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作 者:耿建齐 杨瑞光 李远超 李善清 GENG Jian-qi;YANG Rui-guang;LI Yuan-chao;LI Shan-qing(Shandong Province Key Laboratory of Marine Fine Chemicals,Shandong Ocean Chemical Industry Scientific Research Institute,Weifang 262700,China)
机构地区:[1]山东省海洋精细化工重点实验室,山东省海洋化工科学研究院,山东潍坊262700
出 处:《应用化工》2019年第S02期207-209,共3页Applied Chemical Industry
摘 要:以六氯环三磷腈、苯酚、NaOH为原料,四丁基氯化铵为相转移催化剂,无水氯苯为溶剂,两步法合成了六苯氧基环三磷腈,分别考察了溶剂种类、反应温度、反应时间、四丁基氯化铵用量、物料配比对产品收率的影响。结果表明,在氮气保护、氯苯为溶剂、反应温度130℃,n(苯酚)∶n(NaOH)∶n(六氯环三磷腈)∶n(四丁基氯化铵)=7.5∶7.5∶1∶0.1等条件下,回流反应6.0 h,经过分离和提纯,产品的收率为90.0%,纯度达到99.0%。Hexaphenoxy cyclotriphosphazene was synthesized by two-step method with phosphonitrilic chloride trimer,phenol and NaOH as raw materials,tetrabutyl ammonium chloride as phase transfer catalyst and anhydrous chlorobenzene as solvent.The effects of solvent type,reaction temperature,reaction time,tetrabutyl ammonium chloride dosage and material ratio on product yield were investigated.The results showed that under nitrogen protection,chlorobenzene as solvent,reaction temperature 130℃,n(phenol)∶n(NaOH)∶n(phosphonitrilic chloride trimer)∶n(tetrabutyl ammonium chloride)=7.5∶7.5∶1∶0.1,reflux reaction was conducted for 6.0 h,and the yield was 90.0%and the purity reached 99.0%after separation and purification.
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