Page 181 - 《精细化工》2020年第4期

第 37 卷第 4 期 精 细 化 工 Vol.37, No.4
202 0 年 4 月 FINE CHEMICALS Apr. 2020

纺织染整助剂
磷-氮阻燃剂的合成及整理棉织物性能

邹 旭 1,2,3,4 ，王倩倩 1,2,3,4 ，朱 平 1,2,3,4*

（1. 青岛大学 纺织服装学院, 山东 青岛 266071；2. 青岛大学 功能纺织品与先进材料研究院, 山东 青
岛 266071；3. 生物多糖纤维成形与生态纺织国家重点实验室, 山东 青岛 266071；4. 青岛大学 海洋生
物质纤维材料及纺织品山东省协同创新中心，山东 青岛 266071）

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摘要：以亚磷酸二甲酯、丙烯酰胺和三聚氯氰为原料，合成了无甲醛磷-氮阻燃剂，通过 FTIR、HNMR 和 PNMR
对阻燃剂的结构进行了表征。通过轧烘焙工艺制备了阻燃棉织物，利用 FTIR、SEM 和 EDS 对整理棉织物的结
构、表面形态和元素组成进行了测试。通过极限氧指数（LOI）、垂直燃烧、锥形量热（CCT）研究了整理棉织
物的阻燃性能，采用热重分析法（TG）测试了整理棉织物的热稳定性能。结果表明：整理后纤维表面粗糙，覆
盖有明显颗粒，且均匀分布着磷、氮元素。整理棉织物的极限氧指数由 18%提高到 31%，续燃时间、阴燃时间
由 9 s、25 s 均降到 0 s，损毁长度由 300 mm 降低到 74 mm。在氮气及空气中的残炭率提高了 28.0%和 14.6%，
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最大热降解速率降低了 66.7%及 68.0%。最大热释放速率（PHRR）由 203.5 kW/m 降低到 57.9 kW/m ，总释放
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热（THR）由 6.0 MJ/m 降低到 2.9 MJ/m 。整理后棉织物具有良好的阻燃性能。
关键词：磷-氮阻燃剂；无甲醛；棉织物；阻燃整理；纺织染整助剂
中图分类号：TS195.5 文献标识码：A 文章编号：1003-5214 (2020) 04-0815-07

Synthesis of phosphorus-nitrogen flame retardant and the
properties of treated cotton fabrics by it

ZOU Xu 1,2,3,4 , WANG Qianqian 1,2,3,4 , ZHU Ping 1,2,3,4*
（1. College of Textile & Clothing, Qingdao University, Qingdao 266071, Shandong, China; 2. Institute of Functional
Textiles and Advanced Materials, Qingdao University, Qingdao 266071, Shandong, China; 3. State Key Laboratory of
Bio-Fibers and Eco-Textiles, Qingdao 266071, Shandong, China; 4. Collaborative Innovation Center of Marine Biomass
Fibers Materials and Textiles of Shandong Province, Qingdao University, Qingdao 266071, Shandong, China）

Abstract: A formaldehyde-free phosphorus-nitrogen flame retardant was synthesized using dimethyl
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phosphite, acrylamide and cyanuric chloride as raw materials and characterized by FTIR, HNMR and
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PNMR. Rolling and baking technology was utilized to prepare flame retardant cotton fabrics. The
structure, surface morphology and elemental composition of the treated cotton fabrics were investigated by
FTIR, SEM and EDS, respectively. The flame retardant properties and thermal degradation of treated
fabrics were tested through limiting oxygen index (LOI) test, vertical burning test, cone calorimeter test
(CCT) and thermogravimetry (TG). The results showed that the fibers treated by flame retardant presented
rough surface, covered with obvious particles, and evenly distributed with phosphorus and nitrogen
elements. Compared with those of cotton fabrics, the LOI values of treated cotton fabrics increased from
18% to 31%, the afterflame and afterglow time decreased from 9 s and 25 s to 0 s, respectively, and the
damaged length reduced from 300 mm to 74 mm. Moreover, the char residue rate in nitrogen and air
atmosphere was increased by 28.0% and 14.6%, and the maximum thermal degradation rate was reduced by
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66.7% and 68.0%. The peak heat release rate (PHRR) value decreased from 203.5 kW/m to 57.9 kW/m ,
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and the total heat release (THR) value decreased from 6.0 MJ/m to 2.9 MJ/m . All these indicated that the
treated cotton fabrics exhibited excellent flame retardant properties.

收稿日期：2019-11-12; 定用日期：2020-01-19; DOI: 10.13550/j.jxhg.20191068
基金项目：国家重点研发计划（2017YFB0309001）
作者简介：邹 旭（1995—），男，硕士生，E-mail：zxsdqdu@163.com。联系人：朱 平（1957—），男，教授，E-mail：Pzhu99@163.com。