单宁酸基高效阻燃Lyocell织物的制备及其性能

doi:10.13475/j.fzxb.20250103001

纺织学报 ›› 2025, Vol. 46 ›› Issue (08): 145-153.doi: 10.13475/j.fzxb.20250103001

单宁酸基高效阻燃Lyocell织物的制备及其性能

许云凯¹^,²^,³^,⁴, 宋婉萌¹^,²^,³^,⁴, 张旭¹^,²^,³^,⁴, 刘云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.青岛大学新型防火阻燃材料开发与应用国家地方联合工程研究中心, 山东青岛 266071
4.青岛大学青岛市阻燃纺织材料重点实验室, 山东青岛 266071

收稿日期:2025-01-13 修回日期:2025-04-16 出版日期:2025-08-15 发布日期:2025-08-15
通讯作者: 刘云(1982—),女,教授,博士。主要研究方向为功能纤维及纺织品。E-mail:yliu@qdu.edu.cn。
作者简介:许云凯(2001—),男,硕士生。主要研究方向为阻燃后整理纺织品。
基金资助:
国家自然科学基金面上项目(52373059)

Preparation and properties of high-efficient flame-retardant Lyocell fabrics with tannic acid based flame retardants

XU Yunkai¹^,²^,³^,⁴, SONG Wanmeng¹^,²^,³^,⁴, ZHANG Xu¹^,²^,³^,⁴, LIU Yun¹^,²^,³^,⁴()

1. College of Textiles & Clothing, Qingdao University, Qingdao, Shandong 266071, China
2. Institute of Functional Textiles and Advanced Materials, Qingdao University, Qingdao, Shandong 266071, China
3. National Engineering Research Center for Advanced Fire-Safety Materials D & A (Shandong), Qingdao University, Qingdao, Shandong 266071, China
4. Qingdao Key Laboratory of Flame-Retardant Textile Materials, Qingdao University, Qingdao, Shandong 266071, China

Received:2025-01-13 Revised:2025-04-16 Published:2025-08-15 Online:2025-08-15

摘要/Abstract

摘要： 针对Lyocell织物易燃的缺点,选用生物质多酚单宁酸(TA)和二乙烯三胺五甲叉膦酸(DTPMPA)为原料,制备了阻燃剂(TD),通过轧烘焙的方法对Lyocell织物进行阻燃整理,研究了阻燃Lyocell织物的阻燃、力学、抗菌、抗紫外线和透气等性能。结果表明:阻燃剂可附着到Lyocell织物上,但未阻塞Lyocell纤维之间的空隙,因而可赋予Lyocell织物良好的阻燃性能;阻燃Lyocell织物可实现离火自熄,经100 g/L TD整理的Lyocell织物其损毁长度仅为51 mm,续燃时间和阴燃时间均为0 s,极限氧指数可达到48.2%;TD能够促进阻燃Lyocell织物提前脱水成炭,提高了阻燃Lyocell织物高温区的热稳定性;TD对阻燃Lyocell织物的热释放速率峰值(PHRR)以及总热释放(THR)有良好的抑制效果,经100 g/L TD整理的Lyocell织物的PHRR和THR相比原Lyocell织物分别下降了94.1%和62.4%;TD对Lyocell织物的透气性能影响较小,提高了阻燃Lyocell织物的抗紫外线性能,并对金黄色葡萄球菌和大肠埃希菌的生长起到了一定的抑制效果。

关键词: 阻燃性能, Lyocell织物, 单宁酸, 二乙烯三胺五甲叉膦酸, 生物基阻燃剂, 阻燃织物, 功能纺织品

Abstract:

Objective Lyocell fabrics are used in the clothing and home decoration industries because of their excellent comfort, soft handle and easy coloring. However, the limiting oxygen index (LOI) of Lyocell fabrics is only 19.0%, and it is very easy to be ignited, causing fire accidents. Some of traditional halogenated flame retardants can produce toxic gases and seriously harm to the environment in the process of using, and people are more inclined to choose efficient, green and pollution-free bio-based flame retardants. It is, therefore, necessary to design a biomass flame retardant to improve the flame retardancy of Lyocell fabrics.

Method Tannic acid (TA) and Diethylene triamine pentakis (methyl phosphonic acid) (DTPMPA) were used to prepare flame retardants (named TD). Flame-retardant Lyocell fabrics were prepared by pad-dry-cure finishing method. For comparison,flame-retardant Lyocell fabrics were prepared by 50 g/L and 100 g/L flame-retardant finishing solutions, which were named as L-TDa and L-TDb, respectively. The flame retardancy, mechanical properties and air permeability were investigated for LOI, vertical flame tests (VFT), micro-scale combustion calorimetry test (MCC), universal testing machine and fully automated permeability instrument.

Results The scanning electron microscopy (SEM) results showed that TD adhered to Lyocell fabrics, but the flame retardants did not block the spaces between the fibers, hence the air permeability of flame-retardant Lyocell fabrics was not affected. Due to the lower thermal stability of the flame retardants, TD facilitate the premature dehydration and carbonization of TD, reducing the thermal stability of flame-retardant Lyocell fabrics in low-temperature regions, while improving their thermal stability in high-temperature regions both in nitrogen and air atmosphere. The VFT results indicated that flame-retardant Lyocell fabrics achieved self-extinguishing after ignition, and the after-flame time and the after-glow time were 0 s. The damaged length of L-TDa and L-TDb were only 54 mm and 51 mm, and the LOI values of L-TDa and L-TDb increased to 38.6% and 48.2%. It can be obtained that flame-retardant Lyocell fabrics had better flame retardancy compared with that of control Lyocell fabrics. Meanwhile, the MCC results presented that TD had a significant inhibitory effect on the heat release of flame-retardant Lyocell fabrics. The peak heat release rates of L-TDa and L-TDb were decreased by 76.0% and 94.1% compared with that of control Lyocell fabrics. The retention ratios of breaking force in both the warp and weft direction of L-TDa and L-TDb were over 70%, meeting the daily use expectation. The air permeability results indicated that the air permeability of flame-retardant Lyocell fabrics were not negatively affected, but was even enhanced compared with that of control Lyocell fabrics. The results of anti-ultraviolet tests showed that the UVA and UVB of flame-retardant Lyocell fabrics were significantly lower than those of control Lyocell fabrics, having better anti-ultraviolet properties. The antibacterial results showed that the flame-retardant Lyocell fabrics had certain antibacterial effect on S. aureus and E. coli, in which the antibacterial rate of L-TDb to S. aureus and E. coli reached 97.4% and 93.3%, respectively.

Conclusion It can be concluded that TD treatment improved the flame retardancy of Lyocell fabrics and conferred certain antibacterial and anti-ultraviolet properties on Lyocell fabrics. However, the warp and weft breaking force of these flame-retardant Lyocell fabrics had been decreased, calling for further improvement in the future to reduce the damage of flame retardants to the mechanical properties of Lyocell fabrics. Meanwhile, the handle and whiteness of flame-retardant Lyocell fabrics also need to be further studied. Considering the better performance of flame-retardant Lyocell fabrics in VFT and LOI, it can be concluded that phosphorous-containing biomass flame retardants have excellent flame-retardant effect and give Lyocell fabrics better flame retardancy.

Key words: flame retardancy, Lyocell fabric, tannic acid, diethylene triamine pentakis (methyl phosphonic acid), bio-based flame retardant, flame-retardant fabric, functional textile

中图分类号:

TS195.2

许云凯, 宋婉萌, 张旭, 刘云. 单宁酸基高效阻燃Lyocell织物的制备及其性能[J]. 纺织学报, 2025, 46(08): 145-153.

XU Yunkai, SONG Wanmeng, ZHANG Xu, LIU Yun. Preparation and properties of high-efficient flame-retardant Lyocell fabrics with tannic acid based flame retardants[J]. Journal of Textile Research, 2025, 46(08): 145-153.

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链接本文: http://www.fzxb.org.cn/CN/10.13475/j.fzxb.20250103001

http://www.fzxb.org.cn/CN/Y2025/V46/I08/145

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样品名称	T_5%/ ℃	T_max/ ℃	R_max/ (%·℃^-1)	700 ℃时的残炭量/%
原Lyocell织物	283	353	2.20	9.60
L-TA	262	325	1.16	6.46
L-DTPMPA	206	286	0.46	23.34
L-TDa	200	290	0.47	29.44
L-TDb	205	227	0.38	39.94

样品名称	T_5%/ ℃	T_max1/ ℃	R_max1/ (%·℃^-1)	T_max2/ ℃	R_max2/ (%·℃^-1)	700 ℃时残炭量/%
原Lyocell织物	278	337	1.17	477	0.21	1.20
L-TA	221	317	1.02	499	0.17	0.21
L-DTPMPA	207	286	0.48	512	0.24	0.36
L-TDa	213	288	0.46	511	0.25	0.60
L-TDb	205	227	0.38	530	0.25	2.10

样品名称	增重率/%	续燃时间/s	阴燃时间/s	损毁长度/mm	LOI值/ %
原Lyocell织物	0.0	19	72	300	19.0
L-TA	7.9	0	0	300	19.1
L-DTPMPA	7.5	0	0	92	38.7
L-TDa	8.2	0	0	54	38.6
L-TDb	16.7	0	0	51	48.2
L-TDb(5次水洗)	6.5	0	0	300	25.2

样品名称	PHRR/ (W·g^-1)	T_PHRR/ ℃	THR/ (kJ·g^-1)	残炭量/%
原Lyocell织物	341	362	21.3	5.0
L-TA	346	327	20.1	7.5
L-DTPMPA	90	276	4.6	35.0
L-TDa	82	289	8.7	43.2
L-TDb	20	203	8.0	44.7

样品名称	透过率/%		UPF值
样品名称	UVA	UVB	UPF值
原Lyocell织物	10.98	6.35	13
L-TA	2.93	1.38	63
L-DTPMPA	9.68	5.25	16
L-TDa	4.13	2.71	59
L-TDb	3.23	2.16	74

单宁酸基高效阻燃Lyocell织物的制备及其性能

Preparation and properties of high-efficient flame-retardant Lyocell fabrics with tannic acid based flame retardants

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