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先由双酚A与甲醛反应得到甲阶酚醛树脂,产物再与正丁醇反应制得丁基醚化酚醛树脂,最后再与DOPO反应得到含磷酚醛树脂。通过对产物羟甲基含量,醚化率测定及红外光谱,示差扫描量热和热重分析研究了各步反应因素对合成的影响,结果表明,含磷酚醛树脂的最佳合成工艺为:第1步反应酚、醛物质的量比为4.8∶1,NaOH与双酚A的质量比为2.19∶1,反应温度75℃,反应时间1 h;第2步pH值为4,丁醇与双酚A物质的量比为6∶1,反应时间4 h。当磷质量分数为9%时,含磷酚醛树脂的玻璃化转变温度为176℃,初始分解温度为354℃以上,具有较好的热稳定性,可作为1种优异的阻燃材料。
First, the reaction of bisphenol A with formaldehyde to obtain resol phenolic resin, the product then react with n-butanol butyl etherified phenolic resin, and finally with the DOPO reaction to obtain a phosphorus-containing phenolic resin. The effects of various reaction factors on the synthesis were studied by measuring the content of methylol, the etherification rate and the infrared spectra, differential scanning calorimetry and thermogravimetric analysis. The results showed that the optimum synthesis process of the phosphorus-containing phenolic resin was as follows: The mass ratio of phenol to aldehyde was 4.8:1 in 1-step reaction, the mass ratio of NaOH to bisphenol A was 2.19:1, the reaction temperature was 75 ℃ and the reaction time was 1 h. The second step was pH 4, Phenol A material ratio of 6: 1, the reaction time 4 h. When the mass fraction of phosphorus is 9%, the glass transition temperature of the phosphorus-containing phenolic resin is 176 ℃, the initial decomposition temperature is above 354 ℃, which has good thermal stability and can be used as an excellent flame retardant material.