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Kompozit resol reçinelerinin sentezi ve cam elyaf üretiminde kullanımı

2015
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Advisor: Prof. Dr. Nilgün Kızılcan

Abstract (EN)

This study can be divided into two parts. The first part aims to synthesis resol nanocomposites that can be used for thermal insulation materials, coatings, molding compounds, foundry materials, wood products and aerospace components due to their high strength, thermal stability, heat resistance and solvent resistance. In this study, resol resins were modified with alendronic acid and sepiolite in the presence of base catalyst. Sepiolite is a needle like clay that improves the thermal stability, mechanical properties of polymers and used in the matrix of polyethylene, polypropylene, polyurethane, polyamide, polyvinylalcohol and epoxy resins, however there is not any research that include sepiolite and resol. Alendronic acid that is a phosphorus compound mostly used in drug sector for treatment of hypercalcemia, Paget's disease, parasitic diseases, hypercholesterolemia and atherosclerosis. On the other hand phosphorus containing compounds used as flame retardant materials in engineering plastics, polyurethane foams, phenolic resins, polyamides, coatings and textiles. The influence of sepiolite content and alendronic acid content on spectroscopic, thermal and microscopic properties of resins have been researched and determined. For this reason, with adding the different clay amounts of sepiolite (3wt%, 5wt%, 8 wt%, 10wt%, 15wt%, 20 wt%, 30 wt% and 50wt%) and different amounts of alendronic acid (5wt% and 10wt%) were synthesized. Furthermore, the synergist effect of sepiolite and alendronic acid were studied with 5wt% sepiolite and 5wt% of alendronic acid. In this part the synthesized resins formed the structure of nanocomposites. The characterization of the resin nanocomposite samples have been researched and determined. The characterization of the resin samples were performed by Fourier Transform Infrared Spectroscopy (FTIR-ATR), Thermogravimetric Analysis (TGA), X-ray Diffraction (XRD) and Scanning Electron Microscope (SEM). In addition, the solvent behaviour of these resins were investigated with the solvents of acetone, methanol, tetrahydrofuran (THF), dimethylformamid (DMF), chloroform and dimethyl sulfoxide (DMSO). In FTIR-ATR measurements, with the characteristic peaks of neat resol (PFR), Si-O-Si vibrating characteristics of sepiolite and phosphorus peaks of alendronic acid were obtained in nanocomposite resin samples. The DSC technique was used for determining the maximum cure temperatures and onset of cure temperatures. The cycle was heated from 30°C to 200°C with 10 °C/min heating rate. Due to sepiolite clay and alendronic acid loading, the curing temperarutres were enhanced. The thermal attitude of resins were determined by TGA analysis. All resin samples heated at linear heating rate of 10 oC/min up 30oC to 700oC temperature. The weight loss of the resins were calculated with TGA. The obtained all residues at 700oC were higher than 50%wt of initial resin. The structures and the variations of spacing of the PFR, SEP, PFR-AAs, PFR-SEPs and PFR-AA-SEP were detected by X-ray diffraction. The d-spacings were calculated by Bragg's Equation. All of the PFR-SEPs exhibited intercalated structure. As the loading of sepiolite was increased, the interlayer distance did not change very much due to the layers of sepiolite were bonded covalently and resol has thermoset structure even before curing. In PFR-AAs the nanocomposite structure was changed from exfoliated to intercalated with increasing alendronic acid content. Distribution of clay particles in polymeric resol resin matrix and morphology of resin samples were determined with SEM analysis. The sample that contained 10wt% sepiolite loading had good dispersion in resol matrix that supports the strong interaction between silanol (Si-OH) groups of sepiolite and methylol (-CH2OH) groups of resol. The solubility tests were done with six different solvents that were acetone, methanol, THF, chlorofom, DMF and DMSO. All of the resin samples were not solve in acetone, methanol, THF and chloroform. The neat PFR were soluble in DMF and DMSO. Alendronic acid including nanocomposite resins were soluble in DMF however sepiolite including nanocomposite resins were not soluble in DMF. In DMSO not only PFR-AAs but also most of PFR-SEPs and PFR-AA-SEP were soluble. However, increased sepiolite contents of PFR-SEPs reduced the solubility. The second part of this study aimed to obtain production of glass wool insulation materials with sepiolite and alendronic acid modified phenol formaldehyde resol resins to improve thermal properties. Glass wool that is a fluffy material of discontinuous fibers in random lenghts is very useful in thermal insulation sector. For producing glass wool composites of resol samples in a batch mixer the major ingredients (silica sand, limestone, soda ash, cullet) were blended at 1100oC-1300oC. From the reactor the molten glass was poured into the spinner that consisted of 2000 small holes. The fluid mixture were constrained and fibers were manufactured, owing to the centrifugal force of spinner. To bind glass wools the synthesized liquid nanocomposite resol resins were sprayed. After this step, the glass wool was dried in the curing oven at 180-250oC to obtain composite glass wool – modified resol resin product. Length and width trimmers were cut the size of the composite glass wool insulation product At the end of process glass wool composites gained the colour of resin samples.

Author

Dr. Ümran Burcu Alkan

How to Cite

Ümran Burcu Alkan (Master Thesis). Kompozit resol reçinelerinin sentezi ve cam elyaf üretiminde kullanımı, 2015, Istanbul Technical University.

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