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Study On The Synthesis Of Sodium 5-nitroguaiacol

Posted on:2009-08-27Degree:MasterType:Thesis
Country:ChinaCandidate:M J ChengFull Text:PDF
GTID:2191360302977001Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
5-nitroguaiacol sodium is a new type of plant growth regulators, which can accelerate plant growth to different levels. It applies to cotton, linen, grains, fruits, medicinal herbs, flowers, etc., to increase about 30 percent, with its highly efficient, low toxicity, good market prospects, has been a hot of research. Based on the basic theory of reaction, a route was fixed for the synthesis of 5-nitroguaiacol sodium: guaiacol was used as raw material, was synthesized by means of acylation, nitrification, hydrolysis. Then, in accordance with the reaction sequence, the every step of the reaction was studied in detial, and the intermediate products were fully analysed, which gave a reference to the future research.Firstly, the most important factors of influence on the acylation reaction were investigated by pre-experiment. Then, the better process conditions of synthesizing guaiacol acetate was optimized out by orthogonal design method and single- factor-experiment method. After the separation process was optimized, the yield markedly improved. In this better condition, the product yield is up to 98%, the product purity is over 98%.The product was approved with IR analytical method, and the gas chromatography method was developed for the analysis of guaiacol acetate. With this gas chromatography method the product was qualitative and quantitative analysised.Secondly, the nitric acid and glacial acetic acid were taken as the nitrifying reagents and the influences of different factors on nitration reaction were mainly discussed by single- factor- experiment method, after which the optimal reaction conditions were obtained. In the optimal reaction condition, the product yield is up to 78% and the product purity is up to 99%.The product was adequately analysed by the melting point, the heat analytical method and IR analytical method and the liquid chromatogram analysis method.Thirdly, by the single-factor-experiment method, we studied the most important factors of influence on the hydrolysis reaction, and obtained the optimal reaction conditions. In this better condition, the product yield is up to 83%, the product purity is up to 99%.The product was approved with melting point analysis, the heat analytical method, IR analytical method, and the liquid chromatogram analysis method, and the quantitative analysis for the product with UV method.Finally, the whole process is tested by three parallel experiments, in which the product yield is over 60% and purity is over 97%, confirmed the high reproducibility and feasibility of the process.
Keywords/Search Tags:guaiacol, 5-nitroguaiacol sodium, acylation, nitrification, hydrolysis
PDF Full Text Request
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