大小为30-50微米;具有两亲性的纤维素多孔材料的孔径大小为1-10微米;超亲水纤维素多孔材料孔径大小200-300纳米。
6.根据权利要求4所述复合材料,其特征在于,所述改性的纤维素纳米线采用的硅烷偶联剂为甲基三甲氧基硅烷,甲基二乙氧基硅烷,二甲基二乙烯基硅烷,二甲基二甲氧基硅烷中的一种或几种。
7.一种权利要求1所述方法制备的多层纤维素基多孔复合材料在服装领域中的应用。
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