Bazı metal boratların sentezi ve karakterizasyonu
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Dosyalar
Tarih
2007
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Kırıkkale Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu tezde sunulan çalısma esas olarak yeni alkali metal borat ve alkali metal organoborat sentezlerinin arastırılmasına yöneliktir. stenilen ürünleri elde etmek için, reaksiyonlar sulu ve susuz ortamlarda gerçeklestirilmistir. Çalısmanın ilk bölümünde alkali metal hidroksit veya karbonatlarının borik asit ile sulu ortamdaki reaksiyonları incelenmistir. Yürütülen bu reaksiyonlara ilave olarak ayrıca borik asidin diol, hidroksi karboksilik asit ve dikarboksilik asit içeren organik gruplar ile bazik ortamlardaki reaksiyonları da incelenmistir. Elde edilen analitik ve spektroskopik verilerden, alkali metal boratların sentezlerinin beklenildigi gibi yürüdügü ancak, kullanılan sentez yöntemine baglı olarak organik grubun borat yapısına koordine olmadıgı görülmüstür. Yürütülen bu reaksiyonların sonucunda, mineral adı tinkalkonit, Na2[B4O5(OH)4].3H2O, olarak bilinen bir sodyum tetraborat bilesigi ile bir sezyum tuzu, CsC6H3O4N2.H2O, sentezlenmis, yapıları tek kristal X-ray difraksiyonu ile karakterize edilmistir. Çalısmanın ikinci bölümünde, NaBH4 'ün diol veya karboksilik asit içeren çesitli organik gruplar ile reaksiyonları susuz çözücü ortamında incelenmistir. Mevcut analitik ve spektroskopik veriler esas alındıgında, beklenilen sodyum destekli borat ester bilesiklerinin olusumu basarısız olmustur. Çalısmanın üçüncü bölümünde, potasyum destekli borat esteri elde etmek üzere bir deneme gerçeklestirilmistir. Bu ürüne ait deneysel veriler istenilen bilesigin katı hal sentezi ile üretilemeyecegini göstermistir. Bu reaksiyonlardan elde edilen ürünler, X-ısını kristalografisi, DSC, 1H-NMR, 13C-NMR, LC-MSD, FT-IR ve elementel analiz ile karakterize edilmistir. Anahtar Kelimeler: Metal Boratlar, X-Isını Kristalografisi, Bor Bilesikleri, Katı Hal Sentezi, Tek Kristal
The study presented in this thesis concerns primarily with the investigation of the synthesis of original alkali metal borates and alkali metal organoborates. In order to obtain the desired products, the reactions have been conducted both in aqueous and non aqueous media. In the first part of the study, the reactions of alkali metal hydroxides or carbonates with boric acid in aqueous media were investigated. In addition to these reactions carried out, the reactions of boric acid with organic groups containing diols, hydroxy carboxylic acids and dicarboxylic acids in basic media were also investigated. From the analytical and spectroscopic data obtained so far, the synthesis of alkali metal borates proceeded as might have been anticipated, however it was found that depending on the synthetic method used the coordination of organic groups into the borate structure can not be achieved. As a result of these reactions conducted, a sodium tetraborate compound, the mineral name known as tincalconite, Na2[B4O5(OH)4].3H2O, and a caesium salt, CsC6H3O4N2.H2O were synthesized and their structures were characterized by single crystal X- ray diffraction. In the second part of the study, the reactions of NaBH4 with various organic groups containing diols or carboxylic acids in non-aqueous media were investigated. On the basis of the analytical and spectroscopic data available, the formation of the expected sodium supported borate ester compounds have been unsuccessful. In the third part of the study, an attempt has been made to produce potassium supported borate ester. The experimental data obtained on this product may indicate that the desired compound may not be produced by the solid state synthesis. The products obtained from these reactions were characterized by X-ray Crystallography, DSC, 1H-NMR , 13C-NMR, LC-MSD, FT-IR and elemental analysis, Key Words: Metal Borates, X-ray Crystallography, Boron Compounds, Solid State Synthesis, Single Crystal
The study presented in this thesis concerns primarily with the investigation of the synthesis of original alkali metal borates and alkali metal organoborates. In order to obtain the desired products, the reactions have been conducted both in aqueous and non aqueous media. In the first part of the study, the reactions of alkali metal hydroxides or carbonates with boric acid in aqueous media were investigated. In addition to these reactions carried out, the reactions of boric acid with organic groups containing diols, hydroxy carboxylic acids and dicarboxylic acids in basic media were also investigated. From the analytical and spectroscopic data obtained so far, the synthesis of alkali metal borates proceeded as might have been anticipated, however it was found that depending on the synthetic method used the coordination of organic groups into the borate structure can not be achieved. As a result of these reactions conducted, a sodium tetraborate compound, the mineral name known as tincalconite, Na2[B4O5(OH)4].3H2O, and a caesium salt, CsC6H3O4N2.H2O were synthesized and their structures were characterized by single crystal X- ray diffraction. In the second part of the study, the reactions of NaBH4 with various organic groups containing diols or carboxylic acids in non-aqueous media were investigated. On the basis of the analytical and spectroscopic data available, the formation of the expected sodium supported borate ester compounds have been unsuccessful. In the third part of the study, an attempt has been made to produce potassium supported borate ester. The experimental data obtained on this product may indicate that the desired compound may not be produced by the solid state synthesis. The products obtained from these reactions were characterized by X-ray Crystallography, DSC, 1H-NMR , 13C-NMR, LC-MSD, FT-IR and elemental analysis, Key Words: Metal Borates, X-ray Crystallography, Boron Compounds, Solid State Synthesis, Single Crystal
Açıklama
Anahtar Kelimeler
Enerji, Energy ; Kimya, Chemistry
