CN114182524B - 一种抗菌涤纶梭织坯布及生产工艺 - Google Patents
一种抗菌涤纶梭织坯布及生产工艺 Download PDFInfo
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Abstract
本发明提出了一种抗菌涤纶梭织坯布的生产工艺,包括如下步骤:S1,将氧化石墨烯超声分散在有机溶剂中得到氧化石墨烯分散液,然后加入金属盐溶液和有机配体溶液,搅拌均匀后,加入稳定剂,得到氧化石墨烯金属有机框架化合物;S2,将涤纶梭织坯布浸渍于碱性溶液中,然后洗涤、脱水和烘干;S3,将步骤S1的氧化石墨烯金属有机框架化合物超声分散处理,并加热至90‑120℃,对步骤S2碱处理后的涤纶梭织坯布进行浸渍处理0.5‑2h,然后洗涤和干燥,得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。本发明制备的涤纶梭织坯布对大肠杆菌、金黄色葡萄球菌、白色念珠菌和红色毛癣菌的抑菌率达到97.89‑99.78%,100次洗涤后,抑菌效果仅降低3‑6%。
Description
技术领域
本发明涉及涤纶生产技术领域,尤其涉及一种抗菌涤纶梭织坯布及生产工艺。
背景技术
涤纶,是指以多种二元醇和芳香族二元羧酸或其酯经缩聚而得的成纤高聚物—聚对苯二甲酸乙二醇酯,经纺丝及后处理制成的纤维,简称PET。涤纶纤维具有物理机械性能好、耐磨性好、易洗快干等优良性能,广泛被应用于纺织产品当中。自涤纶纤维问世以来一直受到人们的欢迎,在现代纺织及服饰应用中具有很高的认知度。但是涤纶易被脂肪性油污沾污,滋生细菌,因此进一步研发和推广抗菌涤纶功能性织物,对减少病菌对人类的侵害具有积极的意义。
目前,用于纺织品抗菌处理的抗菌剂主要有季铵盐类、卤胺类、壳聚糖及其衍生物、无机金属及其氧化物等。虽然采用抗菌剂处理方法方便,同时也能达到抗菌的目的,但是随着洗涤次数的增加,抗菌剂容易脱落,抗菌性能的持久性很难得到保证。
发明内容
有鉴于此,本发明提出了一种抗菌剂不易脱落、抗菌性能持久的抗菌涤纶梭织坯布及生产工艺。
本发明的技术方案是这样实现的:本发明提供了一种抗菌涤纶梭织坯布的生产工艺,包括如下步骤:
S1,首先将氧化石墨烯超声分散在有机溶剂中得到浓度为1-5mg/mL的氧化石墨烯分散液,然后加入金属盐溶液和有机配体溶液,在60-80℃下搅拌均匀,加入稳定剂,得到氧化石墨烯金属有机框架化合物;
S2,将涤纶梭织坯布浸渍于碱性溶液中,然后洗涤、脱水和烘干;
S3,将步骤S1的氧化石墨烯金属有机框架化合物超声分散处理,并加热至90-120℃,对步骤S2碱处理后的涤纶梭织坯布进行浸渍处理0.5-2h,然后洗涤和干燥,得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。
在以上技术方案的基础上,优选的,步骤S1所述金属盐为有机铜盐或有机锌盐,选自烯基丁二酸铜、油酸铜、硬脂酸铜、苯磺酸锌、醋酸锌和磷酸锌中的一种或多种组合。
在以上技术方案的基础上,优选的,步骤S1所述有机配体为荭草苷。
在以上技术方案的基础上,优选的,步骤S1所述金属盐和有机配体的溶剂为水、N-甲基吡咯烷酮和N,N-二甲基甲酰胺中的一种或多种组合。
在以上技术方案的基础上,优选的,步骤S1所述金属盐溶液的浓度为0.04-0.08mol/L,有机配体溶液的浓度为0.01-0.05mol/L。
在以上技术方案的基础上,优选的,步骤S1所述氧化石墨烯分散液:金属盐溶液:有机配体溶液的体积比为(50-100):(7-12):(6-8)。
在以上技术方案的基础上,优选的,步骤S3浸渍处理时,每隔0.5h将涤纶梭织坯布取出,放在紫外灯下照射5-10min。
在以上技术方案的基础上,优选的,步骤S1所述有机溶剂为甲醇、乙醇、丙醇和乙二醇乙醚中的一种或多种组合。
在以上技术方案的基础上,优选的,步骤S1所述稳定剂为乙二胺、乙二醇和氨水中的一种或多种组合.
在以上技术方案的基础上,优选的,步骤S1所述氧化石墨烯分散液:稳定剂的体积比为(50-100):(3-5)。
在以上技术方案的基础上,优选的,步骤S2所述碱性溶液的浓度为6-8mol/L,碱性试剂为乙二胺四乙酸二钠、三乙醇胺和乙醇胺中的一种或多种组合,溶剂为水。
本申请还提供了一种抗菌涤纶梭织坯布,由上述抗菌涤纶梭织坯布的生产工艺制备而成。
本发明的一种抗菌涤纶梭织坯布及生产工艺相对于现有技术具有以下有益效果:
(1)本申请根据金属有机骨架材料的多孔结构和较高的表面积的特点,利用氧化石墨烯、有机铜盐、有机锌盐和荭草苷制备的氧化石墨烯金属有机框架化合物对涤纶梭织坯布进行修饰,赋予其良好的抗菌性,对大肠杆菌、金黄色葡萄球菌、白色念珠菌和红色毛癣菌的抑菌率达到97.89-99.78%,100次洗涤后,抑菌效果仅降低3-6%。
(2)涤纶在高温条件下,纤维分子发生剧烈运动,聚合物分子间的空隙增大,纤维结构变得松散;在高温条件下对涤纶进行浸渍处理,依靠金属有机框架化合物之间的羟基与涤纶纤维存在的氢键作用力,使得金属有机框架化合物能很好的吸附到纤维表面和空隙中,降温后,涤纶收缩,增加了金属有机框架化合物与纤维之间的抱合力。
(3)紫外照射可以促进氧化石墨烯金属有机框架化合物与涤纶梭织坯布的结合能力,提高其抗菌能力和防老化能力。
具体实施方式
下面将结合本发明实施方式,对本发明实施方式中的技术方案进行清楚、完整地描述,显然,所描述的实施方式仅仅是本发明一部分实施方式,而不是全部的实施方式。基于本发明中的实施方式,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他实施方式,都属于本发明保护的范围。
实施例1
一种抗菌涤纶梭织坯布的生产工艺,包括如下步骤:
S1,将0.1g氧化石墨烯超声分散在100ml甲醇溶剂中,制备1mg/mL氧化石墨烯分散液;金属盐溶液制备:采用等体积的水和N-甲基吡咯烷酮溶剂制备0.04mol/L的烯基丁二酸铜溶液;有机配体溶液制备:采用等体积的水和N,N-二甲基甲酰胺溶剂制备0.01mol/L的荭草苷溶液;按照氧化石墨烯分散液:金属盐溶液:有机配体溶液的体积比为50:7:6的比例加入到氧化石墨烯分散液中,在60℃下搅拌均匀,按照氧化石墨烯分散液:乙二胺体积比为50:3的比例加入乙二胺,得到氧化石墨烯金属有机框架化合物;
S2,取10cm×10cm的涤纶梭织坯布浸渍于浓度为6mol/L的乙二胺四乙酸二钠的水溶液中,然后洗涤、脱水和烘干;
S3,将氧化石墨烯金属有机框架化合物超声分散20min,然后加热至90℃,并对涤纶梭织坯布进行浸渍处理0.5h,然后将涤纶梭织坯布用10%的丙酮水溶液洗涤1次,置于40℃去离子水中浸泡6d,每2d更换1次去离子水;然后用丙酮浸泡8d,每2d更换1次丙酮,将得到的产物烘干,得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。
实施例2
一种抗菌涤纶梭织坯布的生产工艺,包括如下步骤:
S1,将0.5g氧化石墨烯超声分散在100ml乙醇溶剂中,制备5mg/mL氧化石墨烯分散液;金属盐溶液制备:采用4体积份数的水和1体积份数的N-甲基吡咯烷酮溶剂制备0.08mol/L的油酸铜;有机配体溶液制备:采用4体积份数的水和1体积份数的N,N-二甲基甲酰胺溶剂制备0.05mol/L的荭草苷溶液,按照氧化石墨烯分散液:金属盐溶液:有机配体溶液的体积比为100:12:8的比例加入到氧化石墨烯分散液中,在80℃下搅拌均匀,按照氧化石墨烯分散液:乙二醇体积比为100:5的比例加入乙二胺,得到氧化石墨烯金属有机框架化合物;
S2,取10cm×10cm的涤纶梭织坯布浸渍于浓度为8mol/L的三乙醇胺水溶液中,然后洗涤、脱水和烘干;
S3,将氧化石墨烯金属有机框架化合物超声分散20min,然后加热至120℃,对涤纶梭织坯布进行浸渍处理2h,浸渍处理时,每隔0.5h将涤纶梭织坯布取出,放在紫外灯下照射10min;然后取出涤纶梭织坯布,用10%的丙酮水溶液洗涤1次,置于40℃去离子水中浸泡6d,每2d更换1次去离子水;然后用丙酮浸泡8d,每2d更换1次丙酮,将得到的产物烘干得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。
实施例3
一种抗菌涤纶梭织坯布的生产工艺,包括如下步骤:
S1,将0.3g氧化石墨烯超声分散在100ml丙醇溶剂中,制备3mg/mL氧化石墨烯分散液;金属盐溶液制备:采用3体积份数的水和1体积份数的N-甲基吡咯烷酮溶剂制备0.06mol/L的硬脂酸铜溶液;有机配体溶液制备:采用5体积份数的水和2体积份数的N,N-二甲基甲酰胺溶剂制备0.03mol/L的荭草苷溶液,按照氧化石墨烯分散液:金属盐溶液:有机配体溶液的体积比为75:9:7的比例加入到氧化石墨烯分散液中,在70℃下搅拌均匀,按照氧化石墨烯分散液:氨水体积比为75:4的比例加入氨水,得到氧化石墨烯金属有机框架化合物。
S2,取10cm×10cm的涤纶梭织坯布浸渍于浓度为7mol/L的乙醇胺的水溶液中,然后洗涤、脱水和烘干;
S3,将氧化石墨烯金属有机框架化合物超声分散20min,然后加热至100℃,对涤纶梭织坯布进行浸渍处理1h,浸渍处理时,每隔0.5h将涤纶梭织坯布取出,放在紫外灯下照射5min;然后取出涤纶梭织坯布,用10%的丙酮水溶液洗涤1次,置于40℃去离子水中浸泡6d,每2d更换1次去离子水;然后用丙酮浸泡8d,每2d更换1次丙酮,将得到的产物烘干得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。
实施例4
一种抗菌涤纶梭织坯布的生产工艺,包括如下步骤:
S1,将0.2g氧化石墨烯超声分散在100ml乙二醇乙醚溶剂中,制备2mg/mL氧化石墨烯分散液;金属盐溶液制备:采用2体积份数的水和1体积份数的N-甲基吡咯烷酮溶剂制备0.05mol/L的苯磺酸锌溶液;有机配体溶液制备:采用2体积份数的水和1体积份数的N,N-二甲基甲酰胺溶剂制备0.02mol/L的荭草苷溶液,按照氧化石墨烯分散液:金属盐溶液:有机配体溶液的体积比为60:8:7的比例加入到氧化石墨烯分散液中,在65℃下搅拌均匀,按照氧化石墨烯分散液:乙二胺体积比为55:4的比例加入乙二胺,得到氧化石墨烯金属有机框架化合物。
S2,取10cm×10cm的涤纶梭织坯布浸渍于浓度为6mol/L的乙二胺四乙酸二钠的水溶液中,然后洗涤、脱水和烘干;
S3,将氧化石墨烯金属有机框架化合物超声分散20min,然后加热至110℃,对涤纶梭织坯布进行浸渍处理1.5h,浸渍处理时,每隔0.5h将涤纶梭织坯布取出,放在紫外灯下照射10min;然后取出涤纶梭织坯布,用10%的丙酮水溶液洗涤1次,置于40℃去离子水中浸泡6d,每2d更换1次去离子水;然后用丙酮浸泡8d,每2d更换1次丙酮,将得到的产物烘干得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。
实施例5
一种抗菌涤纶梭织坯布的生产工艺,包括如下步骤:
S1,将0.4g氧化石墨烯超声分散在100ml甲醇溶剂中,制备4mg/mL氧化石墨烯分散液;金属盐溶液制备:采用5体积份数的水和1体积份数的N-甲基吡咯烷酮溶剂制备0.07mol/L的醋酸锌溶液;有机配体溶液制备:采用5体积份数的水和1体积份数的N,N-二甲基甲酰胺溶剂制备0.04mol/L的荭草苷溶液,按照氧化石墨烯分散液:金属盐溶液:有机配体溶液的体积比为90:11:8的比例加入到氧化石墨烯分散液中,在75℃下搅拌均匀,按照氧化石墨烯分散液:乙二醇体积比为65:4的比例加入乙二醇,得到氧化石墨烯金属有机框架化合物。
S2,取10cm×10cm的涤纶梭织坯布浸渍于浓度为8mol/L的乙醇胺的水溶液中,然后洗涤、脱水和烘干;
S3,将氧化石墨烯金属有机框架化合物超声分散20min,然后加热至105℃,对涤纶梭织坯布进行浸渍处理1h,浸渍处理时,每隔0.5h将涤纶梭织坯布取出,放在紫外灯下照射10min;然后取出涤纶梭织坯布,用10%的丙酮水溶液洗涤1次,置于40℃去离子水中浸泡6d,每2d更换1次去离子水;然后用丙酮浸泡8d,每2d更换1次丙酮,将得到的产物烘干得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。
对比例1
在实施例1的基础上,与实施例1相比不同的是,步骤S1中不含氧化石墨烯,性能测试见表1-2。
对比例2
在实施例1的基础上,与实施例1相比不同的是,步骤S1中金属盐为无机盐硝酸铜,有机配体为2,3,6,7,10,11-六羟基三亚苯基苯,性能测试见表1-2。
对比例3
在实施例1的基础上,与实施例1相比不同的是,步骤S3中氧化石墨烯金属有机框架化合物不经超声分散处理和加热,直接将涤纶梭织坯布浸入氧化石墨烯金属有机框架化合物进行浸渍处理,性能测试见表1-2。
对比例4
在实施例1的基础上,与实施例1相比不同的是,步骤S1中不含氧化石墨烯,步骤S1中金属盐为无机盐硝酸铜,有机配体为2,3,6,7,10,11-六羟基三亚苯基苯,步骤S3中氧化石墨烯金属有机框架化合物不经超声分散处理和加热,性能测试见表1-2。
织物抗菌性能指织物具有的能抑制细菌繁殖的能力,本文采用吸收法对涤纶梭织坯布的抗菌性能进行评价,主要为了模拟人穿着时涤纶织物对细菌繁殖的抑制情况。抑菌检测方法参照GB/T20944.2-2007《纺织品抗菌性能的评价第2部分:吸收法》,先将冻干菌融化分散在5mL培养液中,37℃培养18-24h,再用接种环取菌液在培养皿上划线培养1d,再从培养皿上取一个菌接种到试管培养1d,然后测菌液浓度,用移液枪取0.1mL菌液稀释三次后涂布培养1d,用20mL培养液洗脱布上细菌,再从中取0.1mL稀释涂板。培养1d后计数算抑菌率,其中对照组是不加样布的菌液。
表1涤纶梭织坯布的抑菌效果
组别 | 大肠杆菌/% | 金黄色葡萄球菌/% | 白色念珠菌/% | 红色毛癣菌/% |
实施例1 | 96.89 | 97.25 | 93.15 | 96.84 |
实施例2 | 98.14 | 99.17 | 95.78 | 98.75 |
实施例3 | 98.76 | 98.78 | 95.83 | 99.18 |
实施例4 | 99.35 | 99.34 | 96.18 | 99.43 |
实施例5 | 99.43 | 99.78 | 97.89 | 99.72 |
对比例1 | 85.78 | 84.18 | 81.37 | 85.76 |
对比例2 | 80.47 | 82.76 | 81.49 | 80.72 |
对比例3 | 90.15 | 91.29 | 83.56 | 89.39 |
对比例4 | 50.48 | 49.86 | 55.71 | 45.28 |
由表1可知,本发明的涤纶梭织坯布对大肠杆菌、金黄色葡萄球菌、白色念珠菌和红色毛癣菌的抑菌率达到97.89-99.78%,表明氧化石墨烯、有机铜盐、有机锌盐和荭草苷协同具有抑菌性。
涤纶梭织坯布抗菌持久性检测:参照GB/T20944.2-2007《纺织品抗菌性能的评价第2部分:吸收法》,每个实施例和对比例中取3个小样(每个尺寸10cm×10cm,剪成2块),按照GB/T 12490-1990中的试验条件A1M进行洗涤,采用ECE标准洗涤剂,清洗结束后作为5次洗涤(相当于5次洗涤的具体操作条件和步骤:40℃,150ml溶液,钢珠10粒,洗45min,洗涤后去除试样,在40℃和100ml的水中清洗2次,每次1min)。达到规定的洗涤次数后,用水充分清洗样品,晾干并检测其抗菌性,结果见表2。表中抑菌率为大肠杆菌、金黄色葡萄球菌、白色念珠菌和红色毛癣菌抑菌率的平均数。
表2涤纶梭织坯布的抑菌持久性效果
组别 | 10次 | 20次 | 50次 | 100次 |
实施例1 | 95.13 | 94.75 | 93.48 | 90.12 |
实施例5 | 97.87 | 97.01 | 96.28 | 95.89 |
对比例1 | 82.25 | 73.46 | 62.37 | 55.32 |
对比例2 | 75.30 | 47.41 | 32.48 | 22.22 |
对比例3 | 89.24 | 80.34 | 75.76 | 60.38 |
对比例4 | 42.12 | 30.82 | 23.18 | 10.73 |
表2可知,对比例由于不含氧化石墨烯、有机铜盐、有机锌盐和荭草苷,其抑菌持久性表现较差,100次洗涤后,与初始相比,抑菌效果降低了34-78%;实施例仅降低3-6%。
以上所述仅为本发明的较佳实施方式而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (7)
1.一种抗菌涤纶梭织坯布的生产工艺,其特征在于:包括如下步骤:
S1,首先将氧化石墨烯超声分散在有机溶剂中得到浓度为1-5mg/mL的氧化石墨烯分散液,然后加入金属盐溶液和有机配体溶液,在60-80℃下搅拌均匀,加入稳定剂,得到氧化石墨烯金属有机框架化合物;
所述金属盐为有机铜盐或有机锌盐,选自烯基丁二酸铜、油酸铜、硬脂酸铜、苯磺酸锌、醋酸锌和磷酸锌中的一种或多种组合;有机配体为荭草苷;所述金属盐和有机配体的溶剂为水、N-甲基吡咯烷酮和N,N-二甲基甲酰胺中的一种或多种组合;
所述金属盐溶液的浓度为0.07-0.08mol/L,有机配体溶液的浓度为0.04-0.05mol/L;
所述氧化石墨烯分散液:金属盐溶液:有机配体溶液的体积比为(50-100):(7-12):(6-8);
S2,将涤纶梭织坯布浸渍于碱性溶液中,然后洗涤、脱水和烘干;
S3,将步骤S1的氧化石墨烯金属有机框架化合物超声分散处理,并加热至90-120℃,对步骤S2碱处理后的涤纶梭织坯布进行浸渍处理0.5-2h,然后洗涤和干燥,得到氧化石墨烯金属有机框架化合物修饰的涤纶梭织坯布。
2.如权利要求1所述的一种抗菌涤纶梭织坯布的生产工艺,其特征在于:步骤S3浸渍处理时,每隔0.5h将涤纶梭织坯布取出,放在紫外灯下照射5-10min。
3.如权利要求1所述的一种抗菌涤纶梭织坯布的生产工艺,其特征在于:步骤S1所述有机溶剂为甲醇、乙醇、丙醇和乙二醇乙醚中的一种或多种组合。
4.如权利要求1所述的一种抗菌涤纶梭织坯布的生产工艺,其特征在于:步骤S1所述稳定剂为乙二胺、乙二醇和氨水中的一种或多种组合。
5.如权利要求1所述的一种抗菌涤纶梭织坯布的生产工艺,其特征在于:步骤S1所述氧化石墨烯分散液:稳定剂的体积比为(50-100):(3-5)。
6.如权利要求1所述的一种抗菌涤纶梭织坯布的生产工艺,其特征在于:步骤S2所述碱性溶液的浓度为6-8mol/L,碱性试剂为乙二胺四乙酸二钠、三乙醇胺和乙醇胺中的一种或多种组合,溶剂为水。
7.一种抗菌涤纶梭织坯布由权利要求1-6任一所述的一种抗菌涤纶梭织坯布的生产工艺制备。
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