CN117364469A - 一种高耐磨抗菌防污复合纱线及其制备方法 - Google Patents
一种高耐磨抗菌防污复合纱线及其制备方法 Download PDFInfo
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- CN117364469A CN117364469A CN202311299540.XA CN202311299540A CN117364469A CN 117364469 A CN117364469 A CN 117364469A CN 202311299540 A CN202311299540 A CN 202311299540A CN 117364469 A CN117364469 A CN 117364469A
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Abstract
本发明公开了一种高耐磨抗菌防污复合纱线及其制备方法,属于复合纱线加工技术领域,用于解决现有技术中的棉纤维纺织纱线的力学性能差、抗污性能差及抗菌效果有限,在经过多次干洗后,棉纤维纺织材料的抗菌率快速下降,抗菌率保有量低的技术问题;该复合纱线由复合石墨烯对预处理改性得到的改性棉纤维进行修饰改性,制备成复合棉纤维,通过纺纱机对复合棉纤维进行纺纱,本发明是对棉纤维进行改性后制备成纱线,再对纱线进行浸渍改性,不仅有效的提高了复合纱线的疏水抗油污性能与抑菌效果,还有效的提高了复合纱线的力学性能与耐磨性能,使其拓宽了棉纤维复合纱线的应用范围。
Description
技术领域
本发明涉及复合纱线加工技术领域,具体涉及一种高耐磨抗菌防污复合纱线及其制备方法。
背景技术
纱线是一种纺织品的加工原料,广泛应用于纺织、服装及家纺等领域,而棉纤维纱线是一种由棉花纤维制成的纱线,并且棉花作为可再生资源,因此棉纤维纱线的生产相对环保,常用于纺织、制作布料等方面;
但现有技术中的棉纤维复合纱线的耐久性低,在日常对其制成的纺织品进行干洗时易磨损,造成纺织品破损或起毛,不适合户外装备或工业用品的应用需要,而传统的棉纤维复合纱线具有良好的吸水和吸油性能,以致其耐污性差,并且棉纤维纱线不均匀的抗菌性能,在棉纤维纺织材料在加工完成之后,通常会采用抗菌剂对其进行染整,但染整后的棉纤维纺织材料的抗菌效果有限,在经过多个干洗后,棉纤维纺织材料的抗菌率保有量低,棉纤维纺织材料容易在被污染后滋生大量的微生物,增加了感染和过敏的风险;
针对此方面的技术缺陷,现提出一种解决方案。
发明内容
本发明的目的在于提供一种高耐磨抗菌防污复合纱线及其制备方法,以解决背景技术所提出的技术缺陷。
本发明的目的可以通过以下技术方案实现:一种高耐磨抗菌防污复合纱线,由复合石墨烯对预处理改性得到的改性棉纤维进行修饰改性,制备成复合棉纤维,通过纺纱机对复合棉纤维进行纺纱,制备成复合纱线初品,使用防污整理剂对复合纱线进行浸渍改性后,制备得到;
所述复合石墨烯由以下步骤加工而成:
A1、将氧化石墨烯、三甲氧基硅烷剂甲硫醇、三甲氧基硅烷、四甲氧基硅烷和无水乙醇加入到三口烧瓶中,超声分散30-50min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液,室温下反应40-60min,后处理得到中间体I;
中间体I的合成反应原理为:
A2、将中间体I、四氯化钛和纯化水加入到三口烧瓶中,超声分散60-80min,保持超声分散状态,向三口烧瓶中滴加氨水,调节体系pH=10-12,室温下超声分散2-3h,后处理,得到中间体II;
A3、将中间体II、无水乙醇和3-缩水甘油醚氧基丙基三甲氧基硅烷加入到三口烧瓶中,超声分散30-50min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液,室温下反应50-80min,后处理得到改性石墨烯;
改性石墨烯的合成反应原理为:
A4、将改性石墨烯、N,N-二甲基甲酰胺、10wt%氢氧化钠溶液加入到三口烧瓶中,超声分散20-30min,将三口烧瓶固定在带有机械搅拌的铁架台上搅拌,向三口烧瓶中加入复合抗菌剂,三口烧瓶温度升高至50-60℃,保温反应60-80min,后处理得到复合石墨烯。
复合石墨烯的合成反应原理为:
进一步的,步骤A1中氧化石墨烯、三甲氧基硅烷剂甲硫醇、三甲氧基硅烷、四甲氧基硅烷、无水乙醇和5wt%氢氧化钠溶液的用量比为10g:3g:1g:2g:100g:15g,所述后处理操作包括:反应完成之后,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为60-70℃的干燥箱中,真空干燥至恒重,得到中间体I;步骤A2中中间体I、四氯化钛和纯化水的用量比为4g:1g:100g,所述后处理操作包括:反应完成之后,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65-75℃的干燥箱中,真空干燥至恒重,得到中间体II;步骤A3中中间体II、无水乙醇、3-缩水甘油醚氧基丙基三甲氧基硅烷和5wt%氢氧化钠溶液的用量比为10g:100g:3g:15g,所述后处理操作包括:反应完成之后,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为60-70℃的干燥箱中,真空干燥至恒重,得到改性石墨烯;步骤A4中改性石墨烯、N,N-二甲基甲酰胺、10wt%氢氧化钠溶液与复合抗菌剂的用量比为10g:60mL:8g:4g,所述后处理操作包括:反应完成之后,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤三次后抽干,将滤饼转移到温度为65-75℃的干燥箱中,真空干燥至恒重,得到复合石墨烯。
进一步的,复合抗菌剂由以下步骤加工而成:
B1、将对氨基苯甲醛、二异氰基甲烷和丙酮加入到氮气保护的三口烧瓶中搅拌,室温下反应30-50min,后处理得到中间体1;
中间体1的合成反应原理为:
B2、将中间体1和缩二脲、盐酸加入到三口烧瓶中搅拌,室温下反应20-22h,后处理得到复合抗菌剂。
复合抗菌剂的合成反应原理为:
进一步的,步骤B1中对氨基苯甲醛、二异氰基甲烷的摩尔比为2:1,所述丙酮用量为对氨基苯甲醛重量的5倍,所述后处理操作包括:反应完成之后,三口烧瓶温度升高至45-55℃,减压蒸除丙酮,得到中间体1;步骤B2中中间体1、缩二脲的摩尔比为1:1,所述盐酸的浓度为9-11mol/L,盐酸的用量为中间体1重量的10倍,所述后处理操作包括:反应完成之后,抽滤,滤用10vt%醋酸溶液洗涤三次,再使饼用纯化水洗涤三次后抽干,滤饼转移到温度为65-75℃的干燥箱中,真空干燥至恒重,得到复合抗菌剂。
进一步的,棉纤维的预处理改性操作包括以下步骤:
C1、将纯化水、氢氧化钠和十二烷基磺酸钠加入到烧杯中搅拌至体系溶解,向烧瓶中加入棉纤维,室温下,超声分散30-50min,后处理得到预处理棉纤维;
C2、将预处理棉纤维和35wt%氢氧化钠溶液加入烧瓶中,室温下,搅拌30-50min,向烧瓶中缓慢加入环氧氯丙烷,烧瓶温度升高至55-65℃,保温反应2-3h,后处理得到改性棉纤维。
改性棉纤维的合成反应原理为:
进一步的,步骤C1中纯化水、氢氧化钠、十二烷基磺酸钠和棉纤维的用量比为100g:15g:2g:6g,所述后处理操作包括:超声完成之后,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65-75℃的干燥箱中,干燥至恒重,得到预处理棉纤维;步骤C2中预处理棉纤维、35wt%氢氧化钠溶液和环氧氯丙烷的用量比为1g:12g:5g,所述后处理操作包括:反应完成之后,烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65-75℃的干燥箱中,干燥至恒重,得到改性棉纤维。
进一步的,复合棉纤维的制备方法为:将复合石墨烯与纯化水加入到烧瓶中,超声分散30-50min,保持超声状态,向烧瓶中加入改性棉纤维和催化剂,烧瓶温度升高至50-60℃,保温超声反应3-4h,后处理得到复合棉纤维,其中,所述复合石墨烯、纯化水、改性棉纤维和催化剂的用量比为3g:40mL:8g:2g,所述催化剂为对甲苯磺酸,所述后处理操作包括:反应完成之后,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为60-70℃的干燥箱中,干燥至恒重,得到复合棉纤维。
进一步的,防污整理剂由以下步骤加工而成:
D1、将全氟辛基磺酰胺、1,2-环氧基-5-己烯、氢氧化钠和N,N-二甲基甲酰胺加入到氮气保护的三口烧瓶中搅拌,三口烧瓶温度升高至65-75℃,保温反应3-5h,后处理得到改性全氟辛基磺酰胺;
改性全氟辛基磺酰胺的合成反应原理为:
D2、将改性全氟辛基磺酰胺、甲基丙烯酸丁酯、甲基丙烯酸月桂酯、四氢呋喃和引发剂加入到三口烧瓶中搅拌,三口烧瓶温度升高够55-65℃,保温反应10-12h,后处理得到防污剂;
防污剂的合成反应原理为:
D3、将防污剂、氨基改性硅酮、1,4-丁二醇二丙烯酸酯、纳米氧化锌和四氢呋喃加入到烧杯中搅拌均匀,得到防污整理剂。
进一步的,步骤D1中全氟辛基磺酰胺、1,2-环氧基-5-己烯的摩尔比为1:1,所述全氟辛基磺酰胺、氢氧化钠和N,N-二甲基甲酰胺的用量比为3g:2g:10g,所述后处理操作包括:反应完成之后,三口烧瓶温度降低至室温,向三口烧瓶中加入纯化水,有大量固体析出,抽滤,滤饼用纯化水洗涤至中性后,将其转移到温度为70-80℃的干燥箱中,干燥至恒重,得到改性全氟辛基磺酰胺;步骤D2中改性全氟辛基磺酰胺、甲基丙烯酸丁酯、甲基丙烯酸月桂酯的摩尔比为4:2:1,所述改性全氟辛基磺酰胺、四氢呋喃和引发剂的用量比为5g:30mL:0.6g,所述引发剂为偶氮二异丁腈,所述后处理操作包括:反应完成之后,三口烧瓶温度降低至室温,向三口烧瓶中缓慢加入纯化水,有大量固体析出,抽滤,滤饼用无水乙醇洗涤三次后抽干,将滤饼转移到温度为60-70℃的干燥箱中,干燥至恒重,得到防污剂;步骤D3中防污剂、氨基改性硅酮、1,4-丁二醇二丙烯酸酯、纳米氧化锌和四氢呋喃的用量比为5g:3g:1g:1g:60g。
一种高耐磨抗菌防污复合纱线的制备方法,包括以下步骤:
S1、对棉纤维进行预处理改性,制备得到的改性棉纤维;
S2、使用复合石墨烯对改性棉纤维进行修饰改性,制备得到复合棉纤维;
S2、使用纺纱机将复合棉纤维纺织成粗细为30-40Ne的复合纱线初品;
S3、将复合纱线初品完全浸渍到装有防污整理剂的烧杯中,室温辐射状态下,超声浸渍50-60min,将复合纱线初品从烧杯中捞出,用无水乙醇洗涤3次,使用纯化水洗涤3次,抽干,将其转移到温度为75-85℃的干燥箱中,干燥至恒重,得到复合纱线成品。
本发明具备下述有益效果:
1、本发明的高耐磨抗菌防污复合纱线,以棉花的棉纤维为原料,通过十二烷基磺酸钠与氢氧化钠溶液对棉纤维进行处理,包裹住棉纤维表面的杂质和污垢,使其分散在水中,对棉纤维进行清理,然后在碱性环境中与环氧氯丙烷发生取代加成反应,生成具有环氧烷修饰的改性棉纤维,改性棉纤维与复合石墨烯在催化剂的作用下,改性棉纤维上的环氧烷与复合石墨烯上的氨基、羧基、羟基等活性官能团反应,将复合石墨烯接枝修饰在改性棉纤维上,在改性棉纤维表面形成具有抗菌、耐磨的复合石墨烯层,从而提高复合纤维的抗菌与耐磨性能;复合纤维制备成纱线后,通过制备的抗污整理剂对纱线进行浸渍改性,提高复合纤维的抗污性能。
2、本发明的高耐磨抗菌防污复合纱线,在制备时,通过三甲氧基硅烷剂甲硫醇、三甲氧基硅烷、四甲氧基硅烷与氧化石墨烯均匀分散在无水乙醇环境中之后,在碱性环境下,硅氧烷键水解断开后缩合,在氧化石墨烯上形成具有巯基修饰的硅氧烷复合层,巯基的修饰能够进一步的提高氧化石墨烯对钛离子的吸附性能,在氨水环境中,钛离子以固体沉淀的形式附着在氧化石墨烯上,通过后处理,在氧化石墨烯的表面形成钛修饰,3-缩水甘油醚氧基丙基三甲氧基硅烷对石墨烯进行进一步的改性,形成具有环氧烷修饰的改性石墨烯;巯基修饰的聚硅烷层在石墨烯表面形成一种附加层,能够增加石墨烯的抗拉强度和硬度,提高石墨烯的耐磨性,聚硅烷层修饰的巯基能够提高钛元素在氧化石墨烯上的吸附性能的同时,还能够与钛元素相配合,提高抗菌效果,阻止细菌或微生物的附着和生长,从而提高石墨烯的抗菌性能;在制备复合石墨烯过程中,通过对氨基苯甲醛、二异氰基甲烷进行缩合反应,制备得到具有苯甲醛封端的中间体1,中间体1上的苯甲醛与缩二脲发生亲核加成反应,形成6-苯基-2,4-二氧杂-1,3,5-三嗪封端的复合抗菌剂,复合抗菌剂在碱性环境中与改性石墨烯上修饰的环氧乙烷反应,制备成复合石墨烯;复合抗菌剂上的含有的丰富的酮基,具有化学反应的活性,可以与微生物细胞的生化分子发生反应,可能影响细胞的正常功能,进一步的提高复合石墨烯的抗菌性能,并且酮基中含有的碳-氧双键,能够使分子中的碳原子排列更为紧密,分子间相互作用增强,进一步的提高聚硅氧烷层的硬度,从而提高材料的硬度,进而提高复合石墨烯的耐磨性能。
3、本发明的高耐磨抗菌防污复合纱线,在制备时,通过全氟辛基磺酰胺、1,2-环氧基-5-己烯发生取代加成反应,制备成具有烯烃修饰的改性全氟辛基磺酰胺,改性全氟辛基磺酰胺、甲基丙烯酸丁酯、甲基丙烯酸月桂酯在自由基引发剂的作用下发生自由基缩合反应,制备生成具有氟和长烷烃修饰的聚烯烃防污剂;防污剂、氨基改性硅酮、1,4-丁二醇二丙烯酸酯、纳米氧化锌均匀分散在四氢呋喃中,制备成防污整理剂;防污整理剂对复合纱线初品进行浸渍处理,在复合纱线初品上形成膜层,防污剂中含有的长碳氟链段与长烷烃支链具有疏水性,纳米氧化锌的表面具有高度活性的羟基和氧化锌纳米颗粒,这些功能性基团可以与水分子和油分子发生相互作用,吸附水分子,增强薄膜的亲水性,在纱线表面形成疏水疏油双疏的涂层,阻止水分、水性污渍或油性污渍附着在纱线上,氨基改性硅酮是一种硅基化合物,具有表面张力调节作用,其与纱线表面的疏水涂层相互作用,降低液体在纱线表面的表面张力,使污渍不易附着在纱线上,并且氨基改性硅酮能够与1,4-丁二醇二丙烯酸酯、防污剂发生交联聚合,形成三维网状结构,进一步的增强了整理剂的耐磨性和机械强度,进一步保护了纱线不易受损,此外,纳米氧化锌通常具有抗菌性质,将纳米氧化锌均匀分散在整理剂中,可以赋予纱线一定的抗菌性质,有助于抑制微生物的生长,减少污染的风险。
具体实施方式
下面将结合实施例对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,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所有其它实施例,都属于本发明保护的范围。
实施例1
本实施例提高一种高耐磨抗菌防污复合纱线的制备方法,包括以下步骤:
S1、制备改性棉纤维
称取:纯化水1L、氢氧化钠150g和十二烷基磺酸钠20g加入到烧杯中搅拌至体系溶解,向烧瓶中加入棉纤维60g,室温下,超声分散30min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65℃的干燥箱中,干燥至恒重,得到预处理棉纤维;
称取:预处理棉纤维50g和35wt%氢氧化钠溶液600g加入烧瓶中,室温下,搅拌30min,向烧瓶中缓慢加入环氧氯丙烷250g,烧瓶温度升高至55℃,保温反应2h,烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65℃的干燥箱中,干燥至恒重,得到改性棉纤维。
S2、制备复合抗菌剂
称取:对氨基苯甲醛24.7g、二异氰基甲烷10g和丙酮123.5g加入到氮气保护的三口烧瓶中搅拌,室温下反应30min,三口烧瓶温度升高至45℃,减压蒸除丙酮,得到中间体1;
称取:中间体134g和缩二脲10.3g、9-11mol/L盐酸340g加入到三口烧瓶中搅拌,室温下反应20h,抽滤,滤用10vt%醋酸溶液洗涤三次,再使饼用纯化水洗涤三次后抽干,滤饼转移到温度为65℃的干燥箱中,真空干燥至恒重,得到复合抗菌剂。
S3、制备改性石墨烯
称取:氧化石墨烯30g、三甲氧基硅烷剂甲硫醇9g、三甲氧基硅烷3g、四甲氧基硅烷6g和无水乙醇300g加入到三口烧瓶中,超声分散30min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液45g,室温下反应40min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为60℃的干燥箱中,真空干燥至恒重,得到中间体I;
称取:中间体I 20g、四氯化钛5g和纯化水500g加入到三口烧瓶中,超声分散60min,保持超声分散状态,向三口烧瓶中滴加氨水,调节体系pH=10,室温下超声分散2h,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65℃的干燥箱中,真空干燥至恒重,得到中间体II;
称取:中间体II 30g、无水乙醇300g和3-缩水甘油醚氧基丙基三甲氧基硅烷9g加入到三口烧瓶中,超声分散30min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液45g,室温下反应50min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为60℃的干燥箱中,真空干燥至恒重,得到改性石墨烯。
S4、制备复合石墨烯
称取:改性石墨烯50g、N,N-二甲基甲酰胺300mL、10wt%氢氧化钠溶液40g加入到三口烧瓶中,超声分散20min,将三口烧瓶固定在带有机械搅拌的铁架台上搅拌,向三口烧瓶中加入复合抗菌剂20g,三口烧瓶温度升高至50℃,保温反应60min,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤三次后抽干,将滤饼转移到温度为65℃的干燥箱中,真空干燥至恒重,得到复合石墨烯。
S5、制备复合棉纤维
称取:复合石墨烯30g与纯化水400mL加入到烧瓶中,超声分散30min,保持超声状态,向烧瓶中加入改性棉纤维80g和对甲苯磺酸20g,烧瓶温度升高至50℃,保温超声反应3h,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为60℃的干燥箱中,干燥至恒重,得到复合棉纤维。
S6、制备复合纱线初品
使用纺纱机将复合棉纤维纺织成粗细为30-40Ne的复合纱线初品;
S7、制备防污整理剂
称取:全氟辛基磺酰胺49.9g、1,2-环氧基-5-己烯9.8g、氢氧化钠32.9g和N,N-二甲基甲酰胺166.3g加入到氮气保护的三口烧瓶中搅拌,三口烧瓶温度升高至65℃,保温反应3h,三口烧瓶温度降低至室温,向三口烧瓶中加入纯化水250g,有大量固体析出,抽滤,滤饼用纯化水洗涤至中性后,将其转移到温度为70℃的干燥箱中,干燥至恒重,得到改性全氟辛基磺酰胺;
称取:改性全氟辛基磺酰胺47g、甲基丙烯酸丁酯5.5g、甲基丙烯酸月桂酯5g、四氢呋喃282mL和偶氮二异丁腈5.6g加入到三口烧瓶中搅拌,三口烧瓶温度升高够55℃,保温反应10h,三口烧瓶温度降低至室温,向三口烧瓶中缓慢加入纯化水423g,有大量固体析出,抽滤,滤饼用无水乙醇洗涤三次后抽干,将滤饼转移到温度为60℃的干燥箱中,干燥至恒重,得到防污剂;
称取:防污剂10g、氨基改性硅酮6g、1,4-丁二醇二丙烯酸酯2g、纳米氧化锌2g和四氢呋喃120g加入到烧杯中搅拌均匀,得到防污整理剂。
S8、制备复合纱线成品
将复合纱线初品完全浸渍到装有防污整理剂的烧杯中,室温辐射状态下,超声浸渍50min,将复合纱线初品从烧杯中捞出,用无水乙醇洗涤3次,使用纯化水洗涤3次,抽干,将其转移到温度为75℃的干燥箱中,干燥至恒重,得到复合纱线成品。
实施例2
本实施例提高一种高耐磨抗菌防污复合纱线的制备方法,包括以下步骤:
S1、制备改性棉纤维
称取:纯化水1L、氢氧化钠150g和十二烷基磺酸钠20g加入到烧杯中搅拌至体系溶解,向烧瓶中加入棉纤维60g,室温下,超声分散40min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为70℃的干燥箱中,干燥至恒重,得到预处理棉纤维;
称取:预处理棉纤维50g和35wt%氢氧化钠溶液600g加入烧瓶中,室温下,搅拌40min,向烧瓶中缓慢加入环氧氯丙烷250g,烧瓶温度升高至60℃,保温反应2.5h,烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为70℃的干燥箱中,干燥至恒重,得到改性棉纤维。
S2、制备复合抗菌剂
称取:对氨基苯甲醛24.7g、二异氰基甲烷10g和丙酮123.5g加入到氮气保护的三口烧瓶中搅拌,室温下反应40min,三口烧瓶温度升高至50℃,减压蒸除丙酮,得到中间体1;
称取:中间体134g和缩二脲10.3g、9-11mol/L盐酸340g加入到三口烧瓶中搅拌,室温下反应21h,抽滤,滤用10vt%醋酸溶液洗涤三次,再使饼用纯化水洗涤三次后抽干,滤饼转移到温度为70℃的干燥箱中,真空干燥至恒重,得到复合抗菌剂。
S3、制备改性石墨烯
称取:氧化石墨烯30g、三甲氧基硅烷剂甲硫醇9g、三甲氧基硅烷3g、四甲氧基硅烷6g和无水乙醇300g加入到三口烧瓶中,超声分散40min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液45g,室温下反应50min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65℃的干燥箱中,真空干燥至恒重,得到中间体I;
称取:中间体I 20g、四氯化钛5g和纯化水500g加入到三口烧瓶中,超声分散70min,保持超声分散状态,向三口烧瓶中滴加氨水,调节体系pH=11,室温下超声分散2.5h,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为70℃的干燥箱中,真空干燥至恒重,得到中间体II;
称取:中间体II 30g、无水乙醇300g和3-缩水甘油醚氧基丙基三甲氧基硅烷9g加入到三口烧瓶中,超声分散40min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液45g,室温下反应65min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65℃的干燥箱中,真空干燥至恒重,得到改性石墨烯。
S4、制备复合石墨烯
称取:改性石墨烯50g、N,N-二甲基甲酰胺300mL、10wt%氢氧化钠溶液40g加入到三口烧瓶中,超声分散25min,将三口烧瓶固定在带有机械搅拌的铁架台上搅拌,向三口烧瓶中加入复合抗菌剂20g,三口烧瓶温度升高至55℃,保温反应70min,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤三次后抽干,将滤饼转移到温度为70℃的干燥箱中,真空干燥至恒重,得到复合石墨烯。
S5、制备复合棉纤维
称取:复合石墨烯30g与纯化水400mL加入到烧瓶中,超声分散40min,保持超声状态,向烧瓶中加入改性棉纤维80g和对甲苯磺酸20g,烧瓶温度升高至55℃,保温超声反应3.5h,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为65℃的干燥箱中,干燥至恒重,得到复合棉纤维。
S6、制备复合纱线初品
使用纺纱机将复合棉纤维纺织成粗细为30-40Ne的复合纱线初品;
S7、制备防污整理剂
称取:全氟辛基磺酰胺49.9g、1,2-环氧基-5-己烯9.8g、氢氧化钠32.9g和N,N-二甲基甲酰胺166.3g加入到氮气保护的三口烧瓶中搅拌,三口烧瓶温度升高至70℃,保温反应4h,三口烧瓶温度降低至室温,向三口烧瓶中加入纯化水250g,有大量固体析出,抽滤,滤饼用纯化水洗涤至中性后,将其转移到温度为75℃的干燥箱中,干燥至恒重,得到改性全氟辛基磺酰胺;
称取:改性全氟辛基磺酰胺47g、甲基丙烯酸丁酯5.5g、甲基丙烯酸月桂酯5g、四氢呋喃282mL和偶氮二异丁腈5.6g加入到三口烧瓶中搅拌,三口烧瓶温度升高够60℃,保温反应11h,三口烧瓶温度降低至室温,向三口烧瓶中缓慢加入纯化水423g,有大量固体析出,抽滤,滤饼用无水乙醇洗涤三次后抽干,将滤饼转移到温度为65℃的干燥箱中,干燥至恒重,得到防污剂;
称取:防污剂10g、氨基改性硅酮6g、1,4-丁二醇二丙烯酸酯2g、纳米氧化锌2g和四氢呋喃120g加入到烧杯中搅拌均匀,得到防污整理剂。
S8、制备复合纱线成品
将复合纱线初品完全浸渍到装有防污整理剂的烧杯中,室温辐射状态下,超声浸渍55min,将复合纱线初品从烧杯中捞出,用无水乙醇洗涤3次,使用纯化水洗涤3次,抽干,将其转移到温度为80℃的干燥箱中,干燥至恒重,得到复合纱线成品。
实施例3
本实施例提高一种高耐磨抗菌防污复合纱线的制备方法,包括以下步骤:
S1、制备改性棉纤维
称取:纯化水1L、氢氧化钠150g和十二烷基磺酸钠20g加入到烧杯中搅拌至体系溶解,向烧瓶中加入棉纤维60g,室温下,超声分散50min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为75℃的干燥箱中,干燥至恒重,得到预处理棉纤维;
称取:预处理棉纤维50g和35wt%氢氧化钠溶液600g加入烧瓶中,室温下,搅拌50min,向烧瓶中缓慢加入环氧氯丙烷250g,烧瓶温度升高至65℃,保温反应3h,烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为75℃的干燥箱中,干燥至恒重,得到改性棉纤维。
S2、制备复合抗菌剂
称取:对氨基苯甲醛24.7g、二异氰基甲烷10g和丙酮123.5g加入到氮气保护的三口烧瓶中搅拌,室温下反应50min,三口烧瓶温度升高至55℃,减压蒸除丙酮,得到中间体1;
称取:中间体134g和缩二脲10.3g、9-11mol/L盐酸340g加入到三口烧瓶中搅拌,室温下反应22h,抽滤,滤用10vt%醋酸溶液洗涤三次,再使饼用纯化水洗涤三次后抽干,滤饼转移到温度为75℃的干燥箱中,真空干燥至恒重,得到复合抗菌剂。
S3、制备改性石墨烯
称取:氧化石墨烯30g、三甲氧基硅烷剂甲硫醇9g、三甲氧基硅烷3g、四甲氧基硅烷6g和无水乙醇300g加入到三口烧瓶中,超声分散50min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液45g,室温下反应60min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为70℃的干燥箱中,真空干燥至恒重,得到中间体I;
称取:中间体I 20g、四氯化钛5g和纯化水500g加入到三口烧瓶中,超声分散80min,保持超声分散状态,向三口烧瓶中滴加氨水,调节体系pH=12,室温下超声分散3h,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为75℃的干燥箱中,真空干燥至恒重,得到中间体II;
称取:中间体II 30g、无水乙醇300g和3-缩水甘油醚氧基丙基三甲氧基硅烷9g加入到三口烧瓶中,超声分散50min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液45g,室温下反应80min,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为70℃的干燥箱中,真空干燥至恒重,得到改性石墨烯。
S4、制备复合石墨烯
称取:改性石墨烯50g、N,N-二甲基甲酰胺300mL、10wt%氢氧化钠溶液40g加入到三口烧瓶中,超声分散30min,将三口烧瓶固定在带有机械搅拌的铁架台上搅拌,向三口烧瓶中加入复合抗菌剂20g,三口烧瓶温度升高至60℃,保温反应80min,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤三次后抽干,将滤饼转移到温度为75℃的干燥箱中,真空干燥至恒重,得到复合石墨烯。
S5、制备复合棉纤维
称取:复合石墨烯30g与纯化水400mL加入到烧瓶中,超声分散50min,保持超声状态,向烧瓶中加入改性棉纤维80g和对甲苯磺酸20g,烧瓶温度升高至60℃,保温超声反应4h,三口烧瓶温度降低至室温,抽滤,滤饼用纯化水洗涤至中性后抽干,将滤饼转移到温度为70℃的干燥箱中,干燥至恒重,得到复合棉纤维。
S6、制备复合纱线初品
使用纺纱机将复合棉纤维纺织成粗细为30-40Ne的复合纱线初品;
S7、制备防污整理剂
称取:全氟辛基磺酰胺49.9g、1,2-环氧基-5-己烯9.8g、氢氧化钠32.9g和N,N-二甲基甲酰胺166.3g加入到氮气保护的三口烧瓶中搅拌,三口烧瓶温度升高至75℃,保温反应5h,三口烧瓶温度降低至室温,向三口烧瓶中加入纯化水250g,有大量固体析出,抽滤,滤饼用纯化水洗涤至中性后,将其转移到温度为80℃的干燥箱中,干燥至恒重,得到改性全氟辛基磺酰胺;
称取:改性全氟辛基磺酰胺47g、甲基丙烯酸丁酯5.5g、甲基丙烯酸月桂酯5g、四氢呋喃282mL和偶氮二异丁腈5.6g加入到三口烧瓶中搅拌,三口烧瓶温度升高够65℃,保温反应12h,三口烧瓶温度降低至室温,向三口烧瓶中缓慢加入纯化水423g,有大量固体析出,抽滤,滤饼用无水乙醇洗涤三次后抽干,将滤饼转移到温度为70℃的干燥箱中,干燥至恒重,得到防污剂;
称取:防污剂10g、氨基改性硅酮6g、1,4-丁二醇二丙烯酸酯2g、纳米氧化锌2g和四氢呋喃120g加入到烧杯中搅拌均匀,得到防污整理剂。
S8、制备复合纱线成品
将复合纱线初品完全浸渍到装有防污整理剂的烧杯中,室温辐射状态下,超声浸渍60min,将复合纱线初品从烧杯中捞出,用无水乙醇洗涤3次,使用纯化水洗涤3次,抽干,将其转移到温度为85℃的干燥箱中,干燥至恒重,得到复合纱线成品。
对比例1
本对比例与实施例3的区别在于,取消步骤S2,以改性石墨烯等量替代步骤S5中的复合石墨烯。
对比例2
本对比例与实施例3的区别在于,取消步骤S3,以石墨烯等量替代步骤S4中的改性石墨烯。
对比例3
本对比例与实施例3的区别在于,取消步骤S7和S8,以复合纱线初品替代步骤S8的复合纱线成品。
性能测试:
对实施例1-3和对比例1-3制备的复合纱线成品的抗污性能、耐磨性能、抗菌性能与力学性能进行测试,其中,抗污性能参照标准ZBW04015-89《涂层织物拒油性能测定方法》,根据AATCC-118的测试方法,测定试样的拒油等级,并参照标准DB44/T 1872-2016《纺织品表面润湿性能的测定接触角法》测定试样与水的静态接触角,抗菌性能与力学性能参照标准DB35/T 1058-2019《抗菌涤纶长丝通用技术条件》进行测试,耐磨性能为对试样进行30次干洗后,测定试样的拒油等级、抗菌性能与力学性能,具体测试结果见下表:
数据分析:
通过对上表中的数据进行比较分析,本发明制备的复合纱线的拒油等级达到7级,与水的静态接触角达到143°,断裂伸长率达到8.6%,断裂强度达到66.6cN/dtex,对金色球葡萄杆菌的抑菌率达到99.8%,对大肠杆菌的抑菌率达到99.7%,经过30次干洗后,拒油等级达到6级,保有率达到85.7%,断裂强度达到62.5cN/dtex,保有量达到93.8%,对金色球葡萄杆菌的抑菌率达到95.0%,保有量达到95.2%,对大肠杆菌的抑菌率达到93.0%,保有量达到93.2%,各项检测数据均优于对比例,说明,本发明制备的复合纱线,不仅具有良好的疏水抗油污性能,对金色球葡萄杆菌和大肠杆菌起到良好的抑菌效果,还有效的提高了复合纱线的力学性能,拓宽了棉纤维复合纱线的应用范围,在经过30次干洗之后,复合纱线在拒油等级、断裂强度和抑菌率仍有良好的保有率,说明本发明制备的复合纱线的耐磨性能优异。
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节,也不限制该发明仅为的具体实施方式。显然,根据本说明书的内容,可做很多的修改和变化。本说明书选取并具体描述这些实施例,是为了更好地解释本发明的原理和实际应用,从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。
Claims (10)
1.一种高耐磨抗菌防污复合纱线,其特征在于,由复合石墨烯对预处理改性得到的改性棉纤维进行修饰改性,制备成复合棉纤维,通过纺纱机对复合棉纤维进行纺纱,制备成复合纱线初品,使用防污整理剂对复合纱线进行浸渍改性后,制备得到;
所述复合石墨烯由以下步骤加工而成:
A1、将氧化石墨烯、三甲氧基硅烷剂甲硫醇、三甲氧基硅烷、四甲氧基硅烷和无水乙醇加入到三口烧瓶中,超声分散30-50min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液,室温下反应40-60min,后处理得到中间体I;
A2、将中间体I、四氯化钛和纯化水加入到三口烧瓶中,超声分散60-80min,保持超声分散状态,向三口烧瓶中滴加氨水,调节体系pH=10-12,室温下超声分散2-3h,后处理,得到中间体II;
A3、将中间体II、无水乙醇和3-缩水甘油醚氧基丙基三甲氧基硅烷加入到三口烧瓶中,超声分散30-50min,将三口烧瓶固定在带有机械搅拌的铁架台上,搅拌,向三口烧瓶中加入5wt%氢氧化钠溶液,室温下反应50-80min,后处理得到改性石墨烯;
A4、将改性石墨烯、N,N-二甲基甲酰胺、10wt%氢氧化钠溶液加入到三口烧瓶中,超声分散20-30min,将三口烧瓶固定在带有机械搅拌的铁架台上搅拌,向三口烧瓶中加入复合抗菌剂,三口烧瓶温度升高至50-60℃,保温反应60-80min,后处理得到复合石墨烯。
2.根据权利要求1所述的一种高耐磨抗菌防污复合纱线,其特征在于,步骤A1中氧化石墨烯、三甲氧基硅烷剂甲硫醇、三甲氧基硅烷、四甲氧基硅烷、无水乙醇和5wt%氢氧化钠溶液的用量比为10g:3g:1g:2g:100g:15g;步骤A2中中间体I、四氯化钛和纯化水的用量比为4g:1g:100g;步骤A3中中间体II、无水乙醇、3-缩水甘油醚氧基丙基三甲氧基硅烷和5wt%氢氧化钠溶液的用量比为10g:100g:3g:15g;步骤A4中改性石墨烯、N,N-二甲基甲酰胺、10wt%氢氧化钠溶液与复合抗菌剂的用量比为10g:60mL:8g:4g。
3.根据权利要求1所述的一种高耐磨抗菌防污复合纱线,其特征在于,复合抗菌剂由以下步骤加工而成:
B1、将对氨基苯甲醛、二异氰基甲烷和丙酮加入到氮气保护的三口烧瓶中搅拌,室温下反应30-50min,后处理得到中间体1;
B2、将中间体1和缩二脲、盐酸加入到三口烧瓶中搅拌,室温下反应20-22h,后处理得到复合抗菌剂。
4.根据权利要求3所述的一种高耐磨抗菌防污复合纱线,其特征在于,步骤B1中对氨基苯甲醛、二异氰基甲烷的摩尔比为2:1,所述丙酮用量为对氨基苯甲醛重量的5倍;步骤B2中中间体1、缩二脲的摩尔比为1:1,所述盐酸的浓度为9-11mol/L,盐酸的用量为中间体1重量的10倍。
5.根据权利要求1所述的一种高耐磨抗菌防污复合纱线,其特征在于,棉纤维的预处理改性操作包括以下步骤:
C1、将纯化水、氢氧化钠和十二烷基磺酸钠加入到烧杯中搅拌至体系溶解,向烧瓶中加入棉纤维,室温下,超声分散30-50min,后处理得到预处理棉纤维;
C2、将预处理棉纤维和35wt%氢氧化钠溶液加入烧瓶中,室温下,搅拌30-50min,向烧瓶中缓慢加入环氧氯丙烷,烧瓶温度升高至55-65℃,保温反应2-3h,后处理得到改性棉纤维。
6.根据权利要求5所述的一种高耐磨抗菌防污复合纱线,其特征在于,步骤C1中纯化水、氢氧化钠、十二烷基磺酸钠和棉纤维的用量比为100g:15g:2g:6g;步骤C2中预处理棉纤维、35wt%氢氧化钠溶液和环氧氯丙烷的用量比为1g:12g:5g。
7.根据权利要求1所述的一种高耐磨抗菌防污复合纱线,其特征在于,复合棉纤维的制备方法为:将复合石墨烯与纯化水加入到烧瓶中,超声分散30-50min,保持超声状态,向烧瓶中加入改性棉纤维和催化剂,烧瓶温度升高至50-60℃,保温超声反应3-4h,后处理得到复合棉纤维,其中,所述复合石墨烯、纯化水、改性棉纤维和催化剂的用量比为3g:40mL:8g:2g,所述催化剂为对甲苯磺酸。
8.根据权利要求1所述的一种高耐磨抗菌防污复合纱线,其特征在于,防污整理剂由以下步骤加工而成:
D1、将全氟辛基磺酰胺、1,2-环氧基-5-己烯、氢氧化钠和N,N-二甲基甲酰胺加入到氮气保护的三口烧瓶中搅拌,三口烧瓶温度升高至65-75℃,保温反应3-5h,后处理得到改性全氟辛基磺酰胺;
D2、将改性全氟辛基磺酰胺、甲基丙烯酸丁酯、甲基丙烯酸月桂酯、四氢呋喃和引发剂加入到三口烧瓶中搅拌,三口烧瓶温度升高够55-65℃,保温反应10-12h,后处理得到防污剂;
D3、将防污剂、氨基改性硅酮、1,4-丁二醇二丙烯酸酯、纳米氧化锌和四氢呋喃加入到烧杯中搅拌均匀,得到防污整理剂。
9.根据权利要求8所述的一种高耐磨抗菌防污复合纱线,其特征在于,步骤D1中全氟辛基磺酰胺、1,2-环氧基-5-己烯的摩尔比为1:1,所述全氟辛基磺酰胺、氢氧化钠和N,N-二甲基甲酰胺的用量比为3g:2g:10g;步骤D2中改性全氟辛基磺酰胺、甲基丙烯酸丁酯、甲基丙烯酸月桂酯的摩尔比为4:2:1,所述改性全氟辛基磺酰胺、四氢呋喃和引发剂的用量比为5g:30mL:0.6g,所述引发剂为偶氮二异丁腈;步骤D3中防污剂、氨基改性硅酮、1,4-丁二醇二丙烯酸酯、纳米氧化锌和四氢呋喃的用量比为5g:3g:1g:1g:60g。
10.根据权利要求1-9任一项所述的一种高耐磨抗菌防污复合纱线的制备方法,其特征在于,包括以下步骤:
S1、对棉纤维进行预处理改性,制备得到的改性棉纤维;
S2、使用复合石墨烯对改性棉纤维进行修饰改性,制备得到复合棉纤维;
S2、使用纺纱机将复合棉纤维纺织成粗细为30-40Ne的复合纱线初品;
S3、将复合纱线初品完全浸渍到装有防污整理剂的烧杯中,室温辐射状态下,超声浸渍50-60min,将复合纱线初品从烧杯中捞出,用无水乙醇洗涤3次,使用纯化水洗涤3次,抽干,将其转移到温度为75-85℃的干燥箱中,干燥至恒重,得到复合纱线成品。
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