阻燃左旋聚乳酸/季戊四醇磷酸酯纤维及织物的制备与性能

doi:10.13475/j.fzxb.20250503201

纺织学报 ›› 2026, Vol. 47 ›› Issue (1): 63-71.doi: 10.13475/j.fzxb.20250503201

阻燃左旋聚乳酸/季戊四醇磷酸酯纤维及织物的制备与性能

董振峰¹, 张安莹², 魏建斐³, 朱志国¹, 王锐³()

1.北京服装学院材料设计与工程学院, 北京 100029
2.新兴际华(北京)材料技术研究院有限公司, 北京 100078
3.北京服装学院服装材料研究开发与评价北京市重点实验室, 北京 100029

收稿日期:2025-05-20 修回日期:2025-11-03 出版日期:2026-01-15 发布日期:2026-01-15
通讯作者: 王锐(1963—),女,教授,博士。主要研究方向为功能材料及纤维。E-mail:clywangrui@bift.edu.cn。
作者简介:董振峰(1981—),男,高级实验师,硕士。主要研究方向为阻燃材料及纤维。
基金资助:
北京学者团队资助项目(RCQJ20303)

Preparation and properties of flame retardant poly(L-lactic acid)/pentaerythritol phosphate fibers and fabrics

DONG Zhenfeng¹, ZHANG Anying², WEI Jianfei³, ZHU Zhiguo¹, WANG Rui³()

1. School of Materials Design and Engineering, Beijing Institute of Fashion Technology, Beijing 100029, China
2. Xinxing Cathay International (Beijing) Institute of Materials Technology Co., Ltd., Beijing 100078, China
3. Beijing Key Laboratory of Clothing Materials R&D and Assessment, Beijing Institute of Fashion Technology, Beijing 100029, China

Received:2025-05-20 Revised:2025-11-03 Published:2026-01-15 Online:2026-01-15

摘要/Abstract

摘要：

为提高可生物降解左旋聚乳酸(PLLA)材料及其织物的阻燃性能,依据PLLA和季戊四醇磷酸酯(PEPA)的特性设计了PLLA/PEPA体系,采用双螺杆熔融共混制备含40%PEPA的PLLA/PEPA母粒,通过注塑机制备含不同质量分数PEPA的PLLA/PEPA复合物,采用极限氧指数仪、垂直燃烧仪、锥形量热仪和万能试验机等手段研究PEPA质量分数对PLLA阻燃性能和力学性能的影响,并对综合性能最佳复合物的可纺性及纤维的力学性能和织物的阻燃性能进行评价。结果表明:当PEPA质量分数为5%时,复合物的极限氧指数(LOI值)达到32%,UL-94等级为V-0级,引燃时间延长约25 s,且经工业生产线纺丝实验证实该复合物具有良好的可纺性,纤维的断裂强度为2.38 cN/dtex,将其织成153 g/m²的缎纹织物进行性能检测,织物的LOI值约33%,垂直燃烧测试无熔滴且水洗30次后阻燃性能未降低,表明该体系获得的织物具有良好的阻燃耐水洗性。阻燃机制研究表明,PEPA提高PLLA阻燃性能是捕捉自由基机制、凝聚相阻燃机制和交联致熔体增黏三者共同作用的结果。

关键词: 聚乳酸, 季戊四醇磷酸酯, 阻燃性能, 可纺性, 极限氧指数, 引燃时间

Abstract:

Objective Poly (L-lactic acid) (PLLA) is a biodegradable polymer synthesized from renewable biomass resources. Its main raw materials are starch-rich crops. In natural environments, PLLA can be gradually decomposed by microorganisms into carbon dioxide and water, which are non-toxic and harmless to the human body. This aligns with the green development logic of ″coming from nature and returning to nature″. PLLA exhibits good mechanical strength, stiffness, and processing fluidity. It can be processed into products of various forms meeting application needs in different fields. PLA has become a research hotspot and application focus in the field of materials science in recent years.

However, PLLA and its fabrics also has obvious performance shortcomings, among which flammability is the most critical one. Its limiting oxygen index (LOI value) is only 21%, meaning that PLLA is easily flammable when in contact with an open flame. This defect severely restricts its application in fields with explicit fire resistance requirements. In order to improve the flame retardancy of PLA fabrics, a large number of studies have been conducted in the industry. Pentaerythritol phosphate, as a cage-like phosphate flame retardant, not only has extremely low biological toxicity (avoiding the harm of conventional flame retardants to the environment and human body) but also can interact with the terminal hydroxyl groups in the PLA molecular chain to form a stable flame-retardant system. While increasing the LOI value of PLLA and suppressing molten dripping during combustion, it retains the original physical and mechanical properties as well as biodegradability of PLLA to the greatest extent, opening up a new path for the application of PLLA in fields with high fire protection requirements.

Method The PLLA/PEPA masterbatch with 40% PEPA was prepared using a twin-screw extruder, and then the masterbatch was mixed with PLLA followed by injection molding to fabricate a series of PLLA/PEPA composites with different mass percentages of PEPA. The structure and properties of the composites were characterized and tested using differential scanning calorimetry, thermogravimetric analysis, extreme oxygen index analyzer, cone calorimeter, vertical combustion tester, and universal tensile machine. The composite with the best comprehensive performance was optimized for the preparation of fibers and fabrics, and the flame retardant performance of the fabrics was evaluated.

Results When the mass fraction of PEPA added was not greater than 6%, PLLA/PEPA showed good processing performance, and the glass transition temperature, crystallization temperature, melting temperature, and thermal decomposition temperature of the composite were not significantly affected. When the mass percentage of PEPA added was 5%, the LOI value of the composite was 32%, the vertical combustion test reached V-0 level, and the ignition time was prolonged by about 25 s. The composite with 5% PEPA added demonstrated good spinnability. The mechanical testing results showed that the fiber fineness was 185.7 dtex(72 f), and the fiber breaking strength and elongation at break were 2.38 cN/dtex and 21.5%, respectively. Flame retardant performance testing conformed that the LOI value of the fabric was about 33%, the vertical combustion test of the fabric was V-0 level, and the flame retardant performance of the fabric remained unchanged after 30 cycles of water washing. Study on flame retardant mechanism suggested that the improvement of flame retardant performance of PLLA by PEPA was attributed to the combined effect of free radical scavenging mechanism, condensed phase flame retardant mechanism and cross-linking induced melt viscosity increase.

Conclusion After adding PEPA with a mass fraction of 5% to PLLA, the flame retardant performance of the material is significantly improved in effectively increasing the difficulty of ignition, delaying the combustion process, and reducing the flame spread rate. The fabric obtained from the modified PLLA fibers by weaving maintains excellent mechanical properties as well as flame retardant performance, balancing practicality and safety. More importantly, the flame retardant effect of the fabric does not decrease after 30 washing cycles, showing outstanding performance stability. This scheme provides a new method with great application value for preparing safe, harmless, environmentally friendly and biodegradable flame retardant fabrics.

Key words: poly(L-lactic acid), pentaerythritol phosphate, flame retardant performance, spinnability, limiting oxygen index, ignition time

中图分类号:

TQ342.89

董振峰, 张安莹, 魏建斐, 朱志国, 王锐. 阻燃左旋聚乳酸/季戊四醇磷酸酯纤维及织物的制备与性能[J]. 纺织学报, 2026, 47(1): 63-71.

DONG Zhenfeng, ZHANG Anying, WEI Jianfei, ZHU Zhiguo, WANG Rui. Preparation and properties of flame retardant poly(L-lactic acid)/pentaerythritol phosphate fibers and fabrics[J]. Journal of Textile Research, 2026, 47(1): 63-71.

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链接本文: http://www.fzxb.org.cn/CN/10.13475/j.fzxb.20250503201

http://www.fzxb.org.cn/CN/Y2026/V47/I1/63

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样品名称	热焓/(J·g^-1)	样品名称	热焓/(J·g^-1)
PLLA	34.47	PLLA/PEPA4	35.40
PLLA/PEPA2	35.89	PLLA/PEPA5	37.52
PLLA/PEPA3	35.73	PLLA/PEPA6	38.70

样品名称	LOI值/%	垂直燃烧性能测试结果
样品名称	LOI值/%	第1次引燃后自熄时间/s	第2次引燃后自熄时间/s	是否有熔滴	是否引燃脱脂棉	等级	熔滴状态
PLLA	21±1	24.6±4.6	23.0±4.8	是	是	无	液滴
PLLA/PEPA1	26±1	17.0±4.1	2.0±0.5	是	是	V-2	液滴
PLLA/PEPA2	28±1	14.6±2.3	1.7±0.3	是	是	V-2	漫流
PLLA/PEPA3	30±1	8.1±0.9	0	是	否	V-0	漫流
PLLA/PEPA4	31±1	2.9±1.2	0	是	否	V-0	漫流
PLLA/PEPA5	32±1	1.8±0.2	0	是	否	V-0	漫流
PLLA/PEPA6	33±1	1.8±0.3	0	是	否	V-0	漫流
PLLA/PEPA8	33±1	1.6±0.3	0	是	否	V-0	漫流

样品名称	线密度/ (dtex(96 f))	断裂强度/ (cN·dtex^-1)	断裂伸长率/ %
PLLA	113.0	3.31	25.21
PLLA/PEPA3	113.2	2.65	27.14
PLLA/PEPA5	112.8	2.51	23.55

方向	LOI值/%		垂直燃烧性能测试结果
	LOI值/%		续燃时间/s		阴燃时间/s		损毁长度/mm		滴落物
	水洗前	水洗30次后	水洗前	水洗30次后	水洗前	水洗30次后	水洗前	水洗30次后	水洗前	水洗30次后
经向	33.0	32.6	0	0	0	0	156	136	无	无
纬向	32.6	33.1	0	0	0	0	161	132	无	无

阻燃左旋聚乳酸/季戊四醇磷酸酯纤维及织物的制备与性能

Preparation and properties of flame retardant poly(L-lactic acid)/pentaerythritol phosphate fibers and fabrics

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