Journal of Textile Research ›› 2019, Vol. 40 ›› Issue (04): 7-14.doi: 10.13475/j.fzxb.20181103908

• Fiber Materials • Previous Articles     Next Articles

Preparation and structural properties of flame retardant poly(L-lactic acid) and fiber thereof

ZHANG Anying1, WANG Zhaoying1, WANG Rui1(), DONG Zhenfeng1, WEI Lifei2, WANG Deyi3   

  1. 1. School of Materials Science & Engineering, Beijing Institute of Fashion Technology, Beijing 100029, China
    2. College of Polymer Science and Engineering, Sichuan University, Chengdu, Sichuan 610065, China
    3. IMDEA Materials Institute, Madrid 28906, Spain
  • Received:2018-11-14 Revised:2019-01-05 Online:2019-04-15 Published:2019-04-16
  • Contact: WANG Rui E-mail:clywangrui@bift.edu.cn

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Abstract:

In order to study the flame retardancy and spinnability of poly(L-lactic acid) (PLLA), an environmentally [(6-oxo-6H-dibenzo-(c,e)(1,2)-oxaphosphorin-6-one)methyl] butanedioic acid (DDP) flame retardant PLLA system was designed. PLLA/DDP composites were prepared by twin-screw melt extrusion, and the structures and properties thereof were characterized by cone calorimetry, limiting oxygen index, vertical combustion, scanning electron microscopy, differential scanning calorimetry and thermogravimetric analysis. The effect of the flame retardant content on the flame retardant properties of PLLA and the flame retardant mechanism of DDP on PLLA were also investigated. The spinning process and fiber properties at the optimum flame retardant dosage were studied. The results show that when the mass content of DDP is 9%, the LOI of the composite reaches 29% and the UL-94 test reaches grade V-0. The amount of carbon residue of the composite at 800 ℃ increases from 10.7% to 13.5%, and the composite has excellent spinnability. After the nascent fiber is stretched and heat set by 3 times, the breaking strength is 1.77 cN/dtex, and the elongation at break is 44.9%.

Key words: poly(L-lactic acid), halogen-free flame retardant, flame retardancy, spinnability, breaking strength

CLC Number: 

  • TQ342.89

Tab.1

Ratio of composites%"

样品编号 PLLA质量分数 DDP质量分数
1﹟ 100 0
2﹟ 97 3
3﹟ 95 5
4﹟ 93 7
5﹟ 91 9
6﹟ 89 11

Tab.2

Spinning technology parameters"

样品
编号		 纺丝温度/℃ 卷绕速度/
(m·min-1)		 热定型温度/℃
Ⅰ区 Ⅱ区 Ⅲ区 Ⅳ区 管道 组件 上辊 下辊 热辊
1﹟ 160 185 180 180 180 180 500 60 75 85
5﹟ 165 195 210 210 210 210 500 75 80 90

Fig.1

SEM cross section images of flame retardant PLLA composites(×500)"

Fig.2

DSC heating(a) and cooling (b) curves of flame retardant PLLA composites"

Tab.3

Results of DSC of flame retardant PLLA composites℃"

样品
编号		 θg θcc θm θmc θ0 θm-θ0
1﹟ 60 98 174 99 91 83
2﹟ 60 96 173 97 87 86
3﹟ 59 98 172 93 90 82
4﹟ 59 97 172 92 89 83
5﹟ 59 97 172 91 89 83
6﹟ 59 98 170 — 89 81

Fig.3

TG and DTG curves of PLLA, DDP and its composite"

Fig.4

TG and DTG curves of flame retardant PLLA composites"

Fig.5

Cone calorimetry curves of flame retardant PLLA composites. (a) Heat release rate curve;(b) Total heat release curve"

Tab.4

LOI and UL-94 results of flame retardant PLLA composites"

样品
编号		 LOI/
%		 UL-94测试结果 30 s内熔滴数
t1/s t2/s 等级
1﹟ 19 20.9 23.0 V-2 18
2﹟ 22 10.5 4.5 V-2 16
3﹟ 25 17.4 10.5 V-2 16
4﹟ 25 12.4 6.3 V-2 14
5﹟ 29 8.1 4.5 V-0 13(自熄)
6﹟ 27 9.5 4.3 V-0 13(自熄)

Fig.6

FT-IR spectra of 1# and 5# at different temperatures"

Fig.7

FT-IR spectra of gas of thermal degradation of samples at different temperature"

Fig.8

3-D FT-IR spectra of TGA gaseous products of 1# and 5# sample"

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