摘要
对铁基复合氧化物催化苯酚羟基化合成苯二酚反应和产物分离过程生成的酚焦油进行了表征,结果表明,催化剂上所含酚焦油结构与羟基化反应过程生成焦油类似,热失重峰在320℃左右,含有C=O结构物质,形成原因在于羟化液中苯二酚的过度氧化和酚类物质的缩合.用丙酮对蒸馏所得酚焦油进行了抽提,其中溶于丙酮部分呈结晶状,抽余部分不含结晶状物质.蒸馏所得酚焦油中的条状结晶物C∶O原子比为6∶3,背底焦油中C∶O原子比为6∶1.43,废催化剂上沉积的酚焦油,C∶O原子比为6∶4,蒸馏所得酚焦油中氧含量较少,且背底部焦油不溶于热水和丙酮,说明脱水和精馏过程存在进一步的生焦反应。
The characters of phenolic tars in the process for preparing diphenols by the phenol hydroxylation using iron-based composite oxides as catalysts were studied.As a result,phenolic tars deposited in waste catalyst are similar to the ones originated in the hydroxylation in structure,which show peak of weight loss in 320℃ and C=O bond adquired by TG/DrTG and IR analyses,respectively.Accordingly,it was presumed that phenolic tars could be produced by the further oxidation of diphenols and shrink or dehydration of phenolic compounds in the phenol hydroxylation.And then the henolic tars of distillation residue were extracted using acetone as solvent.The crystals in the phenolic tars were soluble by acetone (C/O atomic ratio:6/3) and the remains were not soluble and not crystallizable (C/O atomic ratio:6/1.43).In comparison,the C/O atomic ratio of the phenolic tars deposited waste catalyst was 6/4.Finally,it has been assured that phenolic tars could be formed in the process of evaporation of distillation because of the decrease of oxygen in the phenolic tars of distillation residue.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2005年第3期317-320,共4页
Chemical Research and Application
基金
中国石化股份有限公司燕山分公司资助项目
