Building a Greener Dye Trap: How Replacing N,N-Dimethylformamide with γ-Valerolactone Improves the Ultrasonic-Assisted Synthesis of the Copper-Based Metal-Organic Framework HKUST-1
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| Title: | Building a Greener Dye Trap: How Replacing N,N-Dimethylformamide with γ-Valerolactone Improves the Ultrasonic-Assisted Synthesis of the Copper-Based Metal-Organic Framework HKUST-1 |
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| Language: | English |
| Authors: | Lindsay Weller, Krista H. Brown (ORCID |
| Source: | Journal of Chemical Education. 2026 103(3):1662-1667. |
| Availability: | Division of Chemical Education, Inc. and ACS Publications Division of the American Chemical Society. 1155 Sixteenth Street NW, Washington, DC 20036. Tel: 800-227-5558; Tel: 202-872-4600; e-mail: eic@jce.acs.org; Web site: http://pubs.acs.org/jchemeduc |
| Peer Reviewed: | Y |
| Page Count: | 6 |
| Publication Date: | 2026 |
| Document Type: | Journal Articles Reports - Descriptive |
| Education Level: | Higher Education Postsecondary Education |
| Descriptors: | Inorganic Chemistry, Science Instruction, Laboratory Experiments, College Science |
| DOI: | 10.1021/acs.jchemed.5c00908 |
| ISSN: | 0021-9584 1938-1328 |
| Abstract: | Employing γ-valerolactone (GVL) as a cosolvent in the ultrasonic-assisted synthesis of the metal-organic framework (MOF) [Cu₃(BTC)₂·xH₂O][subscript n] where [BTC]³⁻ = 1,3,5-benzenetricarboxylate = 1,3,5-[C[subscript 6]H₃(CO₂)₃]³⁻ (HKUST-1) enables a "greener" approach than the current published experiment which uses hazardous N,N-dimethylformamide (DMF). Equally important, the revision of the oven-drying step to 200 °C for at least 15 h instead of 1 h at 130 °C removes sequestered solvent from the MOF pores and markedly improves the adsorption characteristics of the final material. A further small gain in adsorption capacity is realized by the inclusion of a second, short ultrasonic treatment during workup as a so-called "swelling step" to maximize the MOF's pore size and thus its effective surface area. The overall student experience is enhanced by incorporating a nontoxic cosolvent derived from biomass and by augmenting the established test of HKUST-1 activity, namely removal of methylene blue from aqueous solution, with an operationally simple determination of water vapor adsorption capacity. A new perspective is suggested to help students understand the complex extended HKUST-1 structure by having them first appreciate the molecular structure of copper(II) acetate hydrate, which is best formulated as Cu₂(O₂CCH₃)[subscript 4]·2H₂O. The revised experiment is flexible and accommodates a variety of laboratory schedules, student skill levels, and pedagogic objectives. |
| Abstractor: | As Provided |
| Entry Date: | 2026 |
| Accession Number: | EJ1499684 |
| Database: | ERIC |
| Abstract: | Employing γ-valerolactone (GVL) as a cosolvent in the ultrasonic-assisted synthesis of the metal-organic framework (MOF) [Cu₃(BTC)₂·xH₂O][subscript n] where [BTC]³⁻ = 1,3,5-benzenetricarboxylate = 1,3,5-[C[subscript 6]H₃(CO₂)₃]³⁻ (HKUST-1) enables a "greener" approach than the current published experiment which uses hazardous N,N-dimethylformamide (DMF). Equally important, the revision of the oven-drying step to 200 °C for at least 15 h instead of 1 h at 130 °C removes sequestered solvent from the MOF pores and markedly improves the adsorption characteristics of the final material. A further small gain in adsorption capacity is realized by the inclusion of a second, short ultrasonic treatment during workup as a so-called "swelling step" to maximize the MOF's pore size and thus its effective surface area. The overall student experience is enhanced by incorporating a nontoxic cosolvent derived from biomass and by augmenting the established test of HKUST-1 activity, namely removal of methylene blue from aqueous solution, with an operationally simple determination of water vapor adsorption capacity. A new perspective is suggested to help students understand the complex extended HKUST-1 structure by having them first appreciate the molecular structure of copper(II) acetate hydrate, which is best formulated as Cu₂(O₂CCH₃)[subscript 4]·2H₂O. The revised experiment is flexible and accommodates a variety of laboratory schedules, student skill levels, and pedagogic objectives. |
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| ISSN: | 0021-9584 1938-1328 |
| DOI: | 10.1021/acs.jchemed.5c00908 |
