四氢噻吩的合成工艺研究

发布时间：2018-03-20 09:15

本文选题：四氢噻吩　切入点：1　出处：《中原工学院》2017年硕士论文　论文类型：学位论文

【摘要】：近年来天然气市场快速增长,天然气在工业生产和日常生活的应用越来越普遍,随着人们对燃气安全性能要求的提高,警示剂行业也迅速发展。四氢噻吩由于其强的抗氧化性质以及气味稳定、添加量少等一系列优点得到广泛的应用,然而由于其生产成本较高,硫醇类毒性较高的警示剂在国内仍然有较多的应用,所以对四氢噻吩合成路线的探究将会有很重大的实际意义。本文以工厂回收的溴化氢废液为原料制备1,4-二溴丁烷,通过对加料温度控制、投料摩尔比(n_((1,4-丁二醇)):n_((氢溴酸)))、催化剂用量(n_((1,4-丁二醇)):n_((浓硫酸)))、反应温度、反应时间的优化,得到最佳工艺收率为88.20%,用气相色谱测得产品纯度为99.48%。用红外光谱、遮光率和沸点确定最终合成物为1,4-二溴丁烷。本论文合成了SO_4~(2-)/ZrO_2-SiO_2固体超强酸并用以催化合成1,4-二溴丁烷,研究了陈化时间、硅锆比例n(Si):n(Zr)、H_2SO_4浓度、预焙烧条件、焙烧温度和焙烧时间对固体超强酸催化性能的影响。用最佳条件制备的固体超强酸催化合成1,4-二溴丁烷的收率为66.57%,用红外光谱及产物沸点、遮光率等对固体超强酸和1,4-二溴丁烷进行表征,用气相色谱测1,4-二溴丁烷纯度为98.95%。用前两步合成的1,4-二溴丁烷合成四氢噻吩,探究了投料方式、催化剂类型、投料物质的量的比、反应温度和时间、催化剂用量对四氢噻吩收率的影响,得到合成四氢噻吩的最佳工艺收率为73.87%。用红外光谱及产物沸点对四氢噻吩进行表征,用气相色谱测得四氢噻吩烷纯度为97.20%。另外,本论文对合成四氢噻吩的废液进行一系列处理,回收溴化氢用于合成1,4-二溴丁烷,收率为38.72%,用气相色谱测得其纯度为98.92%。
[Abstract]:With the rapid growth of natural gas market in recent years, the application of natural gas in industrial production and daily life is becoming more and more common. The industry of warning agents has also developed rapidly. Tetrahydrothiophene has been widely used because of its strong antioxidant properties, stable smell, low addition and so on. However, because of its high production cost, tetrahydrothiophene has been widely used. The warning agent with high toxicity of mercaptan is still used in China, so it will be of great practical significance to explore the synthetic route of tetrahydrothiophene. In this paper, the waste liquid of hydrogen bromide recovered from the factory is used as the raw material to prepare 1h4- dibromobutane. By controlling the feeding temperature, the molar ratio of the feed to the feed is 1 / 4 / 1 / 1 / N / N / N / N / N / T / N / T, and the quantity of catalyst / catalyst is 1 / 4 / 1 / 1 / N / N / T, and the reaction temperature, reaction time and reaction time are optimized for the optimization of the reaction temperature and reaction time. The optimum yield was 88.20, and the purity of the product was 99.48 determined by gas chromatography. The final synthesis was determined by infrared spectroscopy, shading rate and boiling point. In this paper, SO_4~(2-)/ZrO_2-SiO_2 solid superacid was synthesized and used to catalyze the synthesis of 1o 4-dibromobutane. The aging time, the ratio of silicon and zirconium to the ratio of Si to Zirconium, the concentration of S _ 2SO _ 4, and the pre-calcination conditions were studied. The effect of calcination temperature and calcination time on the catalytic performance of solid superacid. The yield of 1,4-dibromobutane prepared under the optimum conditions was 66.57, and the boiling point of the product was obtained. The solid superacid and 1h4- dibromobutane were characterized by shading rate, and the purity of 1h4- dibromobutane was 98.95 by gas chromatography. Tetrahydrothiophene was synthesized from 1o 4- dibromobutane which was synthesized in the first two steps. The feeding method and catalyst type were investigated. The optimum yield of tetrahydrothiophene was 73.87.The optimum yield was 73.87.The tetrahydrothiophene was characterized by infrared spectroscopy and boiling point of the product, and the effect of reaction temperature and time on the yield of tetrahydrothiophene was obtained. The purity of tetrahydrothiophene was 97.20.The purity of tetrahydrothiophene was determined by gas chromatography. In addition, the waste liquid of tetrahydrothiophene was treated by a series of treatments, and hydrogen bromide was recovered for the synthesis of 1H 4- dibromobutane in 38.72% yield, and the purity was 98.92% by gas chromatography.
【学位授予单位】：中原工学院
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TE624.81

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