توسعه و بهینه‌سازی سنتز MIL-101(Cr) به روش فراصوت با استفاده از روش سطح پاسخ

نوع مقاله : مقاله علمی پژوهشی

نویسندگان

گروه شیمی، دانشگاه پیام نور،تهران، ایران.

چکیده

چارچوب MIL-101(Cr) یکی از موردمطالعه‌ترین چارچوب‌های آلی-فلزی با پایه کروم است. این چارچوب از یون کروم و لیگاند ترفتالیک‌اسید تشکیل‌شده‌است. در این مطالعه، به‌منظور توسعه روش‌های کارآمد سنتز جایگزین، از روش فراصوت سنتز استفاده‌شد. بهینه‌سازی بازده این چارچوب آلی-فلزی بامطالعه دو پارامتر اساسی، یعنی دما و زمان، با استفاده از روش سطح پاسخ انجام‌شد. تأثیر این پارامترها از طریق طراحی مرکب مرکزی (CCD) ، بهینه‌شده و رفتار آن‌ها با استفاده از آنالیز واریانس مورد تجزیه ‌و تحلیل قرار‌گرفت. یک معادله درجه دوم برای پیش‌بینی رفتار فرآیند در شرایط مختلف با R2 برابر با 9998/0 ارائه‌شده‌است. که نشان‌دهنده همپوشانی مناسب داده‌های تجربی و مقادیر پیش‌بینی‌شده توسط مدل ارائه‌شده، برای میزان بهینه بازده است. پارامترهای حاصل از آنالیز واریانس، نشان‌می‌دهند که زمان اثر معنی‌دارتر و نقش مؤثرتری در مدل ایفا‌می‌کند. ساختار نانوترکیب تهیه‌شده‌، با استفاده از تکنیک‌های طیف‌سنجی پراش پرتوی ایکس، طیف‌سنج مادون‌قرمز تبدیل فوریه، آنالیز توزین حرارتی، میکروسکوپ الکترونی روبشی و اندازه‌گیری سطح ویژه مواد و تخلخل‌سنجی جذب و واجذب نیتروژن به روش BET شناسایی‌شد. این ماده یک سطح ویژه بسیار بالا (m2.g-1 2143)، حجم حفره بزرگ (cm3.g-1 8/0)، پایداری حرارتی/شیمیایی/آب خوب دارد. همچنین نتایج حاصل از سنتز با استفاده از حمام فراصوت، نشان‌داد که ذرات دارای حفره‌های ریز متخلخل، قفس‌های مزوپور و شکل هشت‌وجهی یکنواخت با اندازه متوسط 125 تا 260 نانومتر هستند. میزان مصرف انرژی تابش فراصوت، بسیار کمتر از روش‌های هیدروترمال و سولوترمال است. بنابراین می‌توان گفت که فن‌آوری فراصوت، سبزتر، سریع‌تر و کارآمدتر از روش‌های گرمایش الکتریکی مرسوم است.

کلیدواژه‌ها

موضوعات

عنوان مقاله [English]

Development and Optimization Synthesis of MIL-101(Cr) by Ultrasound Irradiation Using Response Surface Methodology

نویسندگان [English]

  • Ahmad Nikseresht
  • Hojatolah Normohamadi
Department of Chemistry; Payame Noor University (PNU); P.OBox; 19395-4697 Tehran; Iran
چکیده [English]

MIL-101(Cr) stands as one of the extensively researched chromium-based metal–organic frameworks, comprised of chromium metal ions and terephthalic acid ligands. This study introduces an innovative approach to MIL-101(Cr) synthesis by employing ultrasound (UTS) irradiation. Our primary objective revolved around optimizing key operational parameters, namely time and temperature, using the central composite design method. Subsequently, we conducted an in-depth analysis using variance analysis to understand their respective impacts. To predict process behaviour, we developed quadratic equations under varying conditions, achieving a remarkable R2 value of 0.9998 to relate parameters and synthesis yield. Results revealed a more pronounced influence of time variation compared to temperature on the synthesis process. Moreover, we subjected the synthesized MIL-101(Cr) to rigorous characterization using FT-IR, XRD, SEM, TGA, and N2 physisorption techniques. Our findings showcased the synthesized MIL-101(Cr) possessing exceptional characteristics, including an ultra-high specific surface area (2143 m2. g-1), substantial pore size (0.8 cm3.g-1), and excellent thermal, chemical, and water stability. Further examination indicated the presence of microporous windows, mesoporous cages, and uniform octahedral particles ranging in size between 125-260 nm.
Notably, our study emphasized the energy efficiency of UTS irradiation over conventional electric (CE) heating, highlighting its potential as a quicker, more efficient, and environmentally friendly alternative to conventional synthesis methods.

کلیدواژه‌ها [English]

  • Mil-101(Cr)
  • Ultrasonic irradiation
  • Response surface methodology
  • Metal-organic framework
  • Terephthalic acid
  • Analysis of variance

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شیمى کاربردى روز
دوره 19، شماره 71
تیر 1403
صفحه 223-246

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