新型尼龙66的原位合成
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摘要
作为尼龙类工程塑料中消耗量最大的尼龙66具有强度高、刚性大、耐溶剂和使用温度范围广(-40～100℃)等优点,广泛地用于汽车制造、机械设备、电子电器、医疗器械和精密仪器等领域。但尼龙66也有不足之处,即低温和干态冲击强度低,吸水性强等。因此,通过改性,实现尼龙66的高性能化与功能化,进而促进相关行业的产品向高性能、高质量方向发展,具有重要的实际意义。
本文利用马来酸酐接枝聚乙烯-辛烯弹性体(POE-MAH)合成了带有POE长链的大分子二胺(POE-DHMA),并且用POE-DHMA作为尼龙66的单体代替部分己二胺(HMDA)制备新型尼龙66。
由于POE-MAH中马来酸酐的接枝率很低(＜0.9%),将其二胺化后难以进行结构表征。因此,本文采用聚异丁烯丁二酸酐(PIBSA)作为POE-MAH的模型,研究了PIBSA中丁二酸酐与HMDA反应的条件,以红外光谱表征产物结构。实验结果表明,当PIBSA与HMDA的摩尔比为1∶2,温度为60℃时,所得产物是带有聚异丁烯长链的大分子二胺。
利用PIBSA与HMDA反应所得规律,合成POE-DHMA,并用于制备新型尼龙66。利用差示扫描量热分析(DSC)、场发射扫描电镜(SEM),机械动态力学分析(DMTA)等测试手段对新型尼龙66的结构和性能进行了分析。结果表明,SEM照片中,原位形成的POE颗粒与尼龙66基体结合紧密,并且在用二甲苯刻蚀后,POE颗粒依然存在,说明POE弹性体聚合到尼龙66基体中。
As one of nylon engineering plastics, nylon 66 has the largest wastage. Nylon 66 has many excellent features, such as good intensity, high rigidity, solvent-resistance, wide temperature rage for usage(-40～100℃), et al. It is widely applied in the fields of car manufacture, mechanical apparatus, electrical wiring, medical appliance and fine instrument. But nylon 66 also has some poor performances such as insufficient in the Izod notched impact strength at low temperature and dry form, high water absorption and so on. So it has practical significance to achieve better properties and multi-functional nylon 66 products by modification.
Polyethylene-octane (POE) bearing an two primary amine groups (abbreviate as POE-DHMA) was prepared through a reaction of anhydride -functionalized POE (POE-MAH) with hexamethylenediamine (HMDA). A novel Nylon66 was prepared with the POE-DHMA as a macromere to replace some HMDA.
As the graft ratio of maleic anhydride (MAH) in POE-MAH is very low (less than 0.9%), it was difficult to analysis the product after the reaction of POE-MAH and HMDA by ordinary analyzing methods. So Polyisobutene succinic anhydride (PIBSA) was chosen as a model in order to study the rules of the reaction happened between polymer-g-MAH and HMDA under varied conditions. Then Infrar-red spectrometry (FTIR) was used to characteristic the different products. It was proved that, when PIBSA:HMDA=1:2, and the temperature controlled at 60℃, macrodiamine that with a PIB long chain can be got.
Thus POE-DHMA could be got by means of the rules mentioned above. At last, use it to synthesis the new PA66. Differential scanning calorimeter (DSC), dynamic mechanical thermal analyses (DMTA) and scanning electronic microscope (SEM) were used to investigate the microcosmic structure and the related properties of this new type PA66. The final study shown that, POE particles were combined with PA66 tightly, and they are still exist after eroding by xylene in the SEM photos, which indicated that POE elastomer were polymerized in-situ in the PA66 system.
本文利用马来酸酐接枝聚乙烯-辛烯弹性体(POE-MAH)合成了带有POE长链的大分子二胺(POE-DHMA),并且用POE-DHMA作为尼龙66的单体代替部分己二胺(HMDA)制备新型尼龙66。
由于POE-MAH中马来酸酐的接枝率很低(＜0.9%),将其二胺化后难以进行结构表征。因此,本文采用聚异丁烯丁二酸酐(PIBSA)作为POE-MAH的模型,研究了PIBSA中丁二酸酐与HMDA反应的条件,以红外光谱表征产物结构。实验结果表明,当PIBSA与HMDA的摩尔比为1∶2,温度为60℃时,所得产物是带有聚异丁烯长链的大分子二胺。
利用PIBSA与HMDA反应所得规律,合成POE-DHMA,并用于制备新型尼龙66。利用差示扫描量热分析(DSC)、场发射扫描电镜(SEM),机械动态力学分析(DMTA)等测试手段对新型尼龙66的结构和性能进行了分析。结果表明,SEM照片中,原位形成的POE颗粒与尼龙66基体结合紧密,并且在用二甲苯刻蚀后,POE颗粒依然存在,说明POE弹性体聚合到尼龙66基体中。
As one of nylon engineering plastics, nylon 66 has the largest wastage. Nylon 66 has many excellent features, such as good intensity, high rigidity, solvent-resistance, wide temperature rage for usage(-40～100℃), et al. It is widely applied in the fields of car manufacture, mechanical apparatus, electrical wiring, medical appliance and fine instrument. But nylon 66 also has some poor performances such as insufficient in the Izod notched impact strength at low temperature and dry form, high water absorption and so on. So it has practical significance to achieve better properties and multi-functional nylon 66 products by modification.
Polyethylene-octane (POE) bearing an two primary amine groups (abbreviate as POE-DHMA) was prepared through a reaction of anhydride -functionalized POE (POE-MAH) with hexamethylenediamine (HMDA). A novel Nylon66 was prepared with the POE-DHMA as a macromere to replace some HMDA.
As the graft ratio of maleic anhydride (MAH) in POE-MAH is very low (less than 0.9%), it was difficult to analysis the product after the reaction of POE-MAH and HMDA by ordinary analyzing methods. So Polyisobutene succinic anhydride (PIBSA) was chosen as a model in order to study the rules of the reaction happened between polymer-g-MAH and HMDA under varied conditions. Then Infrar-red spectrometry (FTIR) was used to characteristic the different products. It was proved that, when PIBSA:HMDA=1:2, and the temperature controlled at 60℃, macrodiamine that with a PIB long chain can be got.
Thus POE-DHMA could be got by means of the rules mentioned above. At last, use it to synthesis the new PA66. Differential scanning calorimeter (DSC), dynamic mechanical thermal analyses (DMTA) and scanning electronic microscope (SEM) were used to investigate the microcosmic structure and the related properties of this new type PA66. The final study shown that, POE particles were combined with PA66 tightly, and they are still exist after eroding by xylene in the SEM photos, which indicated that POE elastomer were polymerized in-situ in the PA66 system.
引文
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[3]汪晓东,金东吉,金日光.尼龙6/“壳-核”型聚合物共混合金的力学性能与亚微形态[J].高分子学报,1996,4(1):494-498
[4]樊孝玉,孟大维,吴秀玲.工程塑料尼龙66的增韧改性研究状况[J].广州化工,2004,32(4):46-8
[5]黄健,张云灿,陈俊峰,崔立青.热接枝法MEPDM对尼龙66的增韧行为[J].塑料工业,2000,28(5):13-14
[6]Lu Chengxiang,Chen Li,Wang Yanmei,Cai Xufu.Study on Ethylene-Propylene-Diene Mischpolymer/ Propylene Grafted with Maleic Anhydride and Its Application to Supertough Polyamid[J].Plastic Sci.& Technology,2006,34(2):26-31
[7]Zhang Baowei,Cui Yen,Sun Xinlong,.PA66 Toughened by EVA-g-MAH[J].Plastics Sci,& Technology,2003,4(1):24-26
[8]夏胜利,张云灿.机械力引发官能化POE及其增韧尼龙66的研究[J].南京工业大学学报,2004,26(5):63-67
[9]Tang Weihua,Hu Xiaoyi,Tang Jian,Jin Riguang.Toughening and Compatibilization of Polyphenylene Sulfide/Nylon 66 Blends with SEBS and Maleic Anhydride Grafted SEBS Triblock Copolymers[J].Appl Polym Sci,2007,106(1):2648-2655
[10]解孝林,李伯耿,潘祖仁.液晶共聚醑酰胺对PET/PA66的原位增容、增强、增韧作用[J].合成树脂及塑料,1999,16(4):8-11
[11]Chen Ye,Han Keqing,Lin Jianghin,Wang Linling,Yu Muhuo.Preparation of Nylon66/Montmorillonite Nanocomposites and Study on Their Structures and Properties[J].Application of Engineering Plastics,2002,30(12):5-7
[12]Kiss G.In situ composites:blends of isotropic polymers and thermotropic liquid crystalline polymers[J].Polym.Eng.Sci.,1987,27(6):410-423
[13]Liu Xiaohui,Wu Qiuju[J].Polyamide 66/Clay Nanocomposites via Melt Intercalation[J].Macromol.Mater.Eng.,2002,287(1):180-186
[14]卢会敏,徐翔民,李小红,张治军.尼龙66,纳米SiO2复合材料的形态和力学性能[J].塑料工业,2006,34(4):48-50
[15]曹有名,沈志刚,林尚安.sPS/PA66/g-sPS/纳米Al2O3粒子复合材料性能[J].中南大学学报(自然科学版),2004,35(4):544-547
[16]孟季茹,赵磊,梁国正,贾巧英.无机晶须在聚合物中的应用[J].化工新型材料,2001,29(12):1-6
[17]吕建通,隗学礼,赵宽放.钛酸钾晶须增强PA6的研究[J].工程塑料应用,1995,23(6):5-8
[18]Tjong S.C.,Meng Y.Z..Performance of potassium titanate whisker reinforced polyamide-6 composites[J].Polymer,1998,39(22):5461-5466
[19]魏学礼,赵宽放.晶须及其增强塑料复合材料[J].现代塑料加工应用,2001,13(6):52-56
[20]Li Ning,Gao Chenghui,Lin Youxi.The progress of research on reinforce resin composites with inorganic salt whisker[J].Inorganic Chemicals Inoustry,2006,38(6):8-11
[21]李长生,牟文斌,胡杰.MC尼龙/钛酸钾晶须复合材料制备及其摩擦学性能研究[J],2008,36(1):4-7
[22]杨宁,贵大勇,田军.晶须增强尼龙66及其合金力学性能研究[J].塑料,2006,35(2):14-17
[23]吕家桢,冯新,张云灿,陆小华.钛酸钾晶须—橡胶—尼龙66体系的力学性能[J].南京化工大学学报,2001,23(1):6-9
[24]Xu Zhaoyu.Research Progress of Whisker And its Application[J].Technology &Development of Chemical Industry,2005,34(2):11-17
[25]Liu Yaqin,Dong Juan.Preparation of Glass Fiber Reinforced Nylon 66 with High Impact Strength[J].Plastic SCi.& Tchnology,2002,8(1):16-18
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