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出 处:《应用化工》2009年第8期1153-1155,共3页Applied Chemical Industry
摘 要:以三硝基甲苯(耵汀)为原料,经过氧化、催化氢化、永解等步骤合成间苯三酚。并通过红外、核磁对它的结构进行了确证。考察了氧化剂以及用量、催化剂用量、溶剂、反应温度等对合成间苯三酚的影响。较佳工艺条件:HNO3-KClO3为氧化剂,氧化剂用量与TNT用量比为2:1。水-丙酮为催化氢化溶剂,催化剂用量约为反应物的8%,控制温度在60℃,反应2.5h。水解pH=3—4,反应16—20h。总收率达到60%,纯度达到98%。Using trinitrotoluene as base material, phloroglucinol was synthesized through oxidation, catalytic hydrogenation, hydrolyzing. Its structure was analysized and authenticed by IR, ^1H NMR and ^13C NMR. The effects of oxidant, dosage of oxidant and catalyst, solvent, reaction temperature on the synthesis were studied. The better technology has been obtained as follows: taking nitric acid-chlorate liquor as oxidant, ratio of dosage of it to trinitrotoluene is 2: 1. Taking water-acetone as solvent, the amount of catalyst is 8% of the material, reaction temperature is 60 ℃, reaction time is 2.5 h on the catalytic hydrogenation reaction. At hydrolytic reaction pH is 3 -4, reaction time is 16- 20 h. The yield of phloroglucinol could reach 60%. The purity of phloroglucinol is 98%.
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