CN115182156A - 一种含石墨烯纤维的混纺阻燃面料 - Google Patents

一种含石墨烯纤维的混纺阻燃面料 Download PDF

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CN115182156A
CN115182156A CN202210712229.2A CN202210712229A CN115182156A CN 115182156 A CN115182156 A CN 115182156A CN 202210712229 A CN202210712229 A CN 202210712229A CN 115182156 A CN115182156 A CN 115182156A
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CN115182156B (zh
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从纯纯
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Nantong Ruiyijia Textile Technology Co ltd
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Abstract

本发明公开了一种含石墨烯纤维的混纺阻燃面料,包括如下原料:石墨烯‑聚丙烯腈复合纳米纤维:20‑30份,兔毛纤维:20‑30份,玄武岩纤维:10‑20份,棉纤维:30‑40份,海藻纤维:15‑20份;该阻燃面料的制备工艺具体包括以下步骤:(1)兔毛纤维和海藻纤维的的预处理;(2)棉纤维的预处理;(3)将石墨烯‑聚丙烯腈复合纳米纤维、玄武岩纤维、预处理后的棉纤维、预处理后的兔毛纤维及海藻纤维维通过成条、纺纱、织布制得混纺面料;(4)将混纺面料进行阻燃整理,具体为:采用阻燃剂、树脂、柔软剂和磷酸,通过二浸二轧→烘干→焙烘→纯碱中和,使得pH值7~8→皂洗→水洗→烘干,得到阻燃面;该阻燃面料具有很好的阻燃性、抗菌效果好、舒爽性。

Description

一种含石墨烯纤维的混纺阻燃面料
技术领域
本发明涉及一种面料,具体涉及一种含石墨烯纤维的混纺阻燃面料。
背景技术
纺织品是人们日常生活的必需品,随着时代的发展和人们生活水平的提高,功能纺织品逐渐成为当今纺织产品开发的主流和趋势,所谓功能纺织品是指纺织品除具有保暖和遮盖等基本功能外还具有某些特殊功能,如防静电、阻燃、防紫外线、自清洁、电磁屏蔽和抗菌消臭等功能。根据资料,由于纺织品着火或因纺织品阻燃性不好而引起的火灾占我国历年火灾事故的20%左右;因此,对纤维及织布进行阻燃处理是一项重要而紧迫的研究工程。
石墨烯是从石墨中剥离出来的单层碳原子材料,由碳原子紧密堆积成单层二维蜂窝状晶格结构,它是人类已知的厚度最薄、质地最坚硬、导电性最好的材料。石墨烯具有优异的力学、光学和电学性质,结构非常稳定,迄今为止研究者尚未发现石墨烯中有碳原子缺失的情况,碳原子之间的链接非常柔韧,比钻石还坚硬,强度比世界上最好的钢铁还要高上100倍,如果用石墨烯制成包装袋,它将能承受大约两吨重的物品,几乎完全透明,却极为致密,不透水、不透气,即使原子尺寸最小的氦气也无法通过。当石墨烯层被烧焦时,它会形成连续炭层,这个炭层密集且连续,它会阻挡表面,阻止氧气进入材料的深处。石墨烯传导热量非常好,这意味着局部的热量被传导到其余的材料中并分散,使得火势难以传播。导热和焦炭阻塞产生了所谓的迷宫效应,其中热量和燃烧气体必须遵循通向燃料的曲折路径,并且这有效地防止了火焰的蔓延。除了阻燃效果,石墨烯和氧化石墨烯也具有非常高的表面积。这可以吸附易燃有机挥发物,并阻止其在燃烧过程中的释放和扩散。石墨烯很可能会减少火灾中的有毒气体,将石墨烯组装为宏观的功能结构如纤维、面料等,是实现石墨烯实际应用的重要途径,利用其此种性能,石墨烯的添加可使面料的热物性(导热性和耐热性)提高80%。因此石墨烯及其衍生物被广泛用作阻燃填料,从而使面料具有更高的热稳定性和阻燃性能。然而,目前的石墨烯纤维的缺陷是现有的纤维阻燃性能不佳,不能满足混纺纱线的阻燃需求,现有的纤维的混纺纱线强韧度提升有限,抗抗菌性能一般。
发明内容
本发明所要解决的技术问题是,针对以上现有技术存在的缺点,提出一种含石墨烯纤维的混纺阻燃面料,该阻燃面料具有很好的阻燃性、抗菌效果好、舒爽性。
本发明解决以上技术问题的技术方案是:
一种含石墨烯纤维的混纺阻燃面料,包括如下重量份数计的原料:
石墨烯-聚丙烯腈复合纳米纤维:20-30份,兔毛纤维:20-30份,玄武岩纤维:10-20份,棉纤维:30-40份,海藻纤维:15-20份;
该含石墨烯纤维的混纺阻燃面料的制备工艺具体包括以下步骤:
(1)兔毛纤维和海藻纤维的的预处理
使用前先对兔毛纤维和海藻纤维分别进行开松处理,加入一和毛油和抗静电剂,均匀喷洒到纤维中以减少静电,喷洒后焖放24h以上;
(2)棉纤维的预处理
①将棉纤维在使用前放入十二烷基磺酸钠水溶液中,超声2h,去离子水洗涤,再使用无水乙醇超声洗涤10-20后,用去离子水洗涤,在70℃的烘箱里干燥1h得空白棉纤维备用;
②取硫脲和尿素溶解到无水乙醇中,再加入钛酸丁酯,用5t%稀硝酸调节其pH为3~4,搅拌均匀,然后将去离子水缓慢滴加到上述溶液中,并继续搅拌20-23min,静置0.8-1h,得到湿凝胶;
③将步骤②得到的溶胶液继续搅拌,待出现丁达尔现象后,将步骤(1)准备好的棉纤维浸渍到溶胶液中,浸渍5-7min,烘干,得到处理后的棉纤维;
(3)将石墨烯-聚丙烯腈复合纳米纤维、玄武岩纤维、预处理后的棉纤维、预处理后的兔毛纤维及海藻纤维维通过成条、纺纱、织布制得混纺面料;
(4)将混纺面料进行阻燃整理,具体为:采用阻燃剂、树脂、柔软剂和磷酸,通过二浸二轧→烘干→焙烘→纯碱中和,使得pH值7~8→皂洗→水洗→烘干,得到阻燃面料。
本发明进一步限定的技术方案为:
前述含石墨烯纤维的混纺阻燃面料中,步骤(1)在兔毛纤维和海藻纤维的的预处理时和毛油为纤维质量0.5%的CTA-2886和毛油。
前述含石墨烯纤维的混纺阻燃面料中,步骤(2)棉纤维浸渍溶胶液后进行烘干,烘干时采用低温烘干的方式进行,具体为:
烘干温度为40℃-43℃,且烘干过程中通过风扇保证气流快速流动,烘干后棉纤维含水量为30-33%时停止烘干。
技术效果,低温烘干不损坏织物,保证织物的质感,同时织物保证一定的含水量防止过烘干,提高生产率,可省掉重新给湿工序,又提高了产品质量。
前述含石墨烯纤维的混纺阻燃面料中,步骤(4)混纺面料进行阻燃整理时阻燃剂为聚双三羟甲基丙烷硫代磷酰脲;树脂为脲醛树脂;柔软剂为柔软剂JPBC。
前述含石墨烯纤维的混纺阻燃面料中,步骤(4)阻燃整理时二浸二轧时控制轧余率75%;烘干时烘干温度控制在100-120℃,烘干2-5min;烘焙时控制温度170-175℃,烘焙2-4min。
前述含石墨烯纤维的混纺阻燃面料中,步骤(4)阻燃整理时织物在4g/L皂粉,1g/L纯碱,浴比1∶10的条件下进行皂洗、水洗、晾干。
前述含石墨烯纤维的混纺阻燃面料中,石墨烯-聚丙烯腈复合纳米纤维的制备具体如下:
S1、在冰水浴条件下,在烧杯中加入石墨粉、硝酸钠、浓硫酸搅拌20-30min后,加入高锰酸钾,在40℃下搅拌1h,加入的去离子水搅拌10-15min,加入去离子水和双氧水搅拌10-15min,离心烘干后得到氧化石墨烯片,用硼氢化钠还原得到石墨烯片备用;
S2、将石墨烯加入到甲酰二甲胺中,超声30min,将石墨烯片分散液放在水浴锅中60℃水浴加热,慢慢加入聚丙烯腈,横向搅拌,直至充分溶解,在室温下静止12h去泡,得到石墨烯-聚丙烯腈复合纳米纤维纺丝液;
S3、将石墨烯-聚丙烯腈复合纳米纤维纺丝液转移至注射器采用静电纺制备得到石墨烯-聚丙烯腈复合纳米纤维。
技术效果,石墨烯具有较强的导电性、电阻比铜、银低,是目前室温下较好的导电材料,石墨烯的吸光性也非常强、对紫外光以及其他波段的光可以无选择地吸收,因此具备防紫外线的特性、石墨烯还具有理想的远红外发射功能和良好的阻燃性,石墨烯-PAN复合纳米纤维具有典型的纤维形貌,石墨烯对PAN分子取向具有诱导作用并且不利于PAN分子六方准晶结构的形成,石墨烯-PAN纳米纤维具有一定的抗菌性,对石墨烯-PAN复合纳米纤维进行大肠埃希菌的抗菌测试,石墨烯-PAN复合纳米纤维抑菌带宽度为0.16mm,根据抗菌试验的评判标准,说明这种纤维具有良好的抗菌性能。
前述含石墨烯纤维的混纺阻燃面料中,阻燃面料的后处理,具体为:
(I)将KH570硅烷偶联剂加入到85-90%的乙醇溶液中配制成KH570浓度为0.6-1.5%的浸渍液;
(II)将含石墨烯纤维的混纺阻燃面料浸泡于浸渍液中12-15min后,取出并在鼓风干燥箱中60℃进行烘干,烘干后的面料再进行浸渍及烘干,重复浸渍和烘干操作5-6次后得到后处理后的阻燃面料。
技术效果,硅烷偶联剂KH570化学名称为γ-(甲基丙烯酰氧)丙基三甲氧基硅烷,其形态多为无色或淡黄色液体,液体呈粘稠状,常作为聚合物与天然材料复合的偶联剂,KH570亦可通过物理或化学作用将高分子材料与无机材料相结合,提高复合材料间的结合力度,并提高复合材料的强度,同时也被广泛应用于复合材料的粘接与复合,提高材料间的耐久力、力学强度和粘久力,本发明采用硅烷偶联剂对面料进行后处理,进行改性,KH570会水解成聚硅氧烷,该聚硅氧烷和石墨烯表面以及面料表面的羟基发生脱水缩合反应,使石墨烯与面料紧密结合,提高面料的抗菌性,并改善其耐洗牢度。
本发明的有益效果是:
兔毛是一种现代绿色环保型纺织原料,兔毛纤维本身亲肤舒适,兔毛纤维在宏观上具有质轻、细长、表面光滑、富有光泽、纤维之间蓬松、手感柔软、杂质少等特点,在功能上具有舒适健康,自然环保,透气透湿特性,被称为中国第二大软黄金,但由于可纺性能差导致利用率不高,兔毛与石墨烯-聚丙烯腈复合纳米纤维混纺不仅能够解决兔毛纤维在纺纱过程中静电大、难成网的问题,而且在保留兔毛纤维本身优点的情况下,可以将石墨烯-聚丙烯腈复合纳米纤维的优异特性与兔毛纤维相结合,兔毛与石墨烯-聚丙烯腈复合纳米纤维混纺面料一方面顺应目前纺织面料舒适化"时尚化"环保化"多元化"多功能化的发展趋势,另一方面也能提高兔毛纺织产品的档次。
先与海藻纤维和兔毛纤维进行预处理,因海藻纤维集束较多,使用前先对兔毛纤维和海藻纤维分别进行开松处理,加入一和毛油和抗静电剂,均匀喷洒到纤维中以减少静电,增加纤维抱合力,减少飞花和断头,喷洒后焖放24h以上使其充分渗透,以确保和毛油、水均匀渗透到纤维中,使纤维得到较好的润滑,提高纤维柔软性和韧性,保护纤维在后续梳理时不易被拉断,同时和毛油可提高原料上机回潮率,减少加工过程中的飞毛、落花,提高混纺纱制成率和质量,在使用前控制海藻纤维的回潮率,使纤维在各工序中处于放湿状态,保证细纱生产顺利。
玄武岩纤维是以玄武岩为原料,经过高温熔融拉制成连续纤维材料,其主要成分是二氧化硅、三氧化二铝、三氧化二铁、氧化钙、氧化镁、氧化钾、二氧化钛等多种氧化物,因此,相对于其他化学及矿物材料的化学稳定性和热稳定性更高,玄武岩纤维在强度、耐高低温、阻燃及化学、电绝缘性方面性能优异,选用玄武岩纤维和棉纤维、石墨烯-聚丙烯腈复合纳米纤维、兔毛纤维、海藻纤维混纺开发阻燃面料,不仅可以充分利用到玄武岩纤维的阻燃性能,提高混纺纱线的物理机械性能,降低玄武纤维对人体皮肤的刺激性,同时减少化学药品对人体和环境的危害。
本发明的棉纤维进行了预处理,棉纤维负载掺杂TiO2光催化抗菌机理如下:棉纤维上负载的S-N-TiO2光催化材料与细菌悬液混合振荡,在一定的外界条件下(热、光等),释放带负电的电子e-,同时产生带正电的空穴h+;其次,丰富的空穴在水和空气的环境中发生作用,产生了高活性和强氧化能力的过氧离子自由基(·O2-)和羟基自由基(·HO);这些活泼的自由基能与细胞膜上的磷脂分子与膜蛋白发生作用,从而使膜的流动性变差。由于膜的流动性与细胞的生命活动如营养运输、能量代谢等有着至关紧要的联系。当膜的流动性降低,其传递营养物质的功能也降低,由于不能从外界吸收充足的营养物质,细菌的生长就会受到抑制;再者,细胞膜流动性降低的同时细胞膜的粘度就会相应的增加,而细胞膜上又负载着许多活性酶,膜粘度的增加会使酶的活性降低甚至失活,从而引起细胞的代谢功能发生紊乱,直接影响了细胞的增殖。如果这些自由基在细胞膜的周围达到一定浓度,最终会使细胞死亡,从而达到杀菌的目的,为改善所制Ag-N-TiO2纳米抗菌剂与棉纤维的结合牢度,以及柔性纺织品不耐高温的问题,采用快速溶胶-凝胶法整理棉纤维,使得所制纳米溶胶短时间内在棉纤维表面形成凝胶膜,并通过热处理,二者以共价键或范德华力牢固结合,改善了纤维的抗菌耐久性。
为了降低成本,提高面料的功能,将石墨烯-聚丙烯腈复合纳米纤维与兔毛纤维、棉纤维、玄武岩纤维、海藻纤维进行不同比例的混纺,在保证功能的同时提高阻燃性。
本发明对纤维先进行处理,提高海藻纤维和兔毛纤维纤维柔软性和韧性,提高混纺纱制成率和质量,在对棉纤维进行处理增强其抗菌耐久性,最后混纺面料进行阻燃整理,进一步提高了阻燃性,在石墨烯纤维阻燃的基础上又进行了阻燃整理,进一步调高了阻燃性,满足要求。
具体实施方式
实施例1
本实施例提供一种含石墨烯纤维的混纺阻燃面料,包括如下重量份数计的原料:
石墨烯-聚丙烯腈复合纳米纤维:20份,兔毛纤维:20份,玄武岩纤维:10份,棉纤维:30份,海藻纤维:15份;
该含石墨烯纤维的混纺阻燃面料的制备工艺具体包括以下步骤:
(1)兔毛纤维和海藻纤维的的预处理
使用前先对兔毛纤维和海藻纤维分别进行开松处理,加入纤维质量0.5%的CTA-2886和毛油和纤维质量0.2%的现有技术中抗静电剂,均匀喷洒到纤维中以减少静电,喷洒后焖放24h以上;
(2)棉纤维的预处理
①将棉纤维在使用前放入十二烷基磺酸钠水溶液中,超声2h,去离子水洗涤,再使用无水乙醇超声洗涤10min后,用去离子水洗涤,在70℃的烘箱里干燥1h得空白棉纤维备用;
②取硫脲和尿素溶解到无水乙醇中,再加入钛酸丁酯,用5t%稀硝酸调节其pH为3,搅拌均匀,然后将去离子水缓慢滴加到上述溶液中,并继续搅拌20min,静置0.8h,得到湿凝胶;
③将步骤②得到的溶胶液继续搅拌,待出现丁达尔现象后,将步骤(1)准备好的棉纤维浸渍到溶胶液中,浸渍5min,烘干,得到处理后的棉纤维;
烘干时采用低温烘干的方式进行,具体为:
烘干温度为40℃,且烘干过程中通过风扇保证气流快速流动,烘干后棉纤维含水量为30%时停止烘干;
(3)将石墨烯-聚丙烯腈复合纳米纤维、玄武岩纤维、预处理后的棉纤维、预处理后的兔毛纤维及海藻纤维维通过成条、纺纱、织布制得混纺面料;
(4)将混纺面料进行阻燃整理,具体为:采用阻燃剂、树脂、柔软剂和磷酸,通过二浸二轧(轧余率75%)→烘干(100℃,2min)→焙烘(170℃,2min)→纯碱中和,使得pH值7→皂洗→水洗→烘干,得到阻燃面料;
阻燃剂为聚双三羟甲基丙烷硫代磷酰脲;树脂为脲醛树脂;柔软剂为柔软剂JPBC;
阻燃整理时织物在4g/L皂粉,1g/L纯碱,浴比1∶10的条件下进行皂洗、水洗、晾干。
在本实施例中,石墨烯-聚丙烯腈复合纳米纤维的制备具体如下:
S1、在冰水浴条件下,在200ml烧杯中加入1g石墨粉、0.2g硝酸钠、12ml弄硫酸搅拌20min后,加入1.8g高锰酸钾,在40℃下搅拌1h,加入50ml的去离子水搅拌10min,加入150ml去离子水和1.5ml双氧水搅拌10min,离心烘干后得到氧化石墨烯片,用3g硼氢化钠还原得到石墨烯片备用;
S2、将1g石墨烯加入到40g甲酰二甲胺中,超声30min,将石墨烯片分散液放在水浴锅中60℃水浴加热,慢慢加入15g聚丙烯腈,横向搅拌,直至充分溶解,在室温下静止12h去泡,得到石墨烯-聚丙烯腈复合纳米纤维纺丝液;
S3、将石墨烯-聚丙烯腈复合纳米纤维纺丝液转移至注射器采用静电纺制备得到石墨烯-聚丙烯腈复合纳米纤维。
在本实施例中,阻燃面料的后处理,具体为:
(I)将KH570硅烷偶联剂加入到85-90%的乙醇溶液中配制成KH570浓度为0.6%的浸渍液;
(II)将含石墨烯纤维的混纺阻燃面料浸泡于浸渍液中12min后,取出并在鼓风干燥箱中60℃进行烘干,烘干后的面料再进行浸渍及烘干,重复浸渍和烘干操作5次后得到后处理后的阻燃面料。
将本实施例的阻燃面料纺织成阻燃纱布,将阻燃纱布加入3g/L纯碱,浴比为1∶10,在95℃的热水中处理10min,然后热水洗、温水洗、冷水洗、烘干,处理次数为30次后对其抗菌性采用现有技术进行测定,具体数据见表1所示;
表1面料抗菌性测试结果
Figure BDA0003708505430000081
由表1可知,该面料的抑菌率满足标准,具有很好的抗菌功能。
实施例2
本实施例提供一种含石墨烯纤维的混纺阻燃面料,包括如下重量份数计的原料:
石墨烯-聚丙烯腈复合纳米纤维:30份,兔毛纤维:30份,玄武岩纤维:20份,棉纤维:40份,海藻纤维:20份;
该含石墨烯纤维的混纺阻燃面料的制备工艺具体包括以下步骤:
(1)兔毛纤维和海藻纤维的的预处理
使用前先对兔毛纤维和海藻纤维分别进行开松处理,加入纤维质量0.5%的CTA-2886和毛油和纤维质量0.2%的现有技术中抗静电剂,均匀喷洒到纤维中以减少静电,喷洒后焖放24h以上;
(2)棉纤维的预处理
①将棉纤维在使用前放入十二烷基磺酸钠水溶液中,超声2h,去离子水洗涤,再使用无水乙醇超声洗涤20min后,用去离子水洗涤,在70℃的烘箱里干燥1h得空白棉纤维备用;
②取硫脲和尿素溶解到无水乙醇中,再加入钛酸丁酯,用5t%稀硝酸调节其pH为4,搅拌均匀,然后将去离子水缓慢滴加到上述溶液中,并继续搅拌23min,静置1h,得到湿凝胶;
③将步骤②得到的溶胶液继续搅拌,待出现丁达尔现象后,将步骤(1)准备好的棉纤维浸渍到溶胶液中,浸渍7min,烘干,得到处理后的棉纤维;
烘干时采用低温烘干的方式进行,具体为:
烘干温度为43℃,且烘干过程中通过风扇保证气流快速流动,烘干后棉纤维含水量为33%时停止烘干;
(3)将石墨烯-聚丙烯腈复合纳米纤维、玄武岩纤维、预处理后的棉纤维、预处理后的兔毛纤维及海藻纤维维通过成条、纺纱、织布制得混纺面料;
(4)将混纺面料进行阻燃整理,具体为:采用阻燃剂、树脂、柔软剂和磷酸,通过二浸二轧(轧余率75%)→烘干(120℃,5min)→焙烘(175℃,4min)→纯碱中和,使得pH值8→皂洗→水洗→烘干,得到阻燃面料;
阻燃剂为聚双三羟甲基丙烷硫代磷酰脲;树脂为脲醛树脂;柔软剂为柔软剂JPBC;
阻燃整理时织物在4g/L皂粉,1g/L纯碱,浴比1∶10的条件下进行皂洗、水洗、晾干。
在本实施例中,石墨烯-聚丙烯腈复合纳米纤维的制备具体如下:
S1、在冰水浴条件下,在200ml烧杯中加入1g石墨粉、0.2g硝酸钠、12ml弄硫酸搅拌30min后,加入1.8g高锰酸钾,在40℃下搅拌1h,加入50ml的去离子水搅拌15min,加入150ml去离子水和1.5ml双氧水搅拌15min,离心烘干后得到氧化石墨烯片,用3g硼氢化钠还原得到石墨烯片备用;
S2、将1g石墨烯加入到40g甲酰二甲胺中,超声30min,将石墨烯片分散液放在水浴锅中60℃水浴加热,慢慢加入15g聚丙烯腈,横向搅拌,直至充分溶解,在室温下静止12h去泡,得到石墨烯-聚丙烯腈复合纳米纤维纺丝液;
S3、将石墨烯-聚丙烯腈复合纳米纤维纺丝液转移至注射器采用静电纺制备得到石墨烯-聚丙烯腈复合纳米纤维。
在本实施例中,阻燃面料的后处理,具体为:
(I)将KH570硅烷偶联剂加入到85-90%的乙醇溶液中配制成KH570浓度为1.5%的浸渍液;
(II)将含石墨烯纤维的混纺阻燃面料浸泡于浸渍液中15min后,取出并在鼓风干燥箱中60℃进行烘干,烘干后的面料再进行浸渍及烘干,重复浸渍和烘干操作6次后得到后处理后的阻燃面料。
将本实施例的阻燃面料纺织成阻燃纱布,将阻燃纱布加入2g/L纯碱,浴比为1∶10,在95℃的热水中处理10min,然后热水洗、温水洗、冷水洗、烘干,处理次数为30次后对其抗菌性采用现有技术进行测定,具体数据见表2所示;
表2面料抗菌性测试结果
Figure BDA0003708505430000101
由表2可知,该面料的抑菌率满足标准,具有很好的抗菌功能。
实施例3
本实施例提供一种含石墨烯纤维的混纺阻燃面料,包括如下重量份数计的原料:
石墨烯-聚丙烯腈复合纳米纤维:25份,兔毛纤维:25份,玄武岩纤维:17份,棉纤维:36份,海藻纤维:18份;
该含石墨烯纤维的混纺阻燃面料的制备工艺具体包括以下步骤:
(1)兔毛纤维和海藻纤维的的预处理
使用前先对兔毛纤维和海藻纤维分别进行开松处理,加入纤维质量0.5%的CTA-2886和毛油和纤维质量0.2%的现有技术中抗静电剂,均匀喷洒到纤维中以减少静电,喷洒后焖放24h以上;
(2)棉纤维的预处理
①将棉纤维在使用前放入十二烷基磺酸钠水溶液中,超声2h,去离子水洗涤,再使用无水乙醇超声洗涤15min后,用去离子水洗涤,在70℃的烘箱里干燥1h得空白棉纤维备用;
②取硫脲和尿素溶解到无水乙醇中,再加入钛酸丁酯,用5t%稀硝酸调节其pH为4,搅拌均匀,然后将去离子水缓慢滴加到上述溶液中,并继续搅拌22min,静置0.9h,得到湿凝胶;
③将步骤②得到的溶胶液继续搅拌,待出现丁达尔现象后,将步骤(1)准备好的棉纤维浸渍到溶胶液中,浸渍6min,烘干,得到处理后的棉纤维;
烘干时采用低温烘干的方式进行,具体为:
烘干温度为42℃,且烘干过程中通过风扇保证气流快速流动,烘干后棉纤维含水量为31%时停止烘干;
(3)将石墨烯-聚丙烯腈复合纳米纤维、玄武岩纤维、预处理后的棉纤维、预处理后的兔毛纤维及海藻纤维维通过成条、纺纱、织布制得混纺面料;
(4)将混纺面料进行阻燃整理,具体为:采用阻燃剂、树脂、柔软剂和磷酸,通过二浸二轧(轧余率75%)→烘干(110℃,3min)→焙烘(172℃,3min)→纯碱中和,使得pH值7→皂洗→水洗→烘干,得到阻燃面料;
阻燃剂为聚双三羟甲基丙烷硫代磷酰脲;树脂为脲醛树脂;柔软剂为柔软剂JPBC;
阻燃整理时织物在4g/L皂粉,1g/L纯碱,浴比1∶10的条件下进行皂洗、水洗、晾干。在本实施例中,石墨烯-聚丙烯腈复合纳米纤维的制备具体如下:
S1、在冰水浴条件下,在200ml烧杯中加入1g石墨粉、0.2g硝酸钠、12ml弄硫酸搅拌25min后,加入1.8g高锰酸钾,在40℃下搅拌1h,加入50ml的去离子水搅拌12min,加入150ml去离子水和1.5ml双氧水搅拌12min,离心烘干后得到氧化石墨烯片,用3g硼氢化钠还原得到石墨烯片备用;
S2、将1g石墨烯加入到40g甲酰二甲胺中,超声30min,将石墨烯片分散液放在水浴锅中60℃水浴加热,慢慢加入15g聚丙烯腈,横向搅拌,直至充分溶解,在室温下静止12h去泡,得到石墨烯-聚丙烯腈复合纳米纤维纺丝液;
S3、将石墨烯-聚丙烯腈复合纳米纤维纺丝液转移至注射器采用静电纺制备得到石墨烯-聚丙烯腈复合纳米纤维。
在本实施例中,阻燃面料的后处理,具体为:
(I)将KH570硅烷偶联剂加入到88%的乙醇溶液中配制成KH570浓度为1.1%的浸渍液;
(II)将含石墨烯纤维的混纺阻燃面料浸泡于浸渍液中13min后,取出并在鼓风干燥箱中60℃进行烘干,烘干后的面料再进行浸渍及烘干,重复浸渍和烘干操作5次后得到后处理后的阻燃面料。
将本实施例的阻燃面料纺织成阻燃纱布,将阻燃纱布加入3g/L纯碱,浴比为1∶10,在95℃的热水中处理10min,然后热水洗、温水洗、冷水洗、烘干,处理次数为30次后对其抗菌性采用现有技术进行测定,具体数据见表3所示;
表3面料抗菌性测试结果
Figure BDA0003708505430000121
由表3可知,该面料的抑菌率满足标准,具有很好的抗菌功能。
本发明的阻燃面料在阻燃整理前和整理后面料的性能指标具体见表4所示;
表4实施例1-3中面料阻燃整理前、后的性能指标
Figure BDA0003708505430000122
由表4可见,在阻燃整理后阻燃得到提到达到要求,本发明还加入柔软剂可以有效提高织物的撕破强力指标,本发明经优化阻燃工艺处理后的混纺织物面料达到了阻燃要求,也到达了防护服的要求,具有一定的耐洗性。
对实施例1-3的面料制成织造成织物,对织物服用性能进行检测,具体见表5;
表5织物服用性能
Figure BDA0003708505430000123
Figure BDA0003708505430000131
有表5可见,该阻燃面料性能优异,满足阻燃和服用双重标准。
除上述实施例外,本发明还可以有其他实施方式。凡采用等同替换或等效变换形成的技术方案,均落在本发明要求的保护范围。

Claims (8)

1.一种含石墨烯纤维的混纺阻燃面料,其特征在于,包括如下重量份数计的原料:
石墨烯-聚丙烯腈复合纳米纤维:20-30份,兔毛纤维:20-30份,玄武岩纤维:10-20份,棉纤维:30-40份,海藻纤维:15-20份;
该含石墨烯纤维的混纺阻燃面料的制备工艺具体包括以下步骤:
(1)兔毛纤维和海藻纤维的的预处理
使用前先对兔毛纤维和海藻纤维分别进行开松处理,加入一和毛油和抗静电剂,均匀喷洒到纤维中以减少静电,喷洒后焖放24h以上;
(2)棉纤维的预处理
Figure DEST_PATH_IMAGE001
将棉纤维在使用前放入十二烷基磺酸钠水溶液中,超声2h,去离子水洗涤,再使用无水乙醇超声洗涤10-20min后,用去离子水洗涤,在70℃的烘箱里干燥1h得空白棉纤维备用;
Figure 174125DEST_PATH_IMAGE002
取硫脲和尿素溶解到无水乙醇中,再加入钛酸丁酯,用5t%稀硝酸调节其pH为3~4,搅拌均匀,然后将去离子水缓慢滴加到上述溶液中,并继续搅拌20-23min,静置0.8-1h,得到湿凝胶;
Figure DEST_PATH_IMAGE003
将步骤
Figure 953862DEST_PATH_IMAGE002
得到的溶胶液继续搅拌,待出现丁达尔现象后,将步骤(1)准备好的棉纤维浸渍到溶胶液中,浸渍5-7min,烘干,得到处理后的棉纤维;
(3)将石墨烯-聚丙烯腈复合纳米纤维、玄武岩纤维、预处理后的棉纤维、预处理后的兔毛纤维及海藻纤维维通过成条、纺纱、织布制得混纺面料;
(4)将混纺面料进行阻燃整理,具体为:采用阻燃剂、树脂、柔软剂和磷酸,通过二浸二轧→烘干→焙烘→纯碱中和,使得pH值7~8→皂洗→水洗→烘干,得到阻燃面料。
2.根据权利要求1所述的含石墨烯纤维的混纺阻燃面料,其特征在于:步骤(1)在兔毛纤维和海藻纤维的的预处理时所述和毛油为纤维质量0.5%的CTA-2886和毛油。
3.根据权利要求1所述的含石墨烯纤维的混纺阻燃面料,其特征在于:步骤(2)棉纤维浸渍溶胶液后进行烘干,烘干时采用低温烘干的方式进行,具体为:
烘干温度为40℃-43℃,且烘干过程中通过风扇保证气流快速流动,烘干后棉纤维含水量为30-33%时停止烘干。
4.根据权利要求1所述的含石墨烯纤维的混纺阻燃面料,其特征在于:步骤(4)混纺面料进行阻燃整理时所述阻燃剂为聚双三羟甲基丙烷硫代磷酰脲;所述树脂为脲醛树脂;所述柔软剂为柔软剂JPBC。
5.根据权利要求1所述的含石墨烯纤维的混纺阻燃面料,其特征在于:所述步骤(4)阻燃整理时二浸二轧时控制轧余率75%;烘干时烘干温度控制在100-120℃,烘干2-5min;烘焙时控制温度170-175℃,烘焙2-4min。
6.根据权利要求1所述的含石墨烯纤维的混纺阻燃面料,其特征在于:所述步骤(4)阻燃整理时织物在4g/L皂粉,1g/L纯碱,浴比1∶10的条件下进行皂洗、水洗、晾干。
7.根据权利要求1所述的含石墨烯纤维的混纺阻燃面料,其特征在于:所述石墨烯-聚丙烯腈复合纳米纤维的制备具体如下:
S1、在冰水浴条件下,在烧杯中加入石墨粉、硝酸钠、浓硫酸搅拌20-30min后,加入高锰酸钾,在40℃下搅拌1h,加入去离子水搅拌10-15min,加入去离子水和双氧水搅拌10-15min,离心烘干后得到氧化石墨烯片,用硼氢化钠还原得到石墨烯片备用;
S2、将石墨烯加入到甲酰二甲胺中,超声30min,将石墨烯片分散液放在水浴锅中60℃水浴加热,慢慢加入聚丙烯腈,横向搅拌,直至充分溶解,在室温下静止12h去泡,得到石墨烯-聚丙烯腈复合纳米纤维纺丝液;
S3、将石墨烯-聚丙烯腈复合纳米纤维纺丝液转移至注射器采用静电纺制备得到石墨烯-聚丙烯腈复合纳米纤维。
8.根据权利要求1所述的含石墨烯纤维的混纺阻燃面料,其特征在于:阻燃面料的后处理,具体为:
Figure 286755DEST_PATH_IMAGE004
)将KH570硅烷偶联剂加入到85-90%的乙醇溶液中配制成KH570浓度为0.6-1.5%的浸渍液;
Figure DEST_PATH_IMAGE005
)将含石墨烯纤维的混纺阻燃面料浸泡于浸渍液中12-15min后,取出并在鼓风干燥箱中60℃进行烘干,烘干后的面料再进行浸渍及烘干,重复浸渍和烘干操作5-6次后得到后处理后的阻燃面料。
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