CN108503550A - 一种离子液体型抗静电剂及其制备方法 - Google Patents
一种离子液体型抗静电剂及其制备方法 Download PDFInfo
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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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