饮品级邻氨基苯甲酰胺制备工艺的研究

Research on the Preparation Process of Beverage Grade Ortho Aminobenzamide

摘要

邻氨基苯甲酰胺是目前唯一被批准用作饮品级PET材料中残留AA清除剂的物质。论文以饮品级邻氨基苯甲酰胺的工业生产工艺为研究对象，选择靛红酸酐作为主要反应原料，筛选了加料顺序、氨源种类及其用量、反应温度、反应溶剂种类、混合溶剂配比及其用量，以及母液的套用次数等条件，以邻氨基苯甲酰胺的纯度、收率及亨特白度等为质量技术指标。最终探索出了最佳工艺条件，即质量浓度为26%~28%的工业氨水作为氨源、采用先加靛红酸酐后加氨源的加料顺序，以水与二氯甲烷等体积混合物作为反应溶剂，最佳反应温度为20℃，最大溶剂套用次数为3次，此时，邻氨基苯甲酰胺的收率高于85%，纯度不低于99.9%，亨特白度80，完全满足饮品级邻氨基苯甲酰胺的质量要求。

Abstract

Ortho aminobenzamide is currently the only substance approved for use as a residual AA scavenger in beverage grade PET materials. The paper takes the industrial production process of beverage grade ortho aminobenzamide as the research object, selects indigo carmine anhydride as the main reaction raw material, screens the feeding sequence, ammonia source type and dosage, reaction temperature, reaction solvent type, mixed solvent ratio and dosage, as well as the number of times the mother liquor is used. Quality and technical indicators such as purity, yield, and Hunter whiteness of ortho aminobenzamide are used. The optimal process conditions were ultimately explored, which involved using industrial ammonia water with a mass concentration of 26% to 28% as the ammonia source, followed by the addition of indigo carmine first and then the ammonia source, and using a mixture of water and dichloromethane as the reaction solvent. The optimal reaction temperature was 20 ℃, and the maximum number of solvent applications was 3 times. At this time, the yield of ortho aminobenzamide was higher than 85%, the purity was not less than 99.9%, and the Hunter whiteness was 80, fully meeting the quality requirements of beverage grade ortho aminobenzamide.

关键词

邻氨基苯甲酰胺 / 饮品包材 / 除臭剂 / 靛红酸酐 / 工艺条件

Key words

o-aminobenzamide / PET packaging materials / deodorants / indigo anhydride / process condition

参考文献

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基金资助

滁州学院校级科研启动基金(2020qd07)

滁州市指导计划项目(2021ZD026)

滁州市科技成果转化奖补项目(2022KJ27)