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磺甲基化热塑性酚醛树脂合成与分子结构表征
SYNTHESIS AND MOLECULAR STRUCTURE CHARACTERIZATION OF SULFOMETHYLATED THERMOPLASTIC PHENOLIC RESIN
【摘要】 将苯酚与甲醛在酸性条件下聚合得到热塑性酚醛树脂(TPPR),再在碱性条件下进行磺甲基化处理,制备了磺甲基化热塑性酚醛树脂(STPPR)。考察了磺甲基化条件对产物收率和聚沉值的影响。采用FT-IR和液相色谱-质谱联用对STPPR的分子结构进行了表征,推测了其分子结构。结果表明,磺甲基化较佳反应条件为:反应温度90℃,反应时间60~90 min,pH值10;磺甲基化试剂用量越大,STPPR的耐盐性越好;STPPR是一种聚合度为2~10,M_z为200~1 200的混合物,酚环之间通过亚甲基以对-对位或邻-对位的方式连接;其中一部分TPPR分子未完成磺甲基化过程,已磺化的TPPR分子上只含有一个磺甲基基团。
【Abstract】 Thermoplastic phenolic resin(TPPR) was prepared by polymerization of phenol and formaldehyde under acidic conditions. Then, Sulfomethylated thermoplastic phenolic resin(STPPR) was prepared by sulfomethylation of TPPR under alkaline conditions.The effects of sulfomethylation conditions on the product yield and coagulation value were investigated.The molecular structure of STPPR was characterized by FTIR and liquid chromatography-mass spectrometry.The results showed that the optimum reaction conditions of sulfonated methylation were as follows:reaction temperature 90℃,the reaction time of 60-90 min,pH 10;The higher the dosage of sulfomethylation reagent,the better the salt tolerance of STPPR;STPPR was a mixture with a polymerization degree of 2-10 and an Mz of200-1 200.The phenolic rings were connected by methylene groups in a para-para or ortho-para manner.Some of the TPPR molecules did not complete the sulfomethylation process,and the sulfonated TPPR molecule only contained one sulfomethyl group.
【Key words】 thermoplastic phenolic resin; sulfomethylation; FTIR; liquid chromatography-mass spectrometry; molecular structure;
- 【文献出处】 精细石油化工 ,Speciality Petrochemicals , 编辑部邮箱 ,2019年06期
- 【分类号】TQ323.1
- 【下载频次】261