ABSTRACT: Terpolymer / kaolinite microcomposites were synthesized by 2:2:1 molar ratio of aniline, anthranilic acid and o-phenylenediamine monomers, respectively using various percentages of kaolinite clay via modified in situ oxidative ter-polymerization. The results were confirmed by FT-IR and UV-Vis absorption spectra of terpolymers / kaolinite composites. The thermal behaviour of the terpolymer and composites was studied. Terpolymers / kaolinite composites were thermally more stable than the pristine terpolymer. Surface morphology by SEM of terpolymer composites was recorded at different magnification power and was revealed whitish micrometric beads distributed all over the field with particle size in the range of 0.060 μm to 0.699 μm.
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Initially, the following monomers namely, aniline, anthranilic acid, and crystalline o-phenylenediamine were utilized by 2:2:1 mass ratios. Therefore, 1.82 ml, 20 mmol of pure aniline; 2.74 g, 20 mmol of pure anthranilic acid; 1.08 g, 10 mmol of crystalline o-phenylenediamine were dissolved in 7.5 mL of conc. HCl at room temperature under vigorous magnetic stirrer. Subsequently, 60 mL of potassium dichromate initiator was dissolved in distilled water (K2Cr2O7 8.8 g / 250 mL of distilled water) was gradually added into the reaction solution with continuous stirring at room temperature. The ter-polymerization solution was left for 24 hr at room temperature to complete the polycondensation reaction. Ammonia solution, 10 mL of 33 % NH4OH diluted by 20 mL of distilled water, was added drop wisely until a deep brown precipitate was produced. The filtered precipitate (EB) was washed with sufficient amount of deionized water then washed by ethanol to remove residual oxidant, unreacted monomer and oligomer until the filtrate became colorless and oven dried at 60 °C for overnight. The deep brown dried powder produces PANI-AA-o-PDA (PAAAPDAK1). The gained terpolymer yield was calculated to be 88.3 % utilizing the subsequent compatible …show more content…
At first, aniline, anthranilic acid and crystalline o-phenylenediamine were utilized by 2:2:1 mass ratios. Therefore, 1.82 ml, 20 mmol of pure aniline; 2.74 g, 20 mmol of pure anthranilic acid; 1.08 g, 10 mmol of crystalline o-phenylenediamine were dissolved in 7.5 mL of conc. HCl. After that, the calculated amounts of kaolinite caly, 10 wt. %, 20 wt. %, 30 wt. %, 40 wt. %, and 50 wt. %, were suspended in 25 mL distilled water respectively, under vigorous magnetic stirrer. Then, the suspended system was progressively added to the reactor with continuous stirring at room temperature. At the same time, 60 mL of pure dissolved potassium dichromate initiator, K2Cr2O7 8.8 g / 250 mL distilled water, was slowly dropped into the reaction medium under the above mentioned conditions. Then, the ter-polymerization mixture was left for 24 hr at room temperature in order to complete the ter-polymerization reaction. Ammonia solution, 10 mL of 33 % NH4OH diluted by 20 mL of distilled water, was poured drop wisely until a brown precipitate was formed which was filtered using a Büchner funnel. The obtained precipitates were washed with sufficient amount of deionized water subsequently, washed by ethanol to remove oligomer, unreacted monomer and residual oxidant until the filtrate became
Initially, the following monomers namely, aniline, anthranilic acid, and crystalline o-phenylenediamine were utilized by 2:2:1 mass ratios. Therefore, 1.82 ml, 20 mmol of pure aniline; 2.74 g, 20 mmol of pure anthranilic acid; 1.08 g, 10 mmol of crystalline o-phenylenediamine were dissolved in 7.5 mL of conc. HCl at room temperature under vigorous magnetic stirrer. Subsequently, 60 mL of potassium dichromate initiator was dissolved in distilled water (K2Cr2O7 8.8 g / 250 mL of distilled water) was gradually added into the reaction solution with continuous stirring at room temperature. The ter-polymerization solution was left for 24 hr at room temperature to complete the polycondensation reaction. Ammonia solution, 10 mL of 33 % NH4OH diluted by 20 mL of distilled water, was added drop wisely until a deep brown precipitate was produced. The filtered precipitate (EB) was washed with sufficient amount of deionized water then washed by ethanol to remove residual oxidant, unreacted monomer and oligomer until the filtrate became colorless and oven dried at 60 °C for overnight. The deep brown dried powder produces PANI-AA-o-PDA (PAAAPDAK1). The gained terpolymer yield was calculated to be 88.3 % utilizing the subsequent compatible …show more content…
At first, aniline, anthranilic acid and crystalline o-phenylenediamine were utilized by 2:2:1 mass ratios. Therefore, 1.82 ml, 20 mmol of pure aniline; 2.74 g, 20 mmol of pure anthranilic acid; 1.08 g, 10 mmol of crystalline o-phenylenediamine were dissolved in 7.5 mL of conc. HCl. After that, the calculated amounts of kaolinite caly, 10 wt. %, 20 wt. %, 30 wt. %, 40 wt. %, and 50 wt. %, were suspended in 25 mL distilled water respectively, under vigorous magnetic stirrer. Then, the suspended system was progressively added to the reactor with continuous stirring at room temperature. At the same time, 60 mL of pure dissolved potassium dichromate initiator, K2Cr2O7 8.8 g / 250 mL distilled water, was slowly dropped into the reaction medium under the above mentioned conditions. Then, the ter-polymerization mixture was left for 24 hr at room temperature in order to complete the ter-polymerization reaction. Ammonia solution, 10 mL of 33 % NH4OH diluted by 20 mL of distilled water, was poured drop wisely until a brown precipitate was formed which was filtered using a Büchner funnel. The obtained precipitates were washed with sufficient amount of deionized water subsequently, washed by ethanol to remove oligomer, unreacted monomer and residual oxidant until the filtrate became