CN110747647A - 一种抗菌碳纤维上浆剂乳液及其制备方法与应用 - Google Patents
一种抗菌碳纤维上浆剂乳液及其制备方法与应用 Download PDFInfo
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Abstract
本发明涉及一种抗菌碳纤维上浆剂乳液及其制备方法与应用,其特征是制备了AgO纳米粒子水分散体,将其掺杂在含有机抗菌剂铵根阳离子的水性聚氨酯乳液中,得到抗菌碳纤维上浆剂乳液;将聚丙烯腈基碳纤维浸入本发明制备的上浆剂乳液,制得抗菌聚丙烯腈基碳纤维。本发明制备的抗菌碳纤维对金黄色葡萄球菌、大肠杆菌和白色念珠菌均具有很强的抗菌性能,抑菌率分别达到96%、96%和94%以上。本发明中抗菌碳纤维上浆剂的生产工艺简单,生产过程对环境污染小,原料低廉易得;抗菌碳纤维上浆剂对碳纤维的上浆整理工艺简单,易于操作。
Description
技术领域
本发明属于上浆剂技术领域,具体涉及一种抗菌碳纤维上浆剂乳液及其制备方法与应用。
背景技术
碳纤维是指碳含量在90%以上的纤维状碳材料,其可由聚丙烯腈、纤维素、木质素和沥青等前驱体经一系列纺丝、氧化、热处理和上浆等工艺得到,其直径为5~10μm。碳纤维于20世纪50年代被发明,其具有高强度、高模量、质量轻便等优点,其在航空航天、节能与新能源汽车、风电、军事工业等领域被广泛应用。
碳纤维上浆剂是碳纤维制备工艺中极为重要的助剂,其可以改善碳纤维和基体树脂两相界面的强度,同时,其对碳纤维的集束性、直挺度、耐磨性、幅宽及均匀性等物理工艺性能有重要影响,是碳纤维工业领域极为重要的一种基础配套材料。碳纤维的上浆整理是制备碳纤维的重要步骤,上浆剂的种类繁多,其为碳纤维的性能改性创造了条件。
碳纤维用于一些特殊领域时,如:医用材料、航空航天和防弹衣等领域时,希望碳纤维具有良好的抗菌性,因此,制备出具有抗菌性能的碳纤维是亟待解决的难题,一些学者对此展开了研究。中国专利申请号201711006207.X公布了一种天然抗菌碳纤维及制备方法,该专利将中药提取液与纺丝液混合,然后通过喷丝和碳化制得碳纤维;显然,该方法的碳化过程会破坏中药提取液的结构和性能。中国专利申请号201611073863.7公布了一种多元离子抗菌碳纤维滤芯,该专利也是将多元离子抗菌材料混入母料聚丙烯腈共聚物,当碳化温度达到1700℃,多元离子抗菌材料的稳定性可能会受到影响。为了减少碳化高温时抗菌剂的分解对碳纤维的影响,需寻求新的方法实现碳纤维良好的抗菌性。
发明内容
本发明的目的是克服以往技术的不足,提供一种抗菌碳纤维上浆剂乳液及其制备方法与应用。本发明制备的上浆剂乳液属于水性聚氨酯乳液类型,其与碳纤维的结合力较强,该上浆剂同时含有机类和无机类抗菌剂,且有机类和无机类抗菌剂与碳纤维以化学键形式结合,结合力很强,其耐久性很好。
本发明的目的在于提供一种抗菌碳纤维上浆剂乳液,其主要成分包括水性聚氨酯乳液和AgO纳米粒子,其中,水性聚氨酯中含有机抗菌剂铵根阳离子,纳米级AgO粒子是良好的无机抗菌剂。
本发明的另一个目的在于提供上述所述一种抗菌碳纤维上浆剂乳液的制备方法,所述方法包含如下步骤:
(1)分散剂的制备:将一定质量的丙烯酸和聚合度为45的烯丙基聚氧乙烯醚单体同时溶解于适量的去离子水中配置为单体溶液,备用,优选地,所述丙烯酸与烯丙基聚氧乙烯醚的摩尔比为1∶0.3~0.5;然后在搅拌条件下,控制温度为79~81℃,将配置好的单体与过硫酸铵引发剂分别滴加到装有一定量去离子水的四口烧瓶中,优选地,所述过硫酸铵的质量占单体总质量的0.1~0.5%,滴加时间控制在2~3h,滴加完毕后,保温3~4h;最后冷却,即制得分散剂。
(2)纳米氧化物粒子水分散体的制备:将一定质量的AgO粉体研磨成纳米级别,粒径范围为100~300纳米;将步骤(1)制备的分散剂用水稀释至质量分数为1~2%,将纳米氧化物粒子溶于分散剂溶液,均匀搅拌制备为纳米氧化物粒子水分散体,优选地,所述纳米氧化物粒子与分散剂溶液的料液比为1g∶(30~50)mL;此纳米氧化物粒子水分散体放置一周,不发生分层或沉淀现象即可。
(3)在反应釜中加入聚乙二醇和二羟甲基丙酸,在100~120℃下真空脱水1~2h,缓慢降温至50~60℃,滴加甲苯异氰酸酯、丁酮和催化剂二丁基锡二月桂酸,升温至80~90℃,反应3~4h;优选地,所述聚乙二醇的分子量为400,聚乙二醇、二羟甲基丙酸、甲苯异氰酸酯的摩尔比为1∶1~2∶3~5,二丁基锡二月桂酸用量占单体总量的0.01~0.1%,丁酮(mL)与单体总量(g)的体积质量比为1∶0.3~0.5;然后降温至40~45℃,于1~1.5h内分多次加入扩链剂三羟甲基丙烷,优选地,所述三羟甲基丙烷的用量与二羟甲基丙酸的摩尔比为1∶3~5;升温至60~80℃,保温反应1~2h;自然冷却,即可。
(4)将步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液混合,滴加三乙胺和水溶液至混合溶液中和,优选地,所述步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液的体积比为:1∶3~5;将混合液放入乳化泵进行反向乳化,乳化泵的剪切速率为6000~15000r/min;乳化结束后,采用减压低温蒸馏法脱除丁酮,得到水性聚氨酯乳液。
本发明的另一目的在于提供一种抗菌碳纤维上浆剂乳液的应用,具体方案为:
步骤一:将聚丙烯腈基碳纤维置于臭氧环境中,设置环境温度为100~150℃,放置时间为2~3h;
步骤二:将聚丙烯腈基碳纤维浸入本发明制备的抗菌剂乳液,乳液的固含量为1~5%,浴比:1∶20~30,浸入时间为2~3h,浸入温度为60~80℃;
步骤三:将步骤二处理的纤维取出,自然晾干,得到抗菌聚丙烯腈基碳纤维。
本发明具有如下显著特点:
(1)本发明制备的抗菌碳纤维上浆剂乳液主要成分为水性聚氨酯和AgO纳米粒子,本发明将水性聚氨酯和AgO纳米粒子分散体采用乳化工艺将其结合在一起;水性聚氨酯中含有机抗菌剂铵根阳离子,纳米级AgO粒子是良好的无机抗菌剂。
(2)本发明制备的抗菌碳纤维对金黄色葡萄球菌、大肠杆菌和白色念珠菌均具有很强的抗菌性能,抑菌率分别达到96%、96%和94%以上;上浆后的碳纤维经过10次洗涤后,其仍对金黄色葡萄球菌、大肠杆菌和白色念珠菌表现较强的抗菌性能,抑菌率分别达到94%、92%和91%以上。
(3)本发明中抗菌碳纤维上浆剂的生产工艺简单,生产过程对环境污染小,原料低廉易得,具有较强的推广价值;抗菌碳纤维上浆剂对碳纤维的上浆整理工艺简单,易于操作。
具体实施方式
以下所述实施例详细说明了本发明。
实施例1
在本实施例中,一种抗菌碳纤维上浆剂乳液的制备方法,包括如下步骤:
(1)分散剂的制备:将一定质量的丙烯酸和聚合度为45的烯丙基聚氧乙烯醚单体同时溶解于适量的去离子水中配置为单体溶液,备用,优选地,所述丙烯酸与烯丙基聚氧乙烯醚的摩尔比为1∶0.4;然后在搅拌条件下,控制温度为79~81℃,将配置好的单体与过硫酸铵引发剂分别滴加到装有一定量去离子水的四口烧瓶中,优选地,所述过硫酸铵的质量占单体总质量的0.3%,滴加时间控制在2.5h,滴加完毕后,保温3.5h;最后冷却,即制得分散剂。
(2)纳米氧化物粒子水分散体的制备:将一定质量的AgO粉体研磨成纳米级别,粒径范围为120~200纳米;将步骤(1)制备的分散剂用水稀释至质量分数为1.5%,将纳米氧化物粒子溶于分散剂溶液,均匀搅拌制备为纳米氧化物粒子水分散体,优选地,所述纳米氧化物粒子与分散剂溶液的料液比为1∶40;此纳米氧化物粒子水分散体放置一周,不发生分层或沉淀现象即可。
(3)在反应釜中加入聚乙二醇和二羟甲基丙酸,在110℃下真空脱水1.5h,缓慢降温至55℃,滴加甲苯异氰酸酯、丁酮和催化剂二丁基锡二月桂酸,升温至85℃,反应3.5h;优选地,所述聚乙二醇的分子量为400,聚乙二醇、二羟甲基丙酸、甲苯异氰酸酯的摩尔比为1∶1.5∶4,二丁基锡二月桂酸用量占单体总量的0.05%,丁酮(mL)与单体总量(g)的体积质量比为1∶0.4;然后降温至43℃,于1.2h内分多次加入扩链剂三羟甲基丙烷,优选地,所述三羟甲基丙烷的用量与二羟甲基丙酸的摩尔比为1∶4;升温至65℃,保温反应1.5h;自然冷却,即可。
(4)将步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液混合,滴加三乙胺和水溶液至混合溶液中和,优选地,所述步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液的体积比为:1∶4;将混合液放入乳化泵进行反向乳化,乳化泵的剪切速率为9000r/min;乳化结束后,采用减压低温蒸馏法脱除丁酮,得到水性聚氨酯乳液。
本发明的另一目的在于提供一种抗菌碳纤维上浆剂乳液的应用,具体方案为:
步骤一:将聚丙烯腈基碳纤维置于臭氧环境中,设置环境温度为120℃,放置时间为2.5h;
步骤二:将聚丙烯腈基碳纤维浸入本发明制备的抗菌剂乳液,乳液的固含量为3%,浴比:1∶25,浸入时间为2.5h,浸入温度为70℃;
步骤三:将步骤二处理的纤维取出,自然晾干,得到抗菌聚丙烯腈基碳纤维a。
实施例2
在本实施例中,一种抗菌碳纤维上浆剂乳液的制备方法,包括如下步骤:
(1)分散剂的制备:将一定质量的丙烯酸和聚合度为45的烯丙基聚氧乙烯醚单体同时溶解于适量的去离子水中配置为单体溶液,备用,优选地,所述丙烯酸与烯丙基聚氧乙烯醚的摩尔比为1∶0.3;然后在搅拌条件下,控制温度为79~81℃,将配置好的单体与过硫酸铵引发剂分别滴加到装有一定量去离子水的四口烧瓶中,优选地,所述过硫酸铵的质量占单体总质量的0.1%,滴加时间控制在2h,滴加完毕后,保温3h;最后冷却,即制得分散剂。
(2)纳米氧化物粒子水分散体的制备:将一定质量的AgO粉体研磨成纳米级别,粒径范围为100~200纳米;将步骤(1)制备的分散剂用水稀释至质量分数为1%,将纳米氧化物粒子溶于分散剂溶液,均匀搅拌制备为纳米氧化物粒子水分散体,优选地,所述纳米氧化物粒子与分散剂溶液的料液比为1∶30;此纳米氧化物粒子水分散体放置一周,不发生分层或沉淀现象即可。
(3)在反应釜中加入聚乙二醇和二羟甲基丙酸,在100℃下真空脱水1h,缓慢降温至50℃,滴加甲苯异氰酸酯、丁酮和催化剂二丁基锡二月桂酸,升温至80℃,反应3h;优选地,所述聚乙二醇的分子量为400,聚乙二醇、二羟甲基丙酸、甲苯异氰酸酯的摩尔比为1∶1∶3,二丁基锡二月桂酸用量占单体总量的0.01%,丁酮(mL)与单体总量(g)的体积质量比为1∶0.3;然后降温至40℃,于1h内分多次加入扩链剂三羟甲基丙烷,优选地,所述三羟甲基丙烷的用量与二羟甲基丙酸的摩尔比为1∶3;升温至60℃,保温反应1h;自然冷却,即可。
(4)将步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液混合,滴加三乙胺和水溶液至混合溶液中和,优选地,所述步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液的体积比为:1∶3;将混合液放入乳化泵进行反向乳化,乳化泵的剪切速率为6000r/min;乳化结束后,采用减压低温蒸馏法脱除丁酮,得到水性聚氨酯乳液。
本发明的另一目的在于提供一种抗菌碳纤维上浆剂乳液的应用,具体方案为:
步骤一:将聚丙烯腈基碳纤维置于臭氧环境中,设置环境温度为100℃,放置时间为2h;
步骤二:将聚丙烯腈基碳纤维浸入本发明制备的抗菌剂乳液,乳液的固含量为1%,浴比:1∶20,浸入时间为2h,浸入温度为60℃;
步骤三:将步骤二处理的纤维取出,自然晾干,得到抗菌聚丙烯腈基碳纤维b。
实施例3
在本实施例中,一种抗菌碳纤维上浆剂乳液的制备方法,包括如下步骤:
(1)分散剂的制备:将一定质量的丙烯酸和聚合度为45的烯丙基聚氧乙烯醚单体同时溶解于适量的去离子水中配置为单体溶液,备用,优选地,所述丙烯酸与烯丙基聚氧乙烯醚的摩尔比为1∶0.5;然后在搅拌条件下,控制温度为79~81℃,将配置好的单体与过硫酸铵引发剂分别滴加到装有一定量去离子水的四口烧瓶中,优选地,所述过硫酸铵的质量占单体总质量的0.5%,滴加时间控制在3h,滴加完毕后,保温4h;最后冷却,即制得分散剂。
(2)纳米氧化物粒子水分散体的制备:将一定质量的AgO粉体研磨成纳米级别,粒径范围为200~300纳米;将步骤(1)制备的分散剂用水稀释至质量分数为2%,将纳米氧化物粒子溶于分散剂溶液,均匀搅拌制备为纳米氧化物粒子水分散体,优选地,所述纳米氧化物粒子与分散剂溶液的料液比为1∶50;此纳米氧化物粒子水分散体放置一周,不发生分层或沉淀现象即可。
(3)在反应釜中加入聚乙二醇和二羟甲基丙酸,在120℃下真空脱水2h,缓慢降温至60℃,滴加甲苯异氰酸酯、丁酮和催化剂二丁基锡二月桂酸,升温至90℃,反应4h;优选地,所述聚乙二醇的分子量为400,聚乙二醇、二羟甲基丙酸、甲苯异氰酸酯的摩尔比为1∶2∶5,二丁基锡二月桂酸用量占单体总量的0.1%,丁酮(mL)与单体总量(g)的体积质量比为1∶0.5;然后降温至45℃,于1.5h内分多次加入扩链剂三羟甲基丙烷,优选地,所述三羟甲基丙烷的用量与二羟甲基丙酸的摩尔比为1∶5;升温至80℃,保温反应2h;自然冷却,即可。
(4)将步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液混合,滴加三乙胺和水溶液至混合溶液中和,优选地,所述步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液的体积比为:1∶5;将混合液放入乳化泵进行反向乳化,乳化泵的剪切速率为15000r/min;乳化结束后,采用减压低温蒸馏法脱除丁酮,得到水性聚氨酯乳液。
本发明的另一目的在于提供一种抗菌碳纤维上浆剂乳液的应用,具体方案为:
步骤一:将聚丙烯腈基碳纤维置于臭氧环境中,设置环境温度为150℃,放置时间为3h;
步骤二:将聚丙烯腈基碳纤维浸入本发明制备的抗菌剂乳液,乳液的固含量为5%,浴比:1∶30,浸入时间为3h,浸入温度为80℃;
步骤三:将步骤二处理的纤维取出,自然晾干,得到抗菌聚丙烯腈基碳纤维c。
性能评价实施例:
将实施例1~3制备的上浆剂乳液对碳纤维上浆整理后的碳纤维a、b和c分别做抗菌实验,具体抗菌实验方法为:按GB/T 20944.1-2007《纺织品抗菌性能的评价第1部分:琼脂平皿扩散法》,以琼脂扩散法对织物进行定性检测;按GB/T 20944.3-2008《纺织品抗菌性能的评价第3部分:震荡法》测定织物定量抗菌性能,菌种为白色念珠菌、金黄色葡萄球菌和大肠杆菌。试样的定性检测结果以抑菌圈表示,定量抗菌活性以抑菌率表示,按公式计算:抑菌率=(1-B/A)×100%,式中,A为未处理织物上的活菌数;B为处理织物上的活菌数。参照GB/T 20944.1-2007耐洗色牢度试验机洗涤方法对待测碳纤维进行标准洗涤,测试10次洗涤后的抗菌性能,测试结果如表1、表2和表3所示。
表1整理后的碳纤维a、b和c对大肠杆菌的抑菌率
洗涤次数 | 碳纤维a | 碳纤维b | 碳纤维c | 未上浆整理碳纤维 |
0 | 97.3% | 97.1% | 96.5% | 13.1% |
10 | 93.9% | 94.2% | 94.1% | 10.1% |
由表1可见,上浆整理后的碳纤维对大肠杆菌具有很强的抗菌性能。上浆整理后的碳纤维对大肠杆菌的抑菌率达到96%以上,经过10次的洗涤后,其仍对大肠杆菌表现较强的抗菌性能,抑菌率达94%以上;未上浆整理碳纤维的抑菌率较低。
表2上浆整理后的碳纤维a、b和c对金黄色葡萄球菌的抑菌率
洗涤次数 | 碳纤维a | 碳纤维b | 碳纤维c | 未上浆整理碳纤维 |
0 | 97.1% | 96.8% | 96.5% | 11.2% |
10 | 92.1% | 93.3% | 93.1% | 9.3% |
由表2可见,上浆整理后的碳纤维对金黄色葡萄球菌具有很强的抗菌性能。上浆整理后的碳纤维对大肠杆菌的抑菌率达到96%以上,经过10次的洗涤后,其仍对金黄色葡萄球菌表现较强的抗菌性能,抑菌率达92%以上;未上浆整理碳纤维的抑菌率较低。
表3上浆整理后的碳纤维a、b和c对白色念珠菌的抑菌率
洗涤次数 | 碳纤维a | 碳纤维b | 碳纤维c | 未上浆整理碳纤维 |
0 | 95.7% | 95.2% | 94.8% | 10.3% |
10 | 91.3% | 91.1% | 91.5% | 8.1% |
由表3可见,上浆整理后的碳纤维对白色念珠菌具有很强的抗菌性能。上浆整理后的碳纤维对白色念珠菌的抑菌率达到94%以上,经过10次的洗涤后,其仍对白色念珠菌表现较强的抗菌性能,抑菌率达91%以上;未上浆整理碳纤维的抑菌率较低。
通过研究上浆整理后的碳纤维对金黄色葡萄球菌、大肠杆菌和白色念珠菌抑菌率分析,可以认为,本发明制备的上浆整理后的碳纤维具有很强的抗菌性能。
Claims (5)
1.一种抗菌碳纤维上浆剂乳液的制备方法,其特征在于,所述制备方法包含如下步骤:
(1)分散剂的制备:将丙烯酸和聚合度为45的烯丙基聚氧乙烯醚单体同时溶解于去离子水中配置为单体溶液,所述丙烯酸与烯丙基聚氧乙烯醚的摩尔比为1∶(0.3~0.5);然后在搅拌条件下,控制温度为79~81℃,将配置好的单体与过硫酸铵引发剂分别滴加到装有一定量去离子水的四口烧瓶中,所述过硫酸铵的质量占单体总质量的0.1~0.5%,滴加时间控制在2~3h,滴加完毕后,保温3~4h;最后冷却,制得分散剂;
(2)纳米氧化物粒子水分散体的制备:将AgO粉体研磨成纳米级别,粒径范围为100~300纳米;将步骤(1)制备的分散剂用水稀释至质量分数为1~2%,将纳米氧化物粒子溶于分散剂溶液,均匀搅拌制备为纳米氧化物粒子水分散体;此纳米氧化物粒子水分散体放置一周,不发生分层或沉淀现象即可;
(3)在反应釜中加入聚乙二醇和二羟甲基丙酸,在100~120℃下真空脱水1~2h,缓慢降温至50~60℃,滴加甲苯异氰酸酯、丁酮和催化剂二丁基锡二月桂酸,升温至80~90℃,反应3~4h;然后降温至40~45℃,于1~1.5h内分多次加入扩链剂三羟甲基丙烷,升温至60~80℃,保温反应1~2h;自然冷却,即可;所述三羟甲基丙烷的用量与二羟甲基丙酸的摩尔比为1∶(3~5);所述聚乙二醇的分子量为400,聚乙二醇、二羟甲基丙酸、甲苯异氰酸酯的摩尔比为1∶(1~2)∶(3~5),二丁基锡二月桂酸用量占单体总量的0.01~0.1%,丁酮与单体总量的体积质量比为1mL∶(0.3~0.5)g;
(4)将步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液混合,滴加三乙胺和水溶液至混合溶液中和;所述步骤(2)制备的纳米氧化物粒子水分散体和步骤(3)制备的溶液的体积比为:1∶(3~5);将混合液放入乳化泵进行反向乳化,乳化泵的剪切速率为6000~15000r/min;乳化结束后,采用减压低温蒸馏法脱除丁酮,得到水性聚氨酯乳液。
2.根据权利要求1所述的一种抗菌碳纤维上浆剂乳液的制备方法,其特征在于,所述步骤(2)中纳米氧化物粒子与分散剂溶液的料液比为1g∶(30~50)mL。
3.一种抗菌碳纤维上浆剂乳液,其特征在于,采用权利要求1~2任一项所述的一种抗菌碳纤维上浆剂乳液的制备方法制备而成。
4.一种利用权利要求1所述的抗菌碳纤维上浆剂乳液的应用,其特征在于,所述应用方法如下步骤:
步骤一:将聚丙烯腈基碳纤维置于臭氧环境中,设置合适的环境温度和放置合适的时间;
步骤二:将聚丙烯腈基碳纤维浸入本发明制备的抗菌剂乳液,乳液的固含量为1~5%,浴比:1∶20~30,浸入时间为2~3h,浸入温度为60~80℃;
步骤三:将步骤二处理的纤维取出,自然晾干,得到抗菌聚丙烯腈基碳纤维。
5.根据权利要求4所述的抗菌碳纤维上浆剂乳液的应用,其特征在于,所述步骤一中设置环境温度为100~150℃,放置时间为2~3h。
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