Liquid-liquid extraction in a pilot scale rotating disc contactor

A study of the hydrodynamics and mass transfer characteristics of a liquid-liquid extraction process in a 450 mm diameter, 4.30 m high Rotating Disc Contactor (R.D.C.) has been undertaken. The literature relating to this type of extractor and the relevant phenomena, such as droplet break-up and coalescence, drop mass transfer and axial mixing has been revjewed. Experiments were performed using the system C1airsol-350-acetone-water and the effects of drop size, drop size-distribution and dispersed phase hold-up on the performance of the R.D.C. established. The results obtained for the two-phase system C1airso1-water have been compared with published correlations: since most of these correlations are based on data obtained from laboratory scale R.D.C.'s, a wide divergence was found. The hydrodynamics data from this study have therefore been correlated to predict the drop size and the dispersed phase hold-up and agreement has been obtained with the experimental data to within +8% for the drop size and +9% for the dispersed phase hold-up. The correlations obtained were modified to include terms involving column dimensions and the data have been correlated with the results obtained from this study together with published data; agreement was generally within +17% for drop size and within +14% for the dispersed phase hold-up. The experimental drop size distributions obtained were in excellent agreement with the upper limit log-normal distributions which should therefore be used in preference to other distribution functions. In the calculation of the overall experimental mass transfer coefficient the mean driving force was determined from the concentration profile along the column using Simpson's Rule and a novel method was developed to calculate the overall theoretical mass transfer coefficient Kca1, involving the drop size distribution diagram to determine the volume percentage of stagnant, circulating and oscillating drops in the sample population. Individual mass transfer coefficients were determined for the corresponding droplet state using different single drop mass transfer models. Kca1 was then calculated as the fractional sum of these individual coefficients and their proportions in the drop sample population. Very good agreement was found between the experimental and theoretical overall mass transfer coefficients. Drop sizes under mass transfer conditions were strongly dependant upon the direction of mass transfer. Drop Sizes in the absence of mass transfer were generally larger than those with solute transfer from the continuous to the dispersed phase, but smaller than those with solute transfer in the opposite direction at corresponding phase flowrates and rotor speed. Under similar operating conditions hold-up was also affected by mass transfer; it was higher when solute transfered from the continuous to the dispersed phase and lower when direction was reversed compared with non-mass transfer operation.

Advanced liquid-liquid extraction : studies in a laboratory mixer-settler

A ten stage laboratory mixer-settler has been designed, constructed and operated with efficiencies up to 90%. The phase equilibrium data of the system acetic acid-toluene-water at different temperatures has been determined and correlated. Trials for prediction of these data have been investigated and a good agreement between the experimental data and the predictions obtained by the NRTL equation have been found. Extraction processes have been analysed. A model for determination of the time needed for a countercurrent stage-wise process to come to steady state has been derived. The experimental data was in reasonable agreement with this model. The discrete maximum principle has been applied to optimize the countercurrent extraction process and proved to be highly successful in predicting the optimum operating conditions which were confirmed by the experimental results. The temperature has proved to be a prosolvent for mass transfer in both directions but the temperature profile functioned as an anti solvent.

Organic reactions in ionic liquids: ionic liquid-accelerated facile synthesis of 3-alkyl-2,4-thiazolidinediones

The room temperature ionic liquid [bmim]PF6 is a new green solvent for the N-alkylation of 2,4-thiazolidinones. Significant rate enhancement and improved yields have been observed.

Organic reactions in ionic liquids: ionic liquid-promoted efficient synthesis of N-alkyl and N-arylphthalimides

Phthalic anhydride reacts rapidly with Aromatic and aliphatic amines in ionic liquid [Bmim][PF6] or [Bmim][BF4] at 130 °C to give N-aryl and N-alkylphthalimides in excellent yields.

Organic reactions in ionic liquids: Ionic liquid-promoted three-component condensation of benzotriazole with aldehyde and alcohol

1-(alpha-Alkoxyalkyl)benzotriazoles are readily synthesized from three-component condensation of benzotriazole with aldehyde and alcohol in ionic liquid [Bmim]PF6.

Organic reactions in ionic liquids: ionic liquid-promoted efficient synthesis of disubstituted and trisubstituted thioureas derivatives

In ionic liquid [Bmim][BF4], a series of disubstituted and trisubstituted thiourea derivatives were synthesized from phenyl and butyl isothiocyanate with a variety of amine in excellent yield.

Organic reactions in ionic liquids:Ionic liquid promoted Knoevenagel condensation of aromatic aldehydes with (2-thio)barbituric acid

The Knoevenagel condensation of aromatic aldehydes with (2-thio)barbituric acid proceeded efficiently in reusable ionic liquids, EAN, BmimBF4, and BmimPF6 at room temperature in the absence of any catalyst with high yields.

Organic reactions in ionic liquids: ionic liquid-promoted efficient synthesis of N-alkyl and N-arylimides

In the ionic liquids [Bmim][PF6] or [Bmim][BF4], a series of succinimide, maleimide and phthalimide derivatives were synthesized from corresponding anhydrides with a variety of primary amines in excellent yield.

Ionic liquid-accelerated N-arylation of benzoazoles with diaryliodonium salts, an efficient method for the synthesis of N-aryl azoles

N-Arylation of benzoazoles with diaryliodonium salts can be performed in good yields in the room-temperature ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim]BF4), which provides an efficient method for the synthesis of N-arylbenzoazoles. The ionic liquid can be recycled and reused.

Ionic liquid-accelerated arylation of sodium arenesulfinates with diaryliodonium salts used for the synthesis of diaryl sulfones

Arylation of sodium arenesulfinates with diaryliodonium salts can be performed with good yields in the room-temperature ionic liquid, 1-butyl-3-methylimidazolium tetrafluoroborate ([BMim]BF4), which provides an efficient method for the synthesis of diaryl sulfones; the ionic liquid can be recycled and reused.

Organic reactions in ionic liquids: ionic liquid-accelerated nucleophilic substitution reaction of alpha-tosyloxyketones with potassium salts of aromatic acids

The room temperature ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim][BF4]) is used as a ‘green' recyclable alternative to classical molecular solvents for the nucleophilic substitution reaction of a-tosyloxy ketones with potassium salts of aromatic acids. Significant rate enhancement and improved yields have been observed.

Organic reactions in ionic liquids; Ionic liquid-accelerated three-component reaction: a rapid one-pot synthesis of 3-alkyl-5-[(Z)-arylmethylidene]-1,3-thiazolidine-2,4-diones

A rapid one-pot synthesis of 3-alkyl-5-[(Z)-arylme­thylidene]-1,3-thiazolidine-2,4-dionesis described that occurs in recyclable ionic liquid [bmim]PF6 (1-butyl-3-methylimidazolium hexafluorophosphate).Significant rate enhancement and good selectivity have been observed.

Organic reactions in ionic liquids: ionic liquid-accelerated cyclocondensation of alpha-tosyloxyketones with 2-aminopyridine

The room temperature ionic liquid it-butylpyridinium tetrafluoroborate (BPyBF4) is used as a `green' recyclable alternative to classical molecular solvents for the cyclocondensation of alpha-tosyloxyketones with 2-aminopyridine. Significant rate enhancements and improved yields have been observed.