CN105153692B - 一种可电镀性pa66‑ppo‑mpi工程塑料合金及其制备方法 - Google Patents
一种可电镀性pa66‑ppo‑mpi工程塑料合金及其制备方法 Download PDFInfo
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- CN105153692B CN105153692B CN201510489587.1A CN201510489587A CN105153692B CN 105153692 B CN105153692 B CN 105153692B CN 201510489587 A CN201510489587 A CN 201510489587A CN 105153692 B CN105153692 B CN 105153692B
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Abstract
本发明涉及一种可电镀性PA66‑PPO‑MPI工程塑料合金及其制备方法，工程塑料合金由PA66树脂、PPO树脂、MPI树脂、导电填料、相容剂和助剂组成。制备方法包括：(1)制备MPI树脂；(2)用偶联剂水溶液处理导电填料；(3)将PA66树脂、PPO树脂、MPI树脂、导电填料、相容剂和助剂混合，进行高温熔融混合，造粒，即得。本发明操作工艺简单，生产成本低，产品具有良好的电学性能、力学性能和耐高温性能等，综合性能优异，可应用于新能源汽车翼子板、门把手、保险杆等部件，具有广阔的应用前景。
Description
技术领域
本发明属于工程塑料合金领域，特别涉及一种可电镀性PA66-PPO-MPI工程塑料合金及其制备方法。
背景技术
工程塑料的发展势必是与各种高新技术密切相关，同时也是国家科技与工业水平的重要标志和物质基础。汽车工程塑料的用量是衡量一个国家汽车生产技术水平的标志之一。近30多年来，国际上汽车塑料的用量在不断增加。
目前新能源汽车的发展主要以节能降耗为宗旨，就必须要求汽车轻量化。而全世界范围内PA66/PPO合金材料主要生产是Sabic公司，其牌号是Noryl*GTX系列，它是聚酰胺(PA)和改性聚苯醚(PPO)的合金材料。它结合了PPO材料的尺寸稳定性、耐热性与PA聚合物的耐化学性和易加工特性。这使得此类本身具有良好耐化学性的材料，又具备了良好的硬度、抗撞击性和在线喷涂所要求的耐热性。
汽车车身、翼子板的塑料化就是汽车轻量化的一个重大突破。目前一般的合金工程塑料像PC/ABS、PC/PBT、PA/ABS、PA66/PPO合金等不能满足翼子板的生产加工，主要是缺点是：刚韧性不够，不能进行电镀，耐热低，尺寸不稳定。
尼龙是最重要的汽车工业用工程塑料。汽车零部件也是PA工程塑料最大的消费市场，超过总消费量的三分之一。随着人们对汽车性能要求的不断提高和PA工程塑料自身的发展，汽车用PA正呈逐年上升的趋势。汽车上可使用PA(包括改性产品)制作的部件有门把手、外壳、风扇、车轮罩、导流板、车内装饰、储水器材盖、线卡、各种车内电气接插件等。
改性PPO主要用于制作具有高强、高韧性和良好的电性能的汽车零部件，吸湿小，可用做汽车阀罩、燃油箱导电板、变压器和风力发动机叶片等。而PA66/PPO合金加工性良好，高强、高韧性、吸湿小可用做汽车外饰件的加工。
有关PA66/PPO合金的研究，已有许多公开的文献报道：
梁文虎等人【PPO/PA66合金体系基体的组成与性能关系的研究，北京化工大学机电工程学院的学位论文】，其主要特征在于：研究了聚苯醚(PPO)和尼龙66(PA66)两基体组成比例与合金性能之间的关系。结果表明，在增容剂TGDDM和SEBS-g-MA用量一定的情况下，两基体组份的质量配比为5:5时，共混体系具有较好的综合力学性能。
张伟的中国发明专利CN200910182012.X公开了一种搞抗冲击韧性PPE与PA66的塑料合金及其制备方法，其主要特征在于：本发明公开了一种合成高比浓对数粘度PPTA的方法，在超声波作用环境中，依次进行以下步骤，a.配制溶液体系，先将助溶剂搅拌溶解于极性溶剂中，然后再加入对苯二胺继续搅拌溶解，得溶液体系；b低温缩聚，将a步骤中所得溶液体系继续搅拌，在低温环境中，加入对苯二甲酰氯进行缩聚反应，随后加入酸吸收剂；c熟化，将b步骤中所得的体系转移到水浴中熟化，同时搅拌，最终得到颗粒均匀的高比浓对数粘度PPTA树脂；本发明提高PPTA的合成效率和PPTA的比浓对数粘度，并有助于降低成本。
徐东等人的中国发明专利ZL2010101405464公开了一种高强度PPO/PA66合金材料及其制备方法，其主要特征在于：高强度PPO/PA66合金材料按重量百分比由下述组分组成：聚苯醚树脂20％-40％；尼龙66树脂20％-40％；相容剂5％-10％；增韧剂5％-10％；玻璃纤维5％-15％；玻璃微珠5％-15％；云母粉5％-15％；抗氧剂0.2％-0.4％；其它助剂0.5％-1％。本发明通过采用玻璃纤维复合玻璃微珠，云母粉增强PPO/PA66合金，制得的材料综合性能优异，不仅强度高，耐热性好，易喷涂，同时还具有极佳的尺寸稳定性，翘曲率低，适合成型大型结构制件和受热部件。
聚酰亚胺开发于六十年代，最常用的一种是由均苯四甲酸二酐与芳香族二胺制得。聚酰亚胺分子中含有多重芳香杂环结构单元，因此其耐热性极佳，通常其玻璃化温度在260℃以上。聚酰亚胺树脂是具有极其优异耐热性的一类高分子材料。常规的聚酰亚胺结构，其热分解温度一般均在500℃以上，同时也具有强韧性。因此，也常常用于热固性树脂，如环氧树脂、双马来酰亚胺树脂等的耐热增韧改性剂。
有关聚酰亚胺材料的研究，已有不少公开的文献报道：
中国发明专利CN101921482A公开了一种热固性聚酰亚胺树脂及其制备方法，该树脂由A组分和B组分组成，其重量比为1：2-6；其中A组分为均相透明粘稠状的马来酰亚胺基聚酰亚胺树脂溶液，含固量10％-25％；B组分为四马来酰亚胺基双酚A溶液，含固量30％-40％；马来酰亚胺基聚酰亚胺树脂液(A组分)的制备方法包括如下两个步骤：(1)将2,2-双[4-(2,4-二氨基苯氧基)苯基]丙烷和强极性非质子有机溶剂放入反应釜中，室温下，搅拌溶解完全后，加入马来酸酐固体粉末，室温下搅拌至完全溶解，继续搅拌反应0.5小时后，加入芳香族二元酸酐，室温下搅拌反应5-8小时，获得均相透明粘稠状的树脂溶液；(2)加入共沸脱水剂，共沸回流分水搅拌反应6-8小时后，得到均相透明粘稠状的马来酰亚胺基聚酰亚胺树脂液；四马来酰亚胺基双酚A溶液(B组分)的制备方法包括如下两个步骤：(1)将2,2-双[4-(2,4-二氨基苯氧基)苯基]丙烷和强极性非质子有机溶剂放入反应釜中，室温下，搅拌溶解完全后，加入马来酸酐固体粉末，室温下搅拌至完全溶解，继续搅拌反应3小时后，获得均相透明溶液；(2)加入共沸脱水剂，共沸回流分水搅拌反应5小时后，得到均相透明的四马来酰亚胺基双酚A溶液。
本发明得到的热固性聚酰亚胺树脂不仅可应用于耐高温胶粘剂以及玻璃纤维增强的复合材料的基体树脂，而且也可应用于碳纤维、芳纶纤维等高性能纤维增强的先进复合材料的基体树脂。
中国发明专利CN101973147A公开了一种耐高温聚酰亚胺玻璃布层压板的制备方法，主要包括如下步骤：(1)室温下，将摩尔比为1:2的1,4-双(2,4-二氨基苯氧基)苯和马来酸酐加入强极性非质子有机溶剂中，室温下搅拌反应1小时后，加入芳香族二胺单体，搅拌溶解完全后，加入芳香族二元酸酐，室温下搅拌反应3小时，加入引发剂，搅拌溶解，得到均相透明的粘稠状树脂溶液，即A组分；(2)将摩尔比为1:4的1,4-双(2,4-二氨基苯氧基)苯和马来酸酐加入强极性非质子有机溶剂中，室温下搅拌反应2小时后，得到均相透明的树脂溶液，即B组分；(3)使用时，室温下将A、B组分混合均匀，得聚酰亚胺前驱体树脂溶液，用玻璃布浸渍树脂溶液，预烘半固化得半固化片，层叠后进入高温压机热固化，得到耐高温聚酰亚胺玻璃布层压板。
虞鑫海，许梅芳，樊良子【马来酰亚胺侧基聚酰亚胺薄膜的制备与性能研究，绝缘材料,2011,(4)；1-3】公开了一种马来酰亚胺侧基聚酰亚胺的制备及其性能研究，主要特征在于：利用2,2-双[4-(2,4-二氨基苯氧基)苯基]丙烷(BDAPPP)单体、马来酸酐(MA)、4,4’-二氨基二苯醚(44ODA)及3,3’,4,4’-四羧酸联苯二酐(BPDA)合成制得马来酰胺酸侧基的聚酰胺酸树脂(MPAA)溶液，经涂膜，热亚胺化，得到坚韧透明的马来酰亚胺侧基聚酰亚胺薄膜(MPI)，并对其性能进行研究。
虞鑫海的中国发明专利CN101560298A(2009-10-21)公开了一种热塑性含氟全芳型聚酰亚胺粉末及其制备方法，其主要特征在于：在催化剂的作用下，将含氟芳香族二元伯胺与芳香族二元酸酐在酚类溶剂中，反应5小时-10小时，趁热倒入高速搅拌状态下的沉析剂中，析出固体粉末，过滤、洗涤、浸泡、过滤、干燥，获得热塑性含氟全芳型聚酰亚胺粉末。本发明的热塑性含氟全芳型聚酰亚胺粉末可溶性好，是环氧树脂、不饱和聚酰亚胺树脂、不饱和聚酯树脂等热固性树脂的高性能耐热增韧改性剂，具有良好的应用前景，且操作简单、成本低、环境友好、适用于工业生产。
发明内容
本发明所要解决的技术问题是提供一种可电镀性PA66-PPO-MPI工程塑料合金及其制备方法，该方法操作工艺简单，生产成本低，产品具有良好的电学性能、力学性能和耐高温性能等，综合性能优异，可应用于新能源汽车翼子板、门把手、保险杆等部件，具有广阔的应用前景。
本发明的一种可电镀性PA66-PPO-MPI工程塑料合金，由质量比100:30-100:5-15:10-50:10-30:1-5的PA66树脂、PPO树脂、MPI树脂、导电填料、相容剂和助剂组成；其中，MPI树脂是由摩尔比1:2:7-12:5-10的1,4-双(2,4-二氨基苯氧基)苯、马来酸酐、芳香族二酐、芳香族二胺反应制得的马来酰亚胺基聚酰亚胺树脂。
所述的PA66树脂是由1,6-己二胺与1,6-己二酸通过缩聚反应而得的聚己二酰己二胺树脂。
所述的PPO树脂是由2,6-二甲基苯酚通过自身缩聚反应而成的聚苯醚树脂。
所述的导电填料选自石墨烯、导电炭黑、铜粉、铝粉、银粉、镍粉、镀银铜粉、镀银镍粉、镀银玻璃微珠中的一种或几种。
所述的相容剂选自马来酸酐接枝聚己二酰己二胺树脂、马来酸酐接枝聚苯醚树脂、马来酸酐接枝苯乙烯-乙烯-丁二烯-苯乙烯共聚物树脂中的一种或几种。
所述的助剂选自四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯、三(2,4-二叔丁基苯基)亚磷酸酯、2,6-二叔丁基-4-甲基苯酚、N,N’-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰基]己二胺、二(2-羟基-3-叔丁基-5-甲基苯基)甲烷、4,4’-硫代双(6-叔丁基间甲酚)、1,2-双(3,5-二叔丁基-4-羟基苯基)丙酸肼、硫代二丙酸二月桂酯、丁二酸与4-羟基-2,2,6,6-四甲基-1-哌啶醇的聚合物、双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(3,5-二叔丁基-4-羟基苄基磷酸单乙酯)镍、2,4-二羟基二苯甲酮、2-羟基-4-正辛氧基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-(2’-羟基-5’-甲基苯基)苯并三唑、2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯代苯并三唑、2-(2’-羟基-3’,5’-二戊基苯基)苯并三唑、2-(2’-羟基-5’-叔辛基苯基)苯并三唑、2-苯基苯并咪唑-5-磺酸、2-[2’-羟基-3’,5’-双(α,α-二甲基苄基)苯基]苯并三唑、2-(2H-苯并三唑-2-)-6-(十二烷基)-4-甲基苯酚中的一种或几种。
所述的芳香族二酐选自均苯四甲酸二酐、3,3’,4,4’-四羧基二苯醚二酐、3,3’,4,4’-四羧基联苯二酐、3,3’,4,4’-四羧基二苯甲酮二酐、3,3’,4,4’-四羧基二苯砜二酐、2,2-双(3,4-二羧基苯基)六氟丙烷二酐、2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐、2,2-双[4-(3,4-二羧基苯氧基)苯基]六氟丙烷二酐、1,4-双(3,4-二羧基苯氧基)苯二酐、1,3-双(3,4-二羧基苯氧基)苯二酐、4,4’-双(3,4-二羧基苯氧基)二苯砜二酐、4,4’-双(3,4-二羧基苯氧基)二苯甲酮二酐、4,4’-双(3,4-二羧基苯氧基)联苯二酐、4,4’-双(3,4-二羧基苯氧基)二苯醚二酐中的一种或几种。
所述的芳香族二胺选自对苯二胺、间苯二胺、邻苯二胺、甲基间苯二胺、三甲基间苯二胺、甲基对苯二胺、4,4’-二氨基二苯甲烷、3,3’-二甲基-4,4’-二氨基二苯甲烷、4,4’-二氨基二苯醚、3,4’-二氨基二苯醚、3,3’-二氨基二苯醚、4,4’-二氨基二苯砜、3,3’-二氨基二苯砜、4,4’-二氨基联苯、1,3-双(4-氨基苯氧基)苯、1,4-双(4-氨基苯氧基)苯、1,3-双(3-氨基苯氧基)苯、1,4-双(3-氨基苯氧基)苯、2,2-双[4-(4-氨基苯氧基)苯基]丙烷、2,2-双[4-(3-氨基苯氧基)苯基]丙烷、2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷、2,2-双[4-(3-氨基苯氧基)苯基]六氟丙烷、4,4’-双(4-氨基苯氧基)-3,3’,5,5’-四甲基联苯、4,4’-双(4-氨基苯氧基)联苯、4,4’-双(3-氨基苯氧基)联苯、4,4’-双(4-氨基苯氧基)二苯醚、4,4’-双(3-氨基苯氧基)二苯醚、4,4’-双(4-氨基苯氧基)二苯甲烷、4,4’-双(3-氨基苯氧基)二苯甲烷、4,4’-双(4-氨基苯氧基)二苯砜、4,4’-双(3-氨基苯氧基)二苯砜、2,2’-二(三氟甲基)-4,4’-二氨基联苯、1,4-双(2-三氟甲基-4-氨基苯氧基)苯、1,4-双(3-三氟甲基-4-氨基苯氧基)苯、1,3-双(2-三氟甲基-4-氨基苯氧基)苯、1,3-双(3-三氟甲基-4-氨基苯氧基)苯、2,2-双[4-(2-三氟甲基-4-氨基苯氧基)苯基]丙烷、2,2-双[4-(3-三氟甲基-4-氨基苯氧基)苯基]丙烷、2,2-双[4-(2-三氟甲基-4-氨基苯氧基)-2,6-二甲基苯基]丙烷、2,2-双[4-(3-三氟甲基-4-氨基苯氧基)-2,6-二甲基苯基]丙烷、2,2-双[4-(2-三氟甲基-4-氨基苯氧基)苯基]六氟丙烷、2,2-双[4-(3-三氟甲基-4-氨基苯氧基)苯基]六氟丙烷、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯甲烷、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯甲烷、4,4’-双(2-三氟甲基-4-氨基苯氧基)联苯、4,4’-双(3-三氟甲基-4-氨基苯氧基)-3,3’,5,5’-四甲基联苯、4,4’-双(2-三氟甲基-4-氨基苯氧基)联苯、4,4’-双(3-三氟甲基-4-氨基苯氧基)-3,3’,5,5’-四甲基联苯、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯醚、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯醚、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯砜、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯砜、4,4’-双(2-三氟甲基-4-氨基苯氧基)-3,3’,5,5’-四甲基二苯砜、4,4’-双(3-三氟甲基-4-氨基苯氧基)-3,3’,5,5’-四甲基二苯砜、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯硫醚、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯硫醚、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯甲酮、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯甲酮的一种或几种。
本发明的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，包括如下步骤：
(1)将1,4-双(2,4-二氨基苯氧基)苯和强极性非质子有机溶剂加入反应釜中，室温下搅拌溶解后，冰水浴冷却至5℃以下，加入马来酸酐和芳香族二酐，搅拌反应1小时-2小时后，加入芳香族二胺，继续搅拌反应2.5小时-4小时，随后加入脱水剂和催化剂，移去冰水浴，加热升温至90℃-100℃，搅拌反应4小时-8小时，加入沉析剂，搅拌1小时，过滤，用丙酮洗涤2次-3次，90℃真空干燥，得到MPI树脂；
(2)用偶联剂水溶液处理导电填料，其具体工艺为：将偶联剂水溶液和导电填料放入反应釜中，于60℃-80℃搅拌1小时-2小时后，冷却至室温，过滤，于100℃下干燥1小时-2小时，即得到偶联剂处理的导电填料；其中，偶联剂水溶液与导电填料的质量比为4-8:1；
(3)将PA66树脂、PPO树脂、MPI树脂、导电填料、相容剂和助剂混合，采用双螺杆挤出机，在270℃-290℃进行高温熔融混合，造粒，得到可电镀性PA66-PPO-MPI工程塑料合金。
所述步骤(1)中的强极性非质子有机溶剂选自N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基-2-吡咯烷酮、N-乙基-2-吡咯烷酮、二甲基亚砜中的一种或几种；其中，强极性非质子有机溶剂与总反应物的质量比为3-5：1；总反应物的质量是指1,4-双(2,4-二氨基苯氧基)苯、马来酸酐、芳香族二酐和芳香族二胺的质量之和。
所述步骤(1)中的脱水剂选自乙酸酐、丙酸酐、丁酸酐、三氟醋酐、氯代乙酸酐、二环己基碳二亚胺中的一种或几种；其中，脱水剂与芳香族二酐的摩尔比为2.5-3.5:1。
所述步骤(1)中的催化剂选自三乙胺、三丁胺、吡啶、甲基吡啶、二甲基吡啶、联吡啶、甲基联吡啶中的一种或几种；其中，催化剂与芳香族二酐的摩尔比为0.01-0.1:1。
所述步骤(1)中的沉析剂选自甲醇、乙醇、丙醇、异丙醇、乙二醇、乙二醇单甲醚、乙二醇二甲醚、乙二醇单乙醚、乙二醇二乙醚、甲乙酮中的一种或几种；其中，沉析剂与强极性非质子有机溶剂的质量比为2-5：1。
所述步骤(1)中的丙酮与强极性非质子有机溶剂的质量比为0.5-1:1。
所述步骤(2)中的偶联剂水溶液的质量百分比浓度为1％～10％。
所述的偶联剂选自3-氨丙基三乙氧基硅烷、3-氨丙基三甲氧基硅烷、环氧丙氧基丙基三乙氧基硅烷、环氧丙氧基三甲基氧基硅烷中的一种或几种。
有益效果
(1)本发明的制备工艺简单、成本低、操作方便，反应原料来源方便，可以在通用设备中完成制备过程，有利于实现工业化生产；
(2)本发明具有良好的综合性能，具有高的耐温性、成型加工性、优异的电学性能和力学性能等；
(3)本发明可应用于新能源汽车翼子板、门把手、保险杆等部件，具有广阔的应用前景。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
将32.2克(0.1摩尔)1,4-双(2,4-二氨基苯氧基)苯和1245克N,N-二甲基乙酰胺加入反应釜中，室温下搅拌溶解后，冰水浴冷却至5℃以下，加入19.6克(0.2摩尔)马来酸酐和217.0克(0.7摩尔)3,3’,4,4’-四羧基二苯醚二酐，搅拌反应1小时后，加入146.0克(0.5摩尔)1,3-双(4-氨基苯氧基)苯，继续搅拌反应4小时，随后加入183.6克(1.8摩尔)乙酸酐和0.65克(0.007摩尔)甲基吡啶，移去冰水浴，加热升温至100℃，搅拌反应4小时，加入2490克甲醇，快速搅拌1小时，过滤，用625克丙酮洗涤2次-3次，90℃真空干燥3小时，得到384.5克MPI树脂(理论产量为389.6克)，记作MPI-1，收率为98.7％。
实施例2
将32.2克(0.1摩尔)1,4-双(2,4-二氨基苯氧基)苯、3000克N-甲基-2-吡咯烷酮和690克N,N-二甲基甲酰胺加入反应釜中，室温下搅拌溶解后，冰水浴冷却至5℃以下，加入19.6克(0.2摩尔)马来酸酐、260.2克(0.5摩尔)2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐和217.0克(0.7摩尔)3,3’,4,4’-四羧基二苯醚二酐，搅拌反应2小时后，加入180.0克(0.9摩尔)3,4’-二氨基二苯醚和29.2克(0.1摩尔)1,3-双(3-氨基苯氧基)苯，继续搅拌反应2.5小时，随后加入428.4克(4.2摩尔)乙酸酐和9.48克(0.12摩尔)吡啶，移去冰水浴，加热升温至90℃，搅拌反应8小时，加入18450克乙醇，快速搅拌1小时，过滤，用3690克丙酮洗涤2次-3次，90℃真空干燥5小时，得到689.4克MPI树脂(理论产量为695.0克)，记作MPI-2，收率为99.2％。
实施例3
将400克质量百分比浓度为1％的3-氨丙基三乙氧基硅烷水溶液、50.0克镀银铜粉和50.0克银粉放入反应釜中，于60℃下搅拌1小时后，冷却至室温，过滤，于100℃下干燥1小时，即得到100.0克偶联剂处理的导电填料，记作ECF-1。
将400克质量百分比浓度为3％的3-氨丙基三乙氧基硅烷水溶液、60.0克镀银铜粉和40.0克铝粉放入反应釜中，于80℃下搅拌2小时后，冷却至室温，过滤，于100℃下干燥2小时，即得到100.0克偶联剂处理的导电填料，记作ECF-2。
将800克质量百分比浓度为5％的环氧丙氧基丙基三乙氧基硅烷水溶液、30.0克石墨烯粉末和70.0克镀银玻璃微珠放入反应釜中，于70℃下搅拌2小时后，冷却至室温，过滤，于100℃下干燥2小时，即得到100.0克偶联剂处理的导电填料，记作ECF-3。
将800克质量百分比浓度为10％的环氧丙氧基丙基三乙氧基硅烷水溶液、20.0克石墨烯粉末和80.0克银粉放入反应釜中，于80℃搅拌1小时后，冷却至室温，过滤，于100℃下干燥1小时，即得到100.0克偶联剂处理的导电填料，记作ECF-4。
实施例4
将1000克PA66树脂、300克PPO树脂、50克MPI-1树脂、100克ECF-1导电填料、50克马来酸酐接枝聚己二酰己二胺树脂和50克马来酸酐接枝聚苯醚树脂、5克四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯和5克2-(2’-羟基-5’-甲基苯基)苯并三唑混合，采用双螺杆挤出机，在270℃进行高温熔融混合，造粒，得到1560克可电镀性PA66-PPO-MPI工程塑料合金，记作PPMA-1。其性能数据如表1所示。
将1000克PA66树脂、500克PPO树脂、50克MPI-1树脂、50克MPI-2树脂、100克ECF-2导电填料、100克ECF-3导电填料、100克ECF-4导电填料、120克马来酸酐接枝聚己二酰己二胺树脂和80克马来酸酐接枝聚苯醚树脂、18克三(2,4-二叔丁基苯基)亚磷酸酯和12克2-(2’-羟基-5’-叔辛基苯基)苯并三唑混合，采用双螺杆挤出机，在280℃进行高温熔融混合，造粒，得到2130克可电镀性PA66-PPO-MPI工程塑料合金，记作PPMA-2。其性能数据如表1所示。
将1000克PA66树脂、1000克PPO树脂、50克MPI-1树脂、100克MPI-2树脂、300克ECF-1导电填料、200克ECF-3导电填料、200克马来酸酐接枝聚己二酰己二胺树脂和100克马来酸酐接枝聚苯醚树脂、10克四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、20克1,2-双(3,5-二叔丁基-4-羟基苯基)丙酸肼和20克2-(2’-羟基-5’-甲基苯基)苯并三唑混合，采用双螺杆挤出机，在290℃进行高温熔融混合，造粒，得到3000克可电镀性PA66-PPO-MPI工程塑料合金，记作PPMA-3。其性能数据如表1所示。
表1 可电镀性PA66-PPO-MPI工程塑料合金的性能数据
Claims (15)
1.一种可电镀性PA66-PPO-MPI工程塑料合金，其特征在于：由质量比100:30-100:5-15:10-50:10-30:1-5的PA66树脂、PPO树脂、MPI树脂、导电填料、相容剂和助剂组成；其中，MPI树脂是由摩尔比1:2:7-12:5-10的1,4-双(2,4-二氨基苯氧基)苯、马来酸酐、芳香族二酐、芳香族二胺反应制得的马来酰亚胺基聚酰亚胺树脂；制备方法包括：将1,4-双(2,4-二氨基苯氧基)苯和强极性非质子有机溶剂加入反应釜中，室温下搅拌溶解后，冰水浴冷却至5℃以下，加入马来酸酐和芳香族二酐，搅拌反应1小时-2小时后，加入芳香族二胺，继续搅拌反应2.5小时-4小时，随后加入脱水剂和催化剂，移去冰水浴，加热升温至90℃-100℃，搅拌反应4小时-8小时，加入沉析剂，搅拌1小时，过滤，用丙酮洗涤2次-3次，90℃真空干燥，得到MPI树脂；
助剂选自四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯、三(2,4-二叔丁基苯基)亚磷酸酯、2,6-二叔丁基-4-甲基苯酚、N,N’-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰基]己二胺、二(2-羟基-3-叔丁基-5-甲基苯基)甲烷、4,4’-硫代双(6-叔丁基间甲酚)、1,2-双(3,5-二叔丁基-4-羟基苯基)丙酸肼、硫代二丙酸二月桂酯、丁二酸与4-羟基-2,2,6,6-四甲基-1-哌啶醇的聚合物、双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、双(3,5-二叔丁基-4-羟基苄基磷酸单乙酯)镍、2,4-二羟基二苯甲酮、2-羟基-4-正辛氧基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-(2’-羟基-5’-甲基苯基)苯并三唑、2-(2’-羟基-3’-叔丁基-5’-甲基苯基)-5-氯代苯并三唑、2-(2’-羟基-3’,5’-二戊基苯基)苯并三唑、2-(2’-羟基-5’-叔辛基苯基)苯并三唑、2-苯基苯并咪唑-5-磺酸、2-[2’-羟基-3’,5’-双(α,α-二甲基苄基)苯基]苯并三唑、2-(2H-苯并三唑-2-)-6-(十二烷基)-4-甲基苯酚中的一种或几种。
2.根据权利要求1所述的一种可电镀性PA66-PPO-MPI工程塑料合金，其特征在于：所述的PA66树脂是由1,6-己二胺与1,6-己二酸通过缩聚反应而得的聚己二酰己二胺树脂。
3.根据权利要求1所述的一种可电镀性PA66-PPO-MPI工程塑料合金，其特征在于：所述的PPO树脂是由2,6-二甲基苯酚通过自身缩聚反应而成的聚苯醚树脂。
4.根据权利要求1所述的一种可电镀性PA66-PPO-MPI工程塑料合金，其特征在于：所述的导电填料选自石墨烯、导电炭黑、铜粉、铝粉、银粉、镍粉、镀银铜粉、镀银镍粉、镀银玻璃微珠中的一种或几种。
5.根据权利要求1所述的一种可电镀性PA66-PPO-MPI工程塑料合金，其特征在于：所述的相容剂选自马来酸酐接枝聚己二酰己二胺树脂、马来酸酐接枝聚苯醚树脂、马来酸酐接枝苯乙烯-乙烯-丁二烯-苯乙烯共聚物树脂中的一种或几种。
6.根据权利要求1所述的一种可电镀性PA66-PPO-MPI工程塑料合金，其特征在于：所述的芳香族二酐选自均苯四甲酸二酐、3,3’,4,4’-四羧基二苯醚二酐、3,3’,4,4’-四羧基联苯二酐、3,3’,4,4’-四羧基二苯甲酮二酐、3,3’,4,4’-四羧基二苯砜二酐、2,2-双(3,4-二羧基苯基)六氟丙烷二酐、2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐、2,2-双[4-(3,4-二羧基苯氧基)苯基]六氟丙烷二酐、1,4-双(3,4-二羧基苯氧基)苯二酐、1,3-双(3,4-二羧基苯氧基)苯二酐、4,4’-双(3,4-二羧基苯氧基)二苯砜二酐、4,4’-双(3,4-二羧基苯氧基)二苯甲酮二酐、4,4’-双(3,4-二羧基苯氧基)联苯二酐、4,4’-双(3,4-二羧基苯氧基)二苯醚二酐中的一种或几种。
7.根据权利要求1所述的一种可电镀性PA66-PPO-MPI工程塑料合金，其特征在于：所述的芳香族二胺选自对苯二胺、间苯二胺、邻苯二胺、甲基间苯二胺、三甲基间苯二胺、甲基对苯二胺、4,4’-二氨基二苯甲烷、3,3’-二甲基-4,4’-二氨基二苯甲烷、4,4’-二氨基二苯醚、3,4’-二氨基二苯醚、3,3’-二氨基二苯醚、4,4’-二氨基二苯砜、3,3’-二氨基二苯砜、4,4’-二氨基联苯、1,3-双(4-氨基苯氧基)苯、1,4-双(4-氨基苯氧基)苯、1,3-双(3-氨基苯氧基)苯、1,4-双(3-氨基苯氧基)苯、2,2-双[4-(4-氨基苯氧基)苯基]丙烷、2,2-双[4-(3-氨基苯氧基)苯基]丙烷、2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷、2,2-双[4-(3-氨基苯氧基)苯基]六氟丙烷、4,4’-双(4-氨基苯氧基)-3,3’,5,5’-四甲基联苯、4,4’-双(4-氨基苯氧基)联苯、4,4’-双(3-氨基苯氧基)联苯、4,4’-双(4-氨基苯氧基)二苯醚、4,4’-双(3-氨基苯氧基)二苯醚、4,4’-双(4-氨基苯氧基)二苯甲烷、4,4’-双(3-氨基苯氧基)二苯甲烷、4,4’-双(4-氨基苯氧基)二苯砜、4,4’-双(3-氨基苯氧基)二苯砜、2,2’-二(三氟甲基)-4,4’-二氨基联苯、1,4-双(2-三氟甲基-4-氨基苯氧基)苯、1,4-双(3-三氟甲基-4-氨基苯氧基)苯、1,3-双(2-三氟甲基-4-氨基苯氧基)苯、1,3-双(3-三氟甲基-4-氨基苯氧基)苯、2,2-双[4-(2-三氟甲基-4-氨基苯氧基)苯基]丙烷、2,2-双[4-(3-三氟甲基-4-氨基苯氧基)苯基]丙烷、2,2-双[4-(2-三氟甲基-4-氨基苯氧基)-2,6-二甲基苯基]丙烷、2,2-双[4-(3-三氟甲基-4-氨基苯氧基)-2,6-二甲基苯基]丙烷、2,2-双[4-(2-三氟甲基-4-氨基苯氧基)苯基]六氟丙烷、2,2-双[4-(3-三氟甲基-4-氨基苯氧基)苯基]六氟丙烷、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯甲烷、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯甲烷、4,4’-双(2-三氟甲基-4-氨基苯氧基)联苯、4,4’-双(3-三氟甲基-4-氨基苯氧基)-3,3’,5,5’-四甲基联苯、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯醚、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯醚、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯砜、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯砜、4,4’-双(2-三氟甲基-4-氨基苯氧基)-3,3’,5,5’-四甲基二苯砜、4,4’-双(3-三氟甲基-4-氨基苯氧基)-3,3’,5,5’-四甲基二苯砜、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯硫醚、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯硫醚、4,4’-双(2-三氟甲基-4-氨基苯氧基)二苯甲酮、4,4’-双(3-三氟甲基-4-氨基苯氧基)二苯甲酮的一种或几种。
8.一种如权利要求1所述的可电镀性PA66-PPO-MPI工程塑料合金的制备方法，包括如下步骤：
(1)将1,4-双(2,4-二氨基苯氧基)苯和强极性非质子有机溶剂加入反应釜中，室温下搅拌溶解后，冰水浴冷却至5℃以下，加入马来酸酐和芳香族二酐，搅拌反应1小时-2小时后，加入芳香族二胺，继续搅拌反应2.5小时-4小时，随后加入脱水剂和催化剂，移去冰水浴，加热升温至90℃-100℃，搅拌反应4小时-8小时，加入沉析剂，搅拌1小时，过滤，用丙酮洗涤2次-3次，90℃真空干燥，得到MPI树脂；
(2)用偶联剂水溶液处理导电填料，其具体工艺为：将偶联剂水溶液和导电填料放入反应釜中，于60℃-80℃搅拌1小时-2小时后，冷却至室温，过滤，于100℃下干燥1小时-2小时，即得到偶联剂处理的导电填料；其中，偶联剂水溶液与导电填料的质量比为4-8:1；
(3)将PA66树脂、PPO树脂、MPI树脂、导电填料、相容剂和助剂混合，采用双螺杆挤出机，在270℃-290℃进行高温熔融混合，造粒，得到可电镀性PA66-PPO-MPI工程塑料合金。
9.根据权利要求8所述的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，其特征在于：所述步骤(1)中的强极性非质子有机溶剂选自N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基-2-吡咯烷酮、N-乙基-2-吡咯烷酮、二甲基亚砜中的一种或几种；其中，强极性非质子有机溶剂与总反应物的质量比为3-5：1；总反应物的质量是指1,4-双(2,4-二氨基苯氧基)苯、马来酸酐、芳香族二酐和芳香族二胺的质量之和。
10.根据权利要求8所述的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，其特征在于：所述步骤(1)中的脱水剂选自乙酸酐、丙酸酐、丁酸酐、三氟醋酐、氯代乙酸酐、二环己基碳二亚胺中的一种或几种；其中，脱水剂与芳香族二酐的摩尔比为2.5-3.5:1。
11.根据权利要求8所述的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，其特征在于：所述步骤(1)中的催化剂选自三乙胺、三丁胺、吡啶、甲基吡啶、二甲基吡啶、联吡啶、甲基联吡啶中的一种或几种；其中，催化剂与芳香族二酐的摩尔比为0.01-0.1:1。
12.根据权利要求8所述的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，其特征在于：所述步骤(1)中的沉析剂选自甲醇、乙醇、丙醇、异丙醇、乙二醇、乙二醇单甲醚、乙二醇二甲醚、乙二醇单乙醚、乙二醇二乙醚、甲乙酮中的一种或几种；其中，沉析剂与强极性非质子有机溶剂的质量比为2-5：1。
13.根据权利要求8所述的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，其特征在于：所述步骤(1)中的丙酮与强极性非质子有机溶剂的质量比为0.5-1:1。
14.根据权利要求8所述的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，其特征在于：所述步骤(2)中的偶联剂水溶液的质量百分比浓度为1％～10％。
15.根据权利要求14所述的一种可电镀性PA66-PPO-MPI工程塑料合金的制备方法，其特征在于：所述的偶联剂选自3-氨丙基三乙氧基硅烷、3-氨丙基三甲氧基硅烷、环氧丙氧基丙基三乙氧基硅烷、环氧丙氧基三甲基氧基硅烷中的一种或几种。
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Inventor after: Yu Xinhai Inventor after: Wang Jing Inventor after: Qian Mingjuan Inventor before: Yu Xinhai |
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Effective date of registration: 20160509 Address after: 201620 Shanghai Songjiang new town, North Renmin Road, No. 2999, No. Applicant after: Donghua University Applicant after: Polystar Engineering Plastics (Shanghai) Co., Ltd. Address before: 201620 Shanghai Songjiang new town, North Renmin Road, No. 2999, No. Applicant before: Donghua University |
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Effective date of registration: 20210624 Address after: Room 102, building 1, 299 Zhongchen Road, Songjiang District, Shanghai, 201613 Patentee after: Shanghai Juwei New Material Co.,Ltd. Address before: 201620 No. 2999 North Renmin Road, Songjiang new town, Songjiang District, Shanghai. Patentee before: DONGHUA University Patentee before: POLYSTAR ENGINEERING PLASTICS (SHANGHAI) Co.,Ltd. |
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