title: [Investigation of thermal behaviors of γ-form nylon 6 prepared by ammonia vapor from phosphoric acid solutions].
abstract: In the present work, we prepared nylon 6 crystals via crystallization of nylon from phosphoric acid by using the vapors of ammonium hydroxide as a precipitation regent. Both XRD and FTIR results demonstrate that the obtained nylon 6 sample exhibit characteristic peaks of nylon 6 in gamma form. In addition, treatment of nylon 6 in boiling water for half an hour followed by FTIR and XRD characterization shows that the obtained nylon 6 sample is in gamma form rather than in meta-stable b form. DSC characterization indicates that the nylon 6 sample exhibits two melting peaks (213 and 220 degrees C) when the sample is heated at a heating rate of 10 degrees C x min(-1). The reason for this phenomenon is that the nylon 6 sample has different lamellar thickness. To investigate the thermal behavior of the nylon 6 sample, the sample underwent the following thermal treatment procedure. First, the sample was heated to a pre-set temperature (T(s)) and kept at that temperature for an hour. Subsequently, the sample was cooled down to 100 degrees C at a cooling rate of 1 degrees C x min(-1), and then cooled down to room temperature at a cooling rate of 10 degrees C x min(-1). The treated samples were characterized by FTIR and DSC method. Experimental results show that the treated nylon 6 samples exhibit different crystalline behavior. When T. ranges from 130 to 160 degrees C, no significant changes were observed. When T(s) is 170 degrees C, a small fraction nylon 6 crystals is destroyed and recrystallized into thin lamellae 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 significantly upon increasing T(s) from 170 to 198 degrees C. When T(s) amounts to 200 degrees C, the pre-melting peak and the melting peaks 213 degrees C merge into one melting peak and two melting peaks are observed at 212 and 220 degrees C in the DSC results. FTIR spectra indicate that significant amount of crystalline nylon 6 in a form appears but the majority of crystalline phase of the sample is still gamma phase. As T(s) increases from 200 to 209 degrees C, the melting peak at lower temperature moves to higher temperature with increasing its peak area. On the other hand, the melting peak at 220 degrees C decreases in intensity but does not show any peak shift. As T(s) reaches 209 degrees C, the two melting peaks merge into one peak and FTIR results demonstrate that nylon 6 in a form becomes dominate phase in the sample. In the whole heat-treatment process, the gamma phase nylon 6 sample began to transform to a phase at the heat-treatment temperature of 170 degrees C, which is far below the melting point of the original sample (221 degrees C). This is different from the results reported in the literature, which state that gamma phase nylon 6 will not transform to alpha-phase until nylon is melt.
authors.affiliation: College of Pharmacy, Henan University, Kaifeng 471003, China. iorygjw1985@sina.com
authors.forename: Jia-wen
authors.initials: JW
authors.lastname: Ge
authors.forename: Shao-xuan
authors.initials: SX
authors.lastname: Liu
authors.forename: Cheng-feng
authors.initials: CF
authors.lastname: Zhang
authors.forename: Qin
authors.initials: Q
authors.lastname: Li
authors.forename: Jin-ming
authors.initials: JM
authors.lastname: Xia
authors.forename: Yi-zhuang
authors.initials: YZ
authors.lastname: Xu
authors.forename: Jin-guang
authors.initials: JG
authors.lastname: Wu