CN109137476A - 一种基于TiO2纳米管的仿生超疏水棉织物的制备方法 - Google Patents
一种基于TiO2纳米管的仿生超疏水棉织物的制备方法 Download PDFInfo
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Abstract
本发明提出了一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,包含以下步骤:(1)取TiO2纳米颗粒溶于NaOH溶液中,超声,避光机械搅拌后将上述溶液置于水热反应釜中反应;反应产物用蒸馏水冲洗到pH为7以后用酸洗至上层清夜pH为1,再用蒸馏水冲洗到pH为中性,干燥,制得TiO2纳米管,避光保存;(2)取TiO2纳米管加入到硅烷的乙醇溶液中,超声震荡;加入蒸馏水,经水解反应即可得到疏水化TiO2纳米管整理液;(3)常温下将棉织物浸渍于疏水化TiO2纳米管整理液中,浸渍后取出并60℃烘干,得到超疏水棉织物。本发明所制备的棉织物具有良好的超疏水性能、透气、自清洁、抗紫外和耐磨性好,具有极为显著的应用前景。
Description
技术领域
本发明涉及功能面料技术领域,具体涉及一种基于TiO2纳米管的仿生超疏水棉织物的制备方法。
背景技术
超疏水性是指水滴和固体表面的接触角超过150o且滚动角小于10o的一种润湿性。自然界中的典型代表有:荷叶、水稻叶等。超疏水表面由于具有抗润湿、抗黏附、自清洁、防腐蚀、防覆冰、防污抗菌、流体减阻等优良特性,在纺织、航空、建筑等领域具有广阔的应用潜力。为了在纺织面料表面构筑低表面能微纳米粗糙界面,目前主要方法是将微纳米颗粒整理到纤维表面形成类似荷叶“乳突”的凹凸结构。而实际上,除了点阵式凹凸结构外,线性微纳米阵列如水稻,片状微纳米粗糙结构如蝴蝶,网络状粗糙结构如纳米纤维无纺布,同样可是实现优异超疏水性能甚至是单向导水功能的超疏水结构。然而,纺织面料主要由有机纤维组成,对强酸、强碱耐受性差,织物柔软且表面为粗糙多孔结构,对力学性能和服装舒适性要求高,无法利用刻蚀,镀膜等方法处理。因此,非乳突结构的纳米超疏水纺织面料一直游离于研究这视野之外。
目前关于超疏水织物的相关专利很多,如中国发明专利“一种超疏水抗菌织物的制备方法”(CN 108385375A)中,公开了一种超疏水抗菌织物的制备方法,该方法在室温下利用多巴胺的Tris缓冲溶液对织物进行处理,再将织物浸渍于硝酸银、柠檬酸铵以及硼酸的混合溶液中,取出烘干后获得由纳米银构造的织物粗糙表面;再用无氟拒水剂对纳米银构造的织物粗糙表面进行后处理,赋予织物低表面能;如中国发明专利“一种石墨烯基超疏水织物及其制备方法”(CN 107858825A)中,公开了一种石墨烯基超疏水织物的制备方法,该方法先用含S-H基的硅烷偶联剂对氧化石墨烯进行表面改性,得到表面含S-H基的改性氧化石墨烯;然后,在室温下,将改性氧化石墨烯和端乙烯基聚二甲基硅氧烷分散在溶剂中并均匀搅拌,再加入交联剂和光引发剂,继续搅拌形成均匀的溶液;最后,采用浸涂法将织物浸泡在制备的混合溶液中,取出后通过紫外光照射,使附着在织物上的改性氧化石墨烯上的S-H基与端乙烯基聚二甲基硅氧烷上的C=C双键发生巯烯反应,最终制得石墨烯基超疏水织物。但是目前这些制备超疏水织物的方法具有步骤繁琐、改性层易脱落的问题
发明内容
为了解决上述的技术问题,本发明提供一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,通过用硅烷改性TiO2纳米材料,制得的基于TiO2纳米管的仿生超疏水棉织物不仅具有良好的超疏水性能,还具有良好的透气、自清洁、抗紫外等优点,且通过化学键的连接可有效提升氟硅烷修饰的TiO2纳米管与棉织物之间牢度,提高耐磨性。
本发明提供一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,包含以下步骤:
(1)取TiO2纳米颗粒溶于NaOH溶液,并超声第一时间,避光机械搅拌第二时间后将上述溶液置于水热反应釜中反应;反应产物用蒸馏水冲洗到pH为7以后用酸洗至上层清夜pH为1,再用蒸馏水冲洗到pH为中性,干燥,制得TiO2纳米管,避光保存;
(2)取TiO2纳米管加入到硅烷的乙醇溶液中,超声震荡第三时间;加入蒸馏水,经水解反应第四时间即可得到疏水化TiO2纳米管整理液;
(3)常温下将棉织物浸渍于疏水化TiO2纳米管整理液中,浸渍第五时间后取出并60℃烘干,得到超疏水棉织物。
作为本发明进一步的改进,硅烷包括全氟辛基三乙氧基硅烷,所述硅烷的乙醇溶液为体积介于2-10mL,所述全氟辛基三乙氧基硅烷的质量浓度介于1%-5%。
作为本发明进一步的改进,所述TiO2纳米颗粒与所述NaOH溶液的质量比为1:(80-100),所述TiO2纳米管与所述全氟辛基三乙氧基硅烷的质量比为(3-6):1,所述蒸馏水与所述全氟辛基三乙氧基硅烷(25-50):1,所述棉织物与疏水化TiO2纳米管整理液的质量比为1:(35-45)。
作为本发明进一步的改进,所述棉织物与疏水化TiO2纳米管整理液的浴比为1:(35-45),浸渍时间为3-5h。
作为本发明进一步的改进,步骤(1)中在所述水热反应釜中100-150℃反应24-48h。
作为本发明进一步的改进,所述超声功率为500-700W。
作为本发明进一步的改进,所述搅拌转速为300-500r/min。
作为本发明进一步的改进,所述TiO2纳米颗粒的质量介于0.6g~2g之间。
作为本发明进一步的改进,所述NaOH溶液的体积介于60mL~180mL之间,所述NaOH溶液的浓度介于8-12mol/L。
作为本发明进一步的改进,所述步骤(1)中采用0.1-0.5mol/L HCl酸洗至上层清夜pH为1。
作为本发明进一步的改进,所述第一时间介于0.5-1h,所述第二时间介于12-15h,所述第三时间介于1-2h,所述第四时间介于1-3h,所述第五时间介于3-5h。
本发明具有如下有益效果:本发明方法工艺简单,所制备的棉织物不仅具有良好的超疏水性能,还具有良好的透气、自清洁、抗紫外等优点,且通过化学键的连接可有效提升氟硅烷修饰的TiO2纳米管与棉织物之间牢度,提高耐磨性,其在各种床上用品、卫生材料、装饰材料等领域具有极为显著的应用前景。
附图说明
图1为浸渍前后棉织物的接触角图。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整的描述,显然,所述的实施例只是本发明的部分具有代表性的实施例,而不是全部实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的其他所有实施例都属于本发明的保护范围。
一种硅烷改性TiO2纳米管超疏水材料的制备方法,包含以下步骤:
(1)取(0.6-2)gTiO2纳米颗粒溶于(60-180)mL(8-12)mol/L的NaOH溶液中,(500-700W)超声0.5-1h,避光机械搅拌(300-500r/min)12-15h后将上述溶液置于水热反应釜中,100-150℃反应24-48h;反应产物用蒸馏水冲洗到pH为7以后用(0.1-0.5)mol/LHCl酸洗至上层清夜pH为1,再用蒸馏水冲洗到pH为中性,干燥,制得TiO2纳米管,避光保存;
(2)取TiO2纳米管加入到全氟辛基三乙氧基硅烷质量浓度介于1%-5%的乙醇溶液(2-10)mL中,(500-700W)超声震荡1-2h;加入蒸馏水,经水解反应1-3h即可得到疏水化TiO2纳米管整理液;
(3)常温下将1g棉织物浸渍于(35-45)mL疏水化TiO2纳米管整理液中,浸渍(3-5h)后取出并60℃烘干,得到超疏水棉织物。
实施例1 基于TiO2纳米管的仿生超疏水棉织物的制备
(1)取0.6g TiO2纳米颗粒与60mL 12mol/LNaOH溶液中,500W超声1h,避光机械搅拌(300r/min)15h后将上述溶液置于水热反应釜中,100℃下水热反应24h;反应产物用蒸馏水冲洗到pH为7以后用0.5mol/LHCL酸洗至上层清夜pH为1,再用蒸馏水冲洗到pH为中性,150℃干燥,制得TiO2纳米管,避光保存;
(2)取0.3gTiO2纳米管加入到10mL 10g/L全氟辛基三乙氧基硅烷溶于10mL乙醇中,500W超声震荡2h;加入5g蒸馏水,经水解反应3h即可得到疏水化TiO2纳米管整理液;
(3)常温下将1g棉织物浸渍于35mL疏水化TiO2纳米管整理液中,浸渍3h后取出并60℃烘干,得到超疏水棉织物。
实施例2 基于TiO2纳米管的仿生超疏水棉织物的制备
(1)称取1g TiO2纳米颗粒溶于80mL 8mol/L NaOH溶液中,700W超声30min,避光机械搅拌(500r/min)12h后将上述溶液置于水热反应釜中,150℃下水热反应48h;反应产物用蒸馏水冲洗到pH为7后以0.1mol/LHCL酸洗至上层清夜PH为1,再用蒸馏水冲洗到pH为中性,上述产物150℃干燥,制得TiO2纳米管,避光保存;
(2)取0.6gTiO2纳米管加入到10mL 10g/L全氟辛基三乙氧基硅烷溶于2mL乙醇中,700W超声震荡1h;加入2.5g蒸馏水,经水解反应1h即可得到疏水化TiO2纳米管整理液;
(3)常温下将1g棉织物浸渍于45mL疏水化TiO2纳米管整理液中,浸渍5h后取出60℃烘干,得到超疏水棉织物。
实施例3 基于TiO2纳米管的仿生超疏水棉织物的制备
(1)取2g TiO2纳米颗粒与180mL 10mol/L NaOH溶液中,600W超声45min,避光机械搅拌(400r/min)13h后将上述溶液置于水热反应釜中,120℃反应36h;反应产物用蒸馏水冲洗到pH为7以后用0.3mol/LHCL酸洗至上层清夜pH为1,再用蒸馏水冲洗到pH为中性,150℃干燥,制得TiO2纳米管,避光保存;
(2)取0.45g TiO2纳米管加入到10mL 10g/L全氟辛基三乙氧基硅烷溶于4mL乙醇中,600W超声震荡1.5h;加入4g蒸馏水,经水解反应2h即可得到疏水化TiO2纳米管整理液;
(3)常温下将1g棉织物浸渍于40mL疏水化TiO2纳米管整理液中,浸渍4h后取出并60℃烘干,得到超疏水棉织物。
实施例4 基于TiO2纳米管的仿生超疏水棉织物的制备
(1)取1.5g TiO2纳米颗粒与150mL 10mol/L NaOH溶液中,600W超声50min,避光机械搅拌(400r/min)14h后将上述溶液置于水热反应釜中,130℃反应40h;反应产物用蒸馏水冲洗到pH为7以后用0.4mol/LHCL酸洗至上层清夜pH为1,再用蒸馏水冲洗到pH为中性,150℃干燥,制得TiO2纳米管,避光保存;
(2)取0.45g TiO2纳米管加入到10mL 10g/L全氟辛基三乙氧基硅烷溶于6mL乙醇中,600W超声震荡2h;加入4g蒸馏水,经水解反应3h即可得到疏水化TiO2纳米管整理液;
(3)常温下将1g棉织物浸渍于40mL疏水化TiO2纳米管整理液中,浸渍4h后取出并60℃烘干,得到超疏水棉织物。
本领域的技术人员在不脱离权利要求书确定的本发明的精神和范围的条件下,还可以对以上内容进行各种各样的修改。因此本发明的范围并不仅限于以上的说明,而是由权利要求书的范围来确定的。
Claims (10)
1.一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于,包含以下步骤:
(1)取TiO2纳米颗粒溶于NaOH溶液,并超声第一时间,避光机械搅拌第二时间后将上述溶液置于水热反应釜中反应;反应产物用蒸馏水冲洗到pH为7以后用酸洗至上层清夜pH为1,再用蒸馏水冲洗到pH为中性,干燥,制得TiO2纳米管,避光保存;
(2)取TiO2纳米管加入到硅烷的乙醇溶液中,超声震荡第三时间;加入蒸馏水,经水解反应第四时间即可得到疏水化TiO2纳米管整理液;
(3)常温下将棉织物浸渍于疏水化TiO2纳米管整理液中,浸渍第五时间后取出并60℃烘干,得到超疏水棉织物。
2.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述硅烷包括全氟辛基三乙氧基硅烷,所述硅烷的乙醇溶液为体积介于2-10mL,所述全氟辛基三乙氧基硅烷的质量浓度介于1%-5%。
3.根据权利要求2所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述TiO2纳米颗粒与所述NaOH溶液的质量比为1:(80-100),所述TiO2纳米管与所述全氟辛基三乙氧基硅烷的质量比为(3-6):1,所述蒸馏水与所述全氟辛基三乙氧基硅烷(25-50):1,所述棉织物与疏水化TiO2纳米管整理液的质量比为1:(35-45)。
4.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:步骤(1)中在所述水热反应釜中100-150℃反应24-48h。
5.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述超声功率为500-700W。
6.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述搅拌转速为300-500r/min。
7.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述TiO2纳米颗粒的质量介于0.6g~2g之间。
8.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述NaOH溶液的体积介于60mL~180mL之间,所述NaOH溶液的浓度介于8-12mol/L。
9.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述步骤(1)中采用0.1-0.5mol/LHCl酸洗至上层清夜pH为1。
10.根据权利要求1所述的一种基于TiO2纳米管的仿生超疏水棉织物的制备方法,其特征在于:所述第一时间介于0.5-1h,所述第二时间介于12-15h,所述第三时间介于1-2h,所述第四时间介于1-3h,所述第五时间介于3-5h。
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