磷酸-氨水蒸沉γ晶型聚酰胺6的热行为研究  

Investigation of Thermal Behaviors of γ-Form Nylon 6 Prepared by Ammonia Vapor from Phosphoric Acid Solutions

作　　者：葛佳文[1,2] 刘少轩[2] 章成峰[2,3] 李钦[1] 夏锦明[4] 徐怡庄[2] 吴瑾光[2] 

机构地区：[1]河南大学药学院,河南开封471003 [2]北京大学化学与分子工程学院稀土国家重点实验室,北京100871 [3]中国科学院化学研究所,北京100190 [4]沈阳度太生物制药研究中心,辽宁沈阳110031

出　　处：《光谱学与光谱分析》2012年第1期118-122,共5页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(50973003);国家(863计划)重大项目(2010AA03A406);科技部平台项目(2005DKA32800);北京市专利基金;北京大学先进技术研究院培育项目资助

摘　　要：尼龙6是一种多晶型的半结晶高聚物。实验采用蒸沉法制备出尼龙6,首先通过XRD和FTIR的手段进行表征,与采用沸水处理的尼龙6样品表征结果对比,确定其为γ晶型,然后在130～211℃的温度范围内进行热处理,通过DSC研究其在低于熔点热处理时的整个热行为变化过程,并运用FTIR观察其在不同条件下热处理发生的晶型变化。发现蒸沉法制备的γ晶型尼龙6随着热处理温度的升高,整体结晶完善度以及晶片厚度随着处理温度的升高而增加。而且在这个过程中,样品厚度不同的晶片在不同温度下发生了γ晶型向α晶型的转化,最终在接近熔点(211℃)热处理时,样品变为以α晶型为主。In the present work,we prepared nylon 6 crystal s via crystallization of nylon from phosphoric acid by using the vapors of a mmon ium hydroxide as a precipitation regent.Both XRD and FTIR results demonstrate that the obtained nylon 6 sample exhibit characteristic peaks of nylon 6 in γ f orm.In addition,treatment of nylon 6 in boiling water for half an hour followe d by FTIR and XRD characterization shows that the obtained nylon 6 sample is in γ form rather than in meta-stable b form.DSC characterization indicates that the nylon 6 sample exhibits two melting peaks（213 and 220 ℃） when the sample is heated at a heating rate of 10 ℃·min-1.The reason for this phenomeno n is that the nylon 6 sample has different lamellar thickness.To investigate th e thermal behavior of the nylon 6 sample,the sample underwent the following the rmal treatment procedure.First,the sample was heated to a pre-set temperature （Ts） and kept at that temperature for an hour.Subsequently,the sample w as cooled down to 100 ℃ at a cooling rate of 1 ℃·min-1,and then cooled down to room temperature at a cooling rate of 10 ℃·min-1.The treated s amples were characterized by FTIR and DSC method.Experimental results show that the treated nylon 6 samples exhibit different crystalline behavior.When T s ran ges from 130 to 160 ℃,no significant changes were observed.When Ts is 1 70 ℃, a small fraction nylon 6 crystals is destroyed and recrystallized into thin lam ellae in a form.As a result,a pre-melting peak appears in DSC result.The pre-melting peak moves to higher temperature and its peak area increases significa ntly upon increasing Ts from 170 to 198 ℃.When Ts amounts to 200 ℃,the premelting peak and the melting peaks 213 ℃ merge into one melting peak and two me lting peaks are observed at 212 and 220 ℃ in the DSC results.FTIR spectra ind icate that significant amount of crystalline nylon 6 in a form appears but the m ajority of crystalline phase of the sample is still γ phase.As Ts increa ses fr om 200 to 209 ℃,th

关 键 词：尼龙6 γ晶型 蒸沉法 热行为 红外光谱 

分 类 号：TQ225.26[化学工程—有机化工]