CN110982141A - 一种聚烯烃母粒及其制备方法 - Google Patents
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Abstract
本发明公开一种聚烯烃母粒,按照重量百分比100%计,由以下重量百分比的原料组成:聚烯烃70‑90%,碳纳米材料10‑20%,均质化促进剂0‑5%,耐候稳定剂0‑5%;其中,所述均质化促进剂为马来酸酐接枝聚乙烯、马来酸酐接枝聚丙烯、氧化聚乙烯蜡、聚乙烯改性石蜡、苯乙烯接枝聚丙烯中的至少一种。同时,本发明还公开所述聚烯烃母粒的制备方法。本发明提供的聚烯烃母粒,以聚烯烃作为基材,通过物理混合或化学键连融入碳纳米材料、均质化促进剂和耐候稳定剂,制备的聚烯烃母粒具有良好的导电、传热或力学性能,通过调节聚烯烃和碳纳米材料的比例可以获得同系列的梯级化聚烯烃产品。
Description
技术领域
本发明属于高分子材料技术领域,涉及改性聚烯烃复合材料,具体涉及一种聚烯烃母粒及其制备方法。
背景技术
以聚乙烯和聚丙烯为代表的聚烯烃属于热塑性聚合物,具有优良的电绝缘性、化学稳定性和生物安全性,且热成型性能好,但其热稳定性、耐老化性能、力学性能、耐候性差,限制了其在特定领域的应用。加之,目前国内市场上聚烯烃产品同质化严重、竞争激烈,缺乏高端附加值的特种产品,预计逐渐会由卖方市场转变为买方市场,产品利润率进一步下降。因此,急需对现有普通型的聚烯烃产能进行高端化、功能化深加工,以拓宽应用市场,提高产品收益。
以石墨烯和碳纳米管为代表的新型碳纳米材料,其独特的性能正好能弥补、改善或强化聚烯烃的固有缺陷,人们期望通过物理添加或化学结合的方式将其融入聚烯烃基材以改善其综合应用性能,如超高的弹性模量可改善聚烯烃的力学性能(弯曲模量、冲击强度、拉伸强度、弯曲强度、断裂伸长率等);超大的比表面积可降低聚烯烃对有机蒸汽的透过率,增强材料的密封性;优异的电学性能可以消除聚烯烃在成型和应用过程中的静电积聚,或制成特定用途的导电塑料;超高透光性和显著的界面效应能延缓聚烯烃材料在使用环境中的氧化、降解、老化等进程。碳纳米材料改性聚烯烃的可预见应用领域十分广泛,如侧重电学性能的电子/电器元件防静电包装、防腐胶带基材、油箱/管道抗静电防腐滚塑、防腐导静电涂料、电线电缆耐候增强包覆料等,侧重力学性能的车用轻量化替代产品(保险杠、挡泥板、仪表盘、内饰盖板、座椅、方向盘、立柱装饰等),具备缓冲、吸声、保温等性能的发泡基材,以及改善混凝土综合性能的聚烯烃纤维材料。
然而,多数碳纳米材料与聚烯烃的粘结性、相容性较差,直接混合显然难以达到功能化复合的目的。目前,针对二者的复合材料,国内外的相关研究主要涉及制备方法、溶剂、改性剂、复合添加剂等方面,有关的基础和应用研究热度很高,相关改性材料的专利很多、涉及面也比较广。但现有的改性聚烯烃复合材料存在以下主要问题:1)原料及添加剂的种类及比例固定,可变性差,适用性有限;2)聚烯烃基材及碳纳米材料的来源窄、价格高,如采用超高分子量(200万以上)聚乙烯、改性聚烯烃或极性聚烯烃类前体、改性石墨烯或极性石墨烯;3)所使用的添加剂差异性较小;4)聚烯烃并非唯一基材,碳纳米材料也并非主要改性剂,甚至仅是一种夹层材料。现有的聚烯烃基复合材料的制备方法也存在一些问题:首先,采用环境污染较大、成本较高且难以大规模生产的溶液混合法;其次,已有的熔融混合工艺中没有对聚烯烃和碳纳米材料进行预混/预分散,仅是将所有原料、添加剂同步共混加工,复合材料的均质性较差;最后,制备过程中仅使用一种混合机械,如挤出机/高速混合机/密炼机,难以实现碳纳米材料及添加剂在聚烯烃基材中的均匀分散。
发明内容
针对现有技术的缺陷,本发明提供一种聚烯烃母粒及其制备方法,实现了碳纳米材料和添加剂在聚烯烃中均匀分散。
一种聚烯烃母粒,按照重量百分比100%计,由以下重量百分比的原料组成:聚烯烃70-90 %,碳纳米材料 10-20 %,均质化促进剂 0-5 %,耐候稳定剂 0-5 %;
其中,所述均质化促进剂为马来酸酐接枝聚乙烯、马来酸酐接枝聚丙烯、氧化聚乙烯蜡、聚乙烯改性石蜡、苯乙烯接枝聚丙烯中的至少一种;所述均质化促进剂与聚烯烃相容度高,能挤占空间将其他添加物有效分隔,或在其他添加物与聚烯烃基体间架桥/成键,是促进聚烯烃产品均质化的重要物质。
优选地,所述苯乙烯接枝聚丙烯是通过以下方法制备得到的:将过氧化苯甲酰溶解于苯乙烯中,然后将其加入到聚丙烯粉末中,其中,苯乙烯与聚丙烯的质量比为1:(3-10),过氧化苯甲酰、苯乙烯和聚丙烯的质量和之比为1:(100-125),用氮气置换空气后密封,常温超声分散20-40min,然后在85-95℃下反应3-6h,将反应产物在索氏提取器中用乙酸乙酯抽提24-36 h,将得到的固相产物真空干燥至恒重即可。
优选地,所述耐候稳定剂为粉体亚磷酸酯、聚磷酸铵、季戊四醇硬脂酸酯、三聚氰胺聚磷酸盐中的至少一种;所述耐候稳定剂对热氧自由基链式反应和燃烧反应有抑制和阻断效果,是增强聚烯烃产品耐候性、安全性并延长使用寿命的重要物质。
优选地,所述聚烯烃为高密度聚乙烯、低密度聚乙烯、线性低密度聚乙烯、聚丙烯、聚1-丁烯、聚4-甲基-1-戊烯中的至少一种。
优选地,所述碳纳米材料为纳米石墨烯微片、单壁碳纳米管、多壁碳纳米管、纳米氧化石墨烯、碳纳米纤维中的至少一种;所述碳纳米材料在聚烯烃基体中均匀分散并相互搭接成网络结构,是提高聚烯烃产品电学、导热及力学性能的主要物质。
所述聚烯烃母粒的制备方法,包括以下步骤:
(1)将聚烯烃与碳纳米材料混合搅拌10-30 min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在100-130℃下空气干燥2-4 h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、均质化促进剂、耐候稳定剂加入密炼机,开启滚轴,在10-40 r/min的转速下升温至140-260℃,然后保温20-60 min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在130-250 ℃、10000-20000 r/min下搅拌5-10 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机挤出造粒,即可。
优选地,步骤(5)所述挤出造粒的具体工艺为:在120-240 ℃、15-50 r/min下挤出,然后在喂料速度10-20 r/min下用切粒机在100 -150 r/min下造粒。
本发明中聚烯烃和碳纳米材料作为可调变组分,通过调节二者的质量比例,可获得导电、传热或力学强化的差异化聚烯烃产品,使得最终制备的聚烯烃母粒为可调变功能型聚烯烃母粒。
本发明的优点:
本发明提供的聚烯烃母粒,原料易得,制备方法简单,以聚烯烃作为基材,通过物理混合或化学键连融入碳纳米材料、均质化促进剂和耐候稳定剂,制备的聚烯烃母粒具有良好的导电、传热或力学性能,通过调节聚烯烃和碳纳米材料的比例可以获得同系列的梯级化聚烯烃产品。
具体实施方式
实施例1
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃 70%,碳纳米材料20%,均质化促进剂5%,耐候稳定剂5%;
其中,所述聚烯烃为高密度聚乙烯;所述碳纳米材料为纳米石墨烯微片;所述均质化促进剂为马来酸酐接枝聚乙烯;所述耐候稳定剂为粉体亚磷酸酯;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌10min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在100℃下空气干燥4 h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、均质化促进剂、耐候稳定剂加入密炼机,开启滚轴,在10 r/min的转速下升温至150℃,然后保温60 min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在140℃、10000r/min下搅拌10 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在130℃、15r/min下挤出物料,然后在喂料速度10 r/min下用切粒机在100r/min下造粒,即可。
实施例2
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃 90%,碳纳米材料10%;
其中,所述聚烯烃为聚丙烯;所述碳纳米材料为纳米氧化石墨烯;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌30min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在130℃下空气干燥2 h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料加入密炼机,开启滚轴,在40 r/min的转速下升温至190℃,然后保温40 min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在180℃、15000r/min下搅拌8min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在170℃、30r/min下挤出物料,然后在喂料速度20 r/min下用切粒机在120r/min下造粒,即可。
实施例3
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃80%,碳纳米材料15%,均质化促进剂5%;
其中,所述聚烯烃为低密度聚乙烯;所述碳纳米材料为多壁碳纳米管;所述均质化促进剂为氧化聚乙烯蜡;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌20min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在100℃下空气干燥3 h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、均质化促进剂加入密炼机,开启滚轴,在20 r/min的转速下升温至140℃,然后保温30 min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在130℃、13000r/min下搅拌6 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在120℃、40r/min下挤出物料,然后在喂料速度15 r/min下用切粒机在140r/min下造粒,即可。
实施例4
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃 75%,碳纳米材料20%,耐候稳定剂5%;
其中,所述聚烯烃为聚1-丁烯;所述碳纳米材料为单壁碳纳米管;所述耐候稳定剂为聚磷酸铵;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌15min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在110℃下空气干燥2.5 h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、耐候稳定剂加入密炼机,开启滚轴,在30 r/min的转速下升温至150℃,然后保温20 min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在140℃、18000r/min下搅拌5 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在130℃、20r/min下挤出物料,然后在喂料速度12r/min下用切粒机在130r/min下造粒,即可。
实施例5
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃82%,碳纳米材料12%,均质化促进剂3%,耐候稳定剂3%;
其中,所述聚烯烃为聚4-甲基-1-戊烯;所述碳纳米材料为碳纳米纤维;所述均质化促进剂为马来酸酐接枝聚丙烯;所述耐候稳定剂为季戊四醇硬脂酸酯;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌25min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在130℃下空气干燥3.5h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、均质化促进剂、耐候稳定剂加入密炼机,开启滚轴,在25 r/min的转速下升温至260℃,然后保温50 min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在250℃、20000r/min下搅拌7min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在240℃、50r/min下挤出物料,然后在喂料速度10 r/min下用切粒机在150r/min下造粒,即可。
实施例6
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃 85%,碳纳米材料10%,均质化促进剂2%,耐候稳定剂3%;
其中,所述聚烯烃为线性低密度聚乙烯;所述碳纳米材料为纳米石墨烯微片;所述均质化促进剂为聚乙烯改性石蜡,采购自济南长泰化工有限公司;所述耐候稳定剂为三聚氰胺聚磷酸盐;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌10min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在100℃下空气干燥2h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、均质化促进剂、耐候稳定剂加入密炼机,开启滚轴,在35 r/min的转速下升温至140℃,然后保温35min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在130℃、12000r/min下搅拌9 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在120℃、35r/min下挤出物料,然后在喂料速度20 r/min下用切粒机在135r/min下造粒,即可。
实施例7
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃70%,碳纳米材料20%,均质化促进剂5%,耐候稳定剂5%;
其中,所述聚烯烃为质量比为4:3的高密度聚乙烯和聚丙烯的混合物;所述碳纳米材料为等比例的纳米石墨烯微片、多壁碳纳米管的混合物;所述均质化促进剂为质量比为3:2的马来酸酐接枝聚乙烯和苯乙烯接枝聚丙烯的混合物;所述耐候稳定剂为质量比2:3的粉体亚磷酸酯和季戊四醇硬脂酸酯的混合物;
其中,苯乙烯接枝聚丙烯是通过以下方法制备得到的:将过氧化苯甲酰溶解于苯乙烯中,然后将其加入到聚丙烯粉末中,其中,苯乙烯与聚丙烯的质量比为1:(3-10),过氧化苯甲酰、苯乙烯和聚丙烯的质量和之比为1:(100-125),用氮气置换空气后密封,常温超声分散20-40min,然后在85-95℃下反应3-6h,将反应产物在索氏提取器中用乙酸乙酯抽提24-36 h,将得到的固相产物真空干燥至恒重即可;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌20min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在110℃下空气干燥4h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、均质化促进剂、耐候稳定剂加入密炼机,开启滚轴,在15 r/min的转速下升温至180℃,然后保温30min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在170℃、14000r/min下搅拌5 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在160℃、25r/min下挤出物料,然后在喂料速度13 r/min下用切粒机在100r/min下造粒,即可。
实施例8
一种聚烯烃母粒,由以下重量百分比的原料组成:聚烯烃80%,碳纳米材料10%,均质化促进剂5%,耐候稳定剂5%;
其中,所述聚烯烃为质量比为2:3:3的高密度聚乙烯、低密度聚乙烯、线性低密度聚乙烯的混合物;所述碳纳米材料为质量比为3:4:3的单壁碳纳米管、多壁碳纳米管、碳纳米纤维的混合物;所述均质化促进剂为质量比为2:2:1的马来酸酐接枝聚乙烯、氧化聚乙烯蜡、聚乙烯改性石蜡的混合物;所述耐候稳定剂为质量比1:1:3的聚磷酸铵、季戊四醇硬脂酸酯、三聚氰胺聚磷酸盐的混合物;所述聚乙烯改性石蜡采购自济南长泰化工有限公司;
所述聚烯烃母粒的制备方法如下:
(1)将聚烯烃与碳纳米材料混合搅拌30min,在静电/范德华力的作用下,碳纳米材料会完全粘附在聚烯烃的表面;
(2)将步骤(1)得到的干混物料在100℃下空气干燥4h,去除其所吸附的水分;
(3)将步骤(2)得到的干燥物料、均质化促进剂、耐候稳定剂加入密炼机,开启滚轴,在10 r/min的转速下升温至150℃,然后保温55min,使混合物料在熔融态下均匀分散;
(4)将步骤(3)得到的密炼产物在140℃、10000r/min下搅拌10 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机,在135℃、30r/min下挤出物料,然后在喂料速度15 r/min下用切粒机在145r/min下造粒,即可。
性能检测
以各实施例中只含有聚烯烃,不添加碳纳米材料、均质化促进剂和耐候稳定剂的聚烯烃基材为对比例,分别对应对比例1-8,各实施例相对于各对比例的电导率、热变形温度和抗拉强度的提高值见表1。
表1 聚烯烃母粒的性能改善结果
Claims (7)
1.一种聚烯烃母粒,其特征在于:按照重量百分比100%计,由以下重量百分比的原料组成:聚烯烃 70-90 %,碳纳米材料 10-20 %,均质化促进剂 0-5 %,耐候稳定剂 0-5 %;
其中,所述均质化促进剂为马来酸酐接枝聚乙烯、马来酸酐接枝聚丙烯、氧化聚乙烯蜡、聚乙烯改性石蜡、苯乙烯接枝聚丙烯中的至少一种。
2.根据权利要求1所述聚烯烃母粒,其特征在于:所述苯乙烯接枝聚丙烯是通过以下方法制备得到的:将过氧化苯甲酰溶解于苯乙烯中,然后将其加入到聚丙烯粉末中,其中,苯乙烯与聚丙烯的质量比为1:(3-10),过氧化苯甲酰、苯乙烯和聚丙烯的质量和之比为1:(100-125),用氮气置换空气后密封,常温超声分散20-40min,然后在85-95℃下反应3-6h,将反应产物在索氏提取器中用乙酸乙酯抽提24-36 h,将得到的固相产物真空干燥至恒重即可。
3.根据权利要求1或2所述聚烯烃母粒,其特征在于:所述耐候稳定剂为粉体亚磷酸酯、聚磷酸铵、季戊四醇硬脂酸酯、三聚氰胺聚磷酸盐中的至少一种。
4.根据权利要求1或2所述聚烯烃母粒,其特征在于:所述聚烯烃为高密度聚乙烯、低密度聚乙烯、线性低密度聚乙烯、聚丙烯、聚1-丁烯、聚4-甲基-1-戊烯中的至少一种。
5.根据权利要求1或2所述聚烯烃母粒,其特征在于:所述碳纳米材料为纳米石墨烯微片、单壁碳纳米管、多壁碳纳米管、纳米氧化石墨烯、碳纳米纤维中的至少一种。
6.权利要求1或2所述聚烯烃母粒的制备方法,其特征在于:包括以下步骤:
(1)将聚烯烃与碳纳米材料混合搅拌10-30 min;
(2)将步骤(1)得到的干混物料在100-130℃下空气干燥2-4 h;
(3)将步骤(2)得到的干燥物料、均质化促进剂、耐候稳定剂加入密炼机,开启滚轴,在10-40 r/min的转速下升温至140-260℃,然后保温20-60 min;
(4)将步骤(3)得到的密炼产物在130-250 ℃、10000-20000 r/min下搅拌5-10 min;
(5)将步骤(4)得到的搅拌产物送入双螺杆挤出机挤出造粒,即可。
7.根据权利要求6所述聚烯烃母粒的制备方法,其特征在于:步骤(5)所述挤出造粒的具体工艺为:在120-240 ℃、15-50 r/min下挤出,然后在喂料速度10-20 r/min下用切粒机在100 -150 r/min下造粒。
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