本文選題：四氫噻吩　切入點(diǎn)：1　出處：《中原工學(xué)院》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：近年來(lái)天然氣市場(chǎng)快速增長(zhǎng),天然氣在工業(yè)生產(chǎn)和日常生活的應(yīng)用越來(lái)越普遍,隨著人們對(duì)燃?xì)獍踩阅芤蟮奶岣?警示劑行業(yè)也迅速發(fā)展。四氫噻吩由于其強(qiáng)的抗氧化性質(zhì)以及氣味穩(wěn)定、添加量少等一系列優(yōu)點(diǎn)得到廣泛的應(yīng)用,然而由于其生產(chǎn)成本較高,硫醇類毒性較高的警示劑在國(guó)內(nèi)仍然有較多的應(yīng)用,所以對(duì)四氫噻吩合成路線的探究將會(huì)有很重大的實(shí)際意義。本文以工廠回收的溴化氫廢液為原料制備1,4-二溴丁烷,通過(guò)對(duì)加料溫度控制、投料摩爾比(n_((1,4-丁二醇)):n_((氫溴酸)))、催化劑用量(n_((1,4-丁二醇)):n_((濃硫酸)))、反應(yīng)溫度、反應(yīng)時(shí)間的優(yōu)化,得到最佳工藝收率為88.20%,用氣相色譜測(cè)得產(chǎn)品純度為99.48%。用紅外光譜、遮光率和沸點(diǎn)確定最終合成物為1,4-二溴丁烷。本論文合成了SO_4~(2-)/ZrO_2-SiO_2固體超強(qiáng)酸并用以催化合成1,4-二溴丁烷,研究了陳化時(shí)間、硅鋯比例n(Si):n(Zr)、H_2SO_4濃度、預(yù)焙燒條件、焙燒溫度和焙燒時(shí)間對(duì)固體超強(qiáng)酸催化性能的影響。用最佳條件制備的固體超強(qiáng)酸催化合成1,4-二溴丁烷的收率為66.57%,用紅外光譜及產(chǎn)物沸點(diǎn)、遮光率等對(duì)固體超強(qiáng)酸和1,4-二溴丁烷進(jìn)行表征,用氣相色譜測(cè)1,4-二溴丁烷純度為98.95%。用前兩步合成的1,4-二溴丁烷合成四氫噻吩,探究了投料方式、催化劑類型、投料物質(zhì)的量的比、反應(yīng)溫度和時(shí)間、催化劑用量對(duì)四氫噻吩收率的影響,得到合成四氫噻吩的最佳工藝收率為73.87%。用紅外光譜及產(chǎn)物沸點(diǎn)對(duì)四氫噻吩進(jìn)行表征,用氣相色譜測(cè)得四氫噻吩烷純度為97.20%。另外,本論文對(duì)合成四氫噻吩的廢液進(jìn)行一系列處理,回收溴化氫用于合成1,4-二溴丁烷,收率為38.72%,用氣相色譜測(cè)得其純度為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.
【學(xué)位授予單位】：中原工學(xué)院
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TE624.81

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 張吉東;俞英;黃海燕;張杰;;工業(yè)副產(chǎn)物廢氫溴酸的回收與利用[J];應(yīng)用化工;2014年12期

2 李春華;;轉(zhuǎn)爐煤氣中加臭劑的應(yīng)用和經(jīng)濟(jì)分析[J];天津冶金;2012年04期

3 王小偉;章群丹;王京;田松柏;;南帕斯凝析油硫類型特征及其腐蝕性[J];石油煉制與化工;2012年03期

4 王麗;徐家怡;郭青;;無(wú)硫加臭劑性質(zhì)及應(yīng)用[J];煤氣與熱力;2011年11期

5 王衛(wèi)霞;姚日遠(yuǎn);徐忠娟;;小型煉廠酸性氣回收制硫氫化鈉工藝探討[J];遼寧化工;2011年10期

6 成新云;陳崢;;關(guān)于溴化氫回收利用的探討[J];鹽業(yè)與化工;2011年04期

7 張六一;韓彩蕓;杜東泉;張嚴(yán)嚴(yán);許思維;羅永明;;硫酸化氧化鋯固體超強(qiáng)酸[J];化學(xué)進(jìn)展;2011年05期

8 吳文莉;萬(wàn)輝;管國(guó)鋒;;低溫陳化法制備的SO_4~(2-)/SnO_2-Al_2O_3固體超強(qiáng)酸催化劑表征與評(píng)價(jià)[J];高�；瘜W(xué)工程學(xué)報(bào);2011年02期

9 趙大生;劉海燕;;四氫噻吩合成新工藝[J];黑龍江科學(xué);2010年02期

10 李嵐;;煉油廠酸性廢氣的處理及應(yīng)用[J];化工環(huán)保;2010年01期

，

本文編號(hào)：1638439