Patent GB-760092-A (GB)
Title: Process for crystallization and recovery of hydrocarbons
IPC: B01D9/00
Filed: 1954-10-28
Abstract: <PICT:0760092/III/1> A continuous process for separating a hydrocarbon, which crystallizes below -50 DEG F., from a liquid mixture containing other hydrocarbons, comprises maintaining the liquid mixture in at least two bodies of slurry containing crystals in mother liquor at crystallization temperatures, continuously passing the liquid mixture into the first body of slurry, continuously passing mother liquor and crystals from the first body into the second body of slurry, continuously withdrawing, separating and collecting crystals and mother liquor from the second, or last, body of slurry and recycling at least a portion of the crystals, so separated, to the first of the bodies of slurry.  The process is described as applied to recovering paraxylene from a mixture containing paraxylene with metaxylene, orthoxylene, ethylbenzene, and small amounts of toluene, C9 aromatics and non-aromatics, but durene, cyclohexane, benzene, orthoxylene and naphthalene may be separated from mixtures according to examples.  A feed stock is fractionated in towers A and B to concentrate the paraxylene contained therein, passed by a line 13 through a drier 15, a heat-exchanger 17 and a prechiller 19, mixed with recycled slurry introduced by a line 24, and passed through a scraped surface chiller C into a first crystallization vessel F, where it is held for 30 minutes to three hours at -80 DEG F.  A slurry of paraxylene crystals and mother liquor is continuously withdrawn by a line 22, a part being recycled by line 24, and the remainder passed by a line 25 to a second crystallization vessel G where it is held for 30 minutes to 3 hours at -90 DEG F. to -105 DEG F.  A slurry of paraxylene crystals and mother liquor is continuously withdrawn by a line 26, a part being recycled by a line 28 through a scraped chiller D for admixture with the slurry in line 25, the remainder passing by a line 30 to a first basket centrifuge J.  A part of the filtrate from centrifuge J is passed by a line 31 to dilute the slurry in line 30, while the remainder passes to heat-exchanger 17.  A filter cake is discharged from centrifuge J by a shoot 38, melted in a drum 39, a portion of the melt being passed by a line 43 containing a heater 44 to shoot 38, the remainder passing by a line 45 through a prechiller 46, a line 47, a heat-exchanger E and a line 48 to a third crystallization vessel H, where it is held for 30 minutes at -10 DEG  to 20 DEG F.  A slurry is continuously withdrawn by lines 55 and 56, a portion optionally going by a line 53 to line 47, and the remainder passing to a second basket centrifuge K, from whence a filtrate is passed by a line 58 through a surge drum 59, and lines 60 and 62.  A portion of the filtrate in line 62 passes by a line 14 and is mixed with feed in line 13, while another portion passes by a line 63 to a manifold L having branches 49, 50, 51 and 52 to dilute the slurry entering vessel H.  A filter cake is removed from centrifuge K by a shoot 64 into a melting tank 65 and discharged as desired product by a line 69, a portion being passed by a line 70 containing a heater 71 to shoot 64 to melt the cake therein.  A product of 95 per cent paraxylene may be obtained by the process. The crystallization vessels, centrifuges and drums may be blanketed with an inert gas such as nitrogen or carbon dioxide. Modifications are described where vessels F or G have baffles to allow phase separation to take place so that a high concentration of paraxylene slurry may be maintained therein.  Other modifications have vessels F or G fitted with rotary filters and draw-off lines also to allow high concentrations of paraxylene slurry to be maintained in the crystallization vessels. In a further modification crystallization vessel H is not used, the filter cake from centrifuge J being partially melted and the slurry so obtained passed to centrifuge K where filtrate is obtained and mixed with filter cake from centrifuge J.