Precipitation processes size control

In the polymer industry, post-reaction product treatment processes such as liquid-solid separation, drying, precipitation, particle size control, and polymer purification are very complex and costly. Future polymer plants should be designed such that process equipment can be easily and quickly converted to making new products at minimal cost and with... 

In order to make an efficient Y202 Eu ", it is necessary to start with weU-purifted yttrium and europium oxides or a weU-purifted coprecipitated oxide. Very small amounts of impurity ions, particularly other rare-earth ions, decrease the efficiency of this phosphor. Ce " is one of the most troublesome ions because it competes for the uv absorption and should be present at no more than about one part per million. Once purified, if not already coprecipitated, the oxides are dissolved in hydrochloric or nitric acid and then precipitated with oxaflc acid. This precipitate is then calcined, and fired at around 800°C to decompose the oxalate and form the oxide. EinaHy the oxide is fired usually in air at temperatures of 1500—1550°C in order to produce a good crystal stmcture and an efficient phosphor. This phosphor does not need to be further processed but may be milled for particle size control and/or screened to remove agglomerates which later show up as dark specks in the coating. 

Extra-Fine Precipitated Hydroxide. Very fine (< 1 /im-diameter) particle size hydroxide is produced by precipitation under carefully controlled conditions using specially prepared hydroxide seed. Precipitation is usually carried out at low (30 —40°C) temperatures causing massive nucleation of fine, uniform hydroxide particles (Fig. 5). Tray or tumiel Ape dry ers are used to dry the thorouglily washed filter cake to a granular product wliich is easily pulverized to obtain the fine hydroxide. Alternatively, the washed product is spray dried. Precipitation from an organic-free aluniinate Hquor, such as that obtained from the soda—sinter process, fields a very wliite product. Tlie fine precipitated hydroxide is used by the paper and plastic industries as fillers. 

The pore size, the pore-size distribution, and the surface area of organic polymeric supports can be controlled easily during production by precipitation processes that take place during the conversion of liquid microdroplets to solid microbeads. For example, polystyrene beads produced without cross-linked agents or diluent are nonporous or contain very small pores. However, by using bigb divinylbenzene (DVB) concentrations and monomer diluents, polymer beads with wide porosities and pore sizes can be produced, depending on the proportion of DVB and monomer diluent. Control of porosity by means of monomer diluent has been extensively studied for polystyrene (3-6) and polymethacrylate (7-10). 

It should be clear, then, that the precipitation process needs to be controlled carefully in order to produce a material composed of particles of a desired configuration. Both Ostwald riping and sintering can be utilized to obtain a particle of desired size, dimensions and particle habit. Industrial technologists have taken advantage of these particle forming and altering... 

In 1956 Gerhard Kolbe (1) published the first results that showed that spherical silica particles could be precipitated from tetraethoxysilane in alcohol solutions when ammonia was present as the catalyzing base. Several years later, in 1968, StOber, Fink, and Bohn (2) continued in this research area and published the frequently cited original article for the preparation of monodispersed silica particles form alkoxide solutions. StOber et al. improved the precipitation process and described the formation of exceptionally monodispersed silica particles. The final particle size could be controlled over a wide range from about 50 nm to 1 1/2 p,m. Variations of the particle size could be achieved by different means, e.g., temperature, water and ammonia concentration, type of alcohol (solvent), TEOS (tetraethoxysilane) concentration, or mixing conditions. 

Although it is difficult to precisely explain the phenomena illustrated in Figs. 15.3 and 15.4 at present, the information contained in these figures is helpful for further analysis and investigation on the mechanism and regularities of the reaction-precipitation process, and for searching for a possible method for size-control of the product. 

Cadmium pigments have been manufactured by both a direct calcination process and a precipitation-calcination process. In the first instance, a mixture of cadmium carbonate and sulfur (and zinc oxide and selenium if the hue to be produced requires their addition) is calcined at 520-600°C for 1-2 h. This direct calcination process is complicated by the volatility of cadmium oxide and selenium, both of which are toxic and require special handling. In the precipitation process, an alkali sulfide solution is added to a solution of cadmium and (in the case of green-shade yellows) zinc salts or to a solution of cadmium and (in the case of deep oranges, reds, and maroon) selenium metal to precipitate the appropriate compound. The precipitate is washed, dried, and calcined at 600-700°C in an inert or reducing atmosphere to convert the precipitated cubic structure to a more stable wurtzite crystal. The calcination conditions control particle size, which ranges from 0.2 to 1.0pm. 

Particle size control may also be desirable to facilitate solids handling during formulation. Solids produced by uncontrolled crystallization or precipitation processes can have a broad size distribution that can result in poor flow properties or tendency to segregate. The particle size of APIs can also impact efficiency of blending with excipients, compressibility, flow/ suspension behavior, and compaction performance in downstream equipment. Small particle sizes may be important for controlling dose uniformity in the final formulation, especially for low doses. ... 

Precipitation is carried out by a controlled mixing of the reactants in order to obtain a supersaturated solution from which nucleation takes place. Amorphous primary particles are formed that later crystallise into desired phases and in parallel agglomerate to larger secondary particles. Precipitation processes need in line pH meters and possibilities for automatic particle size distribution analysis coupled to the ageing vessel. 

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