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

RichHTML

15

PDF (PC)

240

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"

[1] 莫达杰, 李旭明, 许增慧. 聚(3-羟基丁酸-co-3-羟基戊酸共聚酯)/聚乳酸阻燃纤维的制备及其性能[J]. 纺织学报, 2019, 40(5):12-17.
MO Dajie, LI Xuming, XU Zenghui. Preparation and properties of poly ( 3-hydroxybutyrate-co-3-hydroxyl valerate)/polylactic acid flame retardant fibers[J]. Journal of Textile Research, 2019, 40(5):12-17.
[2] 余娟娟, 刘淑强, 吴改红, 等. 玄武岩织物增强聚乳酸复合材料的制备及其拉伸断裂性能[J]. 纺织学报, 2019, 40(2):82-86.
YU Juanjuan, LIU Shuqiang, WU Gaihong, et al. Preparation and tensile fracture properties of basalt fabric reinforced polylactic acid composites[J]. Journal of Textile Research, 2019, 40(2):82-86.
[3] ZHAO Xiaomin, GUERRERO Francisco Reyes, LLORCA J, et al. New superefficiently flame-retardant bioplastic poly (lactic acid): flammability, thermal decomposition behavior, and tensile properties[J]. ACS Sustainable Chemistry & Engineering, 2016, 4(1):202-209.
[4] FENG Jiabing, SUN Yiqi, SONG Pingan, et al. Fire-resistant, strong, and green polymer nanocomposites based on poly (lactic acid) and core-shell nanofibrous flame retardants[J]. ACS Sustainable Chemistry & Engineering, 2017, 5(9):7894-7904.
[5] LONG Lijuan, CHANG Qifeng, HE Wentao, et al. Effects of bridged DOPO derivatives on the thermal stability and flame retardant properties of poly (lactic acid)[J]. Polymer Degradation and Stability, 2017, 139:55-66.
doi: 10.1016/j.polymdegradstab.2017.03.016
[6] WU Ningjing, FU Guoliang, YANG Yue, et al. Fire safety enhancement of a highly efficient flame retardant poly (phenylphosphoryl phenylenediamine) in biodegradable poly (lactic acid)[J]. Journal of Hazardous Materials, 2019, 363:1-9.
doi: S0304-3894(18)30777-5 pmid: 30300772
[7] SONG Yan, ZONG Xu, WANG Nan, et al. Preparation of γ-divinyl-3-aminopropyltriethoxysilane modified lignin and its application in flame retardant poly (lactic acid)[J]. Materials, 2018, 11(9):1505-1513.
doi: 10.3390/ma11091505
[8] SHAN Xueying, SONG Lei, XING Weiyi, et al. Effect of nickel-containing layered double hydroxides and cyclophosphazene compound on the thermal stability and flame retardancy of poly (lactic acid)[J]. Industrial & Engineering Chemistry Research, 2012, 51(40):13037-13045.
doi: 10.1021/ie300589p
[9] KANG Benhao, LU Xiang, QU Jinping, et al. Synergistic effect of hollow glass beads and intumescent flame retardant on improving the fire safety of biodegradable poly (lactic acid)[J]. Polymer Degradation and Stability, 2019, 164:167-176.
doi: 10.1016/j.polymdegradstab.2019.04.013
[10] 魏丽菲, 朱志国, 靳昕怡, 等. 基于三(2-羟乙基)异氰尿酸酯的膨胀型阻燃剂对聚合物燃烧性能的影响[J]. 纺织学报, 2017, 38(9):24-31.
WEI Lifei, ZHU Zhiguo, JIN Xinyi, et al. Influence of tris (2-hydroxyethyl) isocyanurate-based intrmescent flame retardants on combustion performance of poly-mers[J]. Journal of Textile Research, 2017, 38(9):24-31.
[11] WANG Chao, WU Yicheng, LI Yingchun, et al. Flame-retardant rigid polyurethane foam with a phosphorus-nitrogen single intumescent flame retardant[J]. Polymers for Advanced Technologies, 2018, 29(1):668-676.
doi: 10.1002/pat.v29.1
[12] LIU Xiaodong, SUN Jun, ZHANG Sheng, et al. Effects of carboxymethyl chitosan microencapsulated melamine polyphosphate on the flame retardancy and water resistance of thermoplastic polyurethane[J]. Polymer Degradation and Stability, 2019, 160:168-176.
doi: 10.1016/j.polymdegradstab.2018.12.019
[13] RAN Guowen, LIU Xiaodong, GUO Jia, et al. Improving the flame retardancy and water resistance of polylactic acid by introducing polyborosiloxane microencapsulated ammonium polyphosphate[J]. Composites Part B: Engineering, 2019, 173:106-113.
[14] ZHU Min, ZHANG Yang, SHENG Haibo, et al. Effect carbon black microencapsulated ammonium polyphosphate on the flame retardancy and mechanical properties of polyurethane composites[J]. Polymer-Plastics Technology and Materials, 2019, 279:1-12.
[15] ZHU Jianqiang, LU Xin, YANG Huayu, et al. Vinyl polysiloxane microencapsulated ammonium polyphosphate and its application in flame retardant polypropylene[J]. Journal of Polymer Research, 2018, 25(4):107-116.
doi: 10.1007/s10965-018-1505-7
[1] LIN Shenggen, LIU Xiaohui, SU Xiaowei, HE Ju, REN Yuanlin. Preparation and properties of Lyocell fibers and fabrics modified with new phytic acid based flame retardant [J]. Journal of Textile Research, 2021, 42(07): 25-30.
[2] ZENG Fanxin, QIN Zongyi, SHEN Yueying, CHEN Yuanyu, HU Shuo. Preparation and flame retardant properties of self-extinguishing cotton fabrics by spray-assisted layer-by-layer self-assembly technology [J]. Journal of Textile Research, 2021, 42(01): 103-111.
[3] XIAO Chuanmin, XIAO Changfa, ZHANG Tai, WANG Xinya. Structure and properties of braided tube reinforced polylactic acid hollow fiber membranes [J]. Journal of Textile Research, 2019, 40(08): 20-26.
[4] MO Dajie, LI Xuming, XU Zenghui. Preparation and properties of poly(3-hydroxybutyrate-co-3-hydroxyl valerate)/polylactic acid flame retardant fibersMO [J]. Journal of Textile Research, 2019, 40(05): 12-17.
[5] DONG Hao, ZHANG Liping, LIU Yining, WANG Lejun, LIU Yayun, FU Shaohai. Preparation and properties of modified carbon black for dope dyeing of polylactic acid fiber [J]. Journal of Textile Research, 2019, 40(05): 64-69.
[6] LI Xiaochuan, QU Qianqian, LI Xuming. Preparation and properties of polylactic acid/polypropylene blend fiber by melt spinning [J]. Journal of Textile Research, 2019, 40(03): 8-12.
[7] WU Qiqi, LI Min, LIU Yining, WANG Lejun, ZHANG Liping, FU Shaohai. Dyeing properties of polylactic acid fabric by carrier dyeing method [J]. Journal of Textile Research, 2019, 40(01): 79-83.
[8] . Fabrication of polylactic acid tree-like nanofiber membrane and its application in filtration [J]. Journal of Textile Research, 2018, 39(12): 139-144.
[9] . Effect of combined anti-dripping additive on properties of flame resistant polyester [J]. JOURNAL OF TEXTILE RESEARCH, 2018, 39(08): 15-21.
[10] . Design on printing parameters of flexible polylactic acid used in 3D printing fabric texture [J]. JOURNAL OF TEXTILE RESEARCH, 2018, 39(05): 38-42.
[11] . Preparation of a novel N-P flame retardant and its flame retardant properties in cotton fabric [J]. JOURNAL OF TEXTILE RESEARCH, 2017, 38(11): 97-101.
[12] . Glass fiber reinforced polylactic acid composites based on 3D printing technology [J]. JOURNAL OF TEXTILE RESEARCH, 2017, 38(10): 13-18.
[13] . Influence of tris (2-hydroxyethyl) isocyanurate-based intrmescent flame retardants on combustion performance of polymers [J]. JOURNAL OF TEXTILE RESEARCH, 2017, 38(09): 24-31.
[14] . Structure and properties of polylactic acid-polycaprolactone/silk fibroin composite nanofibrous scaffolds [J]. JOURNAL OF TEXTILE RESEARCH, 2017, 38(05): 8-13.
[15] . Preparation and properties of reinforcing and toughened polylactic acid fiber [J]. JOURNAL OF TEXTILE RESEARCH, 2017, 38(04): 12-16.
Viewed
Full text


Abstract

Cited
  Shared   
  Discussed   
No Suggested Reading articles found!
京ICP备14006648号
Copyright 2021 © Editorial office of Journal of Textile Research
Supported by Beijing Magtech Co.Ltd