Journal of Textile Research ›› 2019, Vol. 40 ›› Issue (12): 79-85.doi: 10.13475/j.fzxb.20180903207

• Dyeing and Finishing & Chemicals • Previous Articles     Next Articles

Synthesis and characterization of novel phosphorous and nitrogen-containing flame retardant for cotton fabrics

SUN Yufa1,2, ZHOU Xiangdong1,2()   

  1. 1. College of Textile and Clothing Engineering, Soochow University, Suzhou, Jiangsu 215021, China
    2. National Engineering Laboratory for Modern Silk, Soochow University, Suzhou, Jiangsu 215123, China
  • Received:2018-09-13 Revised:2019-08-08 Online:2019-12-15 Published:2019-12-18
  • Contact: ZHOU Xiangdong E-mail:zhouxiangdong@suda.edu.cn

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Abstract:

In order to achieve formaldehyde-free flame retardant finishing on cotton fabrics, a novel phosphorus and nitrogen-containing flame retardant polyether diol(PNFR) was synthesized from dimethyl methylphosphonate(DMMP) and diethanolamine(DEA) by transesterification polymerization using dibutyltin dilaurate as the catalyst, and it is also used for finishing cotton fabric. The structure and application performance of PNFR and the modified cotton were investigated by Fourier infrared spectrometer, thermal analyzer, scanning electron microscope, limited oxygen index tester and vertical burning instrument. The experimental results show that when the molar ratio of DMMP and DEA is 1.0∶1.3, the dosage of catalyst is 0.5% of total mass of reactants, the reaction temperature is 150 ℃, reaction time is 5 h and the dosage of PNFR is 200 g/L, the afterflame time, afterglow time, damaged length and limiting oxygen index(LOI) of the treated cotton fabric are 0 s, 12.1 cm and 28.4% respectively, reaching class B1 of national standard of flame retardant fabrics. Even after 10 washing cycles, class B2 of the treated cotton fabric is achieved while its LOI drops to 25.9%.

Key words: flame retardant, phosphorus and nitrogen-containing polyether diol, transesterification, cotton fabric, synergistic flame retardancy

CLC Number: 

  • TS195.5

Fig.1

Chemical reaction for synthesis of PNFR"

Tab.1

Influence of reaction temperature on synthesis and application of PNFR"

温度/
℃		 阻燃剂颜
色状态		 阻燃剂
数均分
子质量		 整理棉的阻燃效果
续燃
时间/s		 阴燃
时间/s		 损毁
长度/cm
105 黄色黏稠液体 703 13.13 0.00 30.0
120 黄褐色黏稠液体 784 11.07 0.00 30.0
135 黄褐色黏稠液体 825 2.95 0.00 22.3
150 棕色黏稠液体 1 062 0.00 0.00 14.0
165 深棕色黏稠液体 1 034 1.64 0.00 16.1

Tab.2

Influence of reaction time on synthesis and application of PNFR"

反应时
间/h		 阻燃剂颜
色状态		 阻燃剂
数均分
子质量		 整理棉织物的阻燃效果
续燃
时间/s		 阴燃
时间/s		 损毁
长度/cm
3 淡黄色黏稠液体 680 11.94 0.00 30.0
4 黄色黏稠液体 787 10.36 0.00 30.0
5 黄色黏稠液体 1 062 0.00 0.00 14.0
6 黄褐色黏稠液体 1 049 1.56 0.00 15.8
7 黄褐色黏稠液体 1 035 2.37 0.00 16.2

Tab.3

Influence of catalyst concentration on synthesis and application of PNFR"

催化剂
质量分
数/%		 阻燃剂颜
色状态		 阻燃剂
数均分
子质量		 整理棉织物的阻燃效果
续燃
时间/s		 阴燃
时间/s		 损毁
长度/cm
0.00 淡黄色黏稠液体 651 12.81 0.00 30.0
0.25 黄色黏稠液体 783 9.79 0.00 28.9
0.50 黄色黏稠液体 1 062 0.00 0.00 14.0
0.75 黄褐色黏稠液体 824 2.76 0.00 21.1
1.00 棕色黏稠液体 815 3.65 0.00 23.2

Tab.4

Influence of molar ratio on synthesis and application of PNFR"

DMMP
和DEA
的量比		 阻燃剂
颜色
状态		 阻燃剂
数均分
子质量		 整理棉织物的阻燃效果
续燃
时间/s		 阴燃
时间/s		 损毁
长度/cm
1.0∶1.1 淡黄色黏稠液体 827 3.80 0.00 26.3
1.0∶1.2 淡黄色黏稠液体 915 1.04 0.00 18.5
1.0∶1.3 淡黄色黏稠液体 1 062 0.00 0.00 14.0
1.0∶1.4 黄色黏稠液体 834 2.96 0.00 21.3
1.0∶1.5 棕色黏稠液体 751 8.81 0.00 30.0

Fig.2

FT-IR spectrum of PNFR"

Tab.5

Influence of PNFR dosage on application performances of cotton fabrics"

PNFR质量
浓度/(g·L-1)		 白度/
%		 质量增
加率/%		 LOI值/
%		 续燃时
间/s		 阴燃时
间/s		 损毁长
度/cm
100 78.2 8.3 24.9 3.44 0.00 26.3
150 75.9 9.1 26.3 2.13 0.00 22.7
200 73.1 12.7 28.4 0.00 0.00 12.1
250 65.4 13.5 28.7 0.00 0.00 10.8

Tab.6

Chemical compositions of original and PNFR treated cotton fabric%"

整理前后 碳 氧 氮 磷 金
整理前 49.71 41.28 0.00 0.00 9.01
整理后 47.15 38.99 2.64 1.74 9.48

Fig.3

SEM images of control (a) and PNFR treated (b) cotton fabric (×800)"

Fig.4

TG (a) and DTG (b) curves of original and PNFR treated cotton fabrics"

Fig.5

SEM images of residue carbon PNFR treated cotton fabric(×1 000). (a) Residue carbon of control; (b) Residuce carbon of treated cotton fabric"

Tab.7

Physical and flame retardant properties of original and PNFR treated cotton fabrics"

处理方法 白度/
%		 断裂强
力/N		 LOI值/
%		 续燃时
间/s		 阴燃时
间/s		 损毁长
度/cm
整理前 80.2 676.13 18.2 3.86 40.56 30.0
整理后 73.1 662.58 28.4 0.00 0.00 12.1
水洗10次 76.5 652.83 25.9 0.00 0.00 16.8

Fig.6

Vertical burning photographs of control cotton (a), PNFR treated (b) and treated cotton fabricafter 10 washing (c)"

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