磷化纤维素和壳聚糖组合层层自组装技术制备棉织物阻燃材料的性能研究
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摘要
使用磷酸和木质素纤维制备了磷化纤维素(PCL)阴离子溶液,使用甲壳素脱除乙酰基之后得到的壳聚糖制备了壳聚糖(CH)阳离子溶液,然后采用层层自组装(layer by layer self-assembly technique,LBL)技术对无色纯棉织物进行了阻燃处理。首先通过红外光谱(FT-IR)对磷化纤维素进行了结构表征,并通过垂直燃烧(UL94)、热重(TG)、微型燃烧量热仪(MCC)和烟密度测试仪(SDT)等研究阻燃棉织物燃烧和热降解性能。FT-IR测试结果表明:磷化纤维素制备成功。MCC的测试结果表明:试样热释放速率峰值与棉织物相比有大幅降低,显著抑制了棉织物受热分解时的热量释放。TG测试的结果表明:经阻燃处理后的棉织物在700℃的残炭含量明显增加。SDT结果表明:构筑LBL阻燃涂层后,光通量提高了24.9%,最大比光密度降低了65.24%,显著提高了棉织物的抑烟性能。
In this paper,phosphorylated cellulose(PCL)anionic solution was prepared using phosphate and lignin fibers and the chitosan(CH)cation solution was prepared using chitin removal of acetyl groups.Then the fire retardant treatment was applied to non-colored cotton fabric with layers of self-assembly technique.In the experimental part of this paper,the structural characterization of phosphatized cellulose was first made through infrared spectroscopy(FT-IR).The combustion and thermal degradation properties of flame retardant cotton fabrics were investigated by vertical combustion(UL94),thermogravimetry(TG)and micro combustion calorimeter(MCC).The FT-IR test results showed that phosphatingcellulose was successfully prepared.The test results of MCC show that the peak value of the heat release rate of the sample is lower than that of the cotton fabric,which significantly suppresses the heat release of the cotton fabric during thermal decomposition.The results of TG test showed that the content of residual carbon in the cotton fabric treated with flame retardant increased obviously at 700 ℃.SDT results showed that the luminous flux increased by 24.9% and the maximum specific optical density decreased by 65.24% when the LBL flame retardant coating was constructed.The smoke suppression property of cotton fabric was improved remarkably.
In this paper,phosphorylated cellulose(PCL)anionic solution was prepared using phosphate and lignin fibers and the chitosan(CH)cation solution was prepared using chitin removal of acetyl groups.Then the fire retardant treatment was applied to non-colored cotton fabric with layers of self-assembly technique.In the experimental part of this paper,the structural characterization of phosphatized cellulose was first made through infrared spectroscopy(FT-IR).The combustion and thermal degradation properties of flame retardant cotton fabrics were investigated by vertical combustion(UL94),thermogravimetry(TG)and micro combustion calorimeter(MCC).The FT-IR test results showed that phosphatingcellulose was successfully prepared.The test results of MCC show that the peak value of the heat release rate of the sample is lower than that of the cotton fabric,which significantly suppresses the heat release of the cotton fabric during thermal decomposition.The results of TG test showed that the content of residual carbon in the cotton fabric treated with flame retardant increased obviously at 700 ℃.SDT results showed that the luminous flux increased by 24.9% and the maximum specific optical density decreased by 65.24% when the LBL flame retardant coating was constructed.The smoke suppression property of cotton fabric was improved remarkably.
引文
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[13]王文多,陈希磊.碱式钼酸铜的制备及其对膨胀型防火涂料防火抑烟性能的影响[J].青岛科技大学学报(自然科学版),2017,38(4):66-70.WANG Wenduo,CHEN Xilei.Fire and smoke suppression properties of copper molybdate in instumescent flame retardant coating[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2017,38(4):66-70.
[2]CHEN X L,JIANG Y F,LIU J B,et al.Smoke suppression properties of fumed silica on flame-retardant thermoplastic polyurethane based on ammonium polyphosphate[J].Journal of Thermal Analysis and Calorimetry,2015,266(3):114-121.
[3]张军,纪奎江,夏延致.聚合物燃烧与阻燃技术[M].北京:化学工业出版社,2005:57-105,387-389.ZHANG Jun,JI Kuijiang,XIA Yanzhi.Polymer Combustion and Flame Retardant Technology[M].Beijing:Chemistry Industry Press,2005:57-105,387-389.
[4]韩非,辛浩波,张云峰.聚氨酯弹性体的合成及表征[J].青岛科技大学学报(自然科学版),2008,29(1):43-46.HAN Fei,XIN Haobo,ZHANG Yunfeng.Synthesis and characterization of polyurethane elastomers[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2008,29(1):43-46.
[5]王天雷,刘梅堂.层层自组装技术制备水滑石新型薄膜材料的研究发展[J].化工进展,2013,32(7):1584-1590.WANG Tianlei,LIU Meitang.Progress in preparation of hydrotalcite like new thin film materials by layer by layer self-assembly technology[J].Chemical Progress,2013,32(7):1584-1590.
[6]刘宗怀,乔山峰,袁佳琦.层层自组装技术在功能薄膜材料制备中的应用[J].陕西师范大学学报,2010,38(4):65-72.LIU Zonghuai,QIAO Shanfeng,YUAN Jiaqi.Application of layer by layer self-assembly technology in preparation of functional film materials[J].Journal of Shaanxi Normal University,2010,38(4):65-72.
[7]CHEN X L,JIANG Y F,JIAO C M.Synergistic effects between hollow glass microsphere and ammonium polyphosphate on flame-retardant thermoplastic polyurethane[J].Journal of Thermal Analysis and Calorimetry,2014,117(2):875-892.
[8]孙杰,焦传梅.氧化锌与膨胀型阻燃剂对聚丙烯的协效阻燃[J].青岛科技大学学报(自然科学版),2012,32(2):172-176.SUN Jie,JIAO Chuanmei.Synergistic flame resistant effect of zinc oxide and intumescent flame retardant in polypropylene[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2012,32(2):172-176.
[9]李姗姗,陈希磊.以蔗渣为炭源制备膨胀型阻燃乙烯醋酸乙烯酯共聚物[J].青岛科技大学学报(自然科学版),2015,36(5):487-492.LI Shanshan,CHEN Xilei.Preparation and properties of intumescent fire retardant EVA based on bagasse as carbon source[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2015,36(5):487-492.
[10]王洪志,焦传梅.硅胶低聚物阻燃热塑性聚氨酯弹性体的研究[J].青岛科技大学学报(自然科学版),2017,38(1):87-92.WANG Hongzhi,JIAO Chuanmei.Research of flame retardant thermoplastic polyurethane elastomer based on silicone oligomer[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2017,38(1):87-92.
[11]王庆国,张军,张峰.锥形量热仪的工作原理及应用[J].现代科学仪器,2003,6:36-39.WANG Qingguo,ZHANG Jun,ZHANG Feng.The principle and application of the cone calorimeter[J].Modern Scientific Instruments,2003,6:36-39.
[12]李吉祯,刘小刚,付小龙.红外光谱联用技术在材料热分解研究中的应用[J].化学推进剂与高分子材料,2011,9(3):29-32.LI Jizhen,LIU Xiaogang,FU Xiaolong.Application of infrared spectroscopy in the study of thermal decomposition of materials[J].Chemical Propellants and Polymer Materials,2011,9(3):29-32.
[13]王文多,陈希磊.碱式钼酸铜的制备及其对膨胀型防火涂料防火抑烟性能的影响[J].青岛科技大学学报(自然科学版),2017,38(4):66-70.WANG Wenduo,CHEN Xilei.Fire and smoke suppression properties of copper molybdate in instumescent flame retardant coating[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2017,38(4):66-70.