化工专业综合性实验“分离乙醇水溶液”的探究

化工专业综合性实验对于培养学生的创新精神和工程实践能力至关重要。以分离乙醇水溶液为例,将气液相平衡测定实验和萃取精馏过程模拟相结合形成综合性实验,涉及到了三元体系的气液相平衡测定方法、实验数据采用不同热力学模型的回归及评价、萃取精馏过程模拟、各因素对分离效果的影响评价等。加深了学生对理论知识的理解,使学生对萃取精馏工业应用有了一定的认识,提高了学生的实验操作水平和工程实践能力,为应用型人才的培养提供了有力保障。     

异丙醇-水分离技术研究新进展

介绍了萃取精馏法、吸附蒸馏法和膜分离法等用于异丙醇-水分离的新进展,并对这几种方法进行了简单评述,具体分析了各种方法的优缺点,展望了异丙醇-水分离新工艺的前景,认为以乙二醇为萃取剂的萃取精馏技术具有推广价值.     

氯仿萃取分离N,N-二甲基甲酰胺工艺

针对某制药企业生产过程中产生的高浓度含N,N-二甲基甲酰胺(DMF)料液，在折流板萃取塔内进行连续萃取分离，结合精馏工艺，实现了DMF的分离与回收。对于DMF初始质量分数为38.46%的料液，以氯仿作为萃取剂，采用脉冲折流板萃取塔对料液中的DMF进行萃取，研究了不同油水相比、流量和脉冲条件下在折流板萃取塔中DMF的萃取效果。结果表明，DMF的萃取效率随着脉冲的加入、油水相比的升高和两相流速的增大而增大，在优化的条件下DMF的萃取率最高为99.94%，分离后的萃余相DMF质量分数达到0.5%以下。进一步，对于负载了DMF的氯仿溶液，分别进行了间歇精馏实验和模拟计算，结果显示通过精馏可以实现氯仿和DMF的有效分离回收。     

捕集高湿烟气中CO2的变压吸附技术

变压吸附法在捕集烟气中的CO₂这一领域中显示出强大的优越性,但实际电厂烟气含有少量的水蒸气,这对利用常规吸附剂捕集CO₂造成很大挑战。为解决上述瓶颈问题,改进变压吸附工艺以及开发对湿度不敏感、高效的吸附剂成为最主要的途径。本文详细介绍了两种常用的变压吸附工艺,即多层变压吸附及微波辅助真空再生法分离高湿烟气的研究进展,综述了近年来研发的适于捕集高湿烟气的高效吸附剂,系统阐述了各种吸附剂的物理化学特性及其吸附CO₂、H₂O的机制,并在此基础上讨论了变压吸附技术捕集高湿烟气时存在的问题,提出了研究展望。相信随着人们对变压吸附工艺的改进以及对新型高效吸附剂的进一步研发,必将显著降低捕集高湿烟气中CO₂的成本,这将对燃煤电厂等高湿CO₂排放源的温室气体减排具有重要意义。     

基于Aspen Plus的煤层气精馏分离案例教学探讨

为帮助学生掌握“煤矿区煤层气利用技术”基本理论,结合煤层气低温精馏分离科研成果案例,运用Aspen Plus流程模拟软件对煤层气气液相平衡和低温精馏过程进行模拟和案例教学,根据煤层气精馏分离工艺要求,进行精馏塔操作变量计算和灵敏度分析,分析操作变量变化对精馏过程的影响,让学生直观了解塔内各参数的变化,掌握精馏分离操作,加深了对煤层气分离理论的理解,极大地提高了教学效率和质量,提升了学生的综合素质。     

用Excel 2000求解双组分精馏过程的设计型与操作型问题

以精馏过程的设计型与操作型问题为例,介绍Excel 2000的求解过程。计算过程及结果表明,利用Excel 2000解决精馏过程的设计型与操作型问题,不需编程,运算过程简单,结果可靠,具有易学、高效、快速、实用等特点。     

用人工神经网络预测催化精馏塔开工过程的研究

催化精馏是使化学反应过程和精馏分离过程结合在一起,是伴有化学反应的新型特殊精馏过程.“反应精馏”概念自20年代提出以来,从30年代到60年代初,研究都是对特定体系的工艺探索;70年代后,研究扩展到非均相催化反应体系,出现了非均相催化精馏过程,成为了反应精馏的一个重要分支;     

地方高校化工专业“四位一体”实践教学模式的探索

针对当前地方高校化工类专业实践教学中存在的问题,结合地方高校实际,提出了集校内课堂实验、校内仿真实训、校内基地实训与校外基地实践为一体的化工专业实践教学模式,具有"内外结合、虚实结合、循序渐进"等特色。经探索和实践,该模式可走出一条具有地方高校特色的实践教学路径,可形成工科专业实践教学的示范模式,对于提升地方高校的竞争力具有积极意义。     

用Matlab求解化工原理计算问题的教学初探

以管路计算中的设计型问题和精馏过程计算中的操作型问题为例,分析了求解问题的思路,列出了详尽的Matlab计算源程序。计算过程及结果表明,利用Matlab求解化工原理计算问题具有数值稳定性好、使用方便、高效、快速等特点。     

柠檬酸丁酯酯化精馏实验设计及教学探索

通过引入柠檬酸丁酯酯化精馏实验,将高分子材料制备、催化剂制备、材料表征与正交实验引入到课堂。通过本实验可以：(1)熟悉和了解高分子聚合实验,拓宽知识面,将地方产业特色融入到课堂中;(2)了解催化剂的制备方法,同时对高分子材料和催化剂进行表征,掌握仪器分析在催化剂制备中的应用,增强综合实验能力;(3)利用正交实验探索酯化精馏实验最佳的实验条件;(4)以柠檬酸丁酯酯化反应替代乙酸乙酯酯化反应,实现实验内容的更新。本实验将化学工程实验与地方产业需求和研究生阶段的科研能力培养进行有效衔接。通过本实验学生可以将书本知识应用到实际中,增加获得感,提高创新能力与综合素质。     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.     

Synthesis of N-substituted carbazolones from α-iodo enaminones via Pd(0)-catalyzed intramolecular coupling under microwave irradiation

A variety of N-aryl and N-alkyl carbazolones were conveniently achieved in good to high yields via Pd₂(dba)₃-mediated intramolecular coupling of N-substituted α-iodo enaminones under microwave irradiation. The Pd(0)-catalyzed cyclization was found to proceed favorably with the more electron-deficient phenyl ring during the reactions involving unsymmetrical N,N-diaryl α-iodo enaminones. This unique property enables the construction of carbazolone skeleton containing nitro substituted benzenoid ring.     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of substituted 2,4,5,6-tetrahydrocyclopenta[c]pyrazoles and 2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazoles by intramolecular nitrilimine cycloaddition

Both substituted 2,4,5,6-tetrahydrocyclopenta[c]pyrazoles and 2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazoles have been synthesized by the 3+2 intramolecular dipolar cycloaddition of nitrilimines to alkynes. This cyclization has been extended to more versatile 3-bromo derivatives by the use of alkynylbromides as dipolarophiles.