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林产化学与工业 ›› 2021, Vol. 41 ›› Issue (1): 21-28.doi: 10.3969/j.issn.0253-2417.2021.01.004

• 重点研发专栏 • 上一篇    下一篇

松节油基聚酰胺阻燃材料的制备与表征

董阜豪, 周新成, 孙鹏昊, 郭丽珍, 徐徐, 王石发()   

  1. 南京林业大学 化学工程学院; 江苏省生物质绿色燃料与化学品重点实验室, 江苏 南京 210037
  • 收稿日期:2020-09-07 出版日期:2021-02-28 发布日期:2021-03-03
  • 通讯作者: 王石发 E-mail:wsfyyq@njfu.com.cn
  • 作者简介:王石发, 教授, 博士生导师, 研究领域为手性合成等; E-mail: wsfyyq@njfu.com.cn
    董阜豪(1993-), 男(满族), 山东高密人, 博士生, 主要从事天然产物深加工利用的研究工作
  • 基金资助:
    国家重点研发计划资助项目(2018YFD0600402)

Preparation and Characterization of Turpentine-based Polyamide Flame Retardant Material

Fuhao DONG, Xincheng ZHOU, Penghao SUN, Lizhen GUO, Xu XU, Shifa WANG()   

  1. College of Chemical Engineering, Nanjing Forestry University; Jiangsu Key Lab. of Biomass-based Green Fuels and Chemicals, Nanjing 210037, China
  • Received:2020-09-07 Online:2021-02-28 Published:2021-03-03
  • Contact: Shifa WANG E-mail:wsfyyq@njfu.com.cn

摘要:

以莰烯的衍生物N-异冰片基丙烯酰胺(NIBAM)为原料,合成了阻燃单体N-三甲氧基硅丙基-N-异冰片基丙烯酰胺(NPSBAM),与N-异丙基丙烯酰胺(NIPAM)无规共聚制备含硅聚异冰片基酰胺共聚物(P(NIPAM-co-NPSBAM)),分析了其结构、形貌和力学性能,最后对其阻燃性能进行了研究。研究结果表明:红外光谱中发现了Si—O—C的振动峰,且碳碳双键基本消失,表明有机硅单体NPSBAM成功引入到了P(NIPAM-co-NPSBAM)中;通过扫描电镜发现,由于刚性环的引入,导致了聚酰胺膜表面粗糙;随NPSBAM含量的增加,共聚物的水接触角上升,表明了材料疏水性增强。此外,热重分析发现,有机硅单体的引入提高了聚酰胺材料的残炭率。随着阻燃单体NPSBAM的增加,热分解动力学分析可得,平均活化能由123.01 kJ/mol提升到了166.93 kJ/mol,这也表明了聚酰胺材料的热稳定性随着NPSBAM的含量增加而提升;机械性能测试表明,聚酰胺材料的拉伸强度由5.2 MPa提升到7.2 MPa,证明了松节油单体中的刚性环提升了聚酰胺材料的机械性能;阻燃测试发现,聚酰胺材料的阻燃性得到了提升,极限氧指数由16.4%提升到23.9%。

关键词: 松节油, 聚酰胺, 阻燃, 有机硅

Abstract:

By using camphene, a derivative of turpentine, as a raw material; a flame-retardant monomer, N-trimethoxysilylpropyl-N-isobornylacrylamide (NPSBAM); and N-isopropylacrylamide (NIPAM), a flame-retardant copolymer—P(NIPAM-co-NPSBAM)—was prepared through the random copolymerization of NPSBAM and NIPAM. The structure, morphology, mechanical properties, and flame retardancy of the copolymer were analyzed. The results showed that the vibration peak of Si—O—C was found in the infrared spectrum, and the carbon-carbon double bond basically disappeared, which indicated that the turpentine silicone monomer NPSBAM was successfully introduced into the copolymer P(NIPAM-co-NPSBAM). Scanning electron microscopy revealed that the surface of NPSBAM-2 was rough, because of the introduction of the rigid ring.Moreover, as the content of NPSBAM increased, the water contact angle increased, indicating that the hydrophobicityof polyamide materialincreased. In addition, thermogravimetric analysis suggested that the introduction of the organosilicon monomer promoted carbon formation in the polyamide materials, and the amount of the residue increased with increasing organosilicon content. The analysis of the thermal decomposition kinetics indicated that with an increase in the content of the flame-retardant monomer, NPSBAM, the average activation energy increased from 123 to 166 kJ/mol. This indicated that the thermal stability of polyamide increased with an increase in the NPSBAM content. The mechanical property test showed that the tensile strength of polyamide increased from 5.2 to 7.2 MPa, which proved that the presence of the rigid ring in the turpentine monomer caused an improvement of the mechanical properties of polyamide. Furthermore, flame retardancy tests showed that the flame retardancy of the polyamide materials was improved.The limiting oxygen index(LOI)also increased from 16.4% to 23.9%.

Key words: turpentine, palyamide, retardant, organosilicon

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