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材料研究学报  2017, Vol. 31 Issue (5): 387-393    DOI: 10.11901/1005.3093.2016.385
  论文 本期目录 | 过刊浏览 |
LaCl3掺杂聚丙烯酰胺/硅灰基阻燃材料的制备及其阻燃机理
王亚超(), 赵江平, 童媛媛, 丁建雄
西安建筑科技大学材料与矿资学院 西安 710055
Preparation and Flame-retartant Property of LaCl3 Doped Polyacrylamide/Silica Ash-based Flame Retardant Materials
Yachao WANG(), Jiangping ZHAO, Yuanyuan TONG, Jianxiong DING
College of Materials & Mineral Resources, Xi'an University of Architecture and Technology Xi'an 710055, China
引用本文:

王亚超, 赵江平, 童媛媛, 丁建雄. LaCl3掺杂聚丙烯酰胺/硅灰基阻燃材料的制备及其阻燃机理[J]. 材料研究学报, 2017, 31(5): 387-393.
Yachao WANG, Jiangping ZHAO, Yuanyuan TONG, Jianxiong DING. Preparation and Flame-retartant Property of LaCl3 Doped Polyacrylamide/Silica Ash-based Flame Retardant Materials[J]. Chinese Journal of Materials Research, 2017, 31(5): 387-393.

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摘要: 

在Na2SiO39H2O-KOH改性硅灰(溶胶-凝胶法)制备阻燃材料的基础上,基于正交试验L9(34)研究了焦磷酸钠、聚丙烯酰胺(PAM)和LaCl3对其阻燃性能的影响(包括它们的主次顺序和显著水平),合成了稀土元素掺杂的有机-无机杂化阻燃材料LaCl3/PAM/SiO2nH2O。用热重/差示扫描量热(TG/DSC),扫描电镜(SEM),X-射线衍射(XRD)和红外光谱(FT-IR)等手段进行表征,提出并阐明了其阻燃机理。LaCl3/PAM/SiO2nH2O可使帆布的LOI达到39.2%;极差分析表明其主次顺序依次为PAM > LaCl37H2O>Na4P2O710H2O,方差分析表明PAM与其阻燃性能成高度显著影响,LaCl37H2O为显著影响;XRD和SEM结果表明PAM和LaCl3有助于形成片层状的无定型膨胀硅质层,FT-IR和TG/DSC结果证实其具有优良的高温稳定性,进而产生隔热阻燃效应。

关键词 复合材料阻燃方差分析微结构机理    
Abstract

LaCl3 doped organic-inorganic hybrid flame-retardant materials of LaCl3/PAM/ SiO2nH2O were prepared with Na2SiO39H2O-KOH modified silica ash as base material, and with PAM, LaCl37H2O and Na4P2O710H2O as additives. Then the effect of the addition amount of PAM, LaCl37H2O and Na4P2O710H2O on the flame-retardant property of the LaCl3/PAM/ SiO2nH2O was investigated via orthogonal experiments L9(34). In the meanwhile, the flame-retardant materials of LaCl3/PAM/ SiO2nH2O were characterized by using TG/DSC, SEM, XRD and FT-IR. Results show that the LOI of the cotton canvas with an applied surface film of LaCl3/PAM/SiO2nH2O can reach 39.2%; the sequence of the effectiveness of the additives on the flame-retardant property of LaCl3/PAM/SiO2nH2O can be ranked as PAM > LaCl37H2O > Na4P2O710H2O according to the results of range analysis. The results of XRD and SEM showed that the PAM favored the formation of denser amorphous swelling silica layers, the results of FT-IR and TG/DSC confirmed that the prepared flame-retardant materials held excellent high-temperature thermal stability, leading to the occurrence of heat insulation and fire-resistance effects.

Key wordscomposite    flame retardant    variance analysis    microstructure    mechanism
收稿日期: 2016-07-06     
基金资助:陕西省自然科学基金和教育厅自然科学基金
作者简介:

作者简介 王亚超,男,1988年生,讲师,博士

Levels Factors
PAM(A) Na4P2O710H2O (B) LaCl37H2O (C)
1 0.5 0.5 0.3
2 1 1 0.7
3 3 3 1.2
表1  因素水平表
No. A B C Nullable LOI/%
S1 1 1 1 1 26.9
S2 1 2 2 2 27.6
S3 1 3 3 3 29.4
S4 2 1 2 3 36.4
S5 2 2 3 1 39.2
S6 2 3 1 2 32.1
S7 3 1 3 2 32.4
S8 3 2 1 3 28.6
S9 3 3 2 1 31.2
k1 27.97 31.80 29.20 32.43
k2 35.90 31.90 31.73 30.70
k3 30.73 30.90 33.67 31.47
Range (R) 7.93 1 4.47 1.73
表2  实验方案及结果分析
Variance Sum of variances DOF Mean square F value Fa Significance level
A 97.29 2 48.64 30.64 F0.05(2,4)=6.94
F0.01(2,4)=18.0
Highly
B 1.82 2 0.91 0.57 No
C 30.11 2 15.06 9.48 Yes
e 4.53 2 2.27
eΔ 6.35 4 1.59
Total 140.11
表3  方差分析表
图1  实验样品的XRD图谱
图2  实验样品的FT-IR图谱
图3  硅灰基阻燃材料燃烧后的FT-IR图谱
图4  样品的TG/DSC曲线
图5  样品的微观形貌
图6  阻燃机理示意图
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