# US 6,719,954 B2 · Multi-stage counter-current crystallization apparatus > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 6,719,954 B2 - Document ID: US6719954B2 - Status: Granted - Kind: B2 - Application number: 10/132,927 - Filed: 2002-04-25 - Published: 2002-10-31 - Granted: 2004-04-13 - Earliest claimed: 2001-04-27 - Assignees: Korporam B.V. - Inventors: Halbe Anne Jansen - Web page: https://patentgrep.com/patent/US6719954B2 ## CPC - B01D 9/0013: {by indirect heat exchange} - B01D 9/0059: {General arrangements of crystallisation plant, e.g. flow sheets} - Y10T 117/10: Apparatus - B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28) - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract A multi-stage counter-current crystallization apparatus for crystallizing and subsequently separating a component in pure form from a solution comprises a first concentration stage for forming crystals in the solution and a first crystallization vessel for further growth of the crystals to obtain a first crystal suspension mixture containing larger crystals and first separating means for separating the larger crystals from the first crystal suspension mixture to form a concentrated mother liquor. A second concentration stage forms crystals in the concentrated mother liquor solution and includes a second crystallization vessel for further growth of the crystals. A bypass conduit circulates the crystal suspension mixture in a crystal-growing vessel, and includes a filter for extracting part of the mother liquor solution from the crystal suspension mixture. ## Claims ### Claim 1 A multi-stage counter-current crystallization apparatus for crystallizing and subsequently separating a component in pure form from a solution, comprising a first concentration stage including: means for supplying the solution: first crystallization means including a heat exchanger for forming crystals in the solution; a first crystallization vessel for further growth of the crystals formed by the first crystallization means so as to obtain a first crystal suspension mixture containing larger crystals; first separating means for separating the larger crystals from the first crystal suspension mixture so as to obtain a first concentrated mother liquor solution; and at least one second concentration stage including: means for receiving the first concentrated mother liquor solution; second crystallization means including a heat exchanger for forming crystals in the first concentrated mother liquor solution; a second crystallization vessel for further growth of the crystals formed by the second crystallization means; and means for returning crystals from the second crystallization vessel to the first crystallization vessel, characterized in that the crystal-growing vessel of at least one concentration stage is provided with a bypass conduit arranged outside the crystal-growing vessel for circulating the crystal suspension mixture that is present in the crystal-growing vessel and wherein filter means are present in the bypass conduit for extracting at least part of the mother liquor solution from the crystal suspension mixture. ### Claim 2 (depends on 1) A crystallization apparatus according to claim 1 characterized in that the filter cleaning means includes a scraping element which is movable relative to the filter surface. ### Claim 3 An apparatus for separating crystals from a crystal suspension mixture composed of crystals and mother liquor solution, comprising: a fully closed cylinder and a piston which is movable therein, which piston bounds a washing column chamber inside the cylinder; at least one piston rod provided with a longitudinal bore, via which piston rod the piston is moved reciprocatingly in the cylinder by driving means; filter means connected to the piston at the side of the washing column chamber; a supply conduit, which is connected to the end of the piston rod that projects outside the cylinder, which conduit functions to supply the crystal suspension mixture to the washing column chamber through the longitudinal bore; a discharge conduit for discharging mother liquor solution from the washing column chamber after filtration through the filter; means arranged in the washing column chamber, near the closed side of the cylinder, for the controlled removal of an amount of crystals from the crystal bed that has been compacted in the washing column chamber by the piston; a circulation conduit arranged outside the cylinder, which is in communication with the washing column chamber via a connection for the discharge of the removed amount of crystals and via a connection for the supply of a washing liquid to the compacted crystal bed; and a conduit connected to the circulation conduit for discharging the removed crystals, which may or may not be in melted form, characterized in that means for creating a differential liquid pressure across the compacted crystal bed during operation are arranged in the circulation conduit. ### Claim 4 (depends on 3) A separating apparatus according to claim 3, characterized in that the pressure means consist of a restriction valve, which is incorporated in the circulation conduit between the discharge connection and the discharge conduit. ### Claim 5 (depends on 3) A separating apparatus according to claim 3, characterized in that the pressure means consist of an external pump. ### Claim 6 (depends on 3) A separating apparatus according to claim 3, characterized in that the pressure means comprises an expansion vessel connected to the circulation conduit for creating the differential liquid pressure by means of air pressure. ### Claim 7 (depends on 3) A separating apparatus according to claim 3 characterized in that the pressure means can be controlled. ### Claim 8 (depends on 7) A separating apparatus according to claim 7 characterized in that the pressure means can be controlled by means of a sensor which detects the position of the separation interface between the part of the crystal bed in which the washing liquid has displaced the mother liquor solution that is present between the crystals and the part of the crystal bed in which the mother liquor solution is still present between the crystals. ### Claim 9 (depends on 3) A separating apparatus according to claim 3 characterized in that the supply conduit for supplying the crystal suspension mixture is connected to the longitudinal bore of the piston rod by means of a flexible intermediate conduit. ### Claim 10 (depends on 3) A separating apparatus according to claim 3 characterized in that a plate member which moves along with the piston is fitted on the piston rod, which plate member divides the space defined by the piston and the piston rod side of the cylinder into a first filtrate chamber defined by the piston and the plate member and a second filtrate chamber defined by the plate member and the piston rod side of the cylinder and wherein the discharge conduit for filtered liquid extending from the second filtrate chamber includes a conduit which leading to the first filtrate chamber. ### Claim 11 (depends on 10) A separating apparatus according to claim 10, characterized in that said conduit and said discharge conduit can each be closed, for example by means of a valve. ### Claim 12 An apparatus for separating crystals crystal suspension mixture composed of crystals and mother liquor solution, comprising: a fully closed cylinder and a piston which is movable therein, which piston bounds a washing column chamber inside the cylinder; at least one piston rod provided with a longitudinal bore, via which piston rod the piston is moved reciprocatingly in the cylinder by driving means; filter means connected to the piston at the side of the washing column chamber; a supply conduit, which is connected to the end of the piston rod that projects outside the cylinder, which conduit functions to supply the crystal suspension mixture to the washing column chamber through the longitudinal bore; a discharge conduit for discharging mother liquor solution from the washing column chamber after filtration through the filter; means arranged in the washing column chamber, near the closed side of the cylinder for the controlled removal of an amount of crystals from the crystal bed that has been compacted in the washing column chamber by the piston; a circulation conduit arranged outside the cylinder, which is in communication with the washing column chamber via a connection for the discharge of the removed amount of crystals and via a connection for the supply of a washing liquid to the compacted crystal bed; and a conduit connected to the circulation conduit for discharging the removed crystals which may or may not be in melted form, characterized in that a plate member which moves along with the piston is fitted on the piston rod, which plate member divides the space defined by the piston and the piston rod side of the cylinder into a first filtrate chamber defined by the piston and the plate member and a second filtrate chamber defined by the plate member and the piston rod side of the cylinder and wherein the discharge conduit for filtered liquid extending from the second filtrate chamber includes a conduit which leading to the first filtrate chamber. ### Claim 13 (depends on 12) A separating apparatus according claim 12, characterized in that said conduit and said discharge conduit can each be closed, for example by means of a valve. ### Claim 14 A multi-stage counter-current crystallization apparatus for crystallizing and subsequently separating a component in pure form from a solution, comprising a first concentration stage including: means for supplying the solution: first crystallization means including a heat exchanger for forming crystals in the solution; a first crystallization vessel for further growth of the crystals formed by the first crystallization means so as to obtain a first crystal suspension mixture containing larger crystals; first separating means for separating the larger crystals from the first crystal suspension mixture so as to obtain a first concentrated mother liquor solution; and at least one second concentration stage including: means for receiving the first concentrated mother liquor solution; second crystallization means including a heat exchanger for forming crystals in the first concentrated mother liquor solution; a second crystallization vessel for further growth of the crystals formed by the second crystallization means; and means for returning crystals from the second crystallization vessel to the first crystallization vessel, characterized in that the crystal-growing vessel of at least one concentration stage is provided with a bypass conduit that forms part of the first separating means arranged outside the crystal-growing vessel for circulating the crystal suspension mixture that is present in the crystal-growing vessel and wherein filter means are present in the bypass conduit for extracting at least part of the mother liquor solution from the crystal suspension mixture. ### Claim 15 A multi-stage counter-current crystallization apparatus for crystallizing and subsequently separating a component in pure form from a solution, comprising a first concentration stage including: means for supplying the solution: first crystallization means including a heat exchanger for forming crystals in the solution; a first crystallization vessel for further growth of the crystals formed by the first crystallization means so as to obtain a first crystal suspension mixture containing larger crystals; first separating means for separating the larger crystals from the first crystal suspension mixture so as to obtain a first concentrated mother liquor solution; and at least one second concentration stage including: means for receiving the first concentrated mother liquor solution; second crystallization means including a heat exchanger for forming crystals in the first concentrated mother liquor solution; a second crystallization vessel for further growth of the crystals formed by the second crystallization means; and means for returning crystals from the second crystallization vessel to the first crystallization vessel, characterized in that the crystal-growing vessel of at least one concentration stage is provided with a bypass conduit arranged outside the crystal-growing vessel for circulating the crystal suspension mixture that is present in the crystal-growing vessel and wherein filter means are present in the bypass conduit for extracting at least part of the mother liquor solution from the crystal suspension mixture and wherein the crystal-free mother liquor solution can function as the supply solution for a further concentration stage. ### Claim 16 A multi-stage counter-current crystallization apparatus for crystallizing and subsequently separating a component in pure form from a solution, comprising a first concentration stage including: means for supplying the solution: first crystallization means including a heat exchanger for forming crystals in the solution; a first crystallization vessel for further growth of the crystals formed by the first crystallization means so as to obtain a first crystal suspension mixture containing larger crystals; first separating means for separating the larger crystals from the first crystal suspension mixture so as to obtain a first concentrated mother liquor solution; and at least one second concentration stage including: means for receiving the first concentrated mother liquor solution; second crystallization means including a heat exchanger for forming crystals in the first concentrated mother liquor solution; a second crystallization vessel for further growth of the crystals formed by the second crystallization means; and means for returning crystals from the second crystallization vessel to the first crystallization vessel, characterized in that the crystal-growing vessel of at least one concentration stage is provided with a bypass conduit arranged outside the crystal-growing vessel for circulating the crystal suspension mixture that is present in the crystal-growing vessel and wherein filter means are present in the bypass conduit for extracting at least part of the mother liquor solution from the crystal suspension mixture, and wherein the filter means includes a pressure vessel provided with a mixing element and a filter, which filter can be cleaned at its crystal suspension side. ### Claim 17 A multi-stage counter-current crystallization apparatus for crystallizing and subsequently separating a component in pure form from a solution, comprising a first concentration stage including: means for supplying the solution: crystallization means including a heat exchanger for forming crystals in the solution; a first crystallization vessel for further growth of the crystals formed by the first crystallization means so as to obtain a first crystal suspension mixture containing larger crystals; first separating means for separating the larger crystals from the first crystal suspension mixture so as to obtain a first concentrated mother liquor solution; and at least one second concentration stage including: means for receiving the first concentrated mother liquor solution; second crystallization means including a heat exchanger for forming crystals in the first concentrated mother liquor solution; a second crystallization vessel for further growth of the crystals formed by the second crystallization means; and means for returning crystals from the second crystallization vessel to the first crystallization vessel, characterized in that the crystal-growing vessel of at least one concentration stage is provided with a bypass conduit arranged outside the crystal-growing vessel and includes a circulation pump for circulating the crystal suspension mixture that is present in the crystal-growing vessel and wherein filter means are present in the bypass conduit for extracting at least part of the mother liquor solution from the crystal suspension mixture.