Solution, extraction catalyst from

A 500-ml. three-necked flask is fitted with a reflux condenser and a thermometer, the bulb of which reaches far enough into the flask to be covered by the liquid. A solution of 46.0 g. (0.205 mole) of a-phenylcinnamic acid (p. 70) (Note 1) in 280 ml. (307 g., 2.38 moles) of quinoline (Note 2) is added to the flask along with 4.0 g. of copper chromite.2 The reaction flask is heated by means of a mantle or an oil bath until the temperature of the reaction mixture reaches 210-220°. The mixture is kept within this temperature range for 1.25 hours. The solution is then cooled immediately and added to 960 ml. of 10% hydrochloric acid in order to dissolve the quinoline (Note 3). The product is extracted from this mixture with two 200-ml. portions of ether followed by a 100-ml. portion. The combined ether extracts are filtered to remove particles of catalyst, washed with 200 ml. of 10% sodium carbonate, and dried over anhydrous sodium sulfate. The dry solution is removed from the drying agent by filtration and heated on a steam bath to distil the ether. The residue is dissolved in a hexane fraction, b.p. 60-72° (Skellysolve B) the solution is cooled to 0° and filtered to remove /raws-stilbene, if any. The hydrocarbon solvent is removed by distillation, and the czs-stilbene is distilled. The yield is 23-24 g. (62-65%), b.p. 133-136°/10 nun., 95-97°/l mm. tig 1.6183-1.6193, 1.6212-... 

InTox A process for destroying toxic wastes in aqueous solution by oxidation with oxygen at high temperatures and pressures in a pipe reactor. No catalyst is required. The reactions take place at approximately 300°C and 120 atm. Developed by InTox Corporation, UK, based on a process for extracting aluminum from bauxite developed by Lurgi in the 1960s. See also Zimpro. 

The isolation of product is usually possible after evaporation of the solvent and extraction with hexane, ether, or toluene. Supported versions, for example on polystyrene grafted with PPh2 groups, have proved unsatisfactory because the rate of deactivation is greatly enhanced under these conditions [37]. Asymmetric versions exist, but the ee-values tend to be lower than in the Rh series [38]. With acid to neutralize the basic N lone pair, imine reduction is fast. Should it be necessary to remove the catalyst from solutions in order to isolate a strictly metal-free product, a resin containing a thiol group should prove satisfactory. A thiol group in the substrate deactivates the catalyst, however. 

In the classical oxo process the catalyst cohalt carbonyl is formed in situ by introducing divalent cobalt into the reactor. High temperature is required for this catalyst formation that gives a mixture of aldehydes and alcohols containing only 60-70% of linear product. A new BASF process using cobalt carbonyl hydride shows improved selectivity and efficient catalyst recovery. The catalyst is prepared by passing an aqueous solution of cobalt salt over a promoter and extracting the catalyst from the water phase with olefin. 

Step 2 Extraction of the Catalyst from the Aqueous Solution. It is not feasible technically to charge the aqueous solution of cobalt carbonyl hydride directly into the hydroformylation reactor because two phases may form, especially with the long chain olefins. The most direct and most efficient way to eliminate water while permitting full use of the carbonyl catalyst is to extract it from the water phase with the olefin intended for hydroformylation. The extraction is carried out between... 

Well ordered mesoporous silicate films were prepared in supercritical carbon dioxide.[218] In the synthesis in aqueous or alcoholic solution, film morphology of preorganized surfactants on substrate cannot be fully prescribed before silica-framework formation, because structure evolution is coincident with precursor condensation. The rapid and efficient preparation of mesostructured metal oxides by the in situ condensation of metal oxides within preformed nonionic surfactants can be done in supercritical CCU- The synthesis procedure is as follows. A copolymer template is prepared by spin-coating from a solution containing a suitable acid catalyst. Upon drying and annealing to induce microphase separation and enhance order, the acid partitions into the hydrophilic domain of the template. The template is then exposed to a solution of metal alkoxide in humidified supercritical C02. The precursor diffuses into the template and condenses selectively within the acidic hydrophilic domain of the copolymer to form the incipient metal oxide network. The templates did not go into the C02 phase because their solubility is very low. The alcohol by-product of alkoxide condensation is extracted rapidly from the film into the C02 phase, which promotes rapid and extensive network condensation. Because the template and the metal oxide network form in discrete steps, it is possible to pattern the template via lithography or to orient the copolymer domains before the formation of the metal oxide network. 

Leitner reported that lower densities of SCCO2 can be used to extract product from a reaction mixture without coextraction of a homogeneous catalyst. This process, which he called CESS (catalysis and extraction using supercritical solution), was demonstrated with styrene hydroformylation [Eq. (23), ligand L ] and imine hydrogenation [Eq. (22)]. The catalyst was used for three cycles before drops in the conversion and selectivity was observed (101,111,133). Sellin and Cole-Hamilton used catalysts specifically chosen for their insolubility in SCCO2 to facilitate the catalyst/product separation in a CESS process (134). 

The technical realization of telomerizations is not very well investigated. In a recent paper the telomerization of isoprene with methanol was studied in detail and different concepts of realization were proposed both for single phase operation as well as for biphasic catalysis [115]. One possible alternative proved to be the bipha-sic telomerization with an aqueous methanolic solution as catalyst phase, followed by distillation of unreacted isoprene and methanol, then finally extracting the telomers from the aqueous layer with isoprene. The second alternative for the product separation is without any extraction step and uses only phase separation and distillation steps. 

Monocrotalic acid, CJIaOi. A solution of 10.8 g. of monocrotaline in a mixture of 10 cc. of glacial acetic acid and 40 cc. of ethanol was hydrogenated at 2-3 atm. with 0.1 g. of platinum oxide catalyst. Two moles of hydrogen were absorbed in 5 hours. The solution was filtered from the catalyst and evaporated in vacuo. The remaining sirup was taken up in 34 cc. of 1 iV hydrochloric acid and the aqueous solution thus obtained was extracted continuously with ether for 24 hours. The ether solution was dried, the ether was removed, and the crystalline residue of monocrotalic acid was purified by recrystallization from acetone-petroleum ether (b. p. 30-60°) white plates, m.p. 181-182°. 

Hydrogenation reaction a reaction in which hydrogen is added, with a catalyst present, to a carbon-carbon multiple bond. (22.2) Hydrohaiic acid an aqueous solution of a hydrogen halide. (20.7) Hydrometaiiui y a process for extracting metals from ores by use of aqueous chemical solutions. Two steps are involved selective leaching and selective precipitation. (21.8)... 

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