喹啉臭氧化合成烟酸
黄成坤
Subtype硕士
Thesis Advisor吾满江·艾力
2007-06-20
Degree Grantor中国科学院研究生院
Place of Conferral北京
Degree Discipline有机化学
Keyword烟酸 臭氧化 喹啉酸 喹啉
Abstract

烟酸是一种重要的精细化工产品,已广泛应用于医药、食品、饲料和精细化工等领域。近年来随着我国医药化工行业和饲料行业的迅速发展,市场对烟酸的需求量日益增长,原有产量己不能满足市场需求。限于国内相应生产技术的落后和环境保护压力的增大,开发一种新的、对环境友好的、生产成本低的烟酸合成方法已十分迫切。烟酸的合成方法有气相氧化法、液相氧化法、电解氧化法等。这些方法主要采用价格昂贵的3-甲基吡啶为原料。鉴于此,本文以价格低廉的喹啉为原料臭氧化合成烟酸。本文在常压和低温下,在冰乙酸、乙酸乙酯和水的混合溶剂中臭氧化喹啉得到喹啉酸,然后升华脱羧制备烟酸。通过实验考察了温度、浓硫酸和溶剂对烟酸产率的影响,实验最佳反应条件为:n(浓硫酸) : n(喹啉)=1.1~1.5 : 1; V(冰乙酸):V(乙酸乙酯) = 3 :1。该条件下烟酸产率可达65%以上,HPLC测得相对质量分数在95%以上。

Other Abstract
Nicotinic acid is an important fine Chemical product which is widely used in medicine, food, animal feed and Fine Chemical . With the rapid development of pharmaceutical and chemical industry, the demand for nicotinic acid increases quickly. But the existed methods haven't satisfied the market needs. Defined by the backward technology of our country and the increasing pressure on environmental protection, it is urgent to develop new, environment compatible synthesis ways with low capital investment. The synthesis methods of nicotinic acid such as vapor-phase oxidation,liquid-phase oxidation and electro-chemical oxidation were described. Usually, costly 3-methlypyridine was used as material in these methods. So we prepared nicotinic acid by ozonolysis of quinoline. In this paper, nicotinic acid was prepared by subliming quinolinic acid which got from ozonolysis of quinoline in the solvent contained glacial acetic acid, acetic ether and water under a mild reaction condition. In our work, the influences of concentrated sulfuric acid and solvents to the yield of nicotinic acid were investigated. The optimum technological material molar ratio of n (concentrated sulfuric acid): n (quinoline) =1.1~1.5:1; V(glacial acetic acid):V(acetic ether) = 3:1. Under the above conditions the yield of nicotinic acid is up to 65%, and the relative mass fraction is not less than 95% detected by HPLC.
Document Type学位论文
Identifierhttp://ir.xjipc.cas.cn/handle/365002/3493
Collection新疆维吾尔自治区精细化工工程技术研究中心
Affiliation中国科学院新疆理化技术研究所
Recommended Citation
GB/T 7714
黄成坤. 喹啉臭氧化合成烟酸[D]. 北京. 中国科学院研究生院,2007.
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