Journal of Textile Research ›› 2021, Vol. 42 ›› Issue (06): 71-77.doi: 10.13475/j.fzxb.20200902207

Special Issue: Flame Retardant Fibers and Textiles

• Fiber Materials • Previous Articles     Next Articles

Preparation of microencapsulated intumescent flame retardant and its use in polylactic acid

WEN Yufeng, MA Xiaopu, SHENG Fangyuan, ZHU Zhiguo()   

  1. School of Materials Design & Engineering, Beijing Institute of Fashion Technology, Beijing 100029, China
  • Received:2020-09-09 Revised:2021-03-08 Online:2021-06-15 Published:2021-06-28

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Abstract:

In order to improve the flame retardant efficiency, ammonium polyphosphate (marked as A), microcrystal cellulose (marked as C) and melamine cyanourate (marked as M) were selected as the basic components to prepare microencapsulated intumescent flame retardants, noted as M(A&C), via combination of ball-milling and in-situ synthesis techniques. M(A&C) was subsequently incorporated into polylactic acid (PLA) via melt blending method to get the PLA/M(A&C) samples. The structure of MA&C, thermal properties, flame retardancyand residual carbon morphology of flame retardantsamples were characterized with the help of thermogravimetric, Fourier transform infrared, X-ray photoelectron spectroscopy and scanning electron microscope. The results show that PLA/M(A&C) demonstrates better flame retardant ability than PLA/(M+A+C), with the same loadings of flame retardant (3%, 5% and 10% mass fraction, respectively). The limit oxygen index of the former samples was 27%, 29%, and 31.5%, respectively, which is obviously higher than those of the latter samples (24%, 25%, anf 28.5%, respectively). The overall flame retardancy of PLA/M(A&C)-10 is found excellent, achieving UL-94 V-0 grade. The peak heat release rate, total heat release and char residue show obvious flame retardancy properties, with the values of 313 kW/m2, 54 MJ/m2, and 16.1%, respectively.

Key words: intumescent flame retardant, microencapsul, polylactic acid, flame retardant property

CLC Number: 

  • TQ314.24

Fig.1

Preparation and structure scheme of intumescent flame-retardant M(A&C)"

Tab.1

Formulation of flame-retardant PLA blendsg"

样品名称 PLA M(A&C) (M+A+C)
PLA 100 0 0
PLA/M(A&C)-3 97 3 0
PLA/M(A&C)-5 95 5 0
PLA/M(A&C)-10 90 10 0
PLA/(M+A+C)-3 97 0 3
PLA/(M+A+C)-5 95 0 5
PLA/(M+A+C)-10 90 0 10

Fig.2

FTIR spectra of flam eretardants APP, MCA, A&C and M(A&C)"

Fig.3

SEM images of APP,A&C and M(A&C)"

Fig.4

XPS spectra of APP,A&C and M(A&C)"

Tab.2

TG data of different flame retardants"

样品名称 T5%/℃ Tmax/℃ 质量保留率(800 ℃)/%
APP 314.5 610.1 24.9
A+C 292.8 595.3 18.3
A&C 223.2 573.1 24.1
M+A+C 290.9 341.2 26.6
M(A&C) 249.1 295.5 37.6

Fig.5

DSC (a) and TG (b) curves of PLA and flame-retardant PLA samples"

Fig.6

LOI of PLA and flame retardant PLA samples"

Tab.3

UL-94 test data for PLA and flame retardant PLA samples"

样品名称 t1/s t2/s 是否点燃
脱脂棉 		熔滴 UL-94
等级
PLA >30 无 是 ★★★★★ /
PLA/APP-10 6.9 3.9 是 ★★★★ V-2
PLA/(M+A+C)-3 12.8 8.9 是 ★★★★★ /
PLA/(M+A+C)-5 11.5 4.7 是 ★★★★ V-2
PLA/(M+A+C)-10 6.3 1.7 是 ★★★ V-2
PLA/M(A&C)-3 12.1 3.0 是 ★★★★ V-2
PLA/M(A&C)-5 4.1 1.5 是 ★★★ V-2
PLA/M(A&C)-10 1.3 0.9 否 无 V-0

Tab.4

Cone calorimeter data of PLA and flame retardant PLA samples"

样品名称 TTI/
s 		pHRR/
(kW·m-2) 		THR/
(MJ·m-2) 		残炭
量/% 		FGI/FPI
PLA 67 437 73.2 3.7 2.36/0.153
PLA/APP-10 64 443 62.0 10.6 2.70/0.145
PLA/(M+A+C)-10 64 360 62.5 8.4 2.12/0.178
PLA/M(A&C)-10 56 313 54.0 16.1 1.93/0.179

Fig.7

SEM images of residue char of PLA and flame retardant PLA samples(×1 000). (a)Surface morphology;(b)Interior morphology"

Fig.8

XPS spectra of residue char of PLA and PLA/M(A&C)-10"

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