四苯基联苯二酚双磷酸酯的合成研究

用三氯氧磷、4,4’-二羟基联苯、苯酚为原料合成阻燃剂四苯基对联苯二酚双磷酸酯（DBBDP）,采用单因素实验法分别对物质的量之比、反应时间、反应温度进行讨论,确定了最佳的反应条件：三氯氧磷、4,4’-二羟基联苯和苯酚的物质的量之比为6︰1︰4.1;第1步反应温度为105～120℃,反应时间为4 h;第2步反应温度为120～150℃,反应时间为5 h;无水三氯化铝为催化剂,用量为4,4’-二羟基联苯的2%,产品收率为82.1%。产品经红外光谱和元素分析确定其结构和组成,通过热重分析表明产品的耐热性能良好。

Study on Synthesis of Condensed Phosphates Biphenyl bis(diphenyl phosphate)

The synthetic method of oligomeric biphenyl bis（diphenyl phosphate） from 4,4’-Dihydroxy-biphenyl,phosphorus oxychloride and phenol was studied.The effects of reactants molecular ratio,reaction temperature and reaction time on reaction yield were studied.The results show that optimum reaction conditions are as follows：phosphorus oxychloride︰4,4’-Dihydroxy-biphenyl︰phenol=6︰l︰4.1（molar ratio）,reaction temperature is 105~120 ℃ and reaction time is 4 h at the condensation stage.At the end capping stage,reaction temperature is 120~150 ℃,and reaction time is 5 h,AlCl3 is the best catalyst,and its dosage is 2% of 4,4’-dihydroxy-biphenyl amount.Under the optimum reaction conditions,yield of the product can be up to 82.1%.Chemical structure of the product was confirmed by IR and elemental analysis.TG test shows that it has high resistance to heat.