化学教育原油降凝剂合成及性能测定的综合化学实验

根据基础课与专业结合的培养要求,设计了丙烯酸酯三元共聚物的合成、表征及降凝性能测定的综合研究型实验。该实验包括合成条件的考察、产品红外光谱的表征、原油降凝效果的测定、偏光显微镜的观察、流变性质的测定等实验内容。实验通过"合成-表征-性能-机理"4步,使学生对降凝剂的研发有了整体认识,引导学生由理论知识的学习到解决实际问题乃至科学研究步步递进深入。教学实践表明,该实验能够充分调动学生的兴趣和积极性,并培养学生综合运用知识和实践创新的能力。     

淀粉基高吸水树脂微波合成及其性能的综合实验教学设计*

为了达成工程认证教育的培养要求,设计了“淀粉基高吸水树脂微波合成及其性能”综合实验。实验包括淀粉基高吸水树脂的微波辅助合成、结构表征及产品性能测定等内容;要求学生查阅文献,了解各种制备工艺并设计实验方案,掌握衰减全反射傅里叶红外光谱与X射线衍射等表征技术及树脂溶胀性能测定技术,分析实验数据。另外,设计了融合过程考核与结果考核的考核体系,通过实验设计、实验操作与数据分析等环节全面考核学生的综合实验能力。该实验教学方案不仅提高教学质量,还激发学生实验兴趣,培养其创新思维与应用实践能力。     

新型表面活性剂的合成与表征综合实验设计

将专业综合实验与科研成果相结合,设计了新型表面活性剂的合成与表征综合化学实验。实验涉及含羟基基团的表面活性剂的合成、纯化、结构表征和性能测定等操作。该综合实验将有机化学基础知识、表面活性剂的基本性质与前沿科学研究相结合,从而实现学生实验技能的提升、认知视野的拓展和综合能力培养的目标。     

“聚丙烯酸酯的合成及降凝性能评价”综合实验能力考核平台

设计了以柴油中饱和烃含量及碳数分布测定、聚丙烯酸高级醇酯（PTA）的合成与纯化、PTA的红外表征与分子量测定、PTA降凝性能评价等4个模块组成的综合实验，作为化工专业实验的考核及成绩评定平台。这种考核方式将过程考核与结果考核融合，将笔试、操作、设计融合，可以全面准确地考核学生的有机合成、仪器分析等基础实验技能，同时考核综述、数据处理、实验设计等综合实验能力和实验室工作素质。此外，还能够有效训练学生的学习能力、解决问题能力、实践能力和创新能力，并促进了实验教学水平提高。     

综合化学实验:三苯胺衍生物的合成、结构与电致变色性能的研究

介绍了一个综合化学实验。通过乌尔曼缩合反应合成一种具有电致变色性能的三苯胺衍生物。利用红外光谱、核磁共振氢谱、循环伏安法对化合物的结构及电化学性能进行表征。通过将电化学工作站和紫外-可见分光光度计联机进行光谱电化学测试,深入研究该化合物的电致变色性能。本实验充分体现了“合成-表征-分析”的科研思维模式,并打破了传统的单独仪器测试方式,在让学生了解合成化学知识和前沿学术研究的同时,提高学生的基本实验技能和综合运用学科知识的能力。     

大学化学综合实验:Fe/Fe3O4磁性材料的合成、结构性质与磁性能的测定*

推荐一个大学化学综合实验: Fe/Fe3O4磁性材料的合成、结构性质与磁性能的测定,该实验涉及材料的合成、结构表征和磁性能的测定。通过该实验可以使学生掌握一些大型仪器的基本原理和基本操作,掌握材料合成的方法、材料结构及形貌的表征手段以及磁滞曲线的测定方法。使学生在掌握材料研究的基础理论和基本实验技能的同时,培养学生独力实验能力和创新意识,尤其是培养他们综合运用知识的能力。进一步缩短教学与科研的距离。     

pH敏感性丙烯酸-苯乙烯-丙烯酸异辛酯共聚物水凝胶的制备及性能研究综合实验

采用乳液聚合的方法,合成了丙烯酸-苯乙烯-丙烯酸异辛酯共聚物水凝胶,通过红外光谱对水凝胶进行了表征,考察了pH对水凝胶溶胀率的影响,并以该凝胶制备了硫脲缓释体系。结果表明,该凝胶在碱性条件下的溶胀度远大于在中性和酸性条件下的溶胀度,具有pH敏感性,且缓释性能好。将该实验研究过程设计为高职学生的综合实验项目并进行了实践探索,结果表明其在提升学生专业综合能力、开阔专业视野及培养创造性与科学思维等方面效果显著。     

聚苯胺-木质素磺酸复合物的合成及其染料吸附性能——介绍一个综合性研究型实验

以苯胺为单体,木质素磺酸为分散剂,采用化学氧化聚合法合成成本低廉、吸附性能优异的聚苯胺-木质素磺酸(PAL)复合物。要求学生掌握复合物的合成操作步骤、复合物的表征及其染料吸附性能测试的方法。通过对比实验结果,为研究型实验教学提供思路。该实验利于加深学生对高分子学科知识的理解与运用,培养他们的综合实验能力。     

镉配位聚合物的合成及其染料吸附性能研究综合实验*

介绍了一个研究型综合实验,涉及镉配位聚合物的合成及其染料吸附性能研究。该实验使用常见有机配体丁二酸、1,4-二(1-咪唑)苯与硝酸镉四水合物,在溶剂热条件下进行反应得到一例镉配位聚合物。利用X射线单晶衍射、X射线粉末衍射、热重分析、红外光谱对配位聚合物进行结构表征,并对其染料吸附性能进行研究。该实验将科学研究热点融入基础实验教学,既巩固了学生的基础理论知识,提高了实验技能,又拓展了学生的科学视野,加强了他们独立分析问题、解决问题的能力,有利于培养学生的创新精神和实践能力。     

醋酸锰催化合成萘并噻唑衍生物研究型综合实验

设计了“醋酸锰（Ⅲ）催化合成2-邻氯苯甲酰氨基萘并[1，2-d]噻唑”研究型综合化学实验，以自制的醋酸锰（Ⅲ）为催化剂，催化氧化1-萘基-3-邻氯苯甲酰基硫脲合成2-邻氯苯甲酰氨基萘并[1，2-d]噻唑。通过该实验项目的教学，可使学生掌握醋酸锰（Ⅲ）、1-萘基-3-邻氯苯甲酰基硫脲和2-邻氯苯甲酰氨基萘并[1，2-d]噻唑的合成方法，掌握有机化合物结构表征的方法，可以培养学生的实践动手能力、科研创新能力以及综合运用知识的能力。该实验项目集无机合成实验、有机合成实验和仪器分析实验于一体，具有较强的可操作性和实用性，可作为基础化学研究型综合化学实验或开放性实验开设。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Microwave-assisted copper-catalyzed stereoselective ring expansion of three-membered heterocycles with α-diazo-β-dicarbonyl compounds

Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular S_N2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

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%).