CN115028938A - 一种Ag/ZnO改性聚氯乙烯复合抗菌塑料及合成工艺 - Google Patents
一种Ag/ZnO改性聚氯乙烯复合抗菌塑料及合成工艺 Download PDFInfo
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Abstract
本发明涉及聚氯乙烯抗菌技术领域,且公开了一种Ag/ZnO改性聚氯乙烯复合抗菌塑料,将纳米ZnO经过甲苯二异氰酸酯表面改性,然后异氰酸酯基团水解生成氨基,得到NH2‑ZnO;将丙烯酸接枝聚氯乙烯经过氯化亚砜处理,生成酰氯基团与NH2‑ZnO发生酰胺化反应,在纳米ZnO表面修饰了聚氯乙烯分子链,然后与纳米Ag作为协同抗菌剂,对聚氯乙烯树脂抗菌改性,纳米ZnO经过聚氯乙烯修饰后,与聚氯乙烯树脂的相容性很好,分散性优异,显著提高了聚氯乙烯树脂的抗菌性能。
Description
技术领域
本发明涉及聚氯乙烯抗菌技术领域,具体为一种Ag/ZnO改性聚氯乙烯复合抗菌塑料及合成工艺。
背景技术
聚氯乙烯在儿童塑料玩具、包装膜材料、医疗器械等领域有着广泛的应用,因此对聚氯乙烯材料的抗菌改性是研究热点,将抗菌剂与聚氯乙烯复合,可以增强聚氯乙烯材料的抗菌性,如纳米氧化锌、纳米银等抗菌剂抗菌广谱性好,无毒无污染,是一种应用广泛的抗菌剂,改善纳米氧化锌、纳米银在高分子材料基体中的分散性具有重要的意义,如《硅烷偶联剂对Nano-ZnO/PLA复合材料抑菌性能与热降解性的影响》,报道了利用硅烷偶联剂KH550对纳米氧化锌进行表面处理,与聚乳酸复合后,提高nano-ZnO的分散性,改善复合材料的界面相容性,增强其抑菌作用,同时提高了材料的力学性能、热稳定性等性能。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种Ag/ZnO改性聚氯乙烯复合抗菌塑料。
(二)技术方案
为实现上述目的,本发明提供以下技术方案:一种Ag/ZnO改性聚氯乙烯复合抗菌塑料,合成工艺如下:
(1)将纳米ZnO加入到甲苯中,超声分散然后加入甲苯二异氰酸酯和二月桂酸二丁基锡,在50-70℃中反应5-10h,反应后过滤,丙酮洗涤沉淀,得到NCO-ZnO。
(2)将NCO-ZnO加入到蒸馏水中,超声分散然后在80-100℃中回流反应36-72h,反应后过滤,蒸馏水洗涤沉淀,得到NH2-ZnO。
(3)将丙烯酸接枝聚氯乙烯加入到氯化亚砜中,加热回流反应,反应后将酰氯化的聚氯乙烯加入到四氢呋喃中,搅拌溶解后加入NH2-ZnO的四氢呋喃分散液,并滴加三乙胺,搅拌反应后减压浓缩,丙酮洗涤沉淀产物,得到ZnO接枝聚氯乙烯。
(4)将5-20%的ZnO接枝聚氯乙烯、0.2-1%的纳米Ag、聚氯乙烯树脂、助剂进行双辊混炼,将母粒压片,得到Ag/ZnO改性聚氯乙烯复合抗菌塑料。
优选的,所述(1)中纳米ZnO的用量为100重量份、甲苯二异氰酸酯为50-150重量份、二月桂酸二丁基锡1-4重量份。
优选的,所述(3)搅拌反应在0-10℃中进行1-2h,然后在30-50℃中进行6-12h。
优选的,所述(3)酰氯化的聚氯乙烯的用量为100重量份,NH2-ZnO为5-30重量份、三乙胺为10-50重量份。
优选的,所述(4)中助剂包括2-3%的钙锌稳定剂、2-4%的润滑剂、0.2-0.6%的抗氧剂、50-60%的增塑剂。
(三)有益的技术效果
与现有技术相比,本发明具备以下有益技术效果:
该一种Ag/ZnO改性聚氯乙烯复合抗菌塑料,将纳米ZnO经过甲苯二异氰酸酯表面改性,然后异氰酸酯基团水解生成氨基,得到NH2-ZnO;将丙烯酸接枝聚氯乙烯经过氯化亚砜处理,生成酰氯基团与NH2-ZnO发生酰胺化反应,在纳米ZnO表面修饰了聚氯乙烯分子链,然后与纳米Ag作为协同抗菌剂,对聚氯乙烯树脂抗菌改性,纳米ZnO经过聚氯乙烯修饰后,与聚氯乙烯树脂的相容性很好,分散性优异,显著提高了聚氯乙烯树脂的抗菌性能和综合力学性能,通过合成新型高效持久的纳米抗菌剂,采用共混法制备抗菌PVC,在医疗卫生用品、抗菌材料、儿童塑料玩具等方面有着广阔的应用前景,能有效抑制多种细菌的滋生,作为儿童塑料玩具时可以更加安全地保护孩子的健康,有利于推动塑料玩具行业的迅猛发展。
具体实施方式
为实现上述目的,本发明提供以下实施方式
实施例1
(1)将100重量份纳米ZnO加入到甲苯中,超声分散然后加入50重量份的甲苯二异氰酸酯和1重量份的二月桂酸二丁基锡,在70℃中反应8h,反应后过滤,丙酮洗涤沉淀,得到NCO-ZnO。
(2)将NCO-ZnO加入到蒸馏水中,超声分散然后在100℃中回流反应48h,反应后过滤,蒸馏水洗涤沉淀,得到NH2-ZnO。
(3)将丙烯酸接枝聚氯乙烯加入到氯化亚砜中,加热回流反应,反应后将100重量份的酰氯化的聚氯乙烯加入到四氢呋喃中,搅拌溶解后加入含有5重量份的NH2-ZnO的四氢呋喃分散液,并滴加10重量份的三乙胺,在10℃中搅拌反应2h,然后在40℃中搅拌反应8h。后减压浓缩,丙酮洗涤沉淀产物,得到ZnO接枝聚氯乙烯。
(4)将5%的ZnO接枝聚氯乙烯、0.2%的纳米Ag、聚氯乙烯树脂、3%的钙锌稳定剂、3%的润滑剂硬脂酸钙、0.6%的抗氧剂1010、50%的增塑剂邻苯二甲酸二辛酯、进行双辊混炼,将母粒压片,得到Ag/ZnO改性聚氯乙烯复合抗菌塑料。
实施例2
(1)将100重量份纳米ZnO加入到甲苯中,超声分散然后加入100重量份的甲苯二异氰酸酯和2重量份的二月桂酸二丁基锡,在50℃中反应10h,反应后过滤,丙酮洗涤沉淀,得到NCO-ZnO。
(2)将NCO-ZnO加入到蒸馏水中,超声分散然后在80℃中回流反应72h,反应后过滤,蒸馏水洗涤沉淀,得到NH2-ZnO。
(3)将丙烯酸接枝聚氯乙烯加入到氯化亚砜中,加热回流反应,反应后将100重量份的酰氯化的聚氯乙烯加入到四氢呋喃中,搅拌溶解后加入含有20重量份的NH2-ZnO的四氢呋喃分散液,并滴加20重量份的三乙胺,在10℃中搅拌反应2h,然后在40℃中搅拌反应12h。后减压浓缩,丙酮洗涤沉淀产物,得到ZnO接枝聚氯乙烯。
(4)将10%的ZnO接枝聚氯乙烯、0.6%的纳米Ag、聚氯乙烯树脂、2%的钙锌稳定剂、3%的润滑剂硬脂酸钙、0.2%的抗氧剂1010、60%的增塑剂邻苯二甲酸二辛酯进行双辊混炼,将母粒压片,得到Ag/ZnO改性聚氯乙烯复合抗菌塑料。
实施例3
(1)将100重量份纳米ZnO加入到甲苯中,超声分散然后加入150重量份的甲苯二异氰酸酯和2重量份的二月桂酸二丁基锡,在60℃中反应8h,反应后过滤,丙酮洗涤沉淀,得到NCO-ZnO。
(2)将NCO-ZnO加入到蒸馏水中,超声分散然后在100℃中回流反应36h,反应后过滤,蒸馏水洗涤沉淀,得到NH2-ZnO。
(3)将丙烯酸接枝聚氯乙烯加入到氯化亚砜中,加热回流反应,反应后将100重量份的酰氯化的聚氯乙烯加入到四氢呋喃中,搅拌溶解后加入含有30重量份的NH2-ZnO的四氢呋喃分散液,并滴加50重量份的三乙胺,在5℃中搅拌反应1h,然后在50℃中搅拌反应12h。后减压浓缩,丙酮洗涤沉淀产物,得到ZnO接枝聚氯乙烯。
(4)将15%ZnO接枝聚氯乙烯、1%的纳米Ag、聚氯乙烯树脂、2%的钙锌稳定剂、3%的润滑剂硬脂酸、0.5%的抗氧剂1076、55%的增塑剂邻苯二甲酸二丁酯进行双辊混炼,将母粒压片,得到Ag/ZnO改性聚氯乙烯复合抗菌塑料。
实施例4
(1)将100重量份纳米ZnO加入到甲苯中,超声分散然后加入150重量份的甲苯二异氰酸酯和3重量份的二月桂酸二丁基锡,在70℃中反应8h,反应后过滤,丙酮洗涤沉淀,得到NCO-ZnO。
(2)将NCO-ZnO加入到蒸馏水中,超声分散然后在100℃中回流反应48h,反应后过滤,蒸馏水洗涤沉淀,得到NH2-ZnO。
(3)将丙烯酸接枝聚氯乙烯加入到氯化亚砜中,加热回流反应,反应后将100重量份的酰氯化的聚氯乙烯加入到四氢呋喃中,搅拌溶解后加入含有25重量份的NH2-ZnO的四氢呋喃分散液,并滴加50重量份的三乙胺,在5℃中搅拌反应1h,然后在70℃中搅拌反应12h。后减压浓缩,丙酮洗涤沉淀产物,得到ZnO接枝聚氯乙烯。
(4)将20%ZnO接枝聚氯乙烯、1%的纳米Ag、聚氯乙烯树脂、2%的钙锌稳定剂、2%的润滑剂硬脂酸、0.5%的抗氧剂1076、50%的增塑剂邻苯二甲酸二丁酯进行双辊混炼,将母粒压片,得到Ag/ZnO改性聚氯乙烯复合抗菌塑料。
分别以大肠杆菌(106CFU/mL)和金黄色葡萄球菌(106CFU/mL)的菌悬液作为测试菌种,接种到琼脂培养基中,以Ag/ZnO改性聚氯乙烯复合抗菌塑料的薄膜作为实验组,通过抑菌圈试验法,在37℃下培养12h,培养后测定抑菌圈直径。
上述实施例为本发明优选的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (5)
1.一种Ag/ZnO改性聚氯乙烯复合抗菌塑料的合成工艺,其特征在于:所述合成工艺如下:
(1)将纳米ZnO加入到甲苯中,超声分散然后加入甲苯二异氰酸酯和二月桂酸二丁基锡,在50-70℃中反应5-10h,反应后过滤,丙酮洗涤沉淀,得到NCO-ZnO;
(2)将NCO-ZnO加入到蒸馏水中,超声分散然后在80-100℃中回流反应36-72h,反应后过滤,蒸馏水洗涤沉淀,得到NH2-ZnO;
(3)将丙烯酸接枝聚氯乙烯加入到氯化亚砜中,加热回流反应,反应后将酰氯化的聚氯乙烯加入到四氢呋喃中,搅拌溶解后加入NH2-ZnO的四氢呋喃分散液,并滴加三乙胺,搅拌反应后减压浓缩,丙酮洗涤沉淀产物,得到ZnO接枝聚氯乙烯;
(4)将5-20%的ZnO接枝聚氯乙烯、0.2-1%的纳米Ag、聚氯乙烯树脂、助剂进行双辊混炼,将母粒压片,得到Ag/ZnO改性聚氯乙烯复合抗菌塑料。
2.根据权利要求1所述的一种Ag/ZnO改性聚氯乙烯复合抗菌塑料的合成工艺,其特征在于:所述(1)中纳米ZnO的用量为100重量份、甲苯二异氰酸酯为50-150重量份、二月桂酸二丁基锡1-4重量份。
3.根据权利要求1所述的一种Ag/ZnO改性聚氯乙烯复合抗菌塑料的合成工艺,其特征在于:所述(3)搅拌反应在0-10℃中进行1-2h,然后在30-50℃中进行6-12h。
4.根据权利要求1所述的一种Ag/ZnO改性聚氯乙烯复合抗菌塑料的合成工艺,其特征在于:所述(3)酰氯化的聚氯乙烯的用量为100重量份,NH2-ZnO为5-30重量份、三乙胺为10-50重量份。
5.根据权利要求1所述的一种Ag/ZnO改性聚氯乙烯复合抗菌塑料的合成工艺,其特征在于:所述(4)中助剂包括2-3%的钙锌稳定剂、2-4%的润滑剂、0.2-0.6%的抗氧剂、50-60%的增塑剂。
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