CN111058283A - 一种抗菌腈纶纤维的制备方法及其应用 - Google Patents

一种抗菌腈纶纤维的制备方法及其应用 Download PDF

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CN111058283A
CN111058283A CN201911202180.0A CN201911202180A CN111058283A CN 111058283 A CN111058283 A CN 111058283A CN 201911202180 A CN201911202180 A CN 201911202180A CN 111058283 A CN111058283 A CN 111058283A
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antibacterial
acrylic fiber
fiber
towel
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刘彦洋
陈兆文
孙世操
黄国庆
王力
刘大鑫
范海明
白亚楠
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PURIFICATION EQUIPMENT RESEARCH INSTITUTE OF CSIC
718th Research Institute of CSIC
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Abstract

本发明涉及一种抗菌腈纶纤维的制备方法及其应用，属于日用纺织品领域。将腈纶纤维放入含催化剂的有机胺溶液中反应得到网状纤维；然后放入氢氧化钠溶液中反应结束后取出洗涤，得到羧酸钠型腈纶纤维；然后放入含抗菌离子的溶液中反应结束后取出洗涤、晾干，得到一种抗菌除臭腈纶纤维。所述通过催化交联、水解及离子交换过程对腈纶纤维进行化学改性，使得纤维基体上同时存在抗菌基团及亲水基团。所述抗菌腈纶纤维与常规纤维的混纺、整经织布、染整等制备得到一种抗菌除臭毛巾，在不影响毛巾的常规性能的前提下，使得毛巾具有抗菌性能优异、耐洗涤且吸水性强的特点。

Description

一种抗菌腈纶纤维的制备方法及其应用
技术领域
本发明涉及一种抗菌腈纶纤维的制备方法及其应用，属于日用纺织品领域。
背景技术
毛巾是人们使用频次最高的日用品之一，但是在一些特定的工作场所，如出海捕鱼的渔船、作战或演习的舰船等，由于淡水资源有限且出海作业时间较长，渔民及战士无法及时洗涤毛巾，导致毛巾极易滋生细菌，产生难闻的气味并影响人们的身体健康；在炎热的夏季，高温高湿的条件下此类情况更易发生，因此需开发一款具有抗菌除臭功能的毛巾。
目前市场上的抗菌系列毛巾有两大类，一种是采用后整理剂的方式对毛巾进行抗菌处理，这种方式不耐洗涤，多次洗涤使用后，抗菌效果就会完全丧失；另一种是采用将天然抗菌纤维(竹纤维、麻)或人工改性的抗菌纤维(镀银纤维、镀铜纤维、银螯合抗菌纤维等)混纺成纱线后进而纺织得到抗菌毛巾。其中天然抗菌纤维由于自身抗菌性能很差，导致其在混纺纱线中的占比很高，从而严重影响了毛巾的手感；采用现有人工改性的抗菌纤维纺织成的毛巾，如镀银纤维有很强的金属质感，其柔软性、吸水性及回潮率都无法达到毛巾的正常要求。
发明内容
有鉴于此，本发明的目的在于提供一种抗菌腈纶纤维的制备方法及其应用，所述方法是通过人工改性制备得到，该抗菌腈纶纤维表面同时存在抗菌基团及羧酸钠基团，其中抗菌基团以共价键方式连接在纤维基体上，不易脱落；羧酸钠基团具有很强的吸水功能。将所述纤维用于毛巾的制备，纤维的以上特性从而决定了其经过混纺纱线并纺织的毛巾具有抗菌性能好、耐洗涤、吸水性及柔软度高的特性。
为实现上述目的，本发明采取以下技术方案：
1.一种抗菌腈纶纤维的制备方法，所述方法步骤包括：
(1)将腈纶纤维放入含催化剂的有机胺溶液中，80℃-120℃下反应1h-5h，反应结束后取出洗涤；得到网状纤维；其中，所述有机胺的重均分子量大于等于600，所述有机胺为聚乙烯胺、聚乙烯亚胺、多乙烯多胺、氨基酸和多乙烯多酰胺中的一种以上；所述催化剂为四甲基胍、吡啶、二氮杂二环或二氮杂二环的衍生物；
优选的，步骤(1)中所述腈纶纤维为干法纺丝制备得到的腈纶纤维经抽提处理后得到的，抽提时有机溶剂为丙酮、二氯甲烷和二甲基甲酰胺中的一种以上。
优选的，步骤(1)中反应温度为100℃-110℃。
优选的，步骤(1)中所述含催化剂的有机胺溶液中，催化剂的质量分数小于等于10％；有机胺的质量分数小于等于5％。
优选的，步骤(1)中所述有机胺的重均分子量为600-10000。
优选的，步骤(1)中，所述催化剂为二氮杂二环。
(2)将所述网状纤维放入氢氧化钠溶液中，80℃-120℃下反应1h-4h，反应结束后取出洗涤，得到羧酸钠型腈纶纤维；
优选的，步骤(2)氢氧化钠溶液中氢氧化钠的质量分数小于等于10％。
(3)将所述羧酸钠型腈纶纤维放入含抗菌离子的溶液中，于20℃-50℃下震荡反应0.5h-5h，反应结束后取出洗涤、晾干，得到一种抗菌除臭腈纶纤维；其中，所述抗菌离子为银离子和/或铜离子；固液比为1:20-1:50。
优选的，步骤(3)中所述含抗菌离子的溶液为硝酸银溶液或硝酸铜与硝酸银的混合溶液；同时调节混合溶液的pH值为4-6，硝酸银的质量分数为90％-100％，硝酸铜的质量分数为0-10％，且硝酸银浓度小于等于0.1mol/L。
优选的，步骤(3)中所述含抗菌离子的溶液为硝酸铜与硝酸银的混合溶液。
一种抗菌腈纶纤维的应用，所述抗菌腈纶用于纺织制备抗菌除臭毛巾，所述纺织制备方法步骤如下：
(1)混纺纱线的制备：将所述抗菌腈纶纤维与常规纤维在开松机上开松后并混毛均匀，然后疏机上梳理制成混合绒条，混合绒条抽长拉细，反复并条达到设定粗细，然后经过牵伸拉长、加捻及喂入粗纱条得到混纺纱线；其中，所述常规纤维为天然纤维或化学纤维，包括棉、麻、竹纤维、黏胶纤维、涤纶纤维和长绒棉等，优选长绒棉；所述混纺纱线中抗菌腈纶纤维含量为0.5-45％；所述混纺纱线支数为10支-50支。
(2)毛巾胚布的制备：将所述混纺纱线作为地纱或毛圈纱进行织造，得到毛巾胚布。
(3)所述毛巾胚布经过染整、烘干、裁剪缝纫后得到一种抗菌除臭毛巾。染整过程中所使用的染料优选活性染料及还原染料。
有益效果
本发明提供了一种抗菌腈纶纤维的制备方法，即通过催化交联、水解及离子交换过程对腈纶纤维进行化学改性，使得纤维基体上同时存在抗菌基团及亲水基团。
通过催化交联的过程，在催化剂及大分子交联剂的作用下，能够有效保证纤维基体的机械强度，保证了纤维的进一步水解及改性需求。
通过抗菌腈纶纤维与常规纤维的混纺、整经织布、染整等工艺路线成功开发一款抗菌除臭毛巾，在不影响毛巾的常规性能的前提下，使得毛巾具有抗菌性能优异、耐洗涤且吸水性强的特点。
具体实施方式
下面结合具体实施例对本发明作出进一步详细说明。
实施例1
(1)抗菌腈纶纤维的制备：将干法纺丝技术制备的腈纶纤维经过丙酮抽提处理后得到预处理后的腈纶纤维，将20L质量分数为1％聚乙烯亚胺(重均分子量为600)与质量分数为5％二氮杂二环的混合溶液加入到反应釜中，然后将预处理后的腈纶纤维1kg加入到反应釜中，于120℃下反应2h，取出纤维洗涤后再放入50L质量分数为1％的氢氧化钠溶液中，120℃下反应3h，取出洗涤即可制得羧酸钠型腈纶纤维。将该羧酸钠型腈纶纤维放入浓度为0.05mol/L的硝酸银溶液中，所述混合溶液的pH值为4，于35℃下震荡反应2h，取出洗涤、晾干即可制得一种抗菌腈纶纤维，所述抗菌腈纶纤维上的银含量占比为5％，经检测该抗菌腈纶纤维的机械强度与原纤维相比损失为3.6％，且纤维在30s内的吸水率达到了400％。
(2)混纺纱线的制备：将步骤1中的抗菌腈纶纤维与长绒棉在开松机上开松并混毛均匀，后通过疏机梳理制成混合绒条，再将梳理后的混合条子抽长拉细，反复并条达到预定的粗细，而后经过牵伸拉长、加捻及喂入粗纱条得到32支的混纺纱线。该混纺纱线中抗菌腈纶纤维含量为2％。
(3)毛巾胚布的制备：将上述混纺纱线作为地纱，以长绒棉作为毛圈纱进行织造即可制得毛巾胚布。
(4)毛巾的制备：上述毛巾胚布经过染整、烘干、裁剪缝纫常规工艺及工序即可制得一种抗菌除臭毛巾。
经GB/T 22864-2009《毛巾》及FZT 62015-2009《抗菌毛巾》标准检测该毛巾的在水洗50次后对金黄色葡萄球菌的抑菌率≥95％，对大肠杆菌的抑菌率≥85％。
实施例2
(1)抗菌腈纶纤维的制备：将干法纺丝技术制备的腈纶纤维经过二甲基甲酰胺抽提处理后得到预处理后的腈纶纤维，将30L质量分数为3％聚乙烯胺(重均分子量为2000)与质量分数为10％四甲基胍的混合溶液加入到反应釜中，然后将市售腈纶纤维1kg加入到反应液中，于100℃下反应1h，取出纤维洗涤后再放入50L质量分数为10％的氢氧化钠溶液中，100℃下反应1h，取出洗涤即可制得羧酸钠型腈纶纤维。将该羧酸钠型腈纶纤维放入硝酸银浓度为0.01mol/L、硝酸铜的浓度为0.5mmol/L的混合溶液中，混合溶液的pH值为5，于20℃下震荡反应0.5h，取出洗涤、晾干即可制得一种抗菌腈纶纤维，该抗菌腈纶纤维上的银含量占比为0.5％，经检测所述抗菌腈纶纤维的机械强度与原纤维相比损失为2.4％，且纤维在30s内的吸水率达到了300％。
(2)混纺纱线的制备：将步骤1中的抗菌腈纶纤维与竹纤维在开松机上开松并混毛均匀，后通过疏机梳理制成混合绒条，再将梳理后的混合条子抽长拉细，反复并条达到预定的粗细，而后经过牵伸拉长、加捻及喂入粗纱条得到50支的混纺纱线。该混纺纱线中抗菌腈纶纤维含量为45％。
(3)毛巾胚布的制备：将上述混纺纱线作为毛圈纱，以长绒棉作为地纱进行织造即可制得毛巾胚布。
(4)毛巾的制备：上述毛巾胚布经过染整、烘干、裁剪缝纫常规工艺及工序即可制得一种抗菌除臭毛巾。
经GB/T 22864-2009《毛巾》及FZT 62015-2009《抗菌毛巾》检测该毛巾在水洗50次后对金黄色葡萄球菌的抑菌率≥95％，对大肠杆菌的抑菌率≥85％。
实施例3
(1)抗菌腈纶纤维的制备：将干法纺丝技术制备的腈纶纤维经过二氯甲烷抽提处理后得到预处理后的腈纶纤维，将50L质量分数为5％多乙烯多胺(重均分子量为1000)与质量分数为10％吡啶的混合溶液加入到反应釜中，然后将市售腈纶纤维1kg加入到反应液中，于100℃下反应5h，取出纤维洗涤后再放入50L质量分数为10％的氢氧化钠溶液中，100℃下反应4h，取出洗涤即可制得羧酸钠型腈纶纤维。将该羧酸钠型腈纶纤维放入浓度为硝酸银浓度为0.1mol/L、硝酸铜的浓度为0.01mol/L的混合溶液中，混合溶液的pH值为6，于50℃下震荡反应5h，取出洗涤、晾干即可制得一种抗菌腈纶纤维，该抗菌腈纶纤维上的银含量占比为20％，经检测所述抗菌腈纶纤维的机械强度与原纤维相比损失为4.2％，且纤维在30s内的吸水率达到了500％。
(2)混纺纱线的制备：将步骤(1)中的抗菌腈纶纤维与竹纤维在开松机上开松并混毛均匀，后通过疏机梳理制成混合绒条，再将梳理后的混合条子抽长拉细，反复并条达到预定的粗细，而后经过牵伸拉长、加捻及喂入粗纱条得到10支的混纺纱线。该混纺纱线中抗菌腈纶纤维含量为0.5％。
(3)毛巾胚布的制备：将上述混纺纱线作为地纱和毛圈纱进行织造即可制得毛巾胚布。
(4)毛巾的制备：上述毛巾胚布经过染整、烘干、裁剪缝纫常规工艺及工序即可制得一种抗菌除臭毛巾。
经GB/T 22864-2009《毛巾》及FZT 62015-2009《抗菌毛巾》检测该毛巾的在水洗50次后对金黄色葡萄球菌的抑菌率≥95％，对大肠杆菌的抑菌率≥85％。
综上所述，发明包括但不限于以上实施例，凡是在本发明的精神和原则之下进行的任何等同替换或局部改进，都将视为在本发明的保护范围之内。

Claims (10)

1.一种抗菌腈纶纤维的制备方法，其特征在于：所述方法步骤包括：
(1)将腈纶纤维放入含催化剂的有机胺溶液中，80℃-120℃下反应1h-5h，反应结束后取出洗涤；得到网状纤维；其中，所述有机胺的重均分子量大于等于600，所述有机胺为聚乙烯胺、聚乙烯亚胺、多乙烯多胺、氨基酸和多乙烯多酰胺中的一种以上；所述催化剂为四甲基胍、吡啶、二氮杂二环或二氮杂二环的衍生物；
(2)将所述网状纤维放入氢氧化钠溶液中，80℃-120℃下反应1h-4h，反应结束后取出洗涤，得到羧酸钠型腈纶纤维；
(3)将所述羧酸钠型腈纶纤维放入含抗菌离子的溶液中，于20℃-50℃下震荡反应0.5h-5h，同时调节溶液的pH值为5-7，反应结束后取出洗涤、晾干，得到一种抗菌除臭腈纶纤维；其中，所述抗菌离子为银离子和/或铜离子；固液比为1:20-1:50。
2.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(1)中所述腈纶纤维为干法纺丝制备得到的腈纶纤维经抽提处理后得到的，抽提时有机溶剂为丙酮、二氯甲烷和二甲基甲酰胺中的一种以上。
3.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(1)中反应温度为100℃-110℃。
4.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(1)中所述含催化剂的有机胺溶液中，催化剂的质量分数小于等于10％；有机胺的质量分数小于等于5％。
5.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(1)中所述有机胺的重均分子量为600-10000。
6.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(1)中，所述催化剂为二氮杂二环。
7.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(2)氢氧化钠溶液中氢氧化钠的质量分数小于等于10％。
8.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(3)中所述含抗菌离子的溶液为硝酸银溶液或硝酸铜与硝酸银的混合溶液；硝酸银的质量分数为90％-100％，硝酸铜的质量分数为0-10％，且硝酸银浓度小于等于0.1mol/L。
9.如权利要求1所述的一种抗菌腈纶纤维的制备方法，其特征在于：步骤(3)中所述含抗菌离子的溶液为硝酸铜与硝酸银的混合溶液。
10.一种如权利要求1～9任意一项所述的抗菌腈纶纤维的应用，其特征在于：所述抗菌腈纶用于纺织制备抗菌除臭毛巾，所述纺织制备方法步骤如下：
(1)将所述抗菌腈纶纤维与常规纤维在开松机上开松后并混毛均匀，然后疏机上梳理制成混合绒条，混合绒条抽长拉细，反复并条达到设定粗细，然后经过牵伸拉长、加捻及喂入粗纱条得到混纺纱线；其中，所述常规纤维为天然纤维或化学纤维；所述混纺纱线中抗菌腈纶纤维含量为0.5-45％；所述混纺纱线支数为10支-50支；
(2)将所述混纺纱线作为地纱或毛圈纱进行织造，得到毛巾胚布。
(3)所述毛巾胚布经过染整、烘干、裁剪缝纫后得到一种抗菌除臭毛巾。
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