摘要
以三氯氧磷、间苯二酚及苯酚为原料,合成阻燃剂间苯二酚双(二苯基磷酸酯)(RDP);考察了催化剂种类及用量、原料配比、反应温度和时间对合成反应的影响,确定了最佳的工艺条件:n(三氯氧磷)∶n(间苯二酚)∶n(苯酚)=4.5∶1.0∶3.7,催化剂无水氯化镁用量约为间苯二酚质量的2.5%,第一步反应温度85～90℃,反应5h;第二步反应温度120℃,反应8h。在此条件下,合成的RDP质量分数约为74.52%,收率为91.20%。采用FTIR、HPLC和TG-DSC对产物进行了表征和分析,产品质量达到国外同类产品水平。
Flame retardant resorcinol-bis-diphenyphosphate（RDP）was synthesized with phosphous oxychloride,resorcinol and phenol as raw materials.Effects of process parameters,such as catalyst type and dosage,raw materials ratio,reaction temperature and time,on the quality and yield of RDP were studied respectively,The optimum synthesis conditions were defined as follows：mole radio of phosphorus oxychloride and resorcinol and phenol was 4.5∶1.0∶3.7,magnesium chloride was used as catalyst,mass fraction of catalyst（based on resorcinol）was 2.5%,In the first step of the reaction,reaction time was 5 h at 85~90 ℃.In the second step of the reaction,reaction time was 8 h at 120~125 ℃.Under these suitable conditions,the content of RDP can be up 74.52%,the yield be 91.20%.The structure of product was defined by means of FTIR and HPLC.The thermal decomposition temperature of product was high by TG-DSC.The quality of the product can reach the indexes of the oversea product.
出处
《化工科技》
CAS
2011年第5期24-28,共5页
Science & Technology in Chemical Industry
基金
吉林石化公司科学研究与技术开发项目(D200806-101)
