CN107100009A - 一种山梨酸钾改性水性聚氨酯抗菌复合面料及制备方法 - Google Patents

一种山梨酸钾改性水性聚氨酯抗菌复合面料及制备方法 Download PDF

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CN107100009A
CN107100009A CN201710410661.5A CN201710410661A CN107100009A CN 107100009 A CN107100009 A CN 107100009A CN 201710410661 A CN201710410661 A CN 201710410661A CN 107100009 A CN107100009 A CN 107100009A
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potassium sorbate
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乔建军
赵兴旺
许然然
财音青格乐
刘家亨
吴昊
李韡
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Tianjin University
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Abstract

本发明公开了一种山梨酸钾改性水性聚氨酯抗菌复合面料及制备方法，一种山梨酸钾改性水性聚氨酯抗菌复合面料，包括无纺布层，所述无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层。本发明的山梨酸钾改性水性聚氨酯抗菌复合面料具有良好的抗菌性能，能有效对噬菌体Phi‑X174、骨髓灰质炎病毒、枯草杆菌黑色变种芽孢、白色念珠球菌等在检测压力达20KPa时仍具有优良的防护性能，达到GB24539‑2009分级的最高要求。并且对大肠杆菌和金黄色葡萄球菌有良好的抑制作用。

Description

一种山梨酸钾改性水性聚氨酯抗菌复合面料及制备方法
技术领域
本发明涉及新材料开发领域，具体涉及一种山梨酸钾改性水性聚氨酯抗菌复合面料及制备方法。
背景技术
现如今，水性聚氨酯(WPU)是一种在聚氨酯的分子链中含有亲水性基团的聚氨酯树脂,具有很强的亲和性,采用特定的工艺能使之在水中分散并形成稳定的体系。作为一种具有优良性能的涂饰高分子材料已经在木器、皮革、纤维、纺织品、塑料制品等领域广泛应用。水性聚氨酯主要应用于皮革涂饰、纺织印染、造纸业、建筑涂料、胶粘剂等方面,这些领域目前对抗菌性提出了新的要求。
无纺布又称不织布，是由定向的或随机的纤维而构成，是新一代环保材料，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。如多采用聚丙烯(pp材质)粒料为原料，经高温熔融、喷丝、铺纲、热压卷取连续一步法生产而成。因具有布的外观和某些性能而称其为布。
山梨酸(钾)能有效地抑制霉菌，酵母菌和好氧性细菌的活性，还能防止肉毒杆菌、葡萄球菌、沙门氏菌等有害微生物的生长和繁殖，但对厌氧性芽孢菌与嗜酸乳杆菌等有益微生物几乎无效，其抑止发育的作用比杀菌作用更强，从而达到有效地延长物品的保存时间。其防腐效果是同类产品苯甲酸钠的5-10倍。
但目前尚未有山梨酸钾改性水性聚氨酯抗菌复合面料的报道。
发明内容
本发明的目的是克服现有技术的不足，提供一种山梨酸钾改性水性聚氨酯抗菌复合面料。
本发明的第二个目的是提供一种山梨酸钾改性水性聚氨酯抗菌复合面料的制备方法。
本发明的技术方案概述如下：
一种山梨酸钾改性水性聚氨酯抗菌复合面料，包括无纺布层，所述无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层。
两个山梨酸钾改性水性聚氨酯膜层的厚度分别为0.12-0.26mm和0.03-0.12mm。
一种山梨酸钾改性水性聚氨酯抗菌复合面料的制备方法，包括如下步骤：
(1)将水性聚氨酯乳液与二甲基甲酰胺混合，配成水性聚氨酯乳液质量分数为55％-75％的液体,加入山梨酸钾使质量分数为1％-3％，55-70℃恒温水浴下搅拌，测量液体粘度达到1500mpa/s及以上时停止搅拌，制成山梨酸钾改性的水性聚氨酯母液；
(2)用涂布器将山梨酸钾改性的水性聚氨酯母液均匀涂布在无纺布的两面上,58-67℃下恒温干燥；放置于热压机上，32-40MPa压力下滚压，制成无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层的山梨酸钾改性水性聚氨酯抗菌复合面料。
两个山梨酸钾改性水性聚氨酯膜层的厚度分别为0.12-0.26mm和0.03-0.12mm。
本发明的优点：
本发明的山梨酸钾改性水性聚氨酯抗菌复合面料具有良好的抗菌性能，能有效对噬菌体Phi-X174、骨髓灰质炎病毒、枯草杆菌黑色变种芽孢、白色念珠球菌等在检测压力达20KPa时仍具有优良的防护性能，达到GB24539-2009分级的最高要求。并且对大肠杆菌和金黄色葡萄球菌有良好的抑制作用。
具体实施方式
下面结合实施例，对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。
本发明选用的水性聚氨酯乳液可以采用商品化的产品，优选下述方法制成：
(1)将分子量为1000-2000的聚碳酸酯二醇、分子量为1000-2000的聚四氢呋喃醚二醇、分子量为1000-2000的聚醚二醇、异氟尔酮二异氰酸酯、二羟甲基丙酸、1,6-己二醇、三羟甲基丙烷和二月硅酸二丁基锡分别真空干燥脱水；将N-甲基-2-吡咯烷酮、丙酮和三乙胺分别干燥；
(2)按质量份数，将步骤(1)获得的3-4份所述聚碳酸酯二醇、0.8-1.2份聚四氢呋喃醚二醇、1-1.5份聚醚二醇与9-10份异氟尔酮二异氰酸酯混合均匀，在80-100℃下搅拌反应1.5-3h，降温至40-50℃，依次加入0.8-1份二羟甲基丙酸、2-2.5份1,6-己二醇、0.5-0.6份三羟甲基丙烷，0.03-0.04份二月硅酸二丁基锡、100-200份N-甲基-2-吡咯烷酮和0-40份丙酮，将反应温度升至75-90℃反应2-3.5h，降温至20-30℃，加入0.6-1份三乙胺，搅拌分散1-1.5h，制备得到水性聚氨酯乳液。
实施例1
水性聚氨酯乳液，用下述方法制成：
(1)将分子量为1000的聚碳酸酯二醇、分子量为1000的聚四氢呋喃醚二醇、分子量为1000的聚醚二醇、异氟尔酮二异氰酸酯、二羟甲基丙酸、1,6-己二醇、三羟甲基丙烷和二月硅酸二丁基锡分别真空干燥脱水；将N-甲基-2-吡咯烷酮、丙酮和三乙胺分别干燥；
(2)按质量份数，将步骤(1)获得的3.5份所述聚碳酸酯二醇、1份聚四氢呋喃醚二醇、1.25份聚醚二醇与9.5份异氟尔酮二异氰酸酯混合均匀，在90℃下搅拌反应2h，降温至45℃，依次加入0.9份二羟甲基丙酸、2.25份1,6-己二醇、0.55份三羟甲基丙烷，0.035份二月硅酸二丁基锡、150份N-甲基-2-吡咯烷酮和20份丙酮，将反应温度升至80℃反应3h，降温至25℃，加入0.8份三乙胺，搅拌分散1.25h，制备得到水性聚氨酯乳液。
实施例2
水性聚氨酯乳液，用下述方法制成：
(1)将分子量为2000的聚碳酸酯二醇、分子量为2000的聚四氢呋喃醚二醇、分子量为2000的聚醚二醇、异氟尔酮二异氰酸酯、二羟甲基丙酸、1,6-己二醇、三羟甲基丙烷和二月硅酸二丁基锡分别真空干燥脱水；将N-甲基-2-吡咯烷酮、丙酮和三乙胺分别干燥；
(2)按质量份数，将步骤(1)获得的3份所述聚碳酸酯二醇、0.8份聚四氢呋喃醚二醇、1份聚醚二醇与9份异氟尔酮二异氰酸酯混合均匀，在80℃下搅拌反应3h，降温至40℃，依次加入0.8份二羟甲基丙酸、2份1,6-己二醇、0.5份三羟甲基丙烷，0.03份二月硅酸二丁基锡、100份N-甲基-2-吡咯烷酮，将反应温度升至75℃反应3.5h，降温至20℃，加入0.6份三乙胺，搅拌分散1h，制备得到水性聚氨酯乳液。
实施例3
水性聚氨酯乳液，用下述方法制成：
(1)将分子量为2000的聚碳酸酯二醇、分子量为2000的聚四氢呋喃醚二醇、分子量为2000的聚醚二醇、异氟尔酮二异氰酸酯、二羟甲基丙酸、1,6-己二醇、三羟甲基丙烷和二月硅酸二丁基锡分别真空干燥脱水；将N-甲基-2-吡咯烷酮、丙酮和三乙胺分别干燥；
(2)按质量份数，将步骤(1)获得的4份所述聚碳酸酯二醇、1.2份聚四氢呋喃醚二醇、1.5份聚醚二醇与10份异氟尔酮二异氰酸酯混合均匀，在100℃下搅拌反应1.5h，降温至50℃，依次加入1份二羟甲基丙酸、2.5份1,6-己二醇、0.6份三羟甲基丙烷，0.04份二月硅酸二丁基锡、200份N-甲基-2-吡咯烷酮和40份丙酮，将反应温度升至90℃反应2h，降温至30℃，加入1份三乙胺，搅拌分散1.5h，制备得到水性聚氨酯乳液。
实施例4
一种山梨酸钾改性水性聚氨酯抗菌复合面料的制备方法，包括如下步骤：
(1)将水性聚氨酯乳液(实施例1制备)与二甲基甲酰胺混合，配成水性聚氨酯乳液质量分数为65％的液体,加入山梨酸钾使质量分数为2％，60℃恒温水浴下搅拌，测量液体粘度达到1500mpa/s及以上时停止搅拌，制成山梨酸钾改性的水性聚氨酯母液；
(2)用涂布器将山梨酸钾改性的水性聚氨酯母液均匀涂布在无纺布的两面上,63℃下恒温干燥；放置于热压机上，36MPa压力下滚压，制成无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层的山梨酸钾改性水性聚氨酯抗菌复合面料。
其中两个山梨酸钾改性水性聚氨酯膜层的厚度分别为0.2mm(外层)和0.1mm(内层)。
实施例5
一种山梨酸钾改性水性聚氨酯抗菌复合面料的制备方法，包括如下步骤：
(1)将水性聚氨酯乳液(实施例2制备)与二甲基甲酰胺混合，配成水性聚氨酯乳液质量分数为55％的液体,加入山梨酸钾使质量分数为1％，55℃恒温水浴下搅拌，测量液体粘度达到1500mpa/s及以上时停止搅拌，制成山梨酸钾改性的水性聚氨酯母液；
(2)用涂布器将山梨酸钾改性的水性聚氨酯母液均匀涂布在无纺布的两面上,58℃下恒温干燥；放置于热压机上，32MPa压力下滚压，制成无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层的山梨酸钾改性水性聚氨酯抗菌复合面料。
其中两个山梨酸钾改性水性聚氨酯膜层的厚度分别为0.12mm(外层)和0.03mm(内层)。
实施例6
一种山梨酸钾改性水性聚氨酯抗菌复合面料的制备方法，包括如下步骤：
(1)将水性聚氨酯乳液(实施例3制备)与二甲基甲酰胺混合，配成水性聚氨酯乳液质量分数为75％的液体,加入山梨酸钾使质量分数为3％，70℃恒温水浴下搅拌，测量液体粘度达到1500mpa/s及以上时停止搅拌，制成山梨酸钾改性的水性聚氨酯母液；
(2)用涂布器将山梨酸钾改性的水性聚氨酯母液均匀涂布在无纺布的两面上,67℃下恒温干燥；放置于热压机上，40MPa压力下滚压，制成无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层的山梨酸钾改性水性聚氨酯抗菌复合面料。
其中两个山梨酸钾改性水性聚氨酯膜层的厚度分别为0.26mm(外层)和0.12mm(内层)。
参照标准ISO 16604-2004检测实施例4制备的山梨酸钾改性水性聚氨酯抗菌复合面料对血源性病原体的穿透阻力的方法，检测山梨酸钾改性水性聚氨酯复合面料对含微生物液体的阻隔性能。
检测结果如表1所示：
表1
注：“+”代表有微生物检出；“－”代表无微生物检出
实验参照GB/T 19344-2008《第三部分振荡法》，实验微生物采用金黄色葡萄球菌(ATCC6538)和大肠杆菌(8099)。实验结果如表2所示：
表2
由表1可知山梨酸钾改性水性聚氨酯复合面料能有效对噬菌体Phi-X174、脊髓灰质炎病毒、枯草杆菌黑色变种芽孢、白色念珠球菌在检测压力达20KPa时仍具有优良的防护性能，达到GB24539-2009分级的最高要求。经检测，实施例5和实施例6制备的一种山梨酸钾改性水性聚氨酯抗菌复合面料的效果与实施例4的效果相似。
分析表2，结果表明，山梨酸钾改性水性聚氨酯复合面料对大肠杆菌和金黄色葡萄球菌的抑菌率均达到99％以上，显示出良好的抗菌性能。

Claims (4)

1.一种山梨酸钾改性水性聚氨酯抗菌复合面料，其特征在于包括无纺布层，所述无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层。
2.根据权利要求1所述的一种山梨酸钾改性水性聚氨酯抗菌复合面料，其特征在于两个山梨酸钾改性水性聚氨酯膜层的厚度分别为0.12-0.26mm和0.03-0.12mm。
3.权利要求1或2的一种山梨酸钾改性水性聚氨酯抗菌复合面料的制备方法，其特征在于包括如下步骤：
(1)将水性聚氨酯乳液与二甲基甲酰胺混合，配成水性聚氨酯乳液质量分数为55％-75％的液体,加入山梨酸钾使质量分数为1％-3％，55-70℃恒温水浴下搅拌，测量液体粘度达到1500mpa/s及以上时停止搅拌，制成山梨酸钾改性的水性聚氨酯母液；
(2)用涂布器将山梨酸钾改性的水性聚氨酯母液均匀涂布在无纺布的两面上,58-67℃下恒温干燥；放置于热压机上，32-40MPa压力下滚压，制成无纺布层的两个表面分别设置有山梨酸钾改性水性聚氨酯膜层的山梨酸钾改性水性聚氨酯抗菌复合面料。
4.根据权利要求3所述的方法，其特征是两个山梨酸钾改性水性聚氨酯膜层的厚度分别为0.12-0.26mm和0.03-0.12mm。
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