Journal of Textile Research ›› 2022, Vol. 43 ›› Issue (07): 22-28.doi: 10.13475/j.fzxb.20210608607

• Fiber Materials • Previous Articles     Next Articles

Preparation of aqueous dispersion system of bisneopentyl glycol dithiopyrophosphate and its application in flame-retardant viscose fiber

XIONG Yonghui1,2, WANG Dong1, DU Changsen2, FU Shaohai1()   

  1. 1. Key Laboratory of Eco-Textiles (Jiangnan University), Ministry of Education, Wuxi, Jiangsu 214122, China
    2. Suzhou Sunmun Technology Co., Ltd., Kunshan, Jiangsu 215337, China
  • Received:2021-06-30 Revised:2022-02-18 Online:2022-07-15 Published:2022-07-29
  • Contact: FU Shaohai E-mail:shaohaifu@hotmail.com

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Abstract:

To decrease the particle size of bisneopentyl glycol dithiopyrophosphate (DDPS), and improve the interface compatibility with viscose fibers (VF), the DDPS aqueous dispersion was prepared using non-ionic polyoxyethylene ether dispersants through an ultra-fine processing technology. The influence of dispersant structure on the particle size of DDPS was explored, the response surface method was used to optimize the ultra-fine process parameters. The DDPS aqueous dispersion was then blended into viscose spinning dope, and flame-retardant viscose fibers were prepared through the wet spinning process. The flame-retardant properties of the fibers were explored. The results show that the combination of tallow amine polyoxyethylene ether (TA10) and castor oil polyoxyethylene ether (EL90) has better synergistic dispersion effect for DDPS. With 4 h grinding time, 1 700 r/min grinding speed, and 1.2:1 mass ratio of TA10 to EL90, the median particle size of the DDPS dispersion system is 0.310 μm. The DDPS is evenly distributed in the flame-retardant viscose spinning dope and does not affect the spinnability of viscose collagen solution. Compared to VF, the peak heat release rate of flame-retardant viscose fibers decreases by 18.8 % and the limiting oxygen index increases from 19% to 31.31% when DDPS is 20%.

Key words: bisneopentyl glycol dithiopyrophosphate, responce surface experiment, particle size distribution, viscose fiber, flame retardancy

CLC Number: 

  • TS193.5

Tab.1

Analysis factors and levels for response surface"

水平 A
时间/h		 B
转速/(r·min-1)		 C
TA10与EL90质量比
-1 3.5 1 000 1:1
0 4.0 1 500 2:1
+1 4.5 2 000 3:1

Fig.1

Measuring principle of separation analyzer"

Fig.2

D50 trend curve over grinding time.(a)Effect of dispersant type on D50;(b)Effect of type of compound dispersant on D50"

Fig.3

Effect of grinding time(a), grinding speed(b)and mass ratio of TA10 to EL90(c)on D50"

Tab.2

Results of response surface tests"

试验组编号 时间/h 转速/
(r·min-1)		 TA10与
EL90质量比		 粒径/μm
1 3.5 1 500 1:1 0.494
2 3.5 2 000 2:1 0.437
3 4.0 1 000 1:1 0.467
4 4.0 1 500 2:1 0.338
5 4.0 1 500 2:1 0.338
6 4.5 1 500 3:1 0.422
7 4.5 2 000 2:1 0.383
8 4.0 1 500 2:1 0.338
9 4.5 1 500 1:1 0.426
10 3.5 1 000 2:1 0.679
11 4.0 1 500 2:1 0.338
12 4.0 1 500 2:1 0.338
13 3.5 1 500 3:1 0.534
14 4.0 2 000 1:1 0.338
15 4.0 1 000 3:1 0.581
16 4.0 2 000 3:1 0.427
17 4.5 1 000 2:1 0.614

Tab.3

Variance analysis of response surface for particle size"

来源 平方和 自由度 均方 F值 P值 显著性
模型 0.177 7 9 0.019 7 16.33 0.000 7 显著
X 0.011 2 1 0.011 2 9.24 0.018 8
Y 0.071 4 1 0.071 4 59.09 0.000 1
Z 0.007 1 1 0.007 1 5.91 0.045 4
XY 0.000 0 1 0.000 0 0.03 0.878 8
XZ 0.000 5 1 0.000 5 0.40 0.547 0
YZ 0.000 2 1 0.000 2 0.13 0.729 8
X2 0.044 7 1 0.044 7 36.94 0.000 5
Y2 0.032 1 1 0.032 1 26.51 0.001 3
Z2 0.003 3 1 0.003 3 2.73 0.142 5
残差 0.008 5 7 0.001 2
失拟误差 0.008 5 3 0.002 8
纯误差 0.000 0 4 0.000 0
总离差 0.186 1 16

Tab.4

Normalized deviation and standard deviation analysis result for experimental verification"

样品
编号		 时间/
h		 转速/
(r·min-1)		 TA10与
EL90质量比		 粒径中值/μm N/% Ns/%
理论 试验
1# 4.3 1 800 1.6:1 0.325 0.370 8.63 9.77
2# 4.2 1 950 2.2:1 0.331 0.334
3# 4.1 1 850 1.8:1 0.308 0.359
4# 4.0 1 700 1.2:1 0.310 0.335
5# 4.4 1 950 1.9:1 0.360 0.332

Fig.4

Particle size distribution(a)and SEM image (b)of DDPS dispersion system"

Fig.5

Analysis of rheological properties of viscose dope"

Fig.6

Distribution of DDPS in viscose spinning dope. (a)Viscose spinning dope;(b)Flame-retardant viscose spinning dope"

Fig.7

Heat release rate curve of viscose fiber before and after flame-retardant treatment"

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