Research Article
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Kalsiyum floroborat sentezi, kinetik ve alev geciktirici özelliklerinin belirlenmesi

Year 2021, Volume: 6 Issue: 3, 326 - 331, 30.09.2021
https://doi.org/10.30728/boron.880116

Abstract

Bu çalışmada özel bor bileşiklerinden olan kalsiyum floroboratın sentez parametreleri belirlenmiş ve pamuklu kumaştaki alev geciktirici özelliği incelenmiştir. Ayrıca kinetik çalışmalar yapılarak reaksiyon mertebesi ve aktivasyon enerjisi hesaplanmıştır. Kalsiyum floroborat, reaktant olarak kalsiyum oksit ve floroborik asit kullanılarak yaş yöntemle sentezlenmiştir. İncelenen parametreler; reaktant mol oranı (nCaO/nHBF4), sıcaklık ve reaksiyon süresidir. Karakterizasyon çalışmaları için FT-IR, XRD ve BF4- iyon seçici elektrot kullanılmıştır. Termal davranışın karakterize edilmesinde termogravimetrik-diferansiyel termal analiz (TG-DTA) kullanılmıştır. Kalsiyum floroborat, 1:4 reaktant mol oranı, 90˚C sıcaklık ve 100 dakika reaksiyon süresinde %97 verimle sentezlenmiştir. Ayrıca yapılan kinetik çalışmada reaksiyonun birinci mertebeden olduğu belirlenmiş ve reaksiyonun aktivasyon enerjisi 19,14 kJ/mol olarak bulunmuştur. Sentezlenen kalsiyum floroboratın alev geciktirici özelliğini tespit etmek için LOI testinden yararlanılmıştır. Testler sonucunda kalsiyum floroboratın çok iyi alev geciktirici özellik gösterdiği gözlemlenmiştir.

Supporting Institution

Ulusal Bor Araştırma Enstitüsü (BOREN)

Project Number

2017-30-06-30-002.

References

  • Türk Mühendisler Mimarlar Odaları Birliği, Bor Raporu, , Ankara, 2016.
  • Booth, H. S.; Martin, D. R. Boron Trifluoride And Its Derivatives, Wiley, Newyork, The United States of America, 1949.
  • Yünlü, K, Bor ve Bileşikleri Sentez Yöntemleri, Yapı Özellikleri ve Uygulama Alanları, Boren, Ankara, 2016.
  • Achilonu M. C., Umesiobi D. O., The formation of carbon–carbon and carbon–heteroatom bonds using silver tetrafluoroborate as a promoter. Arab. J. Chem., 9(2), 1984-2003. 2010.
  • Aydın Y. D., Gürü M., İpek D., Özyürek D., Obtainment of copper(II) fluoroborate by high-energy impacted ball-milling, Acta Phys. Pol. A, 135, 888-891, 2019.
  • Aydın Y. D., Gürü M., Ipek D., Özyürek D., Synthesis and characterization of zinc fluoroborate from zinc flüoride and boron by mechanochemical reaction, Arab. J. Sci. Eng., 42, 4409-4416, 2017.
  • Krishnapuram P., Jakka S. K., Thummala C., Lalapeta R. M., Photoluminescence characteristics of Eu2O3 doped calcium fluoroborate glasses, J. Mol. Struct., 1028, 170-175, 2012.
  • Kumar J. S., Pavani, K., Babu A. M., Giri N. K., Rai S.B., Moorthy L. R., Fluorescence characteristics of Dy3+ ions in calcium fluoroborate glasses, J. Lumin., 130 (10), 1916-1923, 2010.
  • Kumar J. S., Babu A. M., Sasikala T., Moorthy L. R., NIR fluorescence and visible upconversion studies of Nd3+ ions in calcium fluoroborate glasses, Chem. Phys. Lett., 484(4–6), 207-213, 2010.
  • Prabakar S. J. R., Sohn K.S., Pyo M., Enhancement in high-rate performance of graphite anodes via ınterface modification utilizing Ca(BF4)2 as an electrolyte additive in lithium ion batteries, J. Electrochem. Soc., 166, A591, 2019.
  • Forero-Saboya J. D., Lozinšek M., Ponrouch A., Towards dry and contaminant free Ca(BF4)2-based electrolytes for Ca plating, Journal of Power Sources Advances, 6, 100032, 2020.
  • Sarkar A., Santra S., Kundu S. K., Ghosal N. C., Hajra A., Majee A., Zinc tetrafluoroborate: a versatile and robust catalyst for various organic reactions and transformations. Synthesis, 47,1379-1386, 2015.
  • Pujala B., Rana S., Chakraborti A. K., Zinc tetrafluoroborate hydrate as a mild catalyst For epoxide ring opening with amines: scope and limitations of metal tetrafluoroborates and applications in the synthesis of antihypertensive drugs (RS)/(R)/(S)-metoprolols", J. Org. Chem., 76(21), 8768-8780, 2011.
  • Ranu B. C., Jana U., Majee A., A simple and efficient method for selective deprotection of t-butyldimethylsilyl ethers by zinc tetrafluoroborate in water, Tetrahedron Lett. 40(10), 1985-1988, 1999.
  • Zhang S. S., Xu K., Jow T. R., Study of LiBF4 as an electrolyte salt for a li-ion battery. J Electrochem Soc., 149(5), A586–A590, 2002.
  • Tressaud, A., Functionalized Inorganic Fluorides: Synthesis, Characterization and properties of nanostructured solids, John Wiley & Sons, France, 2010.
  • Chester J. and Van, T, Comprehensive Materials Processing, Elsevier, USA, 2014.
  • Menz W., Mohr J., Paul, O. Microsystem Technology, Wiley, Weinheim, 2001.
  • Wilkie C. A., Morgan A. B., Fire retardancy of polymeric materials. 2nd ed., CRC-Press, Boca Raton, USA, 2009.
  • Aydın D. Y ., Çinko floroborat sentezi ve alev geciktirici olarak kullanılabilirliği , Yüksek Lisans Tezi, Gazi Üniversitesi, Fen Bilimleri Enstitüsü, Ankara, 2015.
  • Aydın Y. D., Patlar K., Gürü M., Akkurt F., Synthesis of antimony fluoroborate and usability as flame retardant, 8th ınternational advanced technologies symposium (IATS’17) Elazığ, Türkiye, 19-22 Ekim, 2017.
  • Aydın Y. D., Kurt H., Kandemir E. B., Gürü M., Synthesis of lead fluoroborate and usability as flame retardant, 8th ınternational advanced technologies symposium (IATS’17) Elazığ, Türkiye, 19-22 Ekim, 2017.
  • Aydın Y. D., Biberoğlu R., Kümbetlioğlu F., Gürü M., Kobalt floroborat sentezi ve alev geciktirici olarak kullanılabilirliği, 1st International Eurasion Conference on Science, Engineering and Technology Ankara, Türkiye, 22-23 Kasım, 2018.
  • A. Abdullah Ceyhan, Safiye Bağcı, Orhan Baytar, Ömer Şahin, Amonyum floroborat üretimi ve üretim parametrelerinin belirlenmesi, Bor Dergisi, 5(2), 63-72, 2020.
  • Aydın D. Y., Gürü M., Ayar B., Çakanyıldırım Ç., Bor bileşiklerinin alev geciktirici ve yüksek sıcaklığa dayanıklı pigment olarak uygulanabilirliği, Bor Dergisi, 1(1), 33-39, 2016.
  • Lu S. Y., Hamerton I., Recent developments in the chemistry of halogen-free flame retardant polymers. Prog. Polym. Sci., 27(8), 1661-1712, 2002.
  • Dogan M., Unlu M., Flame retardant effect of boron compounds on red phosphorus containing epoxy resins. Polym Degrad Stab., 99, 12-17, 2014.
  • Wang X, Song Y., Bao J., Synergistic effects of ZrO 2 or B 2 O 3 on flame-retarded poly (butyl methacrylate) with tricresylphosphate, Fire Mater., 34(7), 357-366, 2010.
  • Ayar B., Gürü M., Çakanyıldırım Ç., Solid phase synthesis of anhydrous zinc borate from zinc and boron oxide and utilization as a flame retardant in dye and textile. GU. J. Sci., 27(3), 987-991, 2014.
  • Bourbigot S., Bras M. L., Leeuwendal R., Shenc K. K., Schubertc D., Recent advances in the use of zinc borates in flame retardancy of EVA. Polym. Degrad. Stabil, 64(3), 419-425, 1999.
  • Leoni P., Sommovigo M., Pasqualli M., Midollini S., Braga D., Sabatino P., Coordinated water/anion hydrogen bonds and Pd-H bond acidity in cationic palladium(II) aquo hydrides and the x-ray crystal and molecular structures of trans- [(Cy3P)2Pd(H)(H2O)]BF4 (Cy = cyclohexyl). Organometallics, 10(4), 1038–1044, 1991.
  • Bozacı E., Borlu bileşiklerin çevre dostu yöntemlerle poliakrilnitril kumaşlarau uygulanması Ebru Bozacı* Bor Dergisi, 3(1), 17-23, 2018.
  • Friedrich K., Breuer U., Multifunctionality of polymer composites: challenges and new solutions. 1st ed., Elsevier, USA, 2015.

Calcium fluoroborate synthesis, determination of kinetics and flame retardant properties

Year 2021, Volume: 6 Issue: 3, 326 - 331, 30.09.2021
https://doi.org/10.30728/boron.880116

Abstract

In this study, the synthesis parameters of calcium fluoroborate, one of the special boron compounds, were determined and its flame retardant properties in cotton fabric were investigated. In addition, kinetic studies were carried out to calculate the reaction order and activation energy. Calcium fluoroborate was synthesized by wet method using calcium oxide and fluoroboric acid as reactants. The parameters examined; reactant mole ratio (nCaO/nHBF4), temperature and reaction time. FT-IR, XRD and BF4-ion selective electrodes were used for characterization studies. Thermogravimetric-differential thermal analysis (TG-DTA) was used to characterize the thermal behavior. Calcium fluoroborate was synthesized with 97% yield when molar ratio of reactants, temperature and reaction time are set as 1:4, 90°C and 100 minutes, respectively. In addition, kinetic experiments reveal that the reaction order obeys to first order kinetics and the activation energy was found as 19.14 kJ/mol. LOI tests were used to determine the flame retardant properties of synthesized calcium fluoroborate. Tests proved that the calcium fluoroborate has very good flame retardant properties.

Project Number

2017-30-06-30-002.

References

  • Türk Mühendisler Mimarlar Odaları Birliği, Bor Raporu, , Ankara, 2016.
  • Booth, H. S.; Martin, D. R. Boron Trifluoride And Its Derivatives, Wiley, Newyork, The United States of America, 1949.
  • Yünlü, K, Bor ve Bileşikleri Sentez Yöntemleri, Yapı Özellikleri ve Uygulama Alanları, Boren, Ankara, 2016.
  • Achilonu M. C., Umesiobi D. O., The formation of carbon–carbon and carbon–heteroatom bonds using silver tetrafluoroborate as a promoter. Arab. J. Chem., 9(2), 1984-2003. 2010.
  • Aydın Y. D., Gürü M., İpek D., Özyürek D., Obtainment of copper(II) fluoroborate by high-energy impacted ball-milling, Acta Phys. Pol. A, 135, 888-891, 2019.
  • Aydın Y. D., Gürü M., Ipek D., Özyürek D., Synthesis and characterization of zinc fluoroborate from zinc flüoride and boron by mechanochemical reaction, Arab. J. Sci. Eng., 42, 4409-4416, 2017.
  • Krishnapuram P., Jakka S. K., Thummala C., Lalapeta R. M., Photoluminescence characteristics of Eu2O3 doped calcium fluoroborate glasses, J. Mol. Struct., 1028, 170-175, 2012.
  • Kumar J. S., Pavani, K., Babu A. M., Giri N. K., Rai S.B., Moorthy L. R., Fluorescence characteristics of Dy3+ ions in calcium fluoroborate glasses, J. Lumin., 130 (10), 1916-1923, 2010.
  • Kumar J. S., Babu A. M., Sasikala T., Moorthy L. R., NIR fluorescence and visible upconversion studies of Nd3+ ions in calcium fluoroborate glasses, Chem. Phys. Lett., 484(4–6), 207-213, 2010.
  • Prabakar S. J. R., Sohn K.S., Pyo M., Enhancement in high-rate performance of graphite anodes via ınterface modification utilizing Ca(BF4)2 as an electrolyte additive in lithium ion batteries, J. Electrochem. Soc., 166, A591, 2019.
  • Forero-Saboya J. D., Lozinšek M., Ponrouch A., Towards dry and contaminant free Ca(BF4)2-based electrolytes for Ca plating, Journal of Power Sources Advances, 6, 100032, 2020.
  • Sarkar A., Santra S., Kundu S. K., Ghosal N. C., Hajra A., Majee A., Zinc tetrafluoroborate: a versatile and robust catalyst for various organic reactions and transformations. Synthesis, 47,1379-1386, 2015.
  • Pujala B., Rana S., Chakraborti A. K., Zinc tetrafluoroborate hydrate as a mild catalyst For epoxide ring opening with amines: scope and limitations of metal tetrafluoroborates and applications in the synthesis of antihypertensive drugs (RS)/(R)/(S)-metoprolols", J. Org. Chem., 76(21), 8768-8780, 2011.
  • Ranu B. C., Jana U., Majee A., A simple and efficient method for selective deprotection of t-butyldimethylsilyl ethers by zinc tetrafluoroborate in water, Tetrahedron Lett. 40(10), 1985-1988, 1999.
  • Zhang S. S., Xu K., Jow T. R., Study of LiBF4 as an electrolyte salt for a li-ion battery. J Electrochem Soc., 149(5), A586–A590, 2002.
  • Tressaud, A., Functionalized Inorganic Fluorides: Synthesis, Characterization and properties of nanostructured solids, John Wiley & Sons, France, 2010.
  • Chester J. and Van, T, Comprehensive Materials Processing, Elsevier, USA, 2014.
  • Menz W., Mohr J., Paul, O. Microsystem Technology, Wiley, Weinheim, 2001.
  • Wilkie C. A., Morgan A. B., Fire retardancy of polymeric materials. 2nd ed., CRC-Press, Boca Raton, USA, 2009.
  • Aydın D. Y ., Çinko floroborat sentezi ve alev geciktirici olarak kullanılabilirliği , Yüksek Lisans Tezi, Gazi Üniversitesi, Fen Bilimleri Enstitüsü, Ankara, 2015.
  • Aydın Y. D., Patlar K., Gürü M., Akkurt F., Synthesis of antimony fluoroborate and usability as flame retardant, 8th ınternational advanced technologies symposium (IATS’17) Elazığ, Türkiye, 19-22 Ekim, 2017.
  • Aydın Y. D., Kurt H., Kandemir E. B., Gürü M., Synthesis of lead fluoroborate and usability as flame retardant, 8th ınternational advanced technologies symposium (IATS’17) Elazığ, Türkiye, 19-22 Ekim, 2017.
  • Aydın Y. D., Biberoğlu R., Kümbetlioğlu F., Gürü M., Kobalt floroborat sentezi ve alev geciktirici olarak kullanılabilirliği, 1st International Eurasion Conference on Science, Engineering and Technology Ankara, Türkiye, 22-23 Kasım, 2018.
  • A. Abdullah Ceyhan, Safiye Bağcı, Orhan Baytar, Ömer Şahin, Amonyum floroborat üretimi ve üretim parametrelerinin belirlenmesi, Bor Dergisi, 5(2), 63-72, 2020.
  • Aydın D. Y., Gürü M., Ayar B., Çakanyıldırım Ç., Bor bileşiklerinin alev geciktirici ve yüksek sıcaklığa dayanıklı pigment olarak uygulanabilirliği, Bor Dergisi, 1(1), 33-39, 2016.
  • Lu S. Y., Hamerton I., Recent developments in the chemistry of halogen-free flame retardant polymers. Prog. Polym. Sci., 27(8), 1661-1712, 2002.
  • Dogan M., Unlu M., Flame retardant effect of boron compounds on red phosphorus containing epoxy resins. Polym Degrad Stab., 99, 12-17, 2014.
  • Wang X, Song Y., Bao J., Synergistic effects of ZrO 2 or B 2 O 3 on flame-retarded poly (butyl methacrylate) with tricresylphosphate, Fire Mater., 34(7), 357-366, 2010.
  • Ayar B., Gürü M., Çakanyıldırım Ç., Solid phase synthesis of anhydrous zinc borate from zinc and boron oxide and utilization as a flame retardant in dye and textile. GU. J. Sci., 27(3), 987-991, 2014.
  • Bourbigot S., Bras M. L., Leeuwendal R., Shenc K. K., Schubertc D., Recent advances in the use of zinc borates in flame retardancy of EVA. Polym. Degrad. Stabil, 64(3), 419-425, 1999.
  • Leoni P., Sommovigo M., Pasqualli M., Midollini S., Braga D., Sabatino P., Coordinated water/anion hydrogen bonds and Pd-H bond acidity in cationic palladium(II) aquo hydrides and the x-ray crystal and molecular structures of trans- [(Cy3P)2Pd(H)(H2O)]BF4 (Cy = cyclohexyl). Organometallics, 10(4), 1038–1044, 1991.
  • Bozacı E., Borlu bileşiklerin çevre dostu yöntemlerle poliakrilnitril kumaşlarau uygulanması Ebru Bozacı* Bor Dergisi, 3(1), 17-23, 2018.
  • Friedrich K., Breuer U., Multifunctionality of polymer composites: challenges and new solutions. 1st ed., Elsevier, USA, 2015.
There are 33 citations in total.

Details

Primary Language Turkish
Subjects Engineering
Journal Section Research Article
Authors

Metin Gürü 0000-0002-7335-7583

Gülden Güngör This is me 0000-0003-1517-7821

Duygu Yılmaz Aydın 0000-0003-0557-5279

Çetin Çakanyıldırım 0000-0001-7040-1369

Project Number 2017-30-06-30-002.
Publication Date September 30, 2021
Acceptance Date June 28, 2021
Published in Issue Year 2021 Volume: 6 Issue: 3

Cite

APA Gürü, M., Güngör, G., Yılmaz Aydın, D., Çakanyıldırım, Ç. (2021). Kalsiyum floroborat sentezi, kinetik ve alev geciktirici özelliklerinin belirlenmesi. Journal of Boron, 6(3), 326-331. https://doi.org/10.30728/boron.880116