二硫代焦磷酸酯水性分散体系的制备及其在阻燃粘胶纤维中的应用

doi:10.13475/j.fzxb.20210608607

纺织学报 ›› 2022, Vol. 43 ›› Issue (07): 22-28.doi: 10.13475/j.fzxb.20210608607

二硫代焦磷酸酯水性分散体系的制备及其在阻燃粘胶纤维中的应用

熊永辉¹^,², 王冬¹, 杜长森², 付少海¹()

1.生态纺织教育部重点实验室(江南大学), 江苏无锡 214122
2.苏州世名科技股份有限公司, 江苏昆山 215337

收稿日期:2021-06-30 修回日期:2022-02-18 出版日期:2022-07-15 发布日期:2022-07-29
通讯作者: 付少海
作者简介:熊永辉(1995—),男,硕士生。主要研究方向为阻燃粘胶纤维及其阻燃浆料的制备。
基金资助:
江苏省自然科学基金项目(BK20190613);国家重点研发计划项目(2017YFB0309503)

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. 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 Published:2022-07-15 Online:2022-07-29
Contact: FU Shaohai

摘要/Abstract

摘要：

针对二硫代焦磷酸酯(DDPS)阻燃剂粒径大,与粘胶纤维(VF)界面相容性差等问题,以聚氧乙烯醚型非离子表面活性剂为分散剂,通过超细加工制备了DDPS水性分散体系;探究了分散剂结构对DDPS粒径的影响,通过响应面试验方法优化超细化工艺参数;然后将DDPS水性分散体系共混添加到粘胶纺丝原液中,通过湿法纺丝制得阻燃粘胶纤维,探究了纤维的阻燃性能。结果表明:牛酯胺聚氧乙烯醚(TA10)和蓖麻油聚氧乙烯醚(EL90)复配对DDPS具有较好的协同分散作用;当研磨时间为4 h,研磨转速为1 700 r/min,分散剂TA10和EL90质量比为1.2:1时,DDPS分散体系粒径中值为0.310 μm;DDPS在阻燃粘胶原液中分布均匀,且不影响粘胶原液的可纺性;与VF相比,当DDPS质量分数为20%时,阻燃粘胶纤维热释放速率峰值下降了18.8%,极限氧指数从19%升高到31.31%。

关键词: 二硫代焦磷酸酯, 响应面试验, 粒径分布, 粘胶纤维, 阻燃性能

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

中图分类号:

TS193.5

熊永辉, 王冬, 杜长森, 付少海. 二硫代焦磷酸酯水性分散体系的制备及其在阻燃粘胶纤维中的应用[J]. 纺织学报, 2022, 43(07): 22-28.

XIONG Yonghui, WANG Dong, DU Changsen, FU Shaohai. Preparation of aqueous dispersion system of bisneopentyl glycol dithiopyrophosphate and its application in flame-retardant viscose fiber[J]. Journal of Textile Research, 2022, 43(07): 22-28.

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参考文献 11

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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

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

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

样品编号	时间/ h	转速/ (r·min^-1)	TA10与 EL90质量比	粒径中值/μm		N/%	N_s/%
样品编号	时间/ h	转速/ (r·min^-1)	TA10与 EL90质量比	理论	试验	N/%	N_s/%
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

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二硫代焦磷酸酯水性分散体系的制备及其在阻燃粘胶纤维中的应用

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

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