CN111826740A - 抗菌阻燃纤维防护服及其制备方法 - Google Patents

抗菌阻燃纤维防护服及其制备方法 Download PDF

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CN111826740A
CN111826740A CN202010603969.3A CN202010603969A CN111826740A CN 111826740 A CN111826740 A CN 111826740A CN 202010603969 A CN202010603969 A CN 202010603969A CN 111826740 A CN111826740 A CN 111826740A
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mixed solution
fiber
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马晓飞
张丽
张志成
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Jixiang Sanbao High Tech Textile Co Ltd
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Abstract

本发明提供一种抗菌阻燃纤维防护服的制备方法，首先将聚酯纤维浸入处理液中改性，再将上述聚酯纤维中加入5wt％过氧乙酸溶液，再加入交联聚维酮，混合得含有丝状纤维的混合液；向上述所制混合液中加入氯化聚氯乙烯，回流保温30min，然后加入三氟甲基磺酸钠和二茂铁，所得混合液送入冷冻干燥机中，干燥所得固体制成微粉，与水混合后制成混合液，在压力泵作用下通过喷嘴以束状形式喷出，形成粗丝制成防护服。通过处理液的使用，将氨基酸或带氨基的二元醇引入到聚酯分子链上，丝氨醇上自带的氨基暴露，将其活化后与无机抗菌剂进行络合反应；实现了抗菌性的提升。同时利用氯化聚氯乙烯、三氟甲基磺酸钠和二茂铁的改性处理，显著增强其抗菌性和阻燃性。

Description

抗菌阻燃纤维防护服及其制备方法
技术领域
本发明属于织造材料技术领域，具体为一种抗菌阻燃纤维防护服及其制备方法。
背景技术
聚酯，即聚对苯二甲酸乙二酯，聚酯纤维因具有诸多优点而被广泛应用于纺织品领域，目前已成为纺织品领域用途最广、耗量最大的纤维原料。人们对聚酯纤维的改性研究一直未从间断过，尤其是对阻燃聚酯纤维的研究，改性之前的聚酯纤维受热容易熔融、分解，燃烧时会出现熔融滴落现象，阻燃聚酯纤维的关键在于阻燃剂的使用，而大多性能良好的阻燃聚酯纤维其阻燃性能改进的关键技术方案仍处于保密状态，目前，聚酯纤维的阻燃改性方法主要有共聚阻燃改性、共混阻燃改性、接枝阻燃改性及后整理阻燃改性，共聚阻燃改性即在聚酯纤维聚合的过程中添加阻燃剂等助剂，以达到阻燃效果，但是该方法容易发生副反应，而且对阻燃剂的稳定性等要求较高；共混阻燃改性，即在纺丝熔融物中添加阻燃助剂；接枝阻燃改性的工艺较复杂，不容易掌握，而且研发周期长，投入较大；阻燃后整理即将聚酯纤维通过浸渍整理剂，赋予其阻燃性能，缺点是很多后整理的阻燃聚酯纤维，其阻燃性能会随着洗涤次数和使用时间而逐渐减弱。
发明内容
针对现有的技术方案存在的问题，本发明的目的在于提供一种抗菌阻燃纤维防护服及其制备方法，实现纤维防护服在改性后阻燃和抗菌性能与一体。
为实现上述目的，本发明提供以下技术方案：
一种抗菌阻燃纤维防护服的制备方法，制备方法包括如下步骤：
步骤一，原料处理：将PET树脂、纳米蒙脱土、纳米硅微粉真空干燥；
步骤二，PET树脂改性：按照质量份数计，将50-60份PET树脂干料、1.2-1.3份纳米蒙脱土干料和0.4-0.8份纳米硅微粉干料混合搅拌均匀后，再加入0.1-0.15份的六(4-醛基苯氧基)环三磷腈，继续混合搅拌均匀，造粒，再经熔融纺丝，制得聚酯纤维；
步骤三，聚酯纤维改性：将步骤二所得聚酯纤维浸入处理液中，于60-70℃下浸渍40-60min，排液，将聚酯纤维真空干燥，得后处理聚酯纤维；
步骤四，丝状纤维制备：向上述所得聚酯纤维中加入5wt％过氧乙酸溶液，充分混合后浸泡24h，并于微波频率2450MHz、输出功率700W下微波回流处理10min，趁热过滤，所得滤液自然冷却至室温，然后利用20wt％碳酸氢钠溶液调节滤液pH值至7，再加入交联聚维酮，混合均匀后于0-5℃环境中静置1h，即得含有丝状纤维的混合液；
步骤五，纤维改性处理：向上述所制含有丝状纤维的混合液中加入氯化聚氯乙烯，继续回流保温混合30min，然后加入三氟甲基磺酸钠和二茂铁，再次回流保温混合15min，并以5℃/min的降温速度降温至40-45℃，所得混合液送入冷冻干燥机中，干燥所得固体经超微粉碎机制成微粉，然后经纳米球磨机研磨成纳米级粉末，即得改性纤维粉；
步骤六，纤维成型：将上述所制改性纤维与水混合后制成混合液，混合液在在压力泵作用下通过喷嘴以束状形式喷出，经凝固后形成粗丝制成防护服。
进一步的，所述步骤四、步骤五中聚酯纤维、5wt％过氧乙酸溶液、交联聚维酮、氯化聚氯乙烯、三氟甲基磺酸钠和二茂铁的重量比为：25-30:60-80:2-3:2-3:0.5-1:0.01-0.02。
进一步的，所述步骤三中处理液由如下重量份数的原料制成：N-羟甲基丙烯酰胺1-2份、羟乙基纤维素1-2份、氨基酸或带氨基的二元醇0.5-1份、陶瓷微粉0.5-1份、水100-150份，其制备方法为：向水中加入羟乙基纤维素、氨基酸或带氨基的二元醇和陶瓷微粉，并升温至回流状态保温混合10min，以5℃/min的降温速度降温至55-60℃后加入N-羟甲基丙烯酰胺，在55-60℃保温混合15min，即得处理液。
进一步的，步骤一中将PET树脂于90-100℃下真空干燥30-35h。
进一步的，步骤一中将纳米蒙脱土于60-65℃下真空干燥3-5h。
进一步的，步骤二中所述混合搅拌用高速混合机进行，搅拌速度为800-1000r/min。
进一步的，步骤二中所述造粒时的温度为240-245℃，熔融纺丝时的温度为290-295℃。
一种抗菌阻燃纤维防护服，其利用上述的抗菌阻燃纤维防护服的制备方法。
与现有技术相比，本发明的有益效果是：本发明通过聚酯纤维处理液的使用，将氨基酸或带氨基的二元醇引入到聚酯分子链上，丝氨醇上自带的氨基暴露出来，将其活化后可以与无机抗菌剂进行络合反应；实现了抗菌性的提升。同时，本发明利用氯化聚氯乙烯、三氟甲基磺酸钠和二茂铁的改性处理，在保证纤维原有轻柔性和保暖性的基础上，显著增强其抗菌性和阻燃性，从而提高所制纤维作为防护制品的使用性能。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，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、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。
实施例1
本实施例提供的一种抗菌阻燃纤维防护服材料，制备步骤：
1、按照质量份数计，将500gPET树脂干料、12g纳米蒙脱土干料和4g纳米硅微粉干料混合搅拌均匀后，再加入10g的六(4-醛基苯氧基)环三磷腈，继续混合搅拌均匀，造粒，再经熔融纺丝，制得聚酯纤维；
2、原料处理：取250g聚酯纤维真空干燥；
3、将聚酯纤维浸入处理液中，于60-70℃下浸渍40-60min，排液，将聚酯纤维真空干燥，得后处理聚酯纤维；
4、向上述所得聚酯纤维中加入650g5wt％过氧乙酸溶液，充分混合后浸泡24h，并于微波频率2450MHz、输出功率700W下微波回流处理10min，趁热过滤，所得滤液自然冷却至室温，然后利用20wt％碳酸氢钠溶液调节滤液pH值至7，再加入30g交联聚维酮，混合均匀后于5℃环境中静置1h，即得含有丝状纤维的混合液；
5、向上述所制含有丝状纤维的混合液中加入20g氯化聚氯乙烯，继续回流保温混合30min，然后加入0.5g三氟甲基磺酸钠和0.1g二茂铁，再次回流保温混合15min，并以5℃/min的降温速度降温至40-45℃，所得混合液送入冷冻干燥机中，干燥所得固体经超微粉碎机制成微粉，然后经纳米球磨机研磨成纳米级粉末，即得改性纤维粉；
6、将上述所制改性纤维与水混合后制成混合液，混合液在在压力泵作用下通过喷嘴以束状形式喷出，经凝固后形成粗丝制成薄片。
处理液的制备：向100g水中加入2g羟乙基纤维素、0.5g氨基酸和0.5g陶瓷微粉，并升温至回流状态保温混合10min，以5℃/min的降温速度降温至55-60℃后加入2gN-羟甲基丙烯酰胺，在55-60℃保温混合15min，即得清洗剂。
实施例2
本实施例提供的一种抗菌阻燃纤维防护服材料，制备步骤：
1、按照质量份数计，将600gPET树脂干料、13g纳米蒙脱土干料和6g纳米硅微粉干料混合搅拌均匀后，再加入15g的六(4-醛基苯氧基)环三磷腈，继续混合搅拌均匀，造粒，再经熔融纺丝，制得聚酯纤维；
2、原料处理：取300g聚酯纤维真空干燥；
3、将聚酯纤维浸入处理液中，于60-70℃下浸渍40-60min，排液，将聚酯纤维真空干燥，得后处理聚酯纤维；
4、向上述所得聚酯纤维中加入800g 5wt％过氧乙酸溶液，充分混合后浸泡24h，并于微波频率2450MHz、输出功率700W下微波回流处理10min，趁热过滤，所得滤液自然冷却至室温，然后利用20wt％碳酸氢钠溶液调节滤液pH值至7，再加入30g交联聚维酮，混合均匀后于5℃环境中静置1h，即得含有丝状纤维的混合液；
5、向上述所制含有丝状纤维的混合液中加入20g氯化聚氯乙烯，继续回流保温混合30min，然后加入0.5g三氟甲基磺酸钠和0.1g二茂铁，再次回流保温混合15min，并以5℃/min的降温速度降温至40-45℃，所得混合液送入冷冻干燥机中，干燥所得固体经超微粉碎机制成微粉，然后经纳米球磨机研磨成纳米级粉末，即得改性纤维粉；
6、将上述所制改性纤维与水混合后制成混合液，混合液在在压力泵作用下通过喷嘴以束状形式喷出，经凝固后形成粗丝制成薄片。
处理液的制备：向100g水中加入2g羟乙基纤维素、0.5g带氨基的二元醇和0.5g陶瓷微粉，并升温至回流状态保温混合10min，以5℃/min的降温速度降温至55-60℃后加入2gN-羟甲基丙烯酰胺，在55-60℃保温混合15min，即得清洗剂。
对照例1
1、原料处理：取250g聚酯纤维真空干燥；
2、向上述所得聚酯纤维中加入650g5wt％过氧乙酸溶液，充分混合后浸泡24h，并于微波频率2450MHz、输出功率700W下微波回流处理10min，趁热过滤，所得滤液自然冷却至室温，然后利用20wt％碳酸氢钠溶液调节滤液pH值至7，再加入30g交联聚维酮，混合均匀后于5℃环境中静置1h，即得含有丝状纤维的混合液；
3、向上述所制含有丝状纤维的混合液中加入20g氯化聚氯乙烯，继续回流保温混合30min，然后加入0.5g三氟甲基磺酸钠和0.1g二茂铁，再次回流保温混合15min，并以5℃/min的降温速度降温至40-45℃，所得混合液送入冷冻干燥机中，干燥所得固体经超微粉碎机制成微粉，然后经纳米球磨机研磨成纳米级粉末；
4、将上述所制纤维与水混合后制成混合液，混合液在在压力泵作用下通过喷嘴以束状形式喷出，经凝固后形成粗丝制成薄片。
对照例2
1、原料处理：取300g聚酯纤维真空干燥；
2、将聚酯纤维浸入处理液中，于60-70℃下浸渍40-60min，排液，将聚酯纤维真空干燥，得后处理聚酯纤维；
3、向上述所得聚酯纤维中加入800g 5wt％过氧乙酸溶液，充分混合后浸泡24h，并于微波频率2450MHz、输出功率700W下微波回流处理10min，趁热过滤，所得滤液自然冷却至室温，然后利用20wt％碳酸氢钠溶液调节滤液pH值至7，再加入30g交联聚维酮，混合均匀后于5℃环境中静置1h，即得含有丝状纤维的混合液；
4、向上述所制混合液送入冷冻干燥机中，干燥所得固体经超微粉碎机制成微粉，然后经纳米球磨机研磨成纳米级粉末；
5、将上述所制纤维与水混合后制成混合液，混合液在在压力泵作用下通过喷嘴以束状形式喷出，经凝固后形成粗丝制成薄片。
处理液的制备：向100g水中加入2g羟乙基纤维素、0.5g带氨基的二元醇和0.5g陶瓷微粉，并升温至回流状态保温混合10min，以5℃/min的降温速度降温至55-60℃后加入2gN-羟甲基丙烯酰胺，在55-60℃保温混合15min，即得清洗剂。
对照例3
1、原料处理：取250g聚酯纤维真空干燥；
2、向上述所得聚酯纤维中加入650g5wt％过氧乙酸溶液，充分混合后浸泡24h，并于微波频率2450MHz、输出功率700W下微波回流处理10min，趁热过滤，所得滤液自然冷却至室温，然后利用20wt％碳酸氢钠溶液调节滤液pH值至7，再加入30g交联聚维酮，混合均匀后于5℃环境中静置1h，即得含有丝状纤维的混合液；
3、向上述所制含有丝状纤维的混合液，所得混合液送入冷冻干燥机中，干燥所得固体经超微粉碎机制成微粉，然后经纳米球磨机研磨成纳米级粉末；
4、将上述所制改性纤维与水混合后制成混合液，混合液在在压力泵作用下通过喷嘴以束状形式喷出，经凝固后形成粗丝制成薄片。
以同批原料，分别利用实施例1、实施例2、对照例1、对照例2和对照例3所述方法进行纤维的制备，测定所制纤维的抗菌性和阻燃性，结果如表1、表2所示。
表1为实施例防护材料薄片微生物分析检测结果：
Figure BDA0002560215860000071
表2为实施例和对照例所述纤维制备方法的应用性能对比数据。
项目 实施例1 实施例2 对照例1 对照例2 对照例3
平均抑菌率(％) ＞99 ＞99 90-95 70-75 ＜50
氧指数(％) 37 36 30 26 22
续燃时间(s) ＜1.8 ＜2.0 ＜3.2 ＜3.5 ＜3.9
其中，平均抑菌率是指对白色念珠菌、金黄色葡萄球菌、大肠杆菌的平均抑制率。
经过上述测试和分析，我们可以得出在采用了本发明的制备工艺后，通过聚酯纤维处理液的使用，将氨基酸或带氨基的二元醇引入到聚酯分子链上，丝氨醇上自带的氨基暴露出来，将其活化后可以与一系列无机抗菌剂进行络合反应；实现了抗菌性的提升。同时，本发明利用氯化聚氯乙烯、三氟甲基磺酸钠和二茂铁的改性处理，在保证纤维原有轻柔性和保暖性的基础上，显著增强其抗菌性和阻燃性，从而提高所制纤维作为防护制品的使用性能。
以上内容仅仅是对本发明结构所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离本发明的结构或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (8)

1.一种抗菌阻燃纤维防护服的制备方法，其特征在于,制备方法包括如下步骤：
步骤一，原料处理：将PET树脂、纳米蒙脱土、纳米硅微粉真空干燥；
步骤二，PET树脂改性：按照质量份数计，将50-60份PET树脂干料、1.2-1.3份纳米蒙脱土干料和0.4-0.8份纳米硅微粉干料混合搅拌均匀后，再加入0.1-0.15份的六(4-醛基苯氧基)环三磷腈，继续混合搅拌均匀，造粒，再经熔融纺丝，制得聚酯纤维；
步骤三，聚酯纤维改性：将步骤二所得聚酯纤维浸入处理液中，于60-70℃下浸渍40-60min，排液，将聚酯纤维真空干燥，得后处理聚酯纤维；
步骤四，丝状纤维制备：向上述所得聚酯纤维中加入5wt％过氧乙酸溶液，充分混合后浸泡24h，并于微波频率2450MHz、输出功率700W下微波回流处理10min，趁热过滤，所得滤液自然冷却至室温，然后利用20wt％碳酸氢钠溶液调节滤液pH值至7，再加入交联聚维酮，混合均匀后于0-5℃环境中静置1h，即得含有丝状纤维的混合液；
步骤五，纤维改性处理：向上述所制含有丝状纤维的混合液中加入氯化聚氯乙烯，继续回流保温混合30min，然后加入三氟甲基磺酸钠和二茂铁，再次回流保温混合15min，并以5℃/min的降温速度降温至40-45℃，所得混合液送入冷冻干燥机中，干燥所得固体经超微粉碎机制成微粉，然后经纳米球磨机研磨成纳米级粉末，即得改性纤维粉；
步骤六，纤维成型：将上述所制改性纤维与水混合后制成混合液，混合液在在压力泵作用下通过喷嘴以束状形式喷出，经凝固后形成粗丝制成防护服。
2.根据权利要求1所述的一种抗菌阻燃纤维防护服的制备方法，其特征在于，所述步骤四、步骤五中聚酯纤维、5wt％过氧乙酸溶液、交联聚维酮、氯化聚氯乙烯、三氟甲基磺酸钠和二茂铁的重量比为：25-30:60-80:2-3:2-3:0.5-1:0.01-0.02。
3.根据权利要求1所述的一种抗菌阻燃纤维防护服的制备方法，其特征在于，所述步骤三中处理液由如下重量份数的原料制成：N-羟甲基丙烯酰胺1-2份、羟乙基纤维素1-2份、氨基酸或带氨基的二元醇0.5-1份、陶瓷微粉0.5-1份、水100-150份，其制备方法为：向水中加入羟乙基纤维素、氨基酸或带氨基的二元醇和陶瓷微粉，并升温至回流状态保温混合10min，以5℃/min的降温速度降温至55-60℃后加入N-羟甲基丙烯酰胺，在55-60℃保温混合15min，即得处理液。
4.根据权利要求1所述的一种抗菌阻燃纤维防护服的制备方法，其特征在于，步骤一中将PET树脂于90-100℃下真空干燥30-35h。
5.根据权利要求1所述的一种抗菌阻燃纤维防护服的制备方法，其特征在于，步骤一中将纳米蒙脱土于60-65℃下真空干燥3-5h。
6.根据权利要求1所述的一种抗菌阻燃纤维防护服的制备方法，其特征在于，步骤二中所述混合搅拌用高速混合机进行，搅拌速度为800-1000r/min。
7.根据权利要求1所述的一种抗菌阻燃纤维防护服的制备方法，其特征在于，步骤二中所述造粒时的温度为240-245℃，熔融纺丝时的温度为290-295℃。
8.一种抗菌阻燃纤维防护服，其特征在于，其利用如权利要求1至7任一项所述的抗菌阻燃纤维防护服的制备方法。
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CN113073473A (zh) * 2021-03-30 2021-07-06 江南大学 一种基于催化接枝实现合纤织物阻燃整理的方法
CN115161876A (zh) * 2022-08-15 2022-10-11 吉祥三宝高科纺织有限公司 一种环保纤维絮片的制备工艺

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113073473A (zh) * 2021-03-30 2021-07-06 江南大学 一种基于催化接枝实现合纤织物阻燃整理的方法
CN115161876A (zh) * 2022-08-15 2022-10-11 吉祥三宝高科纺织有限公司 一种环保纤维絮片的制备工艺
CN115161876B (zh) * 2022-08-15 2023-07-18 吉祥三宝高科纺织有限公司 一种环保纤维絮片的制备工艺

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