合成气制乙二醇的工艺设计和模拟的研究

1、A thesis(dissertation) submitted to Zhengzhou Universityfor the degree of MasterStudy on Process Design and Simulation of Preparation of Ethylene Glycol by SyngasByLi11x.iang YaoSupe1-visor: Prof. Huaijun SongProf. Baozeng Ren Chemical TechnologySchool of Chen1ical Engineering and Energy May,2013帮帮胃 学位论文原创性声明本人郑重声明：所呈交的学位论文，是本人在导师的指导下，独立进行研 究所取得的成果。除文中已经注明引用的内容外，本论文不包含任何其他个人 或集体已经发表或撰写过的科研成果。对本文的研究作出重要贡献的个人和集 体，均已在文中以明确方式标明。本声明的法律责任由本人承担。学位论文作者：七伤袜才干日期：初 3 年 月 5 尸学位论文使用授权声明本人在导师指导下完成的论文及相关的职务作品，

2、知识产权归属郑州大学。根据郑州大学有关保留、使用学位论文的规定，同意学校保留或向国家有关部 门或机构送交论文的复印件和电子版，允许论文被查阅和借阅；本人授权郑州 大学可以将本学位论文的全部或部分编入有关数据库进行检索，可以采用影印、缩印或者其他复制手段保存论文和汇编本学位论文。本人离校后发表、使用学 位论文或与该学位论文直接相关的学术论文或成果时，第一署名单位仍然为郑 州大学。保密论文在解密后应遵守此规定。学位论文作者：挑十未奸日期：为(3 年 月 3/ 日摘要摘要随着石油资源的日益枯竭，以石油为原料生产化工产品的成本越来越高。 鉴于我国相对富煤的能源格局，以煤替代石油为原料生产化工产品成为国内近些年来的发展趋势，其中合成气制乙二醇项目是研究热点之一。目前研究的最具工业化前景的合成气制乙二醇路线为：首先由合成气中分 离出的 co 与亚硝酸甲酷反应合成草酸二甲酷， 然后将草酸二甲酷催化加氢制得乙二醇。本文基千流程模拟系统 Aspen Plus 对上述合成气制乙二醇工艺流程进行了设计与模拟研究。以 Aspen Plus 对合成气制乙二醇工艺中涉及到的亚硝酸甲酷和草酸二甲酷进行了物性估算。对

3、亚硝酸甲酷再生反应精馆塔进行了设计与模拟，优化结果 为：伍的转化率达到 99.99 以上， 反应精熘塔中生成的产物亚硝酸甲酕在塔顶的回收率达到 99.99%。对草酸二甲酷的合成及其相关的分离过程进行了设计与模拟，结果表明用于亚硝酸甲酕再生的循环气物流在流程中可以收敛，通过精馈可以获得摩尔分率为 99.9 的草酸二甲酕。对甲醇和副产物碳酸二甲酷的混合液的分离过程进行了设计与模拟，采用常压加压精馈工艺可以实现二者的分离， 分离所得碳酸二甲酷与甲醇的质量分数均可达 99.9%。对草酸二甲酷加氢制备乙二醇及相关分离过程进行了设计与模拟。在反应器之后设计了三个精馈塔分别用千甲醇的回收、轻组分的脱除以及乙醇酸甲酷和草酸二甲酷的回收。对上述三个精馈塔进行了模拟优化，结果为：甲醇回收塔塔顶甲醇的回收率达到 99.6 %； 脱轻组分塔塔顶 乙醇酸甲 酷的脱除率达 99.9以上， 草酸二甲酣的脱除率为 99.7 %； 乙醇酸甲酕和草酸二甲酷回 收塔塔顶二者的回收率分别达99.7 和99.8 %。在脱轻组分塔的塔底得到含有 1,2- 丙二醇、1,2丁二醇和二甘醇等杂质的粗乙二醇产品， 其流量为 3498.7

4、kg/h， 其中乙二醇的质量分数为98.2 %。关键词：合成气，乙二醇，亚硝酸甲酪，碳酸二甲酷，草酸二甲酷，过程模拟，Aspen PlusAbsractAbstractWith the increasing depletion of oil resources, the cost of production of chemical products with oil as raw material is increasingly high. Given tl 记 relatively rich coal energy st11.1cture in our count1-y, taking coal to replace oil as raw material to produce chemical products has become a hot reasearch in recent years. An1ong the research hots the program of syngas preparation of ethylene glycol is a research p

5、roject with development prospects.At present 出 e most industrialized prospect process route of ethylene glycol preparation by syngas is as follows: first CO separated from syngas reacts with methyl nitrite to synthesize dimethyl oxalate,印 d then ethylene glycol is prepared by catalytic hydrogenation of dimethyl oxalate. In this paper, the desi驴 郘 d sii1mlation of preparation process of ethylene glycol tlnough syngas mentioned above was studied based on process simulation system Aspen Plus.First

6、the physical property of methyl nitrite and dimethyl oxalate involved in the process of syngas prep出ation of ethylene glycol were estimated by Aspen Plus in tliis paper. The regeneration reactive distillation column of methyl nitJ.-ite was designed and simulated, the optimized results are as follows: the 02 conversion rate is higher than 99.99%, the recove1-y rate of metl1yl ni订ite generated in the reactive distillation column in the overhead reaches 99.99%. The syntl1esis of dimethyl oxalate an

7、d the related separation process were designed and simulated, results show that the recycle gas flow for regeneration of methyl nitrite can be converged, by distillation the mole fraction of dimethyl oxalate can reach 99.9%.The separation process of metl1anol and byproduct dimetl1yl carbonate was designed and simulated, results show that the two materialsseparation could be achieved by atmospheric pressure - pressurized distillation process, and the mass fraction of separated dimethyl carbonate

8、a.11d methanol can be up to 99.9%.The process of dimethyl oxalate hydrogenation for ethylene glycol and the related separation process were designed and simulated. After the reactor, threeIIIdistillation columns were designed for recovery of methanol, removal of the light components 叩 d recovery of methyl glycolate and dimethyl oxalate. The tluee columns were simulated and optimized, the results are as follows: the recovery rate of methanol reaches 99.6% in the methanol recovery column overhead,

9、 the removal rate of methyl glycolate and dimethyl oxalate were sep 釭 ately 99.6% and 99.7% in the overhead of off light components column, the recovery of methyl glycolate 皿 d dimetl1yl oxalate were separately 99.7% and 99.8% in the corresponding recovery column overhead. Crude ethylene glycol product which contains little impurity such as 1,2-propylene glycol, 1,2-butylene glycol, diethylene glycol, and so on, is obtained in the bottom of the light component removal column. The flow rate of the crude ethylene glycol product is 3498.7 kg/h,in which the mass fraction of ethyleneglycol is 98.2%.Key words: Syngas; Ethylene glycol; Methyl nitrite; Dimethyl carbonate; Dimethyl oxalate; Process simulation; Aspen Plus目 录目录摘要

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