高等学校化学学报
高等學校化學學報
고등학교화학학보
Chemical Journal of Chinese Universities
2015年
10期
2073-2082
,共10页
韩娜%李慧慧%李传宝%张兴祥%李伟%王栋
韓娜%李慧慧%李傳寶%張興祥%李偉%王棟
한나%리혜혜%리전보%장흥상%리위%왕동
丙烯腈%N-乙烯基咪唑%溶液聚合%熔融纺丝%纤维
丙烯腈%N-乙烯基咪唑%溶液聚閤%鎔融紡絲%纖維
병희정%N-을희기미서%용액취합%용융방사%섬유
Acrylonitrile%N-vinylimidazole%Solution copolymerization%Melt spinning%Fiber
采用自由基溶液聚合法制备了不同投料摩尔比的丙烯腈( AN)-N-乙烯基咪唑( VIM)共聚物[P(AN-co-VIM)].将 n(AN): n(VIM)为82:18和80:20的 P(AN-co-VIM)共聚物于210~220℃熔融纺丝制备了P(AN-co-VIM)初生纤维.通过傅里叶变换红外光谱、核磁共振(1 H NMR)谱、差示扫描量热分析、X 射线衍射分析和热台显微镜对 P(AN-co-VIM)共聚物的组成、热力学和结晶行为进行了表征.结果表明,自由基溶液聚合法可成功制备 P(AN-co-VIM)共聚物,当 VIM 的摩尔分数大于10%时,共聚物具有可熔融加工性.随着 VIM 摩尔分数的增加,共聚物的熔点降低,当 VIM 含量为20%时,共聚物的熔点从317℃降低至180℃,其分解温度最高为313.7℃.扫描电子显微镜(SEM)和电子单纤维强力测试.结果表明,纤维的表面光滑,断面结构致密,初生纤维的断裂强度为1.58 cN/ dtex,断裂伸长率为11.2%,有望广泛应用于碳纤维领域.
採用自由基溶液聚閤法製備瞭不同投料摩爾比的丙烯腈( AN)-N-乙烯基咪唑( VIM)共聚物[P(AN-co-VIM)].將 n(AN): n(VIM)為82:18和80:20的 P(AN-co-VIM)共聚物于210~220℃鎔融紡絲製備瞭P(AN-co-VIM)初生纖維.通過傅裏葉變換紅外光譜、覈磁共振(1 H NMR)譜、差示掃描量熱分析、X 射線衍射分析和熱檯顯微鏡對 P(AN-co-VIM)共聚物的組成、熱力學和結晶行為進行瞭錶徵.結果錶明,自由基溶液聚閤法可成功製備 P(AN-co-VIM)共聚物,噹 VIM 的摩爾分數大于10%時,共聚物具有可鎔融加工性.隨著 VIM 摩爾分數的增加,共聚物的鎔點降低,噹 VIM 含量為20%時,共聚物的鎔點從317℃降低至180℃,其分解溫度最高為313.7℃.掃描電子顯微鏡(SEM)和電子單纖維彊力測試.結果錶明,纖維的錶麵光滑,斷麵結構緻密,初生纖維的斷裂彊度為1.58 cN/ dtex,斷裂伸長率為11.2%,有望廣汎應用于碳纖維領域.
채용자유기용액취합법제비료불동투료마이비적병희정( AN)-N-을희기미서( VIM)공취물[P(AN-co-VIM)].장 n(AN): n(VIM)위82:18화80:20적 P(AN-co-VIM)공취물우210~220℃용융방사제비료P(AN-co-VIM)초생섬유.통과부리협변환홍외광보、핵자공진(1 H NMR)보、차시소묘량열분석、X 사선연사분석화열태현미경대 P(AN-co-VIM)공취물적조성、열역학화결정행위진행료표정.결과표명,자유기용액취합법가성공제비 P(AN-co-VIM)공취물,당 VIM 적마이분수대우10%시,공취물구유가용융가공성.수착 VIM 마이분수적증가,공취물적용점강저,당 VIM 함량위20%시,공취물적용점종317℃강저지180℃,기분해온도최고위313.7℃.소묘전자현미경(SEM)화전자단섬유강력측시.결과표명,섬유적표면광활,단면결구치밀,초생섬유적단렬강도위1.58 cN/ dtex,단렬신장솔위11.2%,유망엄범응용우탄섬유영역.
Polyacrylonitrile(PAN) and acrylonitrile(AN)-N-vinylimidazole(VIM) copolymers[ abbreviated as P(AN-co-VIM)] with various n(AN) : n(VIM)(93 : 7—80 : 20) were synthesized by free-radical solution copolymerization in dimethyl formamide ( DMF). The P ( AN-co-VIM) copolymers (82 : 18 and 80 : 20) possessed good melt processability, which were melt spun at the temperature of 210—220 ℃. The crystallinity, thermodynamics behavior and the composition of P(AN-co-VIM) copolymers were studied and characterized by ubbelodhe viscosimeter, Fourier transform infrared spectroscopy( FTIR), nuclear magnetic resonance ( 1 H NMR), differential scanning calorimetry( DSC), X-ray diffraction( XRD) analyses and hot stage microscope. The results revealed that P(AN-co-VIM) could be synthesized successfully by free-radical solution copolymerization. P( AN-co-VIM) could be melt processable as VIM molar fraction is higher than 10% . The melting temperature of P ( AN-co-VIM) shifts continuously to the lower temperature with the comonomer contents increasing. When the molar fraction of VIM is increased to 20% , the melting point of P (AN-co-VIM) copolymer reduced from 317 ℃ to 180 ℃. The highest decomposition temperature is 313. 7℃. The apparent morphology and mechanical properties of the P(AN-co-VIM) fibers were characterized by scanning electron microscope(SEM) and single fiber electronic tensile strength test. The results show that the fibers have smooth surface and compact cross section. As-spun P(AN-co-VIM) fiber gets the fracture strength of 1. 58 cN/ dtex and the elongation at break attained 11. 2% . After post-treatment, the fiber is expected to be widely used in the field of carbon fiber.