CN117285847A - 一种水性聚丙烯薄膜涂覆用涂层及其制备方法 - Google Patents
一种水性聚丙烯薄膜涂覆用涂层及其制备方法 Download PDFInfo
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- CN117285847A CN117285847A CN202311158316.9A CN202311158316A CN117285847A CN 117285847 A CN117285847 A CN 117285847A CN 202311158316 A CN202311158316 A CN 202311158316A CN 117285847 A CN117285847 A CN 117285847A
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Abstract
本发明公开了一种水性聚丙烯薄膜涂覆用涂层及其制备方法,包括以下组分:石墨烯/聚苯胺复合颗粒、阳离子改性氯化聚丙烯、丙烯酸酯预聚物、光引发剂、流平剂、消泡剂、水;石墨烯/聚苯胺复合颗粒作为丙烯酸酯预聚物pickering乳液的乳化剂,对丙烯酸酯预聚物具有良好的分散稳定性,并且复合颗粒赋予提成良好的耐磨性和抗静电作用;另外阳离子改性氯化聚丙烯使得涂层的抗静电性能进一步提高,且有效提高涂层对油墨的粘附性。
Description
技术领域
本发明属于聚合物涂层材料领域,具体涉及一种水性聚丙烯薄膜涂覆用涂层及其制备方法。
背景技术
双向拉伸聚丙烯薄膜(BOPP)塑料薄膜是目前最为常用的包装原料。然而,塑料等高分子材料的高绝缘性,使其容易产生静电危害,对薄膜的生产加工和使用过程都会产生不便和危害,例如,BOPP薄膜的加工或使用过程中,由于薄膜间的摩擦会产生静电作用,使得BOPP薄膜表面吸附空气中的灰尘或其他脏东西,不仅影响到薄膜的美观,而且薄膜与薄膜之间会产生相互粘结现象,影响正常生产和使用;另外,静电在包装储运过程中的产生是不可避免的,而电子产品的日趋小型化、集成电路的高密度化,使其变得越来越敏感。例如,如果电子线路板的包装材料没有防静电功能,则摩擦产生的静电不容易失散,积累到一定的程度之后,静电放电可能会导致线路板功能损坏。随着电子工业的迅猛发展,电子线路板集成度越来越高,电子线路板和各种电子元件等更容易造成静电损伤,引起产品失效。
除此之外,BOPP薄膜还有如下缺点:(1)表面能低,无极性,印刷油墨在BOPP薄膜上铺展困难,油墨对薄膜的粘结力不好;(2)表面硬度偏低,容易在生产或运输过程中与其他物体摩擦,造成BOPP薄膜表面磨损或刮花,进一步导致BOPP薄膜表面光泽度下降,雾度上升。
发明内容
本发明根据BOPP薄膜作为包装材料而具有的不足之处,提供一种具有综合性能优异的水性涂层,该涂层赋予BOPP薄膜优异的抗静电性、耐磨性和印刷加工性能。
本发明提供的一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
所述石墨烯/聚苯胺复合颗粒作为pickering乳液的乳化剂,对丙烯酸酯预聚物具有良好的分散稳定性,并且提供良好的导电、耐磨性。
所述石墨烯/聚苯胺复合颗粒制备方法如下:将氧化石墨烯分散在水和DMF的混合液中,加入水合肼,在80~100℃下反应6~12h得到石墨烯;将上述石墨烯分散液与一定量聚苯乙烯磺酸混合超声处理12h,得到稳定的黑色分散液;在上述石墨烯分散液中加入一定量苯胺单体,搅拌情况下加入氧化剂过硫酸铵引发苯胺聚合,反应时间为5~10h,将反应后得到的混合液抽滤、去离子水洗涤,得到石墨烯/聚苯胺复合材料。所述聚苯乙烯磺酸和石墨烯的质量比为100:1,苯胺单体与石墨烯的质量比为5:1,苯胺单体与过硫酸铵的质量比为3:1。
所述阳离子改性氯化聚丙烯对抗静电性具有辅助功效,由于印刷油墨通常采用带有大量羟基、羧基的树脂,阳离子改性能够提高涂层对印刷油墨的吸附性。
所述阳离子改性氯化聚丙烯制备方法如下:氯化聚丙烯与丙烯酰氧乙基三甲基氯化铵、丙烯酸丁酯、丙烯酸甲酯溶解于甲苯中,加入过氧化苯甲酰作为氧化催化剂,加热至60~80℃反应12h,纯化后得到阳离子改性氯化聚丙烯。
所述氯化聚丙烯的含氯质量百分比为30%;
所述氯化聚丙烯、丙烯酰氧乙基三甲基氯化铵、丙烯酸丁酯、丙烯酸甲酯、过氧化苯甲酰的投料质量比为20:0.8~2.5:1.5:0.5:1.1。
所述丙烯酸酯预聚物由以下一种或多种单体制备而成:甲基丙烯酸、丙烯酸、甲基丙烯酸丁酯、丙烯酸丁酯、丙烯酸甲酯、丙烯酸异辛酯、苯乙烯、丙烯腈、丁二烯、衣康酸。
所述的光引发剂指α,α-二甲氧基-α-苯基苯乙酮、α,α-二乙氧基苯乙酮、2-苯基-2,2-二甲氨基-1-(4-吗啉苯基)-1-丁酮、2,4,6-三甲基苯甲酰膦酸二乙酯中的至少一种。
所述流平剂指醋酸-丁酸纤维素和聚二甲基硅氧烷中的至少一种。
所述消泡剂指甘油三羟基聚醚和磷酸三丁酯中的至少一种。
本发明还提供上述一种水性聚丙烯薄膜涂覆用涂层的制备方法,包括以下步骤:
(1)将石墨烯/聚苯胺复合颗粒超声分散在水中得到乳化剂分散液,往分散液中加入由丙烯酸酯预聚物单体和过硫酸铵构成的油相,然后使用均质机乳化5min,得到O/W型乳液;将得到的乳液置于60~80℃水浴中静置反应10~15h,加入对苯二酚和四丁基溴化铵,即得到丙烯酸酯预聚物pickering乳液。
所述油相中过硫酸铵的质量分数为2~3%;对苯二酚的加入量为丙烯酸酯预聚物单体质量的0.2~1%;四丁基溴化铵的加入量为丙烯酸酯预聚物单体质量的0.5~1%。
(2)将阳离子改性氯化聚丙烯聚合物溶解于四氢呋喃中,加入四氢呋喃体积3倍的水,然后使用均质机乳化5min,选择合适的真空度,加压旋蒸,将四氢呋喃蒸出回收循环利用,得到阳离子改性氯化聚丙烯聚合物乳液。
(3)在常温下将各组分混合,并在400~600rpm搅拌分散5~10min,混合均匀,制备得到水性聚丙烯薄膜涂覆用涂层。
本发明具有如下优点和有益效果:
本发明提供的一种水性聚丙烯薄膜涂覆用涂层含有石墨烯/聚苯胺复合颗粒作为丙烯酸酯pickering乳液的乳化剂,对丙烯酸酯预聚物具有良好的分散稳定性,并且复合颗粒赋予提成良好的耐磨性和抗静电作用;另外阳离子改性氯化聚丙烯使得涂层的抗静电性能进一步提高,且有效提高涂层对油墨的粘附性。
具体实施方式
下面结合具体实施例对本发明做进一步详细说明,但实施例并不对本发明做任何形式的限定。除非特别说明,本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
制备石墨烯/聚苯胺复合颗粒。
取30mg氧化石墨烯,超声分散在15mL水中,向该棕色的悬浮液中加入100mL的N,N-二甲基甲酰胺得到均匀的氧化石墨烯分散液。向该分散液中加入30μL的水合肼80℃下反应10h,得到黑色的石墨烯分散液,再与3g聚苯乙烯磺酸混合超声波处理12h得到稳定的黑色分散液。随后向聚苯乙烯磺酸稳定的石墨烯水分散液中加入150mg的苯胺单体,剧烈搅拌下加入50mg过硫酸铵引发苯胺聚合,在0℃下反应12h。通过抽滤和去离子水洗涤得到石墨烯/聚苯胺的复合颗粒。
实施例2
按重量份计,取氯化聚丙烯(含氯质量百分比30%)20份,二甲苯100份溶解于带有搅拌器、冷凝管的反应器中,搅拌30min,升温至70℃,加入丙烯酰氧乙基三甲基氯化铵0.8份,丙烯酸丁酯1.5份,丙烯酸甲酯0.5,过氧化苯甲酰1.1份,反应12h,纯化后制得阳离子改性氯化聚丙烯。
实施例3
按重量份计,取氯化聚丙烯(含氯质量百分比30%)20份,二甲苯100份溶解于带有搅拌器、冷凝管的反应器中,搅拌30min,升温至70℃,加入丙烯酰氧乙基三甲基氯化铵1.5份,丙烯酸丁酯1.5份,丙烯酸甲酯0.5份,过氧化苯甲酰1.1份,反应12h,纯化后制得阳离子改性氯化聚丙烯。
实施例4
按重量份计,取氯化聚丙烯(含氯质量百分比30%)20份,二甲苯100份溶解于带有搅拌器、冷凝管的反应器中,搅拌30min,升温至70℃,加入丙烯酰氧乙基三甲基氯化铵2.5份,丙烯酸丁酯1.5份,丙烯酸甲酯0.5份,过氧化苯甲酰1.1份,反应12h,纯化后制得阳离子改性氯化聚丙烯。
实施例5
一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
制备方法如下:
(1)将丙烯酸酯预聚物单体与过硫酸酸铵在50℃下加热混合成均一油相,降至常温备用;所述油相中各成分的质量比例如下:甲基丙烯酸:丙烯酸丁酯:丙烯酸异辛酯:丙烯腈:过硫酸酸铵=10:40:20:5:2。石墨烯/聚苯胺复合颗粒超声分散在水的总质量的60%的水中得到乳化剂分散液,往分散液中加入油相,然后使用均质机乳化5min,得到O/W型乳液;所述油相的质量等于配方中所述的丙烯酸酯预聚物的质量。将得到的乳液置于70℃水浴中静置反应13h,加入对苯二酚和四丁基溴化铵,搅拌均匀即得到丙烯酸酯预聚物pickering乳液。所述对苯二酚的加入量为丙烯酸酯预聚物单体质量的0.5%;四丁基溴化铵的加入量为丙烯酸酯预聚物单体质量的0.7%。
(2)将阳离子改性氯化聚丙烯聚合物溶解于四氢呋喃中,加入剩余的40%的水,然后使用均质机乳化5min,选择合适的真空度,在50℃下加压旋蒸,将四氢呋喃蒸出回收循环利用,得到阳离子改性氯化聚丙烯聚合物乳液。所述四氢呋喃的体积为水的1/3倍。
(3)在常温下混合丙烯酸酯预聚物pickering乳液、阳离子改性氯化聚丙烯聚合物乳液、在500rpm搅拌分散5min后,加入光引发剂、流平剂、消泡剂继续混合5min,制备得到水性聚丙烯薄膜涂覆用涂层。
实施例6
一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
制备过程同实施例5。
实施例7
一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
制备过程同实施例5。
实施例8
一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
制备过程同实施例5。
实施例9
一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
制备过程同实施例5。
实施例10
一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
制备过程同实施例5。
实施例11
一种水性聚丙烯薄膜涂覆用涂层,包括以下组分:
制备过程同实施例5。
对比例1
一种不含复合颗粒的涂层,包括以下组分:
制备方法如下:
(1)将丙烯酸酯预聚物单体与过硫酸酸铵在50℃下加热混合成均一油相,降至常温备用;所述油相中各成分的质量比例如下:甲基丙烯酸:丙烯酸丁酯:丙烯酸异辛酯:丙烯腈:过硫酸酸铵=10:40:20:5:2。称取十二烷基磺酸钠乳化剂溶于水的总质量的60%的水中得到乳化剂分散液(浓度为2wt%),往分散液中加入油相,然后使用均质机乳化5min,得到O/W型乳液;所述油相的质量等于配方中所述的丙烯酸酯预聚物的质量。将得到的乳液置于70℃水浴中静置反应13h,加入对苯二酚和四丁基溴化铵,搅拌均匀即得到丙烯酸酯预聚物乳液。所述对苯二酚的加入量为丙烯酸酯预聚物单体质量的0.5%;四丁基溴化铵的加入量为丙烯酸酯预聚物单体质量的0.7%。
(2)将阳离子改性氯化聚丙烯聚合物溶解于四氢呋喃中,加入剩余的40%的水,然后使用均质机乳化5min,选择合适的真空度,在50℃下加压旋蒸,将四氢呋喃蒸出回收循环利用,得到阳离子改性氯化聚丙烯聚合物乳液。所述四氢呋喃的体积为水的1/3倍。
(3)在常温下混合丙烯酸酯预聚物乳液、阳离子改性氯化聚丙烯聚合物乳液、在500rpm搅拌分散5min后,加入光引发剂、流平剂、消泡剂继续混合5min,制备得到涂层。
对比例2
一种不含阳离子改性氯化聚丙烯的涂层,包括以下组分:
制备方法如下:
(1)将丙烯酸酯预聚物单体与过硫酸酸铵在50℃下加热混合成均一油相,降至常温备用;所述油相中各成分的质量比例如下:甲基丙烯酸:丙烯酸丁酯:丙烯酸异辛酯:丙烯腈:过硫酸酸铵=10:40:20:5:2。石墨烯/聚苯胺复合颗粒超声分散在水的总质量的60%的水中得到乳化剂分散液,往分散液中加入油相,然后使用均质机乳化5min,得到O/W型乳液;所述油相的质量等于配方中所述的丙烯酸酯预聚物的质量。将得到的乳液置于70℃水浴中静置反应13h,加入对苯二酚和四丁基溴化铵,搅拌均匀即得到丙烯酸酯预聚物pickering乳液。所述对苯二酚的加入量为丙烯酸酯预聚物单体质量的0.5%;四丁基溴化铵的加入量为丙烯酸酯预聚物单体质量的0.7%。
(2)在常温下混合光引发剂、流平剂、消泡剂和剩余的40%的水,混合均匀后加入丙烯酸酯预聚物pickering乳液,在500rpm搅拌分散5min,制备得到水性聚丙烯薄膜涂覆用涂层。
对比例3
一种氯化聚丙烯和丙烯酸酯乳液复合涂层,包括以下组分:
制备方法如下:
(1)将丙烯酸酯预聚物单体与过硫酸酸铵在50℃下加热混合成均一油相,降至常温备用;所述油相中各成分的质量比例如下:甲基丙烯酸:丙烯酸丁酯:丙烯酸异辛酯:丙烯腈:过硫酸酸铵=10:40:20:5:2。称取十二烷基磺酸钠乳化剂溶于水的总质量的60%的水中得到乳化剂分散液(浓度为2wt%),往分散液中加入油相,然后使用均质机乳化5min,得到O/W型乳液;所述油相的质量等于配方中所述的丙烯酸酯预聚物的质量。将得到的乳液置于70℃水浴中静置反应13h,加入对苯二酚和四丁基溴化铵,搅拌均匀即得到丙烯酸酯预聚物乳液。所述对苯二酚的加入量为丙烯酸酯预聚物单体质量的0.5%;四丁基溴化铵的加入量为丙烯酸酯预聚物单体质量的0.7%。
(2)将氯化聚丙烯聚合物溶解于四氢呋喃中,加入剩余的40%的水,然后使用均质机乳化5min,选择合适的真空度,在50℃下加压旋蒸,将四氢呋喃蒸出回收循环利用,得到氯化聚丙烯乳液。所述四氢呋喃的体积为水的1/3倍。
(3)在常温下混合丙烯酸酯预聚物乳液、氯化聚丙烯乳液、在500rpm搅拌分散5min后,加入光引发剂、流平剂、消泡剂继续混合5min,制备得到涂层。
测试1:丙烯酸酯乳液钙离子稳定性
稳定性:量取16mL置于试管中,再滴加4ml浓度为0.5%的二氯化钙溶液,混合均匀后放置24h,观察乳液是否有絮凝或分层现象,若没有,则通过钙离子稳定性测试;
测试2:丙烯酸酯乳液储存稳定性
按照GB/T6753.3-1986《涂料储存稳定性试验方法》中的恒温干燥箱加速法测试。
待测试样为实施例5~11和对比例1~3步骤(1)制备的乳液,结果列于表1。
表1
测试3:附着力测试
无水乙醇对聚丙烯塑料板超声清洗30min,去除表面油渍、灰尘,采用30μm的涂膜器将涂层涂覆于聚丙烯塑料板上,干燥成膜。按照GB/T 9286-1998《色漆和清漆漆膜的划格试验》测试涂层在聚丙烯基材上的附着力,所用器材为深圳天友标准光源有限公司的附着力百格刀,涂层附着力=涂层拉掉剩余格数/整体涂层所有格数×100%。涂膜等级分为0级(最优)、1级、2级、3级、4级、5级(最次),测试结果列于表2。
测试4:涂层硬度测试
无水乙醇对聚丙烯塑料板超声清洗30min,去除表面油渍、灰尘,采用30μm的涂膜器将涂层涂覆于聚丙烯塑料板上,干燥成膜。采用东莞市勤兴检测仪器有限公司的QHQ铅笔硬度测试仪按GB/T 6739-1996《涂膜硬度铅笔测定法》测试涂膜的硬度,测试结果列于表2。
测试5:接触角测试(接触角越小,润湿性越好)
无水乙醇对聚丙烯塑料板超声清洗30min,去除表面油渍、灰尘,采用30μm的涂膜器将涂层涂覆于聚丙烯塑料板上,干燥成膜。采用上海中晨数学技术设备有限公司JC2000D型接触角测试仪测试接触角,结果列于表2。
表2
测试6:耐磨测试
将各待测涂层涂布与BOPP薄膜,方法如下:采用19μm的BOPP光膜为基材,使用专业涂布机,基材放卷电晕后,表面张力达到38dyn/cm,在薄膜的正反面涂布待测涂层,涂布量为20g/m2,置于波长为365nm的紫外箱中照射20s,吹干后得到待测涂布BOPP膜。
然后在1.8kg荷重下,包覆待测涂布BOPP膜的滑块来回摩擦纸皮表面(按照GB/T100606-1988的标准进行),待测涂布BOPP膜与纸皮表面接触,记录BOPP薄膜摩擦前后雾度(按照GB/T 2410-2008测试)变化值为1%的时间,结果列于表3。
测试7:表面电阻率
按照GB/T 1410-2006的方法测试待测涂布BOPP膜的表面电阻率,结果列于表3。
测试8:涂层对油墨的粘附性
采用平板印刷机在待测涂布BOPP膜上印刷图案后,静置30min后用3M 600#胶带测试油墨的粘附力,结果列于表3。
表3
以上内容是结合具体的优选技术方案对本发明所作的进一步详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的专业技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单推演或替换,都应当视为属于本发明的保护范围。
Claims (9)
1.一种水性聚丙烯薄膜涂覆用涂层,其特征在于,所述涂层包括以下组分:
石墨烯/聚苯胺复合颗粒2~6份;
阳离子改性氯化聚丙烯20~40份;
丙烯酸酯预聚物100份;
光引发剂1~3份;
流平剂0.1~2份;
消泡剂0.5~1.5份;
水200~400份;
所述石墨烯/聚苯胺复合颗粒制备方法如下:将氧化石墨烯分散在水和DMF的混合液中,加入水合肼,在80~100℃下反应6~12h得到石墨烯;将上述石墨烯分散液与聚苯乙烯磺酸混合超声处理12h,得到稳定的黑色分散液;在上述石墨烯分散液中加入一定量苯胺单体,搅拌情况下加入氧化剂过硫酸铵引发苯胺聚合,反应时间为5~10h,将反应后得到的混合液抽滤、去离子水洗涤,得到石墨烯/聚苯胺复合材料;
所述阳离子改性氯化聚丙烯制备方法如下:氯化聚丙烯与丙烯酰氧乙基三甲基氯化铵、丙烯酸丁酯、丙烯酸甲酯溶解于甲苯中,加入过氧化苯甲酰作为氧化催化剂,加热至60~80℃反应12h,纯化后得到阳离子改性氯化聚丙烯;
所述丙烯酸酯预聚物由以下一种或多种丙烯酸酯预聚物单体制备而成:甲基丙烯酸、丙烯酸、甲基丙烯酸丁酯、丙烯酸丁酯、丙烯酸甲酯、丙烯酸异辛酯、苯乙烯、丙烯腈、丁二烯、衣康酸。
2.根据权利要求1所述的一种水性聚丙烯薄膜涂覆用涂层,其特征在于,所述氧化石墨烯与水合肼的质量比例为1:1;聚苯乙烯磺酸和石墨烯的质量比为100:1,苯胺单体与石墨烯的质量比为5:1,苯胺单体与过硫酸铵的质量比为3:1。
3.根据权利要求1所述的一种水性聚丙烯薄膜涂覆用涂层,其特征在于,所述氯化聚丙烯的含氯质量百分比为30%;所述氯化聚丙烯、丙烯酰氧乙基三甲基氯化铵、丙烯酸丁酯、丙烯酸甲酯、过氧化苯甲酰的投料质量比为20:0.8~2.5:1.5:0.5:1.1。
4.根据权利要求1所述的一种水性聚丙烯薄膜涂覆用涂层,其特征在于,所述的光引发剂指α,α-二甲氧基-α-苯基苯乙酮、α,α-二乙氧基苯乙酮、2-苯基-2,2-二甲氨基-1-(4-吗啉苯基)-1-丁酮、2,4,6-三甲基苯甲酰膦酸二乙酯中的至少一种。
5.根据权利要求1所述的一种水性聚丙烯薄膜涂覆用涂层,其特征在于,所述流平剂指醋酸-丁酸纤维素和聚二甲基硅氧烷中的至少一种。
6.根据权利要求1所述的一种水性聚丙烯薄膜涂覆用涂层,其特征在于,所述消泡剂指甘油三羟基聚醚和磷酸三丁酯中的至少一种。
7.根据权利要求1所述的一种水性聚丙烯薄膜涂覆用涂层的制备方法,其特征在于,包括以下步骤:
(1)将石墨烯/聚苯胺复合颗粒超声分散在水中得到乳化剂分散液,往分散液中加入由丙烯酸酯预聚物单体和过硫酸铵构成的油相,然后使用均质机乳化5min,得到O/W型乳液;将得到的乳液置于60~80℃水浴中静置反应10~15h,加入对苯二酚和四丁基溴化铵,即得到丙烯酸酯预聚物pickering乳液;
(2)将阳离子改性氯化聚丙烯聚合物溶解于四氢呋喃中,加入四氢呋喃体积3倍的水,然后使用均质机乳化5min,选择合适的真空度,加压旋蒸,将四氢呋喃蒸出回收循环利用,得到阳离子改性氯化聚丙烯聚合物乳液;
(3)在常温下将各组分混合,并在400~600rpm搅拌分散5~10min,混合均匀,制备得到水性聚丙烯薄膜涂覆用涂层。
8.根据权利要求7所述的一种水性聚丙烯薄膜涂覆用涂层的制备方法,其特征在于,所述油相中过硫酸铵的质量分数为2~3%;对苯二酚的加入量为丙烯酸酯预聚物单体质量的0.2~1%;四丁基溴化铵的加入量为丙烯酸酯预聚物单体质量的0.5~1%。
9.根据权利要求7所述的一种水性聚丙烯薄膜涂覆用涂层的制备方法,其特征在于,所述油相制备方法如下:将丙烯酸酯预聚物单体与过硫酸酸铵在50℃下加热混合成均一油相,降至常温备用;所述油相中各成分的质量比例如下:甲基丙烯酸:丙烯酸丁酯:丙烯酸异辛酯:丙烯腈:过硫酸酸铵=10:40:20:5:2。
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