Synergistic Flame Retardancy of Amine-based Multi-walled Carbon Nanotubes/DOPO Derivatives and Its Effect on the Properties of Nylon 6

Xin-xin Wang; Wen-tao He; Guo-min Xu; Li-juan Long; Wei-jiang Huang; Jie Yu

doi:10.11777/j.issn1000-3304.2018.18230

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Synergistic Flame Retardancy of Amine-based Multi-walled Carbon Nanotubes/DOPO Derivatives and Its Effect on the Properties of Nylon 6

Research Article | 更新时间：2021-01-26

- Synergistic Flame Retardancy of Amine-based Multi-walled Carbon Nanotubes/DOPO Derivatives and Its Effect on the Properties of Nylon 6
- Acta Polymerica Sinica Vol. 50, Issue 4, Pages: 419-428(2019)
- 作者机构：
  
  1.贵州大学材料与冶金学院　贵阳 550025
  2.国家复合改性聚合物材料工程技术研究中心　贵阳 550014
- 作者简介：
- 基金信息：
- DOI：10.11777/j.issn1000-3304.2018.18230
  CLC：
- Published：2019-4，
  
  Published Online：26 February 2019，
  
  Received：22 November 2018，
  
  Revised：18 January 2019，
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Xin-xin Wang, Wen-tao He, Guo-min Xu, Li-juan Long, Wei-jiang Huang, Jie Yu. Synergistic Flame Retardancy of Amine-based Multi-walled Carbon Nanotubes/DOPO Derivatives and Its Effect on the Properties of Nylon 6. [J]. Acta Polymerica Sinica 50(4):419-428(2019)
DOI：

Xin-xin Wang, Wen-tao He, Guo-min Xu, Li-juan Long, Wei-jiang Huang, Jie Yu. Synergistic Flame Retardancy of Amine-based Multi-walled Carbon Nanotubes/DOPO Derivatives and Its Effect on the Properties of Nylon 6. [J]. Acta Polymerica Sinica 50(4):419-428(2019) DOI： 10.11777/j.issn1000-3304.2018.18230.

摘要

将DOPO衍生物(DIDOPO)和氨基碳纳米管(MWCNTs)以一定的比例进行复配，添加到尼龙6 (PA6)中熔融共混制得复合材料. 运用万能试验机、热重分析仪、示差扫描量热仪、锥形量热仪及扫描电镜测试了各样本的力学性能、热稳定性、结晶性以及燃烧性能，并观察了炭层形貌. 测试结果表明，加入MWCNTs后，复合材料的拉伸强度显著增强，与PA6/DIDOPO复合材料相比，其拉伸强度平均提升了55%. 从非等温结晶曲线可以看出，加入MWCNTs后PA6复合材料的结晶初始温度(

onset

)和结晶峰温(

)都有明显提高，但由于MWCNTs的异相成核作用，结晶度降低. 此外，锥形量热测试表明，当MWCNTs的添加量为2 wt%时，其热释放速率峰值(PHRR)为367.28 kW/m

，较纯PA6降低了58.9%. 扫描电镜和拉曼测试分析表明MWCNTs的加入促进了致密结构炭层的形成，与DIDOPO有协效阻燃的作用.

Abstract

A novel DOPO derivative (DIDOPO) is incorporated together with amine-based multi-walled carbon nanotubes (MWCNTs) into PA6 by melt blending. Mechanical properties

thermal stability

crystallinity

and combustion properties are measured using universal testing machine

thermogravimetric analyzer

differential scanning calorimeter

and cone calorimeter

respectively. After combustion

the morphology of char layer is further observed by a scanning electron microscope. The results show that MWCNTs-incorporated flame-retardant nanocomposites exhibit a tensile strength that is 55% higher than that of the PA6/DIDOPO composites. From the TG and DTG curves

it can be seen that the

5wt%

of PA6 composites increased slightly and the maximum weight loss rate temperature (

max

) gradually improved after adding MWCNTs

indicating that the addition of MWCNTs delays the process of thermal degradation of the PA6 composites. With the incorporation of MWCNTs

the amount of residual carbon is also increased. From the non-isothermal crystallization curve

it can be seen that the crystallization initial temperature (

onset

) and crystallization peak temperature (

) of the PA6 composites are significantly improved with the addition of MWCNTs. However

the crystallinity is lower due to the heterogeneous nucleation of the MWCNTs. From UL-94 datas

the combustion time (

) is increased with the incorporation of MWCNTs into PA6/DIDOPO composites

which results in a V-1 level in the UL-94 test and a slightly increased LOI value. This phenomenon can be attributed to an increment in melt viscosity and a decrement in flow properties. Combined with the curves of effective combustion heat

total smoke release and CO release rate

it can be concluded that the synergistic effect between MWCNTs and DIDOPO weakens the thermal degradation process of the PA6 composites

thus increasing the incomplete combustion and reducing the complete combustion of the PA6 composites

which is beneficial to the flame retardance of the materials. Addition of 2 wt% MWCNTs results in a peak heat release rate (PHRR) of 367.28 kW/m

which corresponds to a 58.9% lower rate than that of pure PA6

as revealed by cone calorimetry. Based on SEM and Raman

a continuous and compact char layer is observed upon addition of MWCNTs

which is ascribed to a synergistic effect between MWCNTs and DIDOPO.

关键词

氨基碳纳米管DOPO衍生物尼龙6热稳定性协效阻燃

Keywords

Amine-based multi-walled carbon nanotubesDOPO derivativesNylon 6Thermal stabilitySynergistic flame retardant

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State Key Lab of Fire Science, University of Science and Technology of China

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