Preparation of DOPO-based Aluminum Phosphinate and Its Flame Retarding Epoxy Resin

Qin-qin LUO; Yu-lin SUN

doi:10.14028/j.cnki.1003-3726.2020.05.004

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Preparation of DOPO-based Aluminum Phosphinate and Its Flame Retarding Epoxy Resin

更新时间：2022-08-31

- Preparation of DOPO-based Aluminum Phosphinate and Its Flame Retarding Epoxy Resin
- Polymer Bulletin Vol. 33, Issue 5, Pages: 31-38(2020)
- 作者机构：
  
  1.岭南师范学院化学化工学院,湛江 524048
  2.岭南师范学院生命科学与技术学院,湛江 524048
- 作者简介：
- 基金信息：
- DOI：10.14028/j.cnki.1003-3726.2020.05.004
  CLC：
- Published：20 May 2020，
  
  Received：05 December 2019，
  
  Revised：19 March 2020，
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Qin-qin LUO, Yu-lin SUN. Preparation of DOPO-based Aluminum Phosphinate and Its Flame Retarding Epoxy Resin. [J]. Polymer Bulletin 33(5):31-38(2020)
DOI：

Qin-qin LUO, Yu-lin SUN. Preparation of DOPO-based Aluminum Phosphinate and Its Flame Retarding Epoxy Resin. [J]. Polymer Bulletin 33(5):31-38(2020) DOI： 10.14028/j.cnki.1003-3726.2020.05.004.

摘要

以10-羟基-9-氧杂-10-磷杂菲-10-氧化物(DOPO-OH)和六水合氯化铝为原料合成了一种DOPO 基膦酸铝盐(DOPO-Al)阻燃剂

通过红外光谱、扫描电镜、能谱、核磁共振磷谱和热失重表征了其结构

并制备了DOPO-Al阻燃的环氧树脂

通过极限氧指数、锥形量热、热失重和差示扫描量热测试分析了该树脂的阻燃和热性能。结果表明

DOPO-Al为高温阻燃剂

其初始热分解温度(

)高达595.5℃。DOPO-Al能提高环氧树脂的阻燃性能和耐热性。当DOPO-Al添加量为7.5% (wt) 时

环氧树脂的LOI值由24.1%提高至31.3%;在燃烧过程中

使其热释放速率峰值、平均热释放速率、总热释放、总烟释放和总烟产量均降低

使残留物增加幅度高达135%。炭层分析表明DOPO-Al存在凝聚相阻燃机理。环氧树脂的

和玻璃化转变温度分别高达368.9℃和161.8℃

所制备阻燃环氧树脂具有较好的热性能。

Abstract

DOPO-based aluminum phosphinate

named as DOPO-Al

was synthesized from 10-hydroxy-9-oxa-10- phosphorphenanthrene-10-oxide (DOPO-OH) and aluminum chloride hexahydrate. Its structure was characterized by the infrared spectrum

scanning electron microscope

energy spectrum

phosphorus nuclear magnetic resonance spectrum and thermogravimetry. The flame-retardant epoxy resin based on DOPO-Al was prepared

and it flame-retardant and thermal properties were analyzed using limiting oxygen index (LOI)

cone calorimetry

thermogravimetry and differential scanning calorimetry. The results showed that DOPO-Al was a high-temperature flame retardant

and its initial thermal decomposition temperature (

) was as high as 595.5℃. The flame-retardant property and heat resistance of epoxy resin were improved by incorporation of DOPO-Al. When 7.5% (wt) DOPO-Al was introduced into the epoxy resin

the LOI value of epoxy resin was increased from 24.1% to 31.3%

and during the combustion

its peak heat release rate

average heat release rate

total heat release

total smoke release and total smoke production were all reduced

and the increase rate of the residue was up to 135%. The analysis of carbon layer suggested that DOPO-Al existed the condensed-phase flameretardant mechanism. Its

and glass transition temperature were up to 368.9℃ and 161.8℃

respectively. The prepared flame-retardant epoxy resin had the good thermal properties.

关键词

DOPO 基膦酸铝盐环氧树脂阻燃性能热性能阻燃机理

Keywords

DOPO-Based aluminum phosphinateEpoxy resinFlame-retardant propertiesThermal propertiesFlame-retardant mechanism

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