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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
Language: English
Authors: Lindsay Weller, Krista H. Brown (ORCID 0009-0004-8288-5718), Anthony L. Fernandez (ORCID 0000-0002-2553-2949), Jason Cooke (ORCID 0000-0002-1847-5966)
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
FullText Text:
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  Data: 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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  Data: <searchLink fieldCode="AR" term="%22Lindsay+Weller%22">Lindsay Weller</searchLink><br /><searchLink fieldCode="AR" term="%22Krista+H%2E+Brown%22">Krista H. Brown</searchLink> (ORCID <externalLink term="https://orcid.org/0009-0004-8288-5718">0009-0004-8288-5718</externalLink>)<br /><searchLink fieldCode="AR" term="%22Anthony+L%2E+Fernandez%22">Anthony L. Fernandez</searchLink> (ORCID <externalLink term="https://orcid.org/0000-0002-2553-2949">0000-0002-2553-2949</externalLink>)<br /><searchLink fieldCode="AR" term="%22Jason+Cooke%22">Jason Cooke</searchLink> (ORCID <externalLink term="https://orcid.org/0000-0002-1847-5966">0000-0002-1847-5966</externalLink>)
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  Data: <searchLink fieldCode="SO" term="%22Journal+of+Chemical+Education%22"><i>Journal of Chemical Education</i></searchLink>. 2026 103(3):1662-1667.
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  Data: 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
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  Data: 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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      – TitleFull: 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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