苯并咪唑类氮-磷膨胀型阻燃剂的合成  

Synthesis of Benzimidazole Nitrogen-phosphorus Intumescent Flame Retardant

作　　者：郑国才 张燕杰[1,2,3] 薛涵与 林棋 ZHENG Guocai;ZHANG Yanjie;XUE Hanyu;LIN Qi(Ocean College,Minjiang University,Fuzhou,Fujian 350108,China;Engineering Research Center of Green Dyeingand Finishing in Fujian Provincial University,Minjiang University,Fuzhou,Fujian 350108,China;FujianEngineering Research Center of New Chinese Lacquer Material,Minjiang University,Fuzhou,Fujian 350108,China)

机构地区：[1]闽江学院海洋学院,福建福州350108 [2]闽江学院绿色染整福建省高校工程研究中心,福建福州350108 [3]闽江学院福建省中国漆新型材料工程研究中心,福建福州350108

出　　处：《闽江学院学报》2018年第5期87-91,共5页Journal of Minjiang University

基　　金：国家自然TUIP基金项目(21503105;51703090);福建省自然基金(2017J01584);福建省中青年教师教育科研项目(JAT170453);闽江学院科技项目(MYK16004)

摘　　要：以新戊二醇、三氯氧磷和苯并咪唑为原料,三乙胺为缚酸剂合成了3-(5,5-二甲基-1,3-二氧杂-2-磷杂环己基磷酰基)苯并咪唑(产物Ⅱ),即首先新戊二醇先与三氯氧磷反应制得5,5-二甲基-1,3-二氧杂-2-磷杂环己内酰氯(新戊二醇磷酰氯或产物Ⅰ),其次以产物Ⅰ与苯并咪唑反应制得产物Ⅱ.通过质谱(MS)、元素分析、傅里叶红外光谱(FT-IR)和核磁共振波谱(1H NMR、13C NMR)等手段表征所制备的目标产物,并考察了缚酸剂种类、缚酸剂滴加时间、溶剂的选择和溶剂的用量等因素对产物收率的影响.3-（5,5-dimethyl-1,3-dioxa-2-phosphacyclohexyl phosphacyl） benzimidazole （productⅡ）was prepared from neopentyl glycol, phosphorus oxychloride and benzimidazole in the presence of triethylamine as the deacid reagent. Thus 5,5-dimethyl-1,3-dioxa-2- phosphacyclohexyl acyl chloride （neopentyl glycol chlorophosphate or productⅠ） was obtained at first by reaction of neopentyl glycol with phosphorus oxychloride, and then reacted it with benzimidazole to prepare productⅡ. Structure of the title compound was confirmed by mass spectrometry（MS）, elementary analysis, Fourier transform infrared spectra（FT-IR） and 1 H and 13 C nuclear magnetic resonance spectrum（ 1 H NMR, 13 C NMR）. The effect of deacid reagent species, deacid reagent dropwise time, solvent select and solvent dosage on the yield were discussed.

关 键 词：新戊二醇 三氯氧磷 苯并咪唑 膨胀型阻燃剂 

分 类 号：TQ314.24[化学工程—高聚物工业]