Semi-Continuous Crystallization Method and Apparatus

Abstract

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.

Claims

1-14. (canceled)

15. 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, comprising the steps of: (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, (g) melting the crystal layer to obtain the separated and purified substance, wherein after step (c) and before step (g) the following steps are carried out: (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 and (f) optionally carrying out a sweating stage and removing a sweating residue.

16. The process in accordance with claim 15, wherein in step (c) 1 to 20% by volume of the mother liquid is removed from the crystallization zone.

17. The process in accordance with claim 15, wherein 1 to 99% by volume of the portion of the mother liquid removed in step (c) is recirculated into the crystallization zone.

18. The process in accordance with claim 15, wherein the liquid feed portion is added in step (d) so that only laminar flow occurs in the liquid contained in the crystallization zone.

19. The process in accordance with claim 15, wherein the steps (c) to (e) are repeated for one or more times.

20. The process in accordance with claim 15, wherein the crystal density after step (e) is at least 20% by volume.

21. The process in accordance with claim 15, wherein the crystallization is carried out in a static crystallizer.

22. The process in accordance with claim 15, wherein the at least one cooled surface is arranged at least substantially vertical in the crystallization zone.

23. The process in accordance with claim 15, wherein the separated and purified substance of step (g) is further purified in a separation process, which is a melt crystallization process.

24. The process in accordance with claim 15, wherein the initial concentration of the substance to be separated and purified in the liquid feed mixture is less than 50% by weight.

25. The process in accordance with claim 15, wherein the liquid feed mixture is derived from a biomass process comprising a fermentation step.

26. The process in accordance with claim 15, wherein the substance to be separated and purified from the liquid feed mixture is selected from the group consisting of xylene, durene, caprolactam, lactic acid, sorbitol, sorbitan, isosorbide, phytosterol, fatty acids, fatty acid esters, paraffins, bisphenols and any arbitrary combination of two or more of the aforementioned substances.

27. A plant for the separation and purification of a substance in a concentration of less than 50% by weight, embodied to be suitable for the process in accordance with claim 15, 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, wherein the circulation loop is embodied to provide at least a partial recirculation between the liquid outlet collection system and the liquid inlet distribution system.

28. The static crystallization apparatus in accordance with claim 27, wherein the static crystallization apparatus additionally comprises an overflow prevention system embodied so as to maintain a desired liquid level in the vessel.

Description

[0060] The invention will be explained in more detail hereinafter with reference to the drawings, in which:

[0061] FIG. 1 schematically shows a crystallization apparatus according to a first embodiment, which is embodied to be suitable for the process in accordance with the present invention, in vertical cross-section,

[0062] FIG. 2 schematically shows the crystallization apparatus of FIG. 1 in horizontal cross-section and

[0063] FIG. 3 schematically shows a crystallization apparatus according to a second embodiment, which is embodied to be suitable for the process in accordance with the present invention, in horizontal cross-section.

[0064] FIGS. 1 and 2 schematically show a crystallization apparatus 10 according to one embodiment of the invention in vertical and horizontal cross-section. The crystallization apparatus 10 comprises a plurality of vertically arranged cooled plates 12, onto which the substance to be separated and purified deposit during the operation of the crystallization apparatus 10. A liquid inlet distribution system 14 is arranged at the upper part of the crystallization apparatus 10 above the cooled plates 12 and embodied so as to distribute the mother liquid substantially homogeneously over the horizontal cross-section of the crystallization apparatus 10. Moreover, the crystallization apparatus 10 comprises on both sides in the bottom part each a liquid outlet collection system 16 embodied so as to collect liquid homogeneously along both sides, which is then withdrawn from the crystallization apparatus 10 via the outlet line 18 or alternatively recirculated via circulation loop 22 by means of pump 24.

[0065] The crystallization apparatus 10 of FIG. 3 is similar to that shown in FIGS. 1 and 2, but comprises on both sides each four outlet lines 18, 18, 18, 18, which merge into one central outlet line 20. This effects an even more homogenous flow field than that obtained with the crystallization apparatus 10 shown in FIGS. 1 and 2.

REFERENCE NUMERALS

[0066] 10 Crystallization apparatus [0067] 12 Cooled plates [0068] 14 Liquid inlet distribution system [0069] 16 Liquid outlet collection system [0070] 18, 18, 18, 18 Outlet line [0071] 20 Central outlet line [0072] 22 Circulation loop [0073] 24 Pump