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2-巯基氧化吡啶钠盐的合成及抑菌性能研究

The Synthesis of 2-Mercapto-Oxide-Pyridine Sodium Salt and Research of Antibacterial Properties

【作者】 赵瑛琛

【导师】 杨蕾;

【作者基本信息】 哈尔滨工业大学 , 高分子化学与物理, 2007, 硕士

【摘要】 2-巯基氧化吡啶钠盐(2-mercapto-oxide-pyridine sodium salt, NaPT)是一种有良好应用前景的新型杀菌剂。本文对2-巯基氧化吡啶钠盐的制备及抑菌性能开展了研究。以2-氨基吡啶为起始原料,经乙酰化、氧化、水解、重氮化、氯化、巯基化和成盐,合成出2-巯基氧化吡啶钠盐,并对关键步骤乙酰化、氧化、水解及巯基化的反应工艺进行了研究。乙酰化反应以冰乙酸为溶剂,不仅解决了乙酰化反应过热的问题,还减少了杂质的引入。氧化反应以顺丁烯二酸酐为催化剂,反应温度在75℃、反应时间3.5h时收率为82.5%;水解反应中温度在80℃、时间2h时收率为87%。巯基化反应中pH值控制在9,收率为85.2%。总反应收率约为61%。使用2-巯基吡啶钠盐,在不同浓度条件下对室内常见细菌(大肠杆菌、白色葡萄球菌、枯草杆菌)和真菌(曲霉、毛霉、根霉)的抑菌性能进行了评价。实验结果表明,所有菌种在CNaPT≥10-3(mass%)时生长全部被抑制,无菌苔生长;杀菌剂在低浓度下对供试菌种即有很好的抑菌效果,在10-4、10-5(mass%)出现明显的抑菌环。采用紫外分光光度计测定杀菌剂的最低抑菌浓度MIC,杀菌剂对各菌种的MIC在5~15mg/L之间,大肠杆菌MIC为11mg/L;枯草杆菌MIC为9mg/L;白色葡萄球菌MIC为15mg/L。曲霉MIC为9mg/L;毛霉MIC为5mg/L;根霉MIC为7mg/L。实验结果表明此种杀菌剂不仅对常见菌(如大肠杆菌)的抑菌性能优秀,而且对抗药性很强枯草杆菌亦有良好的抑制效果。其广谱、高效的杀菌能力决定了2-巯基氧化吡啶钠盐作为杀菌剂在医药卫生、农药抗害、涂料抗菌剂和室内消毒等方面具有广泛的应用。

【Abstract】 2-mercapto-oxide-pyridine sodium salt is a new kind of bactericide which has very good prospect. In this study. 2-mercapto-sodium-oxide pyridine is researched for preparation and antibacterial properties , which provided a product for medicine, paint and indoor bactericide.2-mercapto-oxide-pyridine sodium salt was synthesized by the processes of acetyl, oxidation, hydrolysis, diazotization, chlorination, sulphydryl and salification with the starting material 2-aminopyridine, and the synthetic craft was researched. The yield of oxidation was 82.5%, and the optimal temperature and reaction time of oxidation were 75℃and 3.5h respectively; the yield of hydrolysis was 87%, and the optimal temperature and reaction time of hydrolysis were 80℃and 2h respectively. When pH of solution in Sulfhydryl was 9, the yield is 85.2%. The total yield was 61% under above optimal conditions.Six kinds of indoor common bacteria——bacterial (Escherichia coli, Bacillus subtilis, White staphylococcus) and fungi (Aspergillus, Mucor, Rhizopus) was used to do qualitative tests for the antibacterial effect on 2-mercapto-oxide-pyridine sodium salt. All bacteria was inhibited at CNaPT≥1×10-3(mass%); there were significant inhibition of centrals at 10-4、10-5(mass%), which showed good antibacterial effect at low concentration. Then UV spectrophoto-meter was used to measure the minimum inhibitory concentration (MIC), and the whole MIC of six kinds of indoor common bacteria were 11mg/L, 9mg/L, 15mg/L, 9mg/L, 5mg/L, 7mg/L respectively.Experimental results showed that such compound had good antibacterial properties against common bacteria. And it has better inhibitory effect on fungi than bacteria generally. The performance broad-spectrum, highly antibacterial efficient of NaPT will lead to the extensive application in medicine and health care, anti-pesticide, paint antibacterial agent and indoor bactericide.

  • 【分类号】TQ455.47
  • 【被引频次】1
  • 【下载频次】200
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