Countercurrent crystallization

In the Badger/Niro crystallization unit, the xylenes are fed to a single-stage crystallization section that uses continuous suspension crystallization. In this section, the paraxylene is purified with a single refrigerant compressor system, and the mother liquor rejected. The purified paraxylene is fed to a Niro wash column section where ultra-high-purity paraxylene is produced by countercurrent crystal washing. 

The heat requirement for continuous countercurrent crystallization can be approximated in a manner similar to (hat used for distillation ... 

Figure 90. Flow diagram of new process of physical refining by countercurrent crystallization...

The method to determine the required number of stages for countercurrent crystallization columns is described in [0.1] and [7.1]. 

Figure 4.20 Flow diagram of p-xylene production by countercurrent crystallization using the Phillips process...

Keulemans and van den Oever [36] demonstrated that countercurrent crystallization from the melt can be applied to any semisolid TAG mixture. The principle of their process requires a minimum of two stages, with recycle of the hard fraction from the second stage back to the beginning of the process. This results in a purer highest melting fraction once steady state is reached. 

The Phillips process is a two-stage crystallisation process that uses a pulsed column in the second stage to purify the crystals (79,80). In the pulsed column, countercurrent contact of the high purity PX Hquid with cold crystals results in displacement of impurities. In the first stage, a rotary filter is used. In both stages, scraped surface chillers are used. This process was commercialized in 1957, but no plants in operation as of 1996 use this technology. 

The softened seawater is fed with dry or slaked lime (dolime) to a reactor. After precipitation in the reactor, a flocculating agent is added and the slurry is pumped to a thickener where the precipitate settles. The spent seawater overflows the thickener and is returned to the sea. A portion of the thickener underflow is recirculated to the reactor to seed crystal growth and improve settling and filtering characteristics of the precipitate. The remainder of the thickener underflow is pumped to a countercurrent washing system. In this system the slurry is washed with freshwater to remove the soluble salts. The washed slurry is vacuum-filtered to produce a filter cake that contains about 50% Mg(OH)2. Typical dimensions for equipment used in the seawater process may be found in the Hterature (75). 

The product stream from the kilns is collected in storage bins. Black ash from the bins is fine-ground in a ball mill and fed to a leacher circuit, which is a system of stirred tanks, where it is dissolved in water and the muds are separated by countercurrent decantation. The solution from the decantation is passed through filter presses the muds are washed, centrifuged, and discarded. The filtered product, a saturated solution containing 12—13 wt % strontium sulfide, is sent to an agitation tank where soda ash is added to cause precipitation of strontium carbonate crystals ... 

Ma.nufa.cture. In a typical process, a solution of sodium carbonate is allowed to percolate downward through a series of absorption towers through which sulfur dioxide is passed countercurrently. The solution leaving the towers is chiefly sodium bisulfite of typically 27 wt % combined sulfur dioxide content. The solution is then mn into a stirred vessel where aqueous sodium carbonate or sodium hydroxide is added to the point where the bisulfite is fully converted to sulfite. The solution may be filtered if necessary to attain the required product grade. A pure grade of anhydrous sodium sulfite can then be crystallized above 40°C because the solubiUty decreases with increasing temperature. 

The ice crystals must be separated from the saline solution surrounding them, and washed with freshwater. This is accompHshed by a downward countercurrent flow of a small amount of freshwater through the ice slurry in the washer—melter unit. Keeping that unit at about 0°C limits the needed pressure rise by the compressor to only about 130—260 Pa, and an auxiUary refrigerator is often used to compensate for heat gains from the ambient and the compression. 

In the United States boric acid is produced by United States Borax Chemical Corp. in a 103,000 2 3 ric ton per year plant by reacting cmshed kernite ore with sulfuric acid. Coarse gangue is removed in rake classifiers and fine gangue is removed in thickeners. Boric acid is crystallised from strong hquor, nearly saturated in sodium sulfate, in continuous evaporative crystallizers, and the crystals are washed in a multistage countercurrent wash circuit. 

A suspension of crystals formed from the melt may be contacted by weU-mixed mother Hquor or the crystals may be moved countercurrently to hquor flow ia a vertical or horizontal column. In column crystallizers, crystals are moved ia a specific direction by gravity or rotating blades. The crystals are melted by the addition of heat when they reach a designated end of the crystallizer a portion of the melt is removed as product and the remainder is returned to the system to flow countercurrently to and to wash the product crystals. 

Performance information for the purification of p-xylene indicates that nearly 100 percent of the ciystals in the feed stream are removed as produc t. This suggests that the liquid which is refluxed from the melting section is effectively refrozen oy the countercurrent stream of subcooled crystals. A high-meltingproduct of 99.0 to 99.8 weight percent p-xylene has been obtained from a 65 weight percent p-xyfene feed. The major impurity was m-xylene. Figure 22-12 illustrates the column-cross-section-area-capacity relationship for various product purities. 

The hydrolysis is performed as a continuous countercurrent reaction in tall reaction towers (height 15-20 m, diameter 0.7 m). The reaction time amounts to 60-90 min. Reaction products are as well obtained an aqueous glycerin solution (about 15%) as on a mixture of raw fatty acids [50]. The free fatty acids are carefully distilled with the aid of a thin film evaporator (2-10 mbar, 260°C maximum) [51]. Crystallization and transwetting are additional methods for fractionation of fatty acid mixtures. 

The horizontal continuous Brodie melt crystallizer is basically an indirectly cooled crystallizer with an internal ribbon conveyor to transport crystals countercurrent to the liquid and a vertical purifier for final refining. Figure 20-8 describes the operation of a single tube unit and Fig. 20-13 depicts a multitube unit. The multitube design has been successfully commercialized for a number of organic chemicals. The Brodie purifier configuration requires careful control of process and equipment temperature differences to eliminate internal encrustations and is limited by the inherent equipment geometry to capacities of less than 15,000 tons per year per module. 

In the multistage process described on Fig. 20-14 feed enters one of several crystallizers installed in series. Crystals formed in each crystallizer are transferred to a hotter stage and the liquid collected in the clarified zone of the crystallizer is transferred to a colder stage and eventually discharged as residue. At the hot end, crystals are transferred to a vertical purifier where countercurrent washing is performed by pure, hot-product reflux. TSK refers to this multistage process as the countercurrent cooling crystallization (CCCC) process. In... 

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