CN114369948B - 一种抗菌型医用无纺布及其制备工艺 - Google Patents

一种抗菌型医用无纺布及其制备工艺 Download PDF

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CN114369948B
CN114369948B CN202111663209.2A CN202111663209A CN114369948B CN 114369948 B CN114369948 B CN 114369948B CN 202111663209 A CN202111663209 A CN 202111663209A CN 114369948 B CN114369948 B CN 114369948B
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张春节
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Guangdong Baochuang Environmental Protection New Material Products Co ltd
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Abstract

本发明公开一种抗菌型医用无纺布，属于功能化学纤维材料领域，其制备方法是，在纳米二氧化硅粒子掺杂的聚丙烯纤维上，先通过硅烷偶联剂在所述纳米二氧化硅上引入不饱和的烯基基团，再在引发剂作用下与丙烯酸共聚，在表面引入聚丙烯酸修饰位点，再通过卤代三嗪接枝引入氨基和亚胺基，在次氯酸钠的作用下进行卤化后得到兼具氨基、亚胺基和卤胺基的改性无纺布，基于多种类型的胺基协同作用，极大提高无纺布的抗菌性能。

Description

一种抗菌型医用无纺布及其制备工艺
技术领域
本发明涉及功能化学纤维材料领域，具体涉及一种抗菌型医用无纺布及其制备工艺。
背景技术
无纺布又称非织造布，是利用短纤维或长丝进行定向或随机排列，形成纤维网络结构，接着采用机械、热粘或化学方法进行加固得到无编织的布料。无纺布具有防潮、透气、柔韧、质轻、不助燃、容易分解、无毒无刺激性、色彩丰富、价格低廉、可循环再用等特点，因而被广泛用于医疗卫生、家庭服饰等行业。其中在医疗卫生行业中，诸如一次性口罩、防护服、手术衣、隔离衣、实验服、医用帽、医用包等医用耗材均是由无纺布加工制成的。
当前针对抗菌型医用无纺布的抗菌方式多采用溶出型抗菌，抗菌活性物质溶出速度快，容易脱落，造成安全性问题的同时，使用寿命比较短。另一种方法在纤维内加入抗菌成份，为保证抗菌性能，通常需要加入较大的掺量，这会需要牺牲相当一部分的纤维力学性能，因此，如何在增强无纺布纤维的抗菌活性并保持纤维优良特性，是当前抗菌医用无纺布所急需解决的问题。
发明内容
针对上述问题，本发明提供一种抗菌型医用无纺布及其制备工艺。
本发明的目的采用以下技术方案来实现：
一种抗菌型医用无纺布的制备工艺，包括以下步骤：
S1、二氧化硅纳米粒子制备；
S2、将所述二氧化硅纳米粒子与聚丙烯混合后喂入螺杆挤出机，经所述螺杆挤出机熔融挤出形成熔体，所述熔体恒温保温在管道中，经计量泵计量后通过喷丝板喷出形成纤维，所述纤维经过恒温恒压的热风牵伸，在网帘上形成熔喷布；
S3、配制体积比为(9-10)：1的乙醇-水溶液，加入终浓度为0.04g/mL的乙烯基硅烷偶联剂，充分搅拌水解后，将所述熔喷布浸入，浸泡时间0.5-1h，取出并以无水乙醇洗涤，得到第一改性无纺布；
S4、将所述第一改性无纺布浸入到无水乙醇中，加入丙烯酸和偶氮二异丁腈，在氮气保护气氛下加热至50-60℃并保温搅拌反应16-24h，反应完成后取出并以无水乙醇洗涤，得到第二改性无纺布；
S5、将所述第二改性无纺布浸入到乙二胺和2-氯-4,6-二甲氧基-1,3,5-三嗪的混合溶液中，搅拌反应20-24h，反应完成后取出并以无水乙醇洗涤，得到第三改性无纺布；
S6、将所述第三改性无纺布浸入次氯酸钠溶液中，在冰水浴条件下振荡反应4-8h，反应完成后取出并以依次以无水乙醇和去离子水洗涤，干燥后制得所述抗菌型医用无纺布。
优选的，步骤S1中所述二氧化硅纳米粒子采用Stober法制备。
优选的，所述二氧化硅纳米粒子的制备方法具体包括以下步骤：
在无水乙醇中加入所述无水乙醇体积2％的去离子水和体积3％的氨水，充分混合后加入所述无水乙醇体积10％的正硅酸乙酯，在40-50℃下搅拌反应8-12h，反应完成后分离沉淀并以无水乙醇洗涤，去离子水分散后冻干，制得。
优选的，步骤S2中所述二氧化硅纳米粒子与所述聚丙烯熔体的混合质量比例为(1-3)：100。
优选的，步骤S3中所述乙烯基硅烷偶联剂为乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、甲基乙烯基二乙氧基硅烷、乙烯基三异丙氧基硅烷、甲基丙烯酰氧基丙基三甲氧基硅烷或甲基丙烯酰氧基丙基三乙氧基硅烷。
优选的，步骤S4中所述第一改性无纺布与所述丙烯酸、所述偶氮二异丁腈的质量比例为100：(2-6)：(0.05-0.1)。
优选的，步骤S5中所述第二改性无纺布与所述乙二胺、所述2-氯-4,6-二甲氧基-1,3,5-三嗪的质量比例为100：(15-25)：(2-5)。
优选的，步骤S6中所述次氯酸钠溶液的活性氯浓度为10％。
本发明的另一目的在于提供一种抗菌型医用无纺布，所述无纺布由前述制备方法制备得到。
本发明的有益效果为：
本发明通过在聚丙烯纤维内掺杂少量纳米二氧化硅，在最大保留纤维性能的同时，通过在所述纳米二氧化硅上进行改性接枝，赋予纤维良好的抗菌性能，具体的，先通过硅烷偶联剂在所述纳米二氧化硅上引入不饱和的烯基基团，再在引发剂作用下与丙烯酸共聚，在表面引入聚丙烯酸修饰位点，再通过卤代三嗪接枝引入氨基和亚胺基，在次氯酸钠的作用下进行卤化后得到兼具氨基、亚胺基和卤胺基的改性无纺布，基于多种类型的胺基协同作用，极大提高无纺布的抗菌性能。
具体实施方式
结合以下实施例对本发明作进一步描述。
实施例1
本实施例涉及一种抗菌型医用无纺布，其制备工艺包括以下步骤：
S1、二氧化硅纳米粒子制备；
所述二氧化硅纳米粒子采用Stober法制备，具体包括以下步骤：
在无水乙醇中加入所述无水乙醇体积2％的去离子水和体积3％的氨水，充分混合后加入所述无水乙醇体积10％的正硅酸乙酯，在40-50℃下搅拌反应8-12h，反应完成后分离沉淀并以无水乙醇洗涤，去离子水分散后冻干，制得；
S2、将所述二氧化硅纳米粒子与聚丙烯混合后喂入螺杆挤出机，经所述螺杆挤出机熔融挤出形成熔体，所述熔体恒温保温在管道中，经计量泵计量后通过喷丝板喷出形成纤维，所述纤维经过恒温恒压的热风牵伸，在网帘上形成熔喷布；
所述二氧化硅纳米粒子与所述聚丙烯熔体的混合质量比例为1：50；
S3、配制体积比为(9-10)：1的乙醇-水溶液，加入终浓度为0.04g/mL的KH570，充分搅拌水解后，将所述熔喷布浸入，浸泡时间0.5-1h，取出并以无水乙醇洗涤，得到第一改性无纺布；
S4、将所述第一改性无纺布浸入到无水乙醇中，加入丙烯酸和偶氮二异丁腈，在氮气保护气氛下加热至50-60℃并保温搅拌反应16-24h，反应完成后取出并以无水乙醇洗涤，得到第二改性无纺布；
所述第一改性无纺布与所述丙烯酸、所述偶氮二异丁腈的质量比例为100：5：0.08；
S5、将所述第二改性无纺布浸入到乙二胺和2-氯-4,6-二甲氧基-1,3,5-三嗪的混合溶液中，搅拌反应20-24h，反应完成后取出并以无水乙醇洗涤，得到第三改性无纺布；
所述第二改性无纺布与所述乙二胺、所述2-氯-4,6-二甲氧基-1,3,5-三嗪的质量比例为100：18：4；
S6、将所述第三改性无纺布浸入活性氯浓度为10％的次氯酸钠溶液中，在冰水浴条件下振荡反应4-8h，反应完成后取出并以依次以无水乙醇和去离子水洗涤，干燥后制得所述抗菌型医用无纺布。
实施例2
本实施例涉及一种抗菌型医用无纺布，其制备工艺同实施例1，区别在于，所述二氧化硅纳米粒子与所述聚丙烯熔体的混合质量比例为3：100。
对比例
一种抗菌无纺布，其制备方法同实施例1，区别在于，所述第三改性无纺布。
以未改性的熔喷布为对照，对实施例1、2和对比例制得的抗菌无纺布的抑菌性能进行测试；
以金黄色葡萄球菌ATCC6538和大肠杆菌ATCC25922为测试菌种，菌种培养至OD600＝0.3，无纺布试样灭菌后放置与24孔培养板中，每个孔中接入等量菌液，光照下培养24h，无菌缓冲液漂洗表面，再超声震荡将黏附的细菌震落，测量所得悬液的OD600值，结果如下：
OD600 对照 实施例1 实施例2 对比例
S.aureus 0.99 0.30 0.32 0.41
E.coli 0.71 0.22 0.24 0.30
最后应当说明的是，以上实施例仅用以说明本发明的技术方案，而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细地说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (2)

1.一种抗菌型医用无纺布的制备工艺，其特征在于，包括以下步骤：
S1、二氧化硅纳米粒子制备；
S2、将所述二氧化硅纳米粒子与聚丙烯混合后喂入螺杆挤出机，经所述螺杆挤出机熔融挤出形成熔体，所述熔体恒温保温在管道中，经计量泵计量后通过喷丝板喷出形成纤维，所述纤维经过恒温恒压的热风牵伸，在网帘上形成熔喷布；
S3、配制体积比为(9-10)：1的乙醇-水溶液，加入终浓度为0.04g/mL的乙烯基硅烷偶联剂，充分搅拌水解后，将所述熔喷布浸入，浸泡时间0.5-1h，取出并以无水乙醇洗涤，得到第一改性无纺布；
S4、将所述第一改性无纺布浸入到无水乙醇中，加入丙烯酸和偶氮二异丁腈，在氮气保护气氛下加热至50-60℃并保温搅拌反应16-24h，反应完成后取出并以无水乙醇洗涤，得到第二改性无纺布；
S5、将所述第二改性无纺布浸入到乙二胺和2-氯-4,6-二甲氧基-1,3,5-三嗪的混合溶液中，搅拌反应20-24h，反应完成后取出并以无水乙醇洗涤，得到第三改性无纺布；
S6、将所述第三改性无纺布浸入次氯酸钠溶液中，在冰水浴条件下振荡反应4-8h，反应完成后取出并以依次以无水乙醇和去离子水洗涤，干燥后制得所述抗菌型医用无纺布；
所述二氧化硅纳米粒子的制备方法具体包括以下步骤：
在无水乙醇中加入所述无水乙醇体积2％的去离子水和体积3％的氨水，充分混合后加入所述无水乙醇体积10％的正硅酸乙酯，在40-50℃下搅拌反应8-12h，反应完成后分离沉淀并以无水乙醇洗涤，去离子水分散后冻干，制得；
步骤S2中所述二氧化硅纳米粒子与所述聚丙烯的混合质量比例为(1-3)：100；
步骤S3中所述乙烯基硅烷偶联剂为乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、甲基乙烯基二乙氧基硅烷、乙烯基三异丙氧基硅烷、甲基丙烯酰氧基丙基三甲氧基硅烷或甲基丙烯酰氧基丙基三乙氧基硅烷；
步骤S4中所述第一改性无纺布与所述丙烯酸、所述偶氮二异丁腈的质量比例为100：(2-6)：(0.05-0.1)；
步骤S5中所述第二改性无纺布与所述乙二胺、所述2-氯-4,6-二甲氧基-1,3,5-三嗪的质量比例为100：(15-25)：(2-5)；
步骤S6中所述次氯酸钠溶液的活性氯浓度为10％。
2.根据权利要求1所述制备工艺制得的抗菌型医用无纺布。
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