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原位相容化淀粉/聚丙烯腈复合纤维的干法-湿法纺丝制备。

In-situ compatibilized starch/polyacylonitrile composite fiber fabricated via dry-wet spinning technique.

机构信息

School of Textile and Material Engineering, Dalian Polytechnic University, Dalian 116034, PR China.

School of Textile and Material Engineering, Dalian Polytechnic University, Dalian 116034, PR China.

出版信息

Int J Biol Macromol. 2022 Jul 1;212:412-419. doi: 10.1016/j.ijbiomac.2022.05.091. Epub 2022 May 14.

Abstract

An in-situ compatibilized starch (St) and polyacrylonitrile (PAN) composite spinning solution was designed by preparing starch-graft-polyacrylonitrile (St-g-PAN) through graft copolymerizing acrylonitrile from soluble starch and using ammonium cerium nitrate (CAN) as initiator. As dimethyl sulfoxide (DMSO) was used as the solvent, St/St-g-PAN/PAN/DMSO spinning solution was prepared and St/St-g-PAN/PAN composite fibers were obtained by dry-wet spinning technique. The effects of air gap, coagulation bath, hot drawing and stretching, and thermal-setting process were studied in detail. Fourier transform infrared spectroscopy (FT-IR), solid state nuclear magnetic resonance (C NMR), thermogravimetric analysis (TGA), X-ray diffraction analysis (XRD), and scanning electron microscopy (SEM) were used to characterize the structure and morphology of the copolymer and the fibers. Single fiber strength tester and sonic orientation instrument were performed to measure the fiber mechanical properties and orientation degrees. The results showed that as the grafting ratio ~150.0% and the reacting mixture containing St ~9.8%, St-g-PAN ~81.6%, and homo-PAN ~8.6% in DMSO solution with 6.0 wt% in concentration were used, the spinning parameters such as air gap ~35 mm, coagulation bath concentration ~70%, temperature ~25 °C, and positive stretching ~48%, hot drawing and stretching 6 times at 80 °C, thermal-setting at 90 °C for 3 h under constant length mode were met, composite fibers with breaking strength 3.41 cN·dtex, breaking elongation 14.41%, sonic orientation factor 0.625, moisture recovery ratio 10.53% under standard condition (1 atm, 22 °C, and relative humidity 65%), and boiling water shrinkage ratio 9.60% were obtained. The as prepared composite fiber was better than common viscose fiber 2.11 cN·dtex and cotton fiber ~3.24 cN·dtex and expected to be used in the fields of medical gauze, bandage, protective clothing, et al. besides of common textiles. The in-situ compatibilization method can be applied in preparation of other composite polymer materials.

摘要

采用硝酸铈铵(CAN)为引发剂,通过丙烯腈接枝到可溶性淀粉上制备淀粉接枝聚丙烯腈(St-g-PAN),设计了原位相容化淀粉(St)和聚丙烯腈(PAN)复合纺丝溶液。由于使用二甲基亚砜(DMSO)作为溶剂,制备了 St/St-g-PAN/PAN/DMSO 纺丝溶液,并通过干湿纺丝技术获得了 St/St-g-PAN/PAN 复合纤维。详细研究了空气隙、凝固浴、热拉伸和热定型过程的影响。采用傅里叶变换红外光谱(FT-IR)、固态核磁共振(C NMR)、热重分析(TGA)、X 射线衍射分析(XRD)和扫描电子显微镜(SEM)对共聚物和纤维的结构和形态进行了表征。采用单纤维强力仪和声波取向仪分别测量纤维的力学性能和取向度。结果表明,当接枝率约为 150.0%,反应混合物中含有 St(淀粉)9.8%、St-g-PAN(接枝共聚物)81.6%和均聚 PAN(聚丙烯腈)8.6%,在浓度为 6.0wt%的 DMSO 溶液中使用时,纺丝参数为空气隙35mm、凝固浴浓度70%、温度25°C 和正拉伸48%,在 80°C 下热拉伸和拉伸 6 次,在恒长模式下 90°C 下热定型 3h,可获得断裂强度为 3.41cN·dtex、断裂伸长率为 14.41%、声速取向因子为 0.625、标准条件下(1atm、22°C 和相对湿度 65%)回潮率为 10.53%和沸水收缩率为 9.60%的复合纤维。所制备的复合纤维优于普通粘胶纤维 2.11cN·dtex 和棉纤维3.24cN·dtex,有望除了普通纺织品之外,还可用于医用纱布、绷带、防护服等领域。原位相容化方法可应用于其他复合聚合物材料的制备。

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