Flash precipitation

Coprecipitation Solvent-controlled precipitation technologies, e.g., micropre-cipitated bulk powder (MBP), evaporative precipitation into aqueous solution (EPAS), Nanomorph, and flash precipitation, etc. 

The flash precipitation process, as stated before, was first employed for the production of poly(D,L-lactide) nanoparticles by Fessi et al. [41]. Polymer and drug were dissolved in an organic water-miscible solvent (acetone, tetrahydrofuran) and then the solution was infused into a large volume of water, where the solvent was dispersed quickly into the aqueous phase and stable nanoparticles were formed. As mentioned in the introduction, this process will be described in detail in this section, and in particular the interaction between the particle formation process and hydrodynamics will be discussed as the mixing efficiency is important, nanoparticles production by solvent displacement is often carried out in intensive mixers. 

Catalyst recovery is a major operational problem because rhodium is a cosdy noble metal and every trace must be recovered for an economic process. Several methods have been patented (44—46). The catalyst is often reactivated by heating in the presence of an alcohol. In another technique, water is added to the homogeneous catalyst solution so that the rhodium compounds precipitate. Another way to separate rhodium involves a two-phase Hquid such as the immiscible mixture of octane or cyclohexane and aliphatic alcohols having 4—8 carbon atoms. In a typical instance, the carbonylation reactor is operated so the desired products and other low boiling materials are flash-distilled. The reacting mixture itself may be boiled, or a sidestream can be distilled, returning the heavy ends to the reactor. In either case, the heavier materials tend to accumulate. A part of these materials is separated, then concentrated to leave only the heaviest residues, and treated with the immiscible Hquid pair. The rhodium precipitates and is taken up in anhydride for recycling. 

Lead—copper alloys are also used as tank linings, tubes for acid mist precipitators, steam heating pipes for sulfuric acid or chromate plating baths, and flashing and sheeting (see Tanks AND pressure vessels). 

Examples of similar processes are the decomposition of precipitated aluminum trHiydroxide to alumina, which is the feed for the electrolytic production of aluminum metal, and the drying of wet sulfide concentrates in preparation for flash roasting (see Aluminumand aluminum alloys). 

Tricalcium Phosphate. Commercial tricalcium phosphate (TCP) is actually an amorphous basic calcium phosphate close to hydroxyapatite in composition. Because of its extremely low solubiUty in water, TCP is precipitated almost quantitatively from dilute phosphate solutions with a slurry of hydrated lime. TCP is separated by dmm-, spray-, or flash-drying the TCP slurry, with or without intermediate sedimentation or filtration steps. It is used as an industrial-grade flow conditioner and parting agent. 

The AIF. solution is filtered, AIF. precipitated by heating, flash dried, and calcined. 

Solution Polymerization These processes may retain the polymer in solution or precipitate it. Polyethylene is made in a tubular flow reactor at supercritical conditions so the polymer stays in solution. In the Phillips process, however, after about 22 percent conversion when the desirable properties have been attained, the polymer is recovered and the monomer is flashed off and recyled (Fig. 23-23 ). In another process, a solution of ethylene in a saturated hydrocarbon is passed over a chromia-alumina catalyst, then the solvent is separated and recyled. Another example of precipitation polymerization is the copolymerization of styrene and acrylonitrile in methanol. Also, an aqueous solution of acrylonitrile makes a precipitate of polyacrylonitrile on heating to 80°C (176°F). 

The preferred catalyst is one which contains 5% of chromium oxides, mainly Cr03, on a finely divided silica-alumina catalyst (75-90% silica) which has been activated by heating to about 250°C. After reaction the mixture is passed to a gas-liquid separator where the ethylene is flashed off, catalyst is then removed from the liquid product of the separator and the polymer separated from the solvent by either flashing off the solvent or precipitating the polymer by cooling. 

Purification. The commercial LDPE was dissolved in hot toluene and precipitated in methanol. The resulting small chips were dried in a vacuum oven overnight at 80° C. HDPE was purified in the same manner, except that in this case much of the commercial material was insoluble in toluene, and so significant fractionation apparently occurs during t.he purification. The model compounds were purified by the flash chromatographic technique of Still et al. (10). 

The first step in the precipitator is the addition of polyelectrolyte solution in the flash mix tank [T-98], surge tank [T-99], and then into the slow mix unit [T-100] containing a variable speed mixing paddle. The purpose of this unit is to coagulate and flocculate53 the metal hydroxide precipitates. 

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