综合化学实验设计：氧桥三核铁(III)配合物的便捷制备与表征

引用本文: 楚进锋, 王艺澄, 齐继, 刘余霖, 李言, 靳兰, 何蕾, 宋宇飞. 综合化学实验设计：氧桥三核铁(III)配合物的便捷制备与表征[J]. 大学化学, 2024, 39(7): 299-306. doi: 10.3866/PKU.DXHX202310105 shu

Citation: Jinfeng Chu, Yicheng Wang, Ji Qi, Yulin Liu, Yan Li, Lan Jin, Lei He, Yufei Song. Comprehensive Chemical Experiment Design: Convenient Preparation and Characterization of an Oxygen-Bridged Trinuclear Iron(III) Complex[J]. University Chemistry, 2024, 39(7): 299-306. doi: 10.3866/PKU.DXHX202310105 shu

综合化学实验设计：氧桥三核铁(III)配合物的便捷制备与表征

楚进锋 ^1, ,
王艺澄 ^1, ,
齐继 ^1, ,
刘余霖 ^1, ,
李言 ^1, ,
靳兰 ^1, ,
何蕾 ^1, ,
宋宇飞 ^1,2,

1.
北京化工大学化学学院, 北京 100029;
2.
北京化工大学化工资源有效利用国家重点实验室, 北京 100029
基金项目:
北京化工大学国际教育学院2022年中外合作办学教育教学改革立项资助(HZBX202209,HZBX202204)，北京化工大学基于新工科\新文科建设的实验教学改革研究项目(SYJG2022011)

摘要: 目前本科化学实验教学内容在配合物制备实验方面主要涵盖了单核配合物，而对配合物家族中占有重要地位的多核配合物却很少涉及。基于此，我们依据科研成果设计了一个关于三核铁(III)配合物的综合化学实验，以期通过该实验加深学生对配合物有关知识的理解和运用。本设计以廉价易得的九水合硝酸铁与三水合乙酸钠为原料，通过水浴加热反应、冷却结晶等步骤制备了一种氧桥三核铁(III)配合物[Fe₃O(CH₃COO)₆(H₂O)₃]NO₃·4H₂O，通过配位滴定法测定了其铁元素含量，并对其进行了红外、热重、粉末X射线衍射和电子顺磁共振等表征测试。该实验制备方法简单快捷，易于操作，环保无污染。实验内容蕴含思政元素，目标配合物结构新颖，富有对称美，实验教学时亦可培养学生的审美意识，使其领略化学之美。本设计科教融合，有助于培养学生分析解决问题的能力，为本科生的综合化学实验教学提供了一个可行案例。

关键词:

English

Comprehensive Chemical Experiment Design: Convenient Preparation and Characterization of an Oxygen-Bridged Trinuclear Iron(III) Complex

Jinfeng Chu ^1, ,
Yicheng Wang ^1, ,
Ji Qi ^1, ,
Yulin Liu ^1, ,
Yan Li ^1, ,
Lan Jin ^1, ,
Lei He ^1, ,
Yufei Song ^1,2,

1.
College of Chemistry, Beijing University of Chemical Technology, Beijing 100029, China;
2.
State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China
Received Date: 25 October 2023
Revised Date: 15 November 2023
Available Online: 27 November 2023

Abstract: At present, the undergraduate chemistry experimental teaching predominantly focuses on mononuclear complexes in the field of complex preparation experiments, often overlooking the significantly important polynuclear complexes within the complex family. Addressing this gap, we have designed a comprehensive chemical experiment involving a trinuclear iron(III) complex, drawing from scientific research findings to enrich students’ comprehension and application of complex chemistry. This design involved the preparation of an oxygen-bridged trinuclear iron(III) complex, [Fe₃O(CH₃COO)₆(H₂O)₃]NO₃·4H₂O, utilizing cost-effective and readily available iron(III) nitrate nonahydrate and sodium acetate trihydrate as raw materials through water bath heating, cooling crystallization, and other steps. The iron content in the complex was determined by complexometric titration, and characterized by infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction, and electron paramagnetic resonance. The experimental is notable for its simplicity, efficiency, and eco-friendly approach. It incorporates ideological and political elements, and showcases the complex’s novel and symmetrically aesthetic structure. During experimental teaching, students can also cultivate their appreciation of the intrinsic beauty of chemistry. The integration of science and education in this design helps to foster students’ ability to analyze and solve problems, providing a feasible case for comprehensive chemistry experimental teaching for undergraduate students.

Key words:

Comprehensive chemical experiment
/ Oxygen-bridged trinuclear iron(III) complex
/ Symmetrical structure
/ Electron paramagnetic resonance

1. [1]
  Fujieda, N.; Itoh, S. Bull. Chem. Soc. Jpn. 2016, 89, 733.Fujieda, N.; Itoh, S. Bull. Chem. Soc. Jpn. 2016, 89, 733.
2. [2]
  Fujieda, N.; Umakoshi, K.; Ochi, Y.; Nishikawa, Y.; Yanagisawa, S.; Kubo, M.; Kurisu, G.; Itoh, S. Angew. Chem. Int. Ed. 2020, 59, 13385.Fujieda, N.; Umakoshi, K.; Ochi, Y.; Nishikawa, Y.; Yanagisawa, S.; Kubo, M.; Kurisu, G.; Itoh, S. Angew. Chem. Int. Ed. 2020, 59, 13385.
3. [3]
  刘旭峰, 徐博, 徐航, 李玉龙. 无机化学学报, 2023, 39(8), 1619.
4. [4]
  Wang, P.; Saber, M. R.; VanNatta, P. E.; Yap, G. P. A.; Popescu, C. V.; Scarborough, C. C.; Kieber-Emmons, M. T.; Dunbar, K. R.; Riordan, C. G. Inorg. Chem. 2021, 60, 6480.Wang, P.; Saber, M. R.; VanNatta, P. E.; Yap, G. P. A.; Popescu, C. V.; Scarborough, C. C.; Kieber-Emmons, M. T.; Dunbar, K. R.; Riordan, C. G. Inorg. Chem. 2021, 60, 6480.
5. [5]
  Plamthottam, S.; Sun, D.; Valkenburgh, J. V.; Valenzuela, J.; Ruehle, B.; Steele, D.; Poddar, S.; Marshalik, M.; Hernandez, S.; Radu, C. G.; et al. J. Biol. Inorg. Chem. 2019, 24, 621.Plamthottam, S.; Sun, D.; Valkenburgh, J. V.; Valenzuela, J.; Ruehle, B.; Steele, D.; Poddar, S.; Marshalik, M.; Hernandez, S.; Radu, C. G.; et al. J. Biol. Inorg. Chem. 2019, 24, 621.
6. [6]
  宋天佑, 徐家宁, 程功臻, 王莉. 无机化学(下册). 第4版. 北京: 高等教育出版社, 2019: 514-515.
7. [7]
  严宣申, 王长富. 普通无机化学(重排本). 第2版. 北京: 北京大学出版社, 2016: 166-168.
8. [8]
  北京师范大学, 华中师范大学, 南京师范大学. 无机化学(下册). 第5版. 北京: 高等教育出版社, 2021: 673-675.
9. [9]
  北京大学化学与分子工程学院普通化学实验教学组. 普通化学实验. 第3版. 北京: 北京大学出版社, 2012: 188-190.
10. [10]
  北京师范大学, 东北师范大学, 华中师范大学, 南京师范大学编, 赵新华主编. 无机化学实验. 第4版. 北京: 高等教育出版社, 2014: 147-150.
11. [11]
  范勇, 屈学俭, 徐家宁. 基础化学实验——无机化学实验分册. 北京: 高等教育出版社, 2015: 108-110.
12. [12]
  赵轶臻, 杨皓程, 叶雨锟, 马建功, 邱晓航. 大学化学, 2022, 37(5), 2109100.
13. [13]
  孟祥茹, 李纲. 大学化学, 2021, 36(6), 2008065.
14. [14]
  Turte, K. I.; Shova, S. G.; Spatar, F. A.; Mazus, M. D.; Malinovskii T. I. J. Struct. Chem. 1994, 35, 248.Turte, K. I.; Shova, S. G.; Spatar, F. A.; Mazus, M. D.; Malinovskii T. I. J. Struct. Chem. 1994, 35, 248.
15. [15]
  Golub, A. S.; Lenenko, N. D.; Zaikovskii, V. I.; Efimov, N. N.; Dobrokhotova, Z. V.; Baranchikov, A. E.; Kiskin, M. A.; Eremenko, I. L. Mater. Chem. Phys. 2016, 183, 457.Golub, A. S.; Lenenko, N. D.; Zaikovskii, V. I.; Efimov, N. N.; Dobrokhotova, Z. V.; Baranchikov, A. E.; Kiskin, M. A.; Eremenko, I. L. Mater. Chem. Phys. 2016, 183, 457.
16. [16]
  田文玉. 多酸基离子晶体的构筑及其锂电性能的研究[硕士学位论文]. 北京: 北京化工大学, 2022.
17. [17]
  Deacon, G. B.; Phillips, R. J. Coord. Chem. Rev. 1980, 33, 227.Deacon, G. B.; Phillips, R. J. Coord. Chem. Rev. 1980, 33, 227.
18. [18]
  Sanders-Loehr, J.; Wheeler, W. D.; Shiemke, A. K.; Averill, B. A.; Loehr, T. M. J. Am. Chem. Soc. 1989, 111, 8084.Sanders-Loehr, J.; Wheeler, W. D.; Shiemke, A. K.; Averill, B. A.; Loehr, T. M. J. Am. Chem. Soc. 1989, 111, 8084.
19. [19]
  Johnson, M. K.; Powell, D. B.; Cannon, R. D. Spectrochim. Acta A 1981, 37, 995.Johnson, M. K.; Powell, D. B.; Cannon, R. D. Spectrochim. Acta A 1981, 37, 995.
20. [20]
  Montri, L.; Cannon, R. D. Spectrochim. Acta A 1985, 41, 643.Montri, L.; Cannon, R. D. Spectrochim. Acta A 1985, 41, 643.
21. [21]
  裘祖文. 电子自旋共振波谱. 第1版. 北京: 科学出版社, 1980: 302-307.
22. [22]
  姚尚锋, 李健民. 光谱实验室, 2002, 19(2), 153.

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 104
HTML全文浏览量: 11

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

综合化学实验设计：氧桥三核铁(III)配合物的便捷制备与表征

English

Comprehensive Chemical Experiment Design: Convenient Preparation and Characterization of an Oxygen-Bridged Trinuclear Iron(III) Complex

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

综合化学实验设计：氧桥三核铁(III)配合物的便捷制备与表征

English

Comprehensive Chemical Experiment Design: Convenient Preparation and Characterization of an Oxygen-Bridged Trinuclear Iron(III) Complex

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs