Semi-continuous crystallization method and apparatus
A process for the separation of a substance from a liquid feed mixture and for the purification of the substance by fractional layer crystallization, wherein the liquid feed mixture comprises the substance to be separated and purified in a concentration of less than 50% by weight, which comprises the subsequent steps in the given order: (a) feeding the liquid feed mixture into a crystallization zone, in which at least one surface is provided, so that at least a part of the surface contacts the liquid feed mixture, (b) cooling the at least one surface of the crystallization zone to a temperature below the equilibrium freezing temperature of the liquid feed mixture so that a crystal layer enriched in the substance to be separated and purified is deposited on the at least one cooled surface, whereby a mother liquid having a lower concentration of the substance to be separated and purified than the liquid feed mixture is formed from the liquid feed mixture, (c) removing at least a portion of the mother liquid from the crystallization zone, (d) adding a further portion of liquid feed mixture into the crystallization zone, (e) allowing further deposition of a crystal layer enriched in the substance to be separated and purified to take place on the at least one cooled surface, (f) optionally carrying out a sweating stage and removing a sweating residue and (g) melting the crystal layer to obtain the separated and purified substance.
1. A plant for the separation and purification of a substance in a concentration of less than 50% by weight, the plant comprising:
(a) a source of the liquid feed mixture comprising the substance to be separated and purified in a concentration of less than 50% by weight,
(b) a static crystallization apparatus,
wherein the static crystallization apparatus comprises:
(c) a vessel,
(d) a substantially vertically-disposed cooled surface,
(e) optionally a crystal-retention system for retaining crystals within the vessel,
(f) a liquid inlet distribution system embodied so as to distribute a liquid substantially homogeneously over a horizontal cross-section of the vessel and
(g) a liquid outlet collection system embodied so as to collect liquid homogeneously along an edge between a substantially vertical wall and a bottom of the vessel,
wherein the static crystallization apparatus additionally comprises a circulation loop connected directly between the liquid outlet collection system and the liquid inlet distribution system, wherein the circulation loop is embodied to provide at least a partial recirculation directly between the liquid outlet collection system and the liquid inlet distribution system.
2. The plant of claim 1 , wherein the static crystallization apparatus additionally comprises an overflow prevention system embodied so as to maintain a desired liquid level in the vessel.