Study on Synthesis Process and Properties of Flame Retardant of Dicyclohexenyl Aluminum Hypophosphite at Atmospheric Pressure

Heng ZHANG; Lei XU; Heng YANG; Kai-jie MU; Min-ge TIAN

doi:10.14028/j.cnki.1003-3726.2018.03.008

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Study on Synthesis Process and Properties of Flame Retardant of Dicyclohexenyl Aluminum Hypophosphite at Atmospheric Pressure

更新时间：2022-09-05

- Study on Synthesis Process and Properties of Flame Retardant of Dicyclohexenyl Aluminum Hypophosphite at Atmospheric Pressure
- Polymer Bulletin Vol. 31, Issue 3, Pages: 59-66(2018)
- 作者机构：
  
  1.青岛科技大学海洋科学与生物工程学院，青岛　266042
  2.广西清洁化制浆造纸与污染控制重点实验室，南宁　530004，济南　250353
  3.欣格瑞(山东)环境科技有限公司，济宁　272415
- 作者简介：
- 基金信息：
- DOI：10.14028/j.cnki.1003-3726.2018.03.008
  CLC：
- Published：20 March 2018，
  
  Received：21 February 2017，
  
  Revised：21 December 2017，
扫描看全文
Heng ZHANG, Lei XU, Heng YANG, Kai-jie MU, Min-ge TIAN. Study on Synthesis Process and Properties of Flame Retardant of Dicyclohexenyl Aluminum Hypophosphite at Atmospheric Pressure. [J]. Polymer Bulletin 31(3):59-66(2018)
DOI：

Heng ZHANG, Lei XU, Heng YANG, Kai-jie MU, Min-ge TIAN. Study on Synthesis Process and Properties of Flame Retardant of Dicyclohexenyl Aluminum Hypophosphite at Atmospheric Pressure. [J]. Polymer Bulletin 31(3):59-66(2018) DOI： 10.14028/j.cnki.1003-3726.2018.03.008.

摘要

制备了一种新型二烷基次膦酸盐阻燃剂，以乙酸为反应溶剂，使环己烯与次膦酸钠在自由基引发剂存在及常压条件下发生自由基加成反应，生成二环己基次膦酸钠，再加入硫酸铝溶液进行复分解反应生成二环己基次膦酸铝。通过红外光谱分析了产物结构，利用X射线能谱仪(EDS)测定P、C等元素含量，通过热失重分析其热稳定性，产物添加到聚酰胺(PA6)中进行极限氧指数测定及垂直燃烧实验考察其阻燃效果，讨论了引发剂种类、引发剂用量、实验温度、反应时间等因素对目标产物产率的影响，优化了合成工艺，并且分析了阻燃剂添加量对阻燃效果影响。结果表明：选择过氧化苯甲酰作为自由基引发剂且用量为5%，反应温度85℃ ，反应时间10h，可使产率达到84%。产物添加至PA6中，阻燃剂最佳用量为12%，此时极限氧指数为34. 1%，燃烧等级为FV-0，阻燃效果良好。

Abstract

A new type of dialkyl group hypophosphite flame retardant was synthesized in this paper. The dicyclohexenyl sodium hypophosphite was first prepared via cyclohexene and sodium hypophosphite

and then reacted in free radical initiator and normal pressure conditions with ethanol as the solvent. Dicyclohexenyl aluminum hypophosphite (DCAH) was obtained by adding aluminum sulfate. Molecular structures were characterized by FT-IR. Phosphorus and carbon element contents were measured by energy dispersive X-ray spectroscope. Product thermostability was analyzed via thermogravimetric analyzer. Flame retardant properties were investigated by adding DCAH to polyamide (PA); limiting oxygen index (LOI) and vertical burning were determined. The influences of initiator species

initiator dosage

temperature

and reaction time on target product yield were discussed

and synthesis condition was optimized. The effect of DCAH additive content was also studied. Benzoperoxide was the best initiator

and the optimum dosage was 5%. The product could yield up to 84% when reacted for 10 h at 85℃. LOI was 34. 1 %

and flame class was FV-0

whereas 12% DCAH was added to PA material.

关键词

常压合成自由基加成环己烯次膦酸盐阻燃剂

Keywords

Normal pressure synthesisCyclohexeneEnvironment-friendlyHypophosphiteFlame retardant

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