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SYNTHESIS OF 1,9-BIS [1-PHENYL-3-METHYL-5-HYDROXY-4-PYRAZOLYL] 1,9 NONANEDIONE AND ITS APPLICATION FOR THE EXTRACTION OF COBALT ( II), NICKEL (II), AND CADMIUM (II)

Synthesis of 1,9-bis [1-phenyl-3-methyl-5-hydroxy-4- pyrazolol)-1,9-nonanedione (HL-7-LH) and its application for the extraction of cobalt (II), nickel (II), and cadmium (II) have been carried out. The HL-7-LH were prepared by treating a dioxane solution of 1-phenyl-3-methyl-5-pyrazolone (H2PMP) containing calcium hydroxide catalyst with azelaoyl dichloride [ClCO(CH2)7C0C1l Purification of the HL-7-LH obtained were done by mean recrystallization in etanoltoluena (9:1) at 70°C. Characterization of the HL-7-LH were done by infrared and nuclear magnetic resonance spectroscopic techniques. The application of the HL-7-LH as extractant in the extraction of cobalt, nickel, and cadmium were performed in chloroform and dichloromethane. It was observed that the effectivity of the extraction increases as the extractant concentration and pH increases. Results show that cobalt, nickel, and cadmium extraction in chloroform wereobtained with the extraction constants (log Keks) = -5,37, -5,44, -5,22 and at dichloromethane were -5,19, - 5,24, and -5,08.Key Word : Synthesis, effectivity of the extraction, the extraction constants

SYNTHESIS AND CHARACTERIZATION OF MESOPOROUS ALUMINOSILICATES Al-MCM- 41 AND INVESTIGATION OF ITS THERMAL, HYDROTHERMAL AND ACIDITY STABILITY

The synthesis and characterization of mesoporous aluminosilicates Al-MCM-41 and the investigation of its thermal, hydrothermal and acidity stability have been done. Al-MCM-41 were synthesized by hydrothermal method to the mixture of sodium silicate as Si source, aluminium hydroxide as Al source, sodium hydroxide as a solvent, and cethyltrimethylammoniumbromide (CTAB) as structure directing agent. The reaction were carried out in alkaline condition (pH = 10.2) at 383 K for about 24 h, followed by calcination at 723 K for about 10 h. The synthesized crystals were characterized using FTIR spectroscopy, X-ray diffraction and N2 fisisorption methods. The result showed that Al-MCM-41 sample with hexagonal structure was formed, it has a good in thermal and acid stability, but the structure disintegrated in an alkaline solution (pH = 10) and in boiled water.

EFFECT OF ACID CONCENTRATION ON CHARACTERS OF SILICA GEL SYNTHESIZED FROM SODIUM SILICATE

In this research, synthesis and characterization of silica gel from sodium silicate through sol-gel process using H2SO4, HCl, and citric acid have been investigated. Synthesis was carried out by mixing and stirring 20 mL of H2SO4, HCl or citric acid at certain concentration with 50 mL of sodium silicate solution (Na2O 0.17 M and SiO2 0.61 M) for one hour and let to form gel. The gel was washed with distillated water, and dried in an oven at 100 C. Characterization of silica gel was carried out by determination of acidity, water adsorption capacity, and water content. Identification of functional group and structure were identified using x-ray diffractometer (XRD) and infrared (IR) spectrophotometer, respectively. Results showed that at a range of investigated concentration (0.6 – 3.0 M) the increase of concentration, formation of gel with H2SO4 tended to be faster, but with HCl and citric acid to be slower. The increase of acid concentration caused water content, water adsorption capacity, and acidity of the silica gel resulted with HCl and citric acid tended to be increased, increased, and increased, but with H2SO4 to be decreased, increased, and decreased, respectively. Based on the IR spectra and XRD data, it could concluded that the synthetic silica gels contained silanol (Si-OH) and siloxane (Si-O-Si) and were amorphous, showing similar pattern to kieselgel G 60 produced by Merck.