Master'sOpen Access

Bor içeren metil etil keton formaldehit reçinelerinin sentezi ve karakterizasyonu

2015
0 views
0 downloads
Advisor: Prof. Dr. Nilgün Kızılcan

Abstract (EN)

Methyl ethyl ketone formaldehyde resins are modified in situ and after the polymerization with different modifiers to increase their physical and chemical performances by changing their chemical structures. In this thesis study, methyl ethyl ketone formaldehyde resins including nitrogen and/or boron are synthesized and their phycical and chemical properties are analyzed in a comperative way. The resins are prepared by alkaline-catalysed condensation of methyl ethyl ketone and formalde in a molar ratio of 1: 2 in a batch process. NaOH is used as catalyst for this reaction. During all of the reaction pH value should been kept around 10-11. The medium is kept at 80-90oC. After 4h, the reaction is completed, and yellow resin is formed. For in sitı modifications, the modifer is added to the reaction medium in the beginning of the reaction. For boric acid modification, of resin sample is dissolved in toluene, and boric acid is added. Using deanstag systam, the medium is heated to 150oC, refluxed for about 2h until no water is collected any more. Ten different types of methyl ethyl ketone formaldehyde resins are synthesized for this study, five of which include nitrogen, one includes boron and three include both nitrogen and boron: methyl ethyl ketone formaldehyde resin (MEKFR), MEKFR modified with alendronic acid at a ratio of 5wt% (MEKFR-AA), MEKFR modified with cyclic urea which is synthesized from alendronic acid at a ratio of 5wt% (MEKFR-CUAA), MEKFR modified with diethanolamine at ratios of 5wt%, 10wt% and 20wt% (MEKFR-DEA), MEKFR and three MEKFR-DEA modified with boric acid (MEKFR-BA and MEKFR-DEA-BA, respectively). After the synthesis and modifications of resins, their chemical structures are analyzed, and Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance Spectroscopy (NMR) are used for this purpose. When the spectums of resins obtained are looked through the characteristics peaks and their corresponding functional groups, it is concluded that the estimated chemical structures as the product of synthesis and modification reactions match with the results obtained. In the terms of physical properties, solubility analyses are carried out in five different solvents, namely ethanol, acetone, dichloromethane (DCM), tetrahydrofuran (THF) and dimethylsulfoxide (DMS), and it is seen that depending on the modifier type and ratio, the solubility of resins change, as a result of the changes in the chemical structures. Lastly, in order to get information about thermal behaviour of the resins and effects of modifications on thermal degradation of them, thermogravimetric analyses (TGA ) and Methyl ethyl ketone formaldehyde resins are modified in situ and after the polymerization with different modifiers to increase their physical and chemical performances by changing their chemical structures. In this thesis study, methyl ethyl ketone formaldehyde resins including nitrogen and/or boron are synthesized and their phycical and chemical properties are analyzed in a comperative way. The resins are prepared by alkaline-catalysed condensation of methyl ethyl ketone and formalde in a molar ratio of 1: 2 in a batch process. NaOH is used as catalyst for this reaction. During all of the reaction pH value should been kept around 10-11. The medium is kept at 80-90oC. After 4h, the reaction is completed, and yellow resin is formed. For in sitı modifications, the modifer is added to the reaction medium in the beginning of the reaction. For boric acid modification, of resin sample is dissolved in toluene, and boric acid is added. Using deanstag systam, the medium is heated to 150oC, refluxed for about 2h until no water is collected any more. Ten different types of methyl ethyl ketone formaldehyde resins are synthesized for this study, five of which include nitrogen, one includes boron and three include both nitrogen and boron: methyl ethyl ketone formaldehyde resin (MEKFR), MEKFR modified with alendronic acid at a ratio of 5wt% (MEKFR-AA), MEKFR modified with cyclic urea which is synthesized from alendronic acid at a ratio of 5wt% (MEKFR-CUAA), MEKFR modified with diethanolamine at ratios of 5wt%, 10wt% and 20wt% (MEKFR-DEA), MEKFR and three MEKFR-DEA modified with boric acid (MEKFR-BA and MEKFR-DEA-BA, respectively). After the synthesis and modifications of resins, their chemical structures are analyzed, and Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance Spectroscopy (NMR) are used for this purpose. When the spectums of resins obtained are looked through the characteristics peaks and their corresponding functional groups, it is concluded that the estimated chemical structures as the product of synthesis and modification reactions match with the results obtained. In the terms of physical properties, solubility analyses are carried out in five different solvents, namely ethanol, acetone, dichloromethane (DCM), tetrahydrofuran (THF) and dimethylsulfoxide (DMS), and it is seen that depending on the modifier type and ratio, the solubility of resins change, as a result of the changes in the chemical structures. Lastly, in order to get information about thermal behaviour of the resins and effects of modifications on thermal degradation of them, thermogravimetric analyses (TGA ) and Methyl ethyl ketone formaldehyde resins are modified in situ and after the polymerization with different modifiers to increase their physical and chemical performances by changing their chemical structures. In this thesis study, methyl ethyl ketone formaldehyde resins including nitrogen and/or boron are synthesized and their phycical and chemical properties are analyzed in a comperative way. The resins are prepared by alkaline-catalysed condensation of methyl ethyl ketone and formalde in a molar ratio of 1: 2 in a batch process. NaOH is used as catalyst for this reaction. During all of the reaction pH value should been kept around 10-11. The medium is kept at 80-90oC. After 4h, the reaction is completed, and yellow resin is formed. For in sitı modifications, the modifer is added to the reaction medium in the beginning of the reaction. For boric acid modification, of resin sample is dissolved in toluene, and boric acid is added. Using deanstag systam, the medium is heated to 150oC, refluxed for about 2h until no water is collected any more. Ten different types of methyl ethyl ketone formaldehyde resins are synthesized for this study, five of which include nitrogen, one includes boron and three include both nitrogen and boron: methyl ethyl ketone formaldehyde resin (MEKFR), MEKFR modified with alendronic acid at a ratio of 5wt% (MEKFR-AA), MEKFR modified with cyclic urea which is synthesized from alendronic acid at a ratio of 5wt% (MEKFR-CUAA), MEKFR modified with diethanolamine at ratios of 5wt%, 10wt% and 20wt% (MEKFR-DEA), MEKFR and three MEKFR-DEA modified with boric acid (MEKFR-BA and MEKFR-DEA-BA, respectively). After the synthesis and modifications of resins, their chemical structures are analyzed, and Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance Spectroscopy (NMR) are used for this purpose. When the spectums of resins obtained are looked through the characteristics peaks and their corresponding functional groups, it is concluded that the estimated chemical structures as the product of synthesis and modification reactions match with the results obtained. In the terms of physical properties, solubility analyses are carried out in five different solvents, namely ethanol, acetone, dichloromethane (DCM), tetrahydrofuran (THF) and dimethylsulfoxide (DMS), and it is seen that depending on the modifier type and ratio, the solubility of resins change, as a result of the changes in the chemical structures. Lastly, in order to get information about thermal behaviour of the resins and effects of modifications on thermal degradation of them, thermogravimetric analyses (TGA ) and differential scanning calorimetry (DSC) analyses are carried out for each of resins. T50 values and residue amounts of them obtained from TGA curves as well as glass transition and melting temperatures obtained from DSC curves are the crucial parameters used during the evaluation of thermal properties of the resins.

Author

Dr. Hatay Cöcen

How to Cite

Hatay Cöcen (Master Thesis). Bor içeren metil etil keton formaldehit reçinelerinin sentezi ve karakterizasyonu, 2015, Istanbul Technical University.

Keywords

License

Tüm Hakları Saklıdır

This work is shared under the specified license terms.

More theses from Istanbul Technical University