CN108641506A - 一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法 - Google Patents
一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，将聚四氟乙烯微粉制备成分散液，在碱性条件下，加入硝酸银溶液，通过在微粉表面原位生成纳米银颗粒，形成所述基于聚四氟乙烯的复合纳米抗菌分散剂。所述基于聚四氟乙烯的复合纳米抗菌分散剂在溶剂中具有良好的分散性及便利的操作性，可制备成耐污、抗菌的喷剂直接使用，也可以在涂料和油墨中添加，制备耐磨、防污、抗菌的纳米复合材料。
Description
技术领域
本发明涉及高分子抗菌纳米材料领域，尤其涉及一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法。
背景技术
聚四氟乙烯微粉常作为润滑油、油墨、涂料添加，用于提高润滑油、油墨、涂料的防粘、耐磨、润滑、减摩等效果。通常聚四氟乙烯微粉主要通过电子束等辐照的方法，将高分子量的聚四氟乙烯转化为低分子量，再经过粉碎来制备。这些经过辐照产生的低分子量的聚四氟乙烯具有与高分子量的聚四氟乙烯几乎同样的使用温度范围、耐候性、耐化学药品性、滑动性及不粘性，但由于辐照后分子量降低，结晶度升高，具有更好的粉碎加工性，便于制备成容易添加的微粉，具有了广泛的用途。
添加了少量聚四氟乙烯微粉的油墨或涂料，表面具有较好的疏水、耐污性能，能够阻止细菌在这些材料表面的黏附及生长，具备部分抗菌能力，但这种效果并不特别显著，主要的原因在于尽管由于添加了聚四氟乙烯可以减少细菌的黏附，但一旦有部分细菌粘附后可以继续存活和增殖，随着时间的延长，表面依然会产生霉斑，影响人类健康及制品的使用寿命和外观。为了进一步提高聚四氟乙烯微粉的抗菌耐污性能，需要对微粉进行必要的改性，使添加微粉后的油墨、或涂料，对黏附在表面的细菌具备持久的杀菌能力。
目前使用的抗菌分散剂有负载纳米银的PE/PTFE蜡微粉，使用6nm的银液体分散体与PE和PTFE蜡共混，经熔融后，通过机械加工将纳米银负载在蜡中，经过研磨加工后获得。由于使用的载体主体为PE蜡，在塑料、油墨、或涂料的添加中较难起到很好的抗黏附效果，而且使用商品化的纳米银成本较高，另外熔融处理同样增加了较多的能耗，此外制备的粉体在实际使用时较难添加。
发明内容
本发明提供了一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，用以解决上述问题。
为了解决上述技术问题，本发明的技术方案是：
一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，包括如下步骤：
将聚四氟乙烯微粉制备成分散液，调节所述分散液的pH值为7～9，加入AgNO3溶液，通过还原在所述聚四氟乙烯微粉表面原位生成纳米银颗粒，制备所述基于聚四氟乙烯的复合纳米抗菌分散剂。
作为优选，所述聚四氟乙烯纳米微粉的制备方法如下：通过在空气气氛的条件下通过电子束辐照聚四氟乙烯，经粉碎后在通风环境下堆放至少一个月，获得所述聚四氟乙烯微粉。
作为优选，所述聚四氟乙烯微粉的粒径为200nm。
作为优选，所述分散液包括溶剂和所述聚四氟乙烯微粉，所述聚四氟乙烯微粉和溶剂的质量份数之比为1:4～16。
作为优选，所述溶剂为甲醇、乙醇、正丙醇、异丙醇和正丁醇中的至少一种溶剂。
作为优选，所述AgNO3溶液的质量份数为所述分散液中所述聚四氟乙烯微粉质量份数的0.01～1％。
作为优选，还原采用的还原剂为抗坏血酸、葡萄糖、盐酸羟胺和硼氢化钠中的一种。
作为优选，所述还原剂的质量份数为所述分散液中所述聚四氟乙烯微粉质量份数的0.02～2％。
与现有技术相比，本发明具有以下优点：本发明公开了一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，将聚四氟乙烯微粉制备成分散液，在碱性条件下，加入硝酸银溶液，通过还原在所述聚四氟乙烯微粉表面原位生成纳米银颗粒，形成所述基于聚四氟乙烯的复合纳米抗菌分散剂，制备方法简单。所述基于聚四氟乙烯的复合纳米抗菌分散剂在溶剂中具有良好的分散性及便利的操作性，可制备成耐污、抗菌的喷剂直接使用，也可以直接在涂料和油墨中添加，制备耐磨、防污、抗菌的纳米复合材料。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂，下面对本发明的具体实施方式做详细的说明。
一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，包括如下步骤：
步骤一：将在空气气氛中用高剂量辐照聚四氟乙烯，经气流粉碎后形成粒径为200nm的微粉，在通风环境下堆放至少一个月，辐照产生的聚四氟乙烯微粉酰氟键转化为羧基。所述的聚四氟乙烯原料优选自分散聚合所制备的聚四氟乙烯。
步骤二：将所述聚四氟乙烯微粉经过高速搅拌或超声分散，分散于溶剂中制备分散液。所述溶剂为甲醇、乙醇、正丙醇、异丙醇、正丁醇中的至少一种溶剂。所述分散液包括溶剂和所述聚四氟乙烯微粉。所述聚四氟乙烯微粉和溶剂的质量份数之比为1:4～16；所述聚四氟乙烯微粉的质量份数为50～200份，优选50～100份；所述溶剂的质量份数为200～800份，优选200～400份。
步骤三：用氨水调整所述分散液pH值呈弱碱性，pH值范围为7～9，优选7～8。
步骤四：向所述分散液中加入一定量的AgNO3溶液充分搅拌，所述AgNO3的质量份数为所述分散液中所述聚四氟乙烯微粉质量份数的0.01～1％，优选0.1～0.5％。所述AgNO3溶液中AgNO3的浓度为10％。
步骤五：加入还原剂，在所述聚四氟乙烯纳米微粉表面原位生成纳米银颗粒，获得所述基于聚四氟乙烯的复合纳米抗菌分散剂。所述还原剂为抗坏血酸、葡萄糖、盐酸羟胺和硼氢化钠中的一种。所述还原剂的质量份数为所述分散液中所述聚四氟乙烯微粉质量份数的0.02～2％，优选0.2～1％。
实施例一
(1)分散聚四氟乙烯树脂用GJ-2型电子加速器辐照，辐照剂量60Mrad，完成后通过粉碎机粉碎，获得粒径约200nm的辐照聚四氟乙烯微粉，堆放一个月。
(2)100份聚四氟乙烯微粉经过超声和高速搅拌分散于400份乙醇溶剂中制备分散液。
(3)滴加28％的氨水，调整所述分散液的pH值为7.4，继续搅拌2h。
(4)加入0.5份10％AgNO3乙醇溶液，继续搅拌2h。
(5)加入1份10％抗坏血酸乙醇溶液，继续搅拌5h，溶液变为浅灰色，得到所述基于聚四氟乙烯的复合纳米抗菌分散剂的溶液。
(6)将10份所述基于聚四氟乙烯的复合纳米抗菌分散剂的溶液，加入100份涂料中，设置转速400-600rpm，搅拌2h。
(7)将涂料涂覆到聚碳酸酯或尼龙表面，真空烘箱干燥10h。
(8)用大肠杆菌和金色葡萄糖球菌做抗菌实验，实验结果表明有明显的持久抗菌效果，总有效抗菌率达95％以上。
本领域的技术人员可以对发明进行各种改动和变型而不脱离本发明的精神和范围。这样，倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内，则本发明也意图包括这些改动和变型在内。
Claims (9)
1.一种基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，包括如下步骤：
将聚四氟乙烯微粉制备成分散液，调节所述分散液的pH值为7～9，加入AgNO3溶液，通过还原，在所述聚四氟乙烯微粉表面原位生成纳米银颗粒，制备所述基于聚四氟乙烯的复合纳米抗菌分散剂。
2.根据权利要求1所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，所述聚四氟乙烯微粉的制备方法如下：在空气气氛的条件下通过电子束辐照聚四氟乙烯，经粉碎后在通风环境下堆放，获得所述聚四氟乙烯微粉。
3.根据权利要求2所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，所述聚四氟乙烯经粉碎后在通风环境下堆放至少一个月。
4.根据权利要求2所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，所述聚四氟乙烯微粉的粒径为200nm。
5.根据权利要求1所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，所述分散液包括溶剂和所述聚四氟乙烯微粉，所述聚四氟乙烯微粉和溶剂的质量份数之比为1:4～16。
6.根据权利要求5所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，所述溶剂为甲醇、乙醇、正丙醇、异丙醇和正丁醇中的至少一种溶剂。
7.根据权利要求5所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，所述AgNO3溶液的质量份数为所述分散液中所述聚四氟乙烯微粉质量份数的0.01～1％。
8.根据权利要求5所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，还原采用的还原剂的质量份数为所述分散液中所述聚四氟乙烯微粉质量份数的0.02～2％。
9.根据权利要求1所述的基于聚四氟乙烯的复合纳米抗菌分散剂的制备方法，其特征在于，采用的还原剂为抗坏血酸、葡萄糖、盐酸羟胺和硼氢化钠中的一种。
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