摘要
以邻苯基苯酚和三氯化磷通过傅-克反应、水解反应,合成9,10-二氢-9-氧杂-10-磷酰杂菲(DOPO),用衣康酸(ITA)与DOPO加成反应制备阻燃单体9,10-二氢-9-氧杂-10-磷酰杂菲-丁二酸(DDP)。通过红外光谱、核磁共振及质谱对合成产物进行了结构表征。并进行了中试生产,产品质量指标与实验室合成产物一致,表明配比和工艺路线完全可行。
9,10- dihydro- 10- phosphaphenanthrene- 10 -oxide （DOPO） was prepared though Friedel- Crafts reaction and hydrolyzed reaction with the main reactants of o - phenyl phenol and PC13. The flame - retardant monomer 9,10 - dihydro - 10 [2,3-di （hydroxycarbonyl） propyl] 10 -phosphaphenanthrene- 10- oxide （DDP） was synthesized by the addition reaction with itaconie acid （ITA） and DOPO. The structure of DDP was characterized by element analysis, FT - IR, mass spectroscopy （MS） and nuclear magnetic resonance spectroscopy （NMR）. And the pilot production of DDP with high quality has been finished. The monomer quality was very close to the lab product, which indicates that the proportion and the process route was feasible.
出处
《山东化工》
CAS
2017年第13期1-2,5,共3页
Shandong Chemical Industry
基金
山东省自然科学基金项目(ZR2012EML09)
关键词
阻燃剂
9
10-二氢-9-氧杂-10-磷酰杂菲-丁二酸(DDP)
衣康酸(ITA)
制备
表征
flame retardant
9,10 - dihydro - 10 [ 2,3 - di （hydroxycarbonyl） propyl ] 10 - phosphaphenanthrene - 10 - oxide （DDP）
itaconic acid（ITA）
preparation
characterization
