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木质素基含氮磷阻燃剂的合成及热重分析

Synthesis and Thermal Analysis of Lignin-based Flame Retardant Containing Nitrogen and Phosphorus

  • 摘要: 以解聚木质素(DL)为原料,采用相转移超声波法制备了席夫碱型含氮木质素(N-DL),再进一步与9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)反应,合成氮磷改性DL(NP-DL),NP-DL是一种新型膨胀型木质素基含氮磷阻燃剂。采用FT-IR、1H NMR、31P NMR、TG、TG/FT-IR、TG/MS、GPC和XPS方法对NP-DL的结构和性能进行表征。研究结果表明:DL中成功地引入了N、P元素;TG分析表明600和800℃时NP-DL残炭率比DL残炭率分别提高了1 285.5%和362.6%。TG/FT-IR联用和TG/MS联用测试结果表明:NP-DL受热降解产生含磷物OP+m/z=47)、H3PO(m/z=50)、O2P+m/z=63)和HO2P+m/z=64),证明NP-DL在热解过程中产生的含磷化合物抑制了燃烧。

     

    Abstract: Using depolymerized lignin(DL) as raw material, Schiff base nitrogen-containing lignin(N-DL) was prepared by phase transfer ultrasonic method, and then further reacted with 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide(DOPO) to synthesize nitrogen-phosphorus modified DL(NP-DL). NP-DL was a new type of expanded lignin-based nitrogen and phosphorus flame retardant. The structure and performance of NP-DL were characterized by FT-IR, 1H NMR, 31P NMR, TG, TG/FT-IR, TG/MS, GPC and XPS. The results showed that N and P were successfully introduced into the depolymerized lignin; TG analysis showed that the carbon residue rates of NP-DL at 600 and 800℃ were increased by 1 285.5% and 362.6% compared with those of DL, respectively. The test results of TG/FT-IR and TG/MS showed that NP-DL was thermally degraded to produce phosphorus: OP+ with m/z=47, H3PO with m/z=50, O2P+ with m/z=63 andHO2P+ with m/z=64 proved that the phosphorus-containing compounds produced during the pyrolysis of NP-DL inhibited combustion.

     

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