CN103360759B - 一种发泡用高熔体强度聚酰胺材料及其制备方法 - Google Patents
一种发泡用高熔体强度聚酰胺材料及其制备方法 Download PDFInfo
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Abstract
本发明属于高分子材料技术领域,公开了一种发泡用高熔体强度聚酰胺材料及其制备方法。该材料由包括以下重量份的组分制成:聚酰胺100份,聚酯0~30份,玻璃纤维0~40份,相容剂0~10份,扩链剂0.3~3份和助剂0.2~2份。制备方法如下:称取100份聚酰胺、0‑30份聚酯、0‑10份相容剂、0.3‑3份扩链剂、0.2‑2份助剂高速混匀;将混合物和0‑40份玻璃纤维加入双螺杆挤出机挤出造粒,制得组合物;然后将组合物进行固相缩聚反应,得到聚酰胺材料。本发明的聚酰胺材料具有高强度,耐热、耐化学药品等优点。
Description
技术领域
本发明属于高分子材料技术领域,涉及一种发泡用高熔体强度聚酰胺材料及其制备方法。
背景技术
泡沫材料由于其内部存在大量的泡沫结构而具有质轻、隔热保温、吸音、减震等性能对于保护环境、节能减排具有非常重要的意义,而被广泛应用于社会生活的各个领域。市场上现有的发泡产品多为聚苯乙烯、PVC以及PP、PE等聚烯烃泡沫材料,然而这些材料大多存在力学性能不足、耐热性不高、长期使用稳定较低等问题。而聚酰胺材料本身因其具有高强度、高耐热、高耐疲劳、耐化学药品和耐油性突出等性能而被广泛的应用于制造业。然而普通的聚酰胺由于相对分子质量较低,约在两万以下,相对粘度较低2.3~2.6,熔融指数大,熔体强度极低,难以满足发泡材料的要求。聚酰胺发泡材料能够极大的扩展发泡材料的应用领域,并且聚酰胺材料的轻量化能够极大的减少能源消耗,具有较高的经济价值和社会价值。
发明内容
针对现有技术的缺陷,本发明的目的是提供一种发泡用高熔体强度聚酰胺材料,该材料具有高强度,耐热、耐化学药品等优点。
本发明的第二个目的是提供一种上述发泡用高熔体强度聚酰胺材料的制备方法。
本发明的技术方案如下:
本发明提供了一种发泡用高熔体强度聚酰胺材料,该材料由包括以下重量份的组分制成:
聚酰胺 100份,
聚酯 0~30份,
玻璃纤维 0~40份,
相容剂 0~10份,
扩链剂 0.3~3份,
助剂 0.2~2份。
所述的聚酰胺为聚己内酰胺(PA6)或聚己二酸己二胺(PA66)中的一种或一种以上。
所述的聚酯为聚对苯乙二醇酯(PET)或聚对苯丁二醇酯(PBT)中的一种或一种以上。
所述的玻璃纤维为无碱玻璃纤维,直径为6~18μm。
所述的相容剂为马来酸酐接枝聚丙烯(PP-g-MAH)、马来酸酐接枝乙烯-辛烯共聚物(POE-g-MAH)或丙烯酸缩水甘油酯接枝聚丙烯(PP-g-GMA)中的一种或一种以上。
所述的扩链剂选自聚乙二醇环氧树脂、双酚A二缩水甘油醚、1,3-双噁唑啉苯、1,4-双噁唑啉苯、2,6-甲苯二异氰酸酯(TDI)或二苯基甲烷二异氰酸酯(MDI)中的一种或一种以上。
所述的助剂选自抗氧剂或润滑剂中的一种或一种以上;其中:抗氧剂进一步选自磷酸氢二钠(H10)、N,N′-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺(1098)、三[2.4-二叔丁基苯基]亚磷酸酯(168)或四(2,4-二叔丁基苯基)4,4′-联苯基二亚磷酸酯(P-EPQ)中的一种或一种以上;润滑剂进一步选自乙撑双脂肪酸酰胺(TAF)、乙烯-丙烯酸共聚物、共聚物和褐煤酸衍生物(P12)或硅酮粉中的一种或一种以上。
本发明还提供了一种上述发泡用高熔体强度聚酰胺材料的制备方法,该方法包括以下步骤:
称取100份聚酰胺、0-30份聚酯、0-10份相容剂、0.3-3份扩链剂、0.2-2份助剂高速混匀;将混合物和0-40份玻璃纤维加入双螺杆挤出机挤出造粒,制得组合物;然后将组合物进行固相缩聚反应,得到聚酰胺材料。
所述的高速混匀的混合温度为50~75℃,混合时间为2~5min,混合速率为1500~3000rmp。
所述的玻璃纤维由双螺杆挤出机的侧喂料口加入。
所述的双螺杆挤出机自喂料口至挤出机模头的挤出温度分别是240~260℃,260~290℃,280~310℃,280~310℃,270~290℃,主机转速20~50Hz。
所述的固相缩聚的反应温度为200~245℃,反应时间为4~20h。
本发明与现有技术相比,具有以下优点和有益效果:
本发明克服了聚酰胺熔体强度低的缺点,提供了一种高熔体强度满足发泡要求的聚酰胺材料,制得的发泡材料强度更好,耐热、耐化学药品等性能更突出,同时聚酰胺材料的轻量化具有极大的经济价值和社会价值,有利于减少能源消耗,符合低碳经济和可持续发展的需要。
具体实施方式
以下结合实施例对本发明作进一步的说明。
实施列1
按照以下重量份称取原料:
聚酰胺(PA66) 100份,
扩链剂(双酚A二缩水甘油醚) 0.3份,
抗氧剂(H10) 0.2份;
按上述重量份的聚酰胺、扩链剂、抗氧剂投入高速混合机中混合温度为50℃,混合时间为3min,混合速率为1500rmp,高速混匀后,下料至双螺杆挤出机挤出机料斗,控制各区温度(自喂料口至挤出机模头)分别为260℃,280℃,300℃,300℃,285℃,主机转速50Hz,经双螺杆挤出机挤出造粒得到该组合物后;将组合物投入固相缩聚反应釜中,固相缩聚的反应温度为220℃,反应10h后,得到发泡用高熔体强度聚酰胺材料,其熔体强度见表1。
实施例2
按照以下重量份称取原料:
聚酰胺(PA66)100份,
聚酯(PET)30份,
无碱玻璃纤维(直径为7μm)40份,
相容剂(PP-g-MAH)10份,
扩链剂(1,3-双噁唑啉苯)3份,
抗氧剂10980.6份,
抗氧剂1680.3份,
硅酮粉11份;
按上述重量份的聚酰胺、聚酯、相容剂、扩链剂、助剂(1098、168、硅酮粉)投入高速混合机中混合温度为75℃,混合时间为5min,混合速率为2800rmp,高速混匀后,下料至双螺杆挤出机挤出机料斗,同时由双螺杆挤出机挤的侧喂料口加入玻璃纤维,控制各区温度(自喂料口至挤出机模头)分别为240℃,260℃,280℃,280℃,270℃,主机转速30Hz,经双螺杆挤出机挤出造粒得到该组合物后;将组合物投入固相缩聚反应釜中,固相缩聚的反应温度为210℃,反应12h后,得到发泡用高熔体强度聚酰胺材料,其熔体强度见表1。
实施例3
按照以下重量份称取原料:
聚酰胺(PA66)100份,
聚酯(PET)15份,
无碱玻璃纤维(直径为10μm)20份,
相容剂(POE-g-MAH)5份,
扩链剂(TDI)1.5份,
抗氧剂1098 0.4份,
抗氧剂P-EPQ 0.2份,
乙烯-丙烯酸共聚物0.5份;
按上述重量份的聚酰胺、聚酯、相容剂、扩链剂、助剂(1098,P-EPQ,乙烯-丙烯酸共聚物)投入高速混合机中混合温度为50℃,混合时间为2min,混合速率为3000rmp,高速混匀后,下料至双螺杆挤出机挤出机料斗,同时由双螺杆挤出机挤的侧喂料口加入玻璃纤维,控制各区温度(自喂料口至挤出机模头)分别为250℃,280℃,290℃,290℃,280℃,主机转速20Hz,经双螺杆挤出机挤出造粒得到该组合物后;将组合物投入固相缩聚反应釜中,固相缩聚的反应温度为245℃,反应4h后,得到发泡用高熔体强度聚酰胺材料,其熔体强度见表1。
实施例4
按照以下重量份称取原料:
聚酰胺(PA66) 80份,
聚酰胺(PA6) 20份,
无碱玻璃纤维(直径为13μm) 30份,
相容剂(PP-g-GMA) 8份,
扩链剂(MDI) 1份,
抗氧剂H10 0.2份,
润滑剂TAF 0.6份;
按上述重量份的聚酰胺、相容剂、扩链剂、助剂(H10,TAF)投入高速混合机中混合温度为60℃,混合时间为4min,混合速率为2000rmp,高速混匀后,下料至双螺杆挤出机挤出机料斗,同时由双螺杆挤出机挤的侧喂料口加入玻璃纤维,控制各区温度(自喂料口至挤出机模头)分别为250℃,280℃,290℃,290℃,280℃,主机转速40Hz,经双螺杆挤出机挤出造粒得到该组合物后;将组合物投入固相缩聚反应釜中,固相缩聚的反应温度为200℃,反应20h后,得到发泡用高熔体强度聚酰胺材料,其熔体强度见表1。
实施例5
按照以下重量份称取原料:
聚酰胺(PA6)100份,
聚酯(PBT)20份,
无碱玻璃纤维(直径为18μm)10份,
相容剂(POE-g-MAH)5份,
扩链剂(聚乙二醇环氧树脂)2份,
抗氧剂1098 0.6份,
抗氧剂168 0.3份,
乙烯-丙烯酸共聚物 0.5份;
按上述重量份的聚酰胺、聚酯、相容剂、扩链剂、助剂(1098,168,乙烯-丙烯酸共聚物)投入高速混合机中混合温度为70℃,混合时间为4min,混合速率为1800rmp,高速混匀后,下料至双螺杆挤出机挤出机料斗,同时由双螺杆挤出机挤的侧喂料口加入玻璃纤维,控制各区温度(自喂料口至挤出机模头)分别为260℃,280℃,290℃,290℃,280℃,主机转速50Hz,经双螺杆挤出机挤出造粒得到该组合物后;将组合物投入固相缩聚反应釜中,固相缩聚的反应温度为230℃,反应10h后,得到发泡用高熔体强度聚酰胺材料,其熔体强度见表1。
表1
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | |
熔体强度(N) | 1.47 | 1.52 | 1.60 | 1.54 | 1.61 |
由表1可知,本发明中所制备的发泡用高熔体强度聚酰胺材料,克服了熔体强度低的缺点,最大的熔体强度可以达到1.61N,满足了发泡要求,具有强度更好,耐热、耐化学药品等优点,同时聚酰胺材料的轻量化具有极大的经济价值和社会价值,有利于减少能源消耗,符合低碳经济和可持续发展的需要。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改,并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此,本发明不限于这里的实施例,本领域技术人员根据本发明的揭示,不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (4)
1.一种发泡用高熔体强度聚酰胺材料,其特征在于:该材料由以下重量份的组分制成:
所述的聚酰胺为聚己内酰胺或聚己二酸己二胺中的一种以上;
所述的聚酯为聚对苯二甲酸乙二醇酯或聚对苯二甲酸丁二醇酯中的一种以上;
所述的玻璃纤维为无碱玻璃纤维,直径为6~18μm;
所述的相容剂为丙烯酸缩水甘油酯接枝聚丙烯;
所述的扩链剂选自聚乙二醇环氧树脂、双酚A二缩水甘油醚、1,3-双噁唑啉苯、或1,4-双噁唑啉苯中的一种以上;
所述的助剂选自抗氧剂或润滑剂中的一种以上;抗氧剂选自磷酸氢二钠、N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺、三[2,4-二叔丁基苯基]亚磷酸酯或四(2,4-二叔丁基苯基)4,4′-联苯基二亚磷酸酯中的一种以上;
所述的发泡用高熔体强度聚酰胺材料的制备方法,其包括以下步骤:
称取100份聚酰胺、15-30份聚酯、5-10份相容剂、0.3-3份扩链剂、0.2-2份助剂高速混匀,得到混合物;将所述混合物和20-40份玻璃纤维加入双螺杆挤出机挤出造粒,制得组合物;然后将所述组合物进行固相缩聚反应,得到所述发泡用高熔体强度聚酰胺材料;
所述的高速混匀的混合温度为50~75℃,混合时间为2~5min,混合速率为1500~3000rmp;所述的玻璃纤维由双螺杆挤出机的侧喂料口加入。
2.根据权利要求1所述的发泡用高熔体强度聚酰胺材料,其特征在于:所述的润滑剂选自乙撑双脂肪酸酰胺、乙烯-丙烯酸共聚物和褐煤酸衍生物或硅酮粉中的一种以上。
3.一种如权利要求1或2所述的发泡用高熔体强度聚酰胺材料的制备方法,其特征在于:该方法包括以下步骤:
称取100份聚酰胺、15-30份聚酯、5-10份相容剂、0.3-3份扩链剂、0.2-2份助剂高速混匀,得到混合物;将所述混合物和20-40份玻璃纤维加入双螺杆挤出机挤出造粒,制得组合物;然后将所述组合物进行固相缩聚反应,得到所述聚酰胺材料;
所述的高速混匀的混合温度为50~75℃,混合时间为2~5min,混合速率为1500~3000rmp;所述的玻璃纤维由双螺杆挤出机的侧喂料口加入。
4.根据权利要求3所述的发泡用高熔体强度聚酰胺材料的制备方法,其特征在于:所述的双螺杆挤出机自喂料口至挤出机模头的挤出温度分别是240~260℃,260~290℃,280~310℃,280~310℃和270~290℃,主机转速20~50Hz;所述的固相缩聚的反应温度为200~245℃,反应时间为4~20h。
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