Phase separation by gas evolution

• US 5,360,554 A
• Filed: 02/07/1994
• Issued: 11/01/1994
• Est. Priority Date: 02/07/1994
• Status: Expired due to Fees

• Current Assignee: Parhelion Incorporated
• Original Assignee: Parhelion Incorporated
• Inventors: Sloan, Jack C., Lurie, Walter, Ferramosca, Adrian C.
• Primary Examiner(s): Dawson, Robert A.
• Assistant Examiner(s): KIM, SUN U
• Application Number:
  US08/192,725
• Time in Patent Office: 267 Days
• Field of Search: 210/742, 210/768, 210/774, 210/805, 210/808, 62/532, 62/533, 62/535, 62/537, 62/542, 62/48.2
• US Class Current: 210/768
• CPC Class Codes: B01D 9/04 concentrating solutions by removing frozen solvent therefrom
• CPC Class Codes: C02F 1/22 by freezing

Abstract

A solute can be separated from a solute/solvent solution by dissolving a gas-forming material into said solution and then adjusting the temperature, pressure and solute concentration of the resulting solution such that a Joule-Thompson free expansion of the gas-forming material released from the solution will produce a three-phase separation of the components of said solution.

Claims

1. A process for separating a solute from a solvent which together constitute a solute/solvent solution starting material having an initial solute concentration, said process comprising:

(1) dissolving a gas-forming material into the solute/solvent solution to produce a dissolved gas/solute/solvent solution;

(2) lowering the temperature of the dissolved gas/solute/solvent solution to a jumping off temperature to produce a liquid having a solute concentration and temperature that are such that a release of a nominal high pressure on the solution to a nominal low pressure results in evaporation of a major portion of the gas-forming material as well as evaporation of a minor portion of the solvent as vapors that take their heats of vaporization in amounts such that the temperature of an entire mass of the solution is lowered to a temperature that approximates the triple point temperature of said solution;

(3) placing the solution in a pressure vessel;

(4) bringing the solution in the pressure vessel to the nominal high pressure;

(5) rapidly releasing the nominal high pressure and thereby allowing a major portion of the gas-forming material and a minor portion of the solvent to form vapors that undergo a Joule-Thompson free expansion into a closed second vessel having a nominal low pressure and thereby obtaining three phases of resultant materials that each have a temperature approximating the triple point temperature of the solution and wherein said three phases of resultant materials comprise a gas-phase product containing the gas-forming material originally dissolved in the solute/solvent solution starting material and vapors of the solvent, a portion of which flow into the second vessel, a liquid-phase product having a solute concentration greater than the initial concentration of the solute/solvent solution starting material and a solid-phase form of the solvent;

(6) collecting at least one of the three phases of resultant materials as a product of the process;

(7) collecting at least a portion of the gas-phase product for reuse in the process; and

(8) recycling at least one of the three phases of resultant materials back into an earlier stage of the process via a heat exchanger that heat exchanges a relatively cold resultant material with a relatively warm solute/solvent solution.

2. The process of claim 1 wherein the gas-forming material is liquid carbon dioxide.

3. The process of claim 1 wherein the gas-forming material is gaseous carbon dioxide.

4. The process of claim 1 wherein the solution in the pressure vessel is a single-phase liquid.

5. The process of claim 1 wherein an additional portion of a gas-forming material is introduced into the solution while it is in the pressure vessel.

6. The process of claim 1 wherein the second vessel is under a pressure greater than atmospheric pressure, but less than the nominal high pressure, when it receives vapors resulting from the Joule-Thompson free expansion.

7. The process of claim 1 wherein the second vessel is under atmospheric pressure when it receives vapors resulting from the Joule-Thompson free expansion.

8. The process of claim 1 wherein the second vessel is under a vacuum pressure when it receives vapors resulting from the Joule-Thompson free expansion.

9. The process of claim 1 wherein the second vessel is under a vacuum pressure originally supplied by a jet eductor when said second vessel receives vapors resulting from the Joule-Thompson free expansion.

10. The process of claim 1 wherein the gas phase product in the second vessel is introduced into the solute/solvent solution by a suction action supplied by a jet eductor.

11. The process of claim 1 wherein an incoming portion of the solute/solvent solution liquid is heat exchanged against two or more cold materials created by a Joule-Thompson free expansion of the process, before said solution is delivered to the pressure vessel.

12. The process of claim 1 wherein the pressure vessel is a part of a battery of pressure vessels such that the pressure vessel can be filled while another pressure vessel is being emptied.

13. The process of claim 1 wherein the pressure vessel is connected to a second vessel that is also used by other pressure vessels to collect vapor products produced by Joule-Thompson free expansions performed in the other pressure vessels.

14. The process of claim 1 wherein the lowering of the temperature of the solute/solvent solution to a jumping off temperature is done in at least two stages and wherein the first stage involves heat exchanging said solution against an external heat sink.

15. The process of claim 1 wherein the lowering of the temperature of the solute/solvent solution to a jumping off temperature is done in at least two stages and wherein the first stage involves heat exchanging said solution against an external heat sink comprised of a body of water from which the initial solute/solvent solution is drawn.

16. The process of claim 1 wherein the solute/solvent solution starting material is seawater.

17. The process of claim 1 wherein the solute/solvent solution liquid is a potassium sulfate solution obtained as a by-product of a cement manufacturing process.

18. The process of claim 1 wherein the solute/solvent solution starting material is an aqueous solution containing dissolved minerals and the solid-phase product is ice that is thereafter melted and used in the production of a carbonated beverage.

19. The process of claim 1 wherein the solute/solvent solution starting material is a nonaqueous industrial waste fluid.

20. The process of claim 1 wherein the solute/solvent solution is a brine of nearly eutectic solute concentration from which magnesium carbonate is recovered.

21. The process of claim 1 wherein a quantity of the liquid phase product containing a solute concentration greater than the initial concentration of the solute/solvent solution starting material is recycled to an earlier stage of the process as a constant recycle quantity of said liquid-phase product.

22. The process of claim 1 wherein a liquid-phase product is subjected to a blow-down procedure and a product of said blow-down procedure is recycled back to an earlier stage of the process as a constant recycle quantity of said product.

23. The process of claim 1 wherein the liquid-phase product is separated into a constant recycle quantity and a remaining blow-down quantity comprised of the starting material total solute and a unsolidified liquid remainder of starting material solvent in proportions up to and approaching eutectic (solubility) composition of the starting material.

24. The process of claim 1 wherein the liquid product of the Joule-Thompson expansion is entirely returned to an inventory of starting material following separation of a solid phase of purified component originally present in excess of eutectic composition.

25. The process of claim 1 wherein the solid-phase product is not a solid-phase form of the solvent having a solute concentration substantially less than the initial concentration of the solute/solvent solution starting material, but rather, because of solute concentration, temperature and/or pressure adjustments to the solute/solvent solution, is a solid-phase product of substantially pure solid-phase solute that is precipitated from the liquid-phase product as a result of the Joule-Thompson free expansion.

26. A process for separating a solute from a solvent that together constitute a solute/solvent solution starting material having an initial solute concentration and an initial temperature, said process comprising:

(1) combining the solute/solvent solution with a constant recycle quantity of a liquid product of increased solute concentration obtained from a Joule-Thompson free expansion step of this process and used as a circulating inventory of said liquid product of increased solute concentration that is recycled in an amount adjusted to control a solute concentration of a combined solution comprised of a portion of the solute/solvent solution and a portion of the liquid product of increased solute concentration;

(2) dissolving into said combined solution a controlled amount of a gas-forming material that will constitute a vapor phase at a system low temperature and pressure state that exists after the Joule-Thompson free expansion step, to produce a gas-forming material/solute/solvent solution;

(3) removing at least a portion of the heat of condensation arising from dissolving vapors of the gas-forming material and solvent into the combined solution by means of heat exchange with an external heat sink;

(4) removing heat from the gas-forming material/solute/solvent solution by means of an internal heat exchange against at least one product of the Joule-Thompson free expansion to bring said solution to a temperature that approaches a jumping off temperature;

(5) placing the solution in a pressure vessel;

(6) bringing the solution in the pressure vessel to a nominal high pressure;

(7) rapidly releasing the nominal high pressure on the solution in the pressure vessel and thereby allowing a major portion of the gas-forming material and a minor portion of the solvent to form vapors that undergo a Joule-Thompson free expansion into a closed second vessel having a nominal low pressure and thereby obtaining three phases of resultant materials that each have a temperature approximating the triple point temperature of the solution and wherein said three phases of resultant materials comprise;

a gas-phase product containing the gas-forming material originally dissolved in the solute/solvent solution starting material and vapors of the solvent, a portion of which flow into the second vessel, a liquid-phase product having a solute concentration greater than the initial concentration of the solute/solvent solution starting material and a solid-phase form of the solvent;

(8) collecting at least a portion of the gas-phase product via a jet eductor for reuse in the process;

(9) collecting at least one of the three phases of resultant materials as a product of the process; and

(10) recycling the liquid product back into an earlier stage of the process via a heat exchanger that heat exchanges relatively cold liquid-phase product with relatively warm solute/solvent solution.

27. A process for separating a solute from a solvent that together constitute a solute/solvent solution starting material having an initial solute concentration and an initial temperature, said process comprising:

(1) combining the solute/solvent solution with a constant recycle quantity of a liquid product of increased solute concentration obtained from a Joule-Thompson free expansion step of this process and used as a circulating inventory of said liquid product of increased solute concentration that is recycled in an amount adjusted to control a solute concentration of a combined solution comprised of a portion of the solute/solvent solution and a portion of the liquid product of increased solute concentration;

(2) dissolving into said combined solution a controlled amount of a gas-forming material that will constitute a vapor phase at a system low temperature and pressure state that exists after the Joule-Thompson free expansion step, to produce a gas-forming material/solute/solvent solution;

(3) removing heat of condensation arising from dissolving vapors of the gas-forming material and solvent into the combined solution by means of heat exchange with an external heat sink;

(4) removing heat from the gas-forming material/solute/solvent solution by means of an internal heat exchange against at least one product of the Joule-Thompson free expansion to bring said solution to a temperature that approaches a jumping off temperature;

(5) placing the solution in a pressure vessel;

(6) bringing the solution in the pressure vessel to a nominal high pressure;

(7) rapidly releasing the nominal high pressure on the solution in the pressure vessel and thereby allowing a major portion of the gas-forming material and a minor portion of the solvent to form vapors that undergo a Joule-Thompson free expansion into a closed second vessel having a nominal low pressure and thereby obtaining three phases of resultant materials that each have a temperature approximating the triple point temperature of the solution and wherein said three phases of resultant materials comprise;

a gas-phase product containing the gas-forming material originally dissolved in the solute/solvent solution starting material and vapors of the solvent, a portion of which flow into the second vessel, a liquid-phase product having a solute concentration greater than the initial concentration of the solute/solvent solution starting material and a solid-phase product that does not have a solute concentration substantially less than the initial concentration of the solute/solvent solution starting material but rather, because of solute concentration, temperature and/or pressure adjustments to the liquid, is a solid-phase product of substantially pure solid-phase, solute that is precipitated from the liquid-phase product as a result of said Joule-Thompson free expansion;

(8) collecting at least a portion of the gas-phase product via a jet eductor for reuse in the process;

(9) collecting at least one of the three phases of resultant materials as a product of the process; and

(10) separating the liquid phase into a constant recycle quantity and a remaining "blow-down" quantity comprised of total solute of the starting material and unsolidified remaining solvent of the starting material in proportions up to and approaching the eutectic (solubility) proportion of the starting material solute/solvent solution.