CN108503550A - 一种离子液体型抗静电剂及其制备方法 - Google Patents
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Abstract
本发明涉及一种离子液体型抗静电剂及其制备方法。该方法是通过两种离子型前驱体化合物A和B通过离子液体交换得到目标产物离子液体型抗静电剂。本发明所制备的离子型抗静电剂具有蒸汽压极低，不可燃，电导率高；且制备工艺简单，转化率高，选择性好，利于中试放大及大规模工业化生产；具有良好的热稳定性和化学稳定性，在使用过程中不影响塑料制品的其他性质(如拉伸性能、冲击性能等机械性能，透明性、着色性等表观性能)；且易于后处理，不会对环境造成污染等优点。
Description
技术领域
本发明属于工程塑料行业中抗静电剂的设计与开发领域，具体涉及一种 离子液体型抗静电剂及其制备方法。
背景技术
由于塑料制品具有重量轻、成本低以及良好的可塑性、绝缘性、抗腐蚀 性等特点，近年来已被广泛应用于电子电气、汽车、建筑、家电、医疗、办 公设备、机械、航空航天等众多领域。在“以塑代钢”、“以塑代木”的发展 趋势下，塑料行业已成为当今世界工业中增长速度较快的领域，其发展不仅 对国家支柱产业和现代高新技术产业起着支撑作用，同时也推动传统产业改 造和产品结构的调整。
同时，我们应该注意到的是：塑料通常具有很好的电绝缘性，既不能电 离，又不能传递电子。在其加工和使用过程中,当同其它物体或自身接触和摩 擦时,会因电子的得失而带电,并且很难通过传导而消失,从而产生静电。由于 静电吸引力，塑料制品会吸附空气中的灰尘，影响制品美观；电影胶片和唱 片由于静电吸尘会使清晰度和音质变劣。另外，静电还会导致精密仪器失真， 电子元件报废等，从而带来巨大损失，如在美国塑料电子部件在储运过程中 废品率达到50％，损失高达50亿美元。静电甚至会危及人的生命，有些塑 料制品产生的静电电压高达几千伏，人一旦接触就会触电，严重时会造成死 亡。因此，研究开发经济高效的抗静电剂具有十分重要的经济意义和社会意 义。
常用的抗静电剂多为表面活性剂类，可以分为：非离子型、阳离子型和 阴离子型。非离子型抗静电剂虽然具有热稳定性良好、价格较便宜、使用方 便等优点，但是因自身不带电荷，故抗静电性能都比不上离子型抗静电剂， 所以其所需添加量较大。阴离子型抗静电剂具有热稳定性高的优点，但吸湿 性大、加工困难、透明性能差等缺点也较为明显。阳离子型抗静电剂抗静电 的效果最好，吸附能力强，耐摩擦及洗涤，但是其不耐高温，这也严重限制 了阳离子型抗静电剂的实际应用。
因此，有必要提出有效的技术方案，解决上述问题。
发明内容
本发明针对上述现有技术的不足，提供一种离子液体型抗静电剂的制备 方法。该方法得到的离子液体型抗静电剂产品性能优良。
本发明解决上述技术问题的技术方案如下：
一种离子液体型抗静电剂的制备方法，步骤如下：
(1)采用具有式(a)结构的季铵阳离子、具有式(b)结构的季膦阳 离子、具有式(c)结构的咪唑阳离子和具有式(d)结构的吡啶阳离子结构 中的一种的卤化物作为前驱体A；
式中R1、R2、R3、R4为氢原子或烷基取代基；
(2)采用具有[BF4]-、[PF6]-、[CF3SO3]-和[Tf2N]-阴离子中的一种的金 属盐作为前驱体B；
(3)将所述前驱体A和前驱体B按照一定的摩尔比混合，再加入一定 量的水，在一定温度下恒温搅拌一段时间，静置后溶液分为两相，除去上层 水相，再将下层粘稠液体用水洗涤，最后在一定温度下真空干燥即可得到目 标产物离子液体型抗静电剂。
优选地，所述的阳离子中烷基取代基的烷基链长度为C1～C16。
优选地，所述的前驱体A中卤化物为Cl-、Br-或I-，优选Br-。
优选地，所述的前驱体B中金属盐为Li+、Na+或K+，优选Li+、Na+。
优选地，所述的前驱体A和前驱体B的摩尔比为1:1.1。
优选地，所述的前驱体A和前驱体B反应温度为50～70℃，反应时间 为8～12h。
优选地，所述的真空干燥温度为90℃，干燥时间为12h。
本发明还提供一种离子液体型抗静电剂，所述离子液体型抗静电剂的阳 离子为具有式(a)结构的季铵阳离子、具有式(b)结构的季膦阳离子、具 有式(c)结构的咪唑阳离子、具有式(d)结构的吡啶阳离子中的一种，
式中R1、R2、R3、R4为氢原子或烷基取代基；
所述离子液体型抗静电剂的阳离子为[BF4]-、[PF6]-、[CF3SO3]-、[Tf2N]-中的一种。
本发明所制备的离子型抗静电剂具有如下优点：
(1)蒸汽压极低，不可燃，电导率高；且制备工艺简单，转化率高， 选择性好，利于中试放大及大规模工业化生产。
(2)具有良好的热稳定性和化学稳定性，在使用过程中不影响塑料制 品的其他性质(如拉伸性能、冲击性能等机械性能，透明性、着色性等表观 性能)；且易于后处理，不会对环境造成污染。
具体实施方式
下面结合实施例对本发明作进一步地详细说明，但本发明的实施方式不 限于此。对于未特别注明的工艺参数，可参照常规技术进行。
实施例1
本实施例提供了一种离子液体型抗静电剂的制备方法，该制备方法具体 包括以下步骤：
将0.1mol三丁基甲基溴化铵与0.11mol双(三氟甲磺酰亚胺)锂加入 到装有回流装置的三口圆底烧瓶中，再加入500mL水，在70℃下恒温磁力 搅拌12h。静置后溶液分为两相，下层为离子液体型抗静电剂相，上层为水 相，用分液漏斗进行分离，再将下层离子液体型抗静电剂相反复用水洗涤， 直到用AgNO3滴定不再有沉淀产生，然后旋转蒸发去除水，最后在90℃下 真空干燥12h，即可得到目标产物离子液体型抗静电剂。
实施例2
本实施例提供了一种离子液体型抗静电剂的制备方法，该制备方法具体 包括以下步骤：
将0.1mol三丁基甲基溴化鏻与0.11mol四氟硼酸钠加入到装有回流装 置的三口圆底烧瓶中，再加入500mL水，在50℃下恒温磁力搅拌12h。静 置后溶液分为两相，下层为离子液体型抗静电剂相，上层为水相，用分液漏 斗进行分离，再将下层离子液体型抗静电剂相反复用水洗涤，直到用AgNO3滴定不再有沉淀产生，然后旋转蒸发去除水，最后在90℃下真空干燥12h， 即可得到目标产物离子液体型抗静电剂。
实施例3
本实施例提供了一种离子液体型抗静电剂的制备方法，该制备方法具体 包括以下步骤：
将0.1mol1-十六烷基3-甲基咪唑溴盐与0.11mol双(三氟甲磺酰亚胺) 锂加入到装有回流装置的三口圆底烧瓶中，再加入500mL水，在60℃下恒 温磁力搅拌8h。静置后溶液分为两相，下层为浅黄色油状液体——离子液 体型抗静电剂相，上层为水相。冷却后，下层为白色固体相，将水除去，并 用水对固体相进行反复冲洗，直到用AgNO3滴定不再有沉淀产生，得到的 白色固体最后在90℃下真空干燥12h，即可得到目标产物离子液体型抗静电剂，并用适量乙醇溶解待用。
实施例4
本实施例提供了一种离子液体型抗静电剂的制备方法，该制备方法具体 包括以下步骤：
将0.1mol1-丁基吡啶与0.11mol六氟硼酸钠加入到装有回流装置的三 口圆底烧瓶中，再加入500mL水，在70℃下恒温磁力搅拌12h。静置后溶 液分为两相，下层为离子液体型抗静电剂相，上层为水相，用分液漏斗进行 分离，再将下层离子液体型抗静电剂相反复用水洗涤，直到用AgNO3滴定 不再有沉淀产生，然后旋转蒸发去除水，最后在90℃下真空干燥12h，即可 得到目标产物离子液体型抗静电剂。
实施例5
本实施例提供了一种离子液体型抗静电剂的制备方法，该制备方法具体 包括以下步骤：
将0.1mol 1-丁基-3-甲基咪唑溴盐与0.11mol三氟磺酸钠加入到装有回 流装置的三口圆底烧瓶中，再加入500mL水，在70℃下恒温磁力搅拌12h。 静置后溶液分为两相，下层为离子液体型抗静电剂相，上层为水相，用分液 漏斗进行分离，再将下层离子液体型抗静电剂相反复用水洗涤，直到用AgNO3滴定不再有沉淀产生，然后旋转蒸发去除水，最后在90℃下真空干 燥12h，即可得到目标产物离子液体型抗静电剂。
实施例6
本实施例提供了一种离子液体型抗静电剂的制备方法，该制备方法具体 包括以下步骤：
将0.1mol 1-丁基-3-甲基咪唑溴盐与0.11mol双(三氟甲磺酰亚胺)锂 加入到装有回流装置的三口圆底烧瓶中，再加入500mL水，在60℃下恒温 磁力搅拌8h。静置后溶液分为两相，下层为离子液体型抗静电剂相，上层 为水相，用分液漏斗进行分离，再将下层离子液体型抗静电剂相反复用水洗 涤，直到用AgNO3滴定不再有沉淀产生，然后旋转蒸发去除水，最后在90℃ 下真空干燥12h，即可得到目标产物离子液体型抗静电剂。
上述实施例为本发明较佳的实施方式，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 (8)
1.一种离子液体型抗静电剂的制备方法，其特征在于，步骤如下：
(1)采用具有式(a)结构的季铵阳离子、具有式(b)结构的季膦阳离子、具有式(c)结构的咪唑阳离子和具有式(d)结构的吡啶阳离子结构中的一种的卤化物作为前驱体A；
式中R1、R2、R3、R4为氢原子或烷基取代基；
(2)采用具有[BF4]-、[PF6]-、[CF3SO3]-和[Tf2N]-阴离子中的一种的金属盐作为前驱体B；
(3)将所述前驱体A和前驱体B按照一定的摩尔比混合，再加入一定量的水，在一定温度下恒温搅拌一段时间，静置后溶液分为两相，除去上层水相，再将下层粘稠液体用水洗涤，最后在一定温度下真空干燥即可得到目标产物离子液体型抗静电剂。
2.如权利要求1所述的制备方法，其特征在于，所述的阳离子中烷基取代基的烷基链长度为C1～C16。
3.如权利要求1所述的制备方法，其特征在于，所述的前驱体A中卤化物为Cl-、Br-或I-。
4.如权利要求1所述的制备方法，其特征在于，所述的前驱体B中金属盐为Li+、Na+或K+。
5.如权利要求1所述的制备方法，其特征在于，所述的前驱体A和前驱体B的摩尔比为1:1.1。
6.如权利要求1所述的制备方法，其特征在于，所述的前驱体A和前驱体B反应温度为50～70℃，反应时间为8～12h。
7.如权利要求1所述的制备方法，其特征在于，所述的真空干燥温度为90℃，干燥时间为12h。
8.一种离子液体型抗静电剂，其特征在于，所述离子液体型抗静电剂的阳离子为具有式(a)结构的季铵阳离子、具有式(b)结构的季膦阳离子、具有式(c)结构的咪唑阳离子、具有式(d)结构的吡啶阳离子中的一种，
式中R1、R2、R3、R4为氢原子或烷基取代基；
所述离子液体型抗静电剂的阳离子为[BF4]-、[PF6]-、[CF3SO3]-、[Tf2N]-中的一种。
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| CN115650887A (zh) * | 2022-10-25 | 2023-01-31 | 默尼化工科技(上海)有限公司 | 一种光学透明耐温长效小分子型抗静电剂及其制备方法和应用 |
| CN115894933A (zh) * | 2022-12-07 | 2023-04-04 | 世晨材料技术(上海)有限公司 | 一种有机硅材料用反应型抗静电剂化合物 |
| CN116041708A (zh) * | 2022-12-07 | 2023-05-02 | 世晨材料技术(上海)有限公司 | 一种反应型有机硅材料用抗静电剂化合物的制备方法 |
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