Solid-liquid, suspension extraction

The entropically driven disorder-order transition in hard-sphere fluids was originally discovered in computer simulations [58, 59]. The development of colloidal suspensions behaving as hard spheres (i.e., having negligible Hamaker constants, see Section VI-3) provided the means to experimentally verify the transition. Experimental data on the nucleation of hard-sphere colloidal crystals [60] allows one to extract the hard-sphere solid-liquid interfacial tension, 7 = 0.55 0.02k T/o, where a is the hard-sphere diameter [61]. This value agrees well with that found from density functional theory, 7 = 0.6 0.02k r/a 2 [21] (Section IX-2A). 

The concept of extractive reaction, which was conceived over 40 years ago, has connections with acid hydrolysis of pentosans in an aqueous medium to give furfural, which readily polymerizes in the presence of an acid. The use of a water-immiscible solvent, such as tetralin allows the labile furfural to be extracted and thus prevents polymerization, increases the yield, and improves the recovery procedures. In the recent past an interesting and useful method has been suggested by Rivalier et al. (1995) for acid-catalysed dehydration of hexoses to 5-hydroxy methyl furfural. Here, a new solid-liquid-liquid extractor reactor has been suggested with zeolites in protonic form like H-Y-faujasite, H-mordenite, H-beta, and H-ZSM-5, in suspension in the aqueous phase and with simultaneous extraction of the intermediate product with a solvent, like methyl Aobutyl ketone, circulating countercurrently. 

Leoni [366] observed that in the extraction preconcentration of organochlo-rine insecticides and PCB s from surface and coastal waters in the presence of other pollutants such as oil, surface active substances, etc., the results obtained with an absorption column of Tenax-Celite are equivalent to those obtained with the continuous liquid-liquid extraction technique. For non-saline waters that contain solids in suspension that absorb pesticides, it may be necessary to filter the water before extraction with Tenax and then to extract the suspended solids separately. Analyses of river and estuarine sea waters, filtered before extraction, showed the effectiveness of Tenax, and the extracts obtained for pesticide analysis prove to be much less contaminated by interfering substances than corresponding extracts obtained by the liquid-liquid technique. Leoni et al. [365] showed that for the extraction of organic micro pollutants such as pesticides and aromatic polycyclic hydrocarbons from waters, the recoveries of these substances from unpolluted waters (mineral and potable waters) when added at the level of 1 xg/l averaged 90%. 

As observed above, in order to quench HMF produced in situ, dealuminated H-form mordenites were investigated in a water/MIBK mixture (1/5) [84, 85]. In this case, a maximum conversion of fructose of 54% (along with 90% selectivity to HMF) was obtained over an H-mordenite with a Si/Al ratio of 11. HMF was continuously extracted with a flow of MIBK circulating in a countercurrent way through a catalytic heterogeneous reactor containing the H-mordenite zeolite. On the continuation of their efforts, the same authors then set up a new continuous solid-liquid-liquid reactor where the zeolite was now in suspension in the aqueous phase while the HMF was continuously extracted with MIBK in a countercurrent way to the aqueous phase and catalyst feed. 

To investigate the presence of organo-mineral compounds, specimens of fine earth and the five separates (coarse, medium and fine sand, silt and clay) from bulk, LAR and TAR of the 2C horizons were shaken for 30 min in 1.2 M HCl solution (solid/liquid ratio, 1 10) the suspensions were centrifuged and the supernatants filtered at 0.45 pm. Aliquots of 2 mL were oven-dried (120°C) on glass slides and analyzed by X-ray diffraction using a Philips PW 1710 diffractometer (Fe-filtered Co-Kaj radiation). The acid extracts were also analyzed by gas chromatography, following the procedure of Ferntodez Sanjurjo et al. 

Once a liquid sample has been obtained, either from an original liquid object or by dissolution of a soHd object, the various species of interest must be isolated for analysis. In the case of a liquid suspension, filtration, or centrifugation are often performed prior to analysis to remove any solid particles. In the case of a solution, there are many methods available for isolating analytes, including complexation, separation or extraction. These procedures are performed prior to analysis, for many reasons. Most often these procedures are performed either to remove any species which may cause interferences in the particular analysis or to provide a means of concentrating the analyte prior to analysis. 

To a vigorously stirred suspension of 2 mol of lithium amide in 2 1 of liquid atimonia (see II, Exp. 11) was added in 15 min 1 mol of propargyl alcohol (commercial product, distilled in a partial vacuum before use). Subsequently, 1 mol of butyl bromide was added dropwise in 75 min. After an additional 1.5 h, stirring was stopped and the ammonia was allovied to evaporate. To the solid residue were added 500 ml of ice-water. After the solid mass had dissolved, six extractions with diethyl ether were performed. The (unwashed) combined extracts were dried over magnesium sulfate and then concentrated in a water-pump vacuum. Distillation of the residue through a 40-cm Vigreux column afforded 2-heptyn-l-ol, b.p. 

A solution of the monosodium salt of diacetylene in 300 ml of liquid ammonia is prepared from 13.8 g (0.6 g-atoms) sodium and 24.6 g (0.2 moles) l,4-dichlorobut-2-yne. To this mixture is added a suspension of 5 g (17.6 mmoles) 3-methoxyestra-l,3,5(10)-trien-17-one in anhydrous tetrahydrofuran at —40° and the reaction mixture is stirred and maintained at this temperature for 2 hr. Ammonium chloride is then added and the ammonia is allowed to evaporate overnight. The residual solids are extracted with methylene dichloride and the extracts washed with water, dried over magnesium sulfate, and evaporated at 70°. The resultant dark gum is... 

Operations such as blending, solids-suspension, dissolving, heat transfer and liquid-liquid extraction are typical of systems requiring high flow relative to turbulence, while gas-liquid reactions and some liquid-liquid contacting require high turbulence relative to flow. The case of (1) 100% of suspension—requires head to keep particles suspended and (2) 100% uniformity of distribution of particles—requires head for suspension plus flow for dis-tiibution. 

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