Removal of thermal stable salts from organic solvents

• US 9,427,696 B2
• Filed: 01/29/2011
• Issued: 08/30/2016
• Est. Priority Date: 02/26/2010
• Status: Active Grant

• Current Assignee: Thyssenkrupp Uhde GmbH (Thyssenkrupp AG)
• Original Assignee: Thyssenkrupp Uhde GmbH (Thyssenkrupp AG)
• Inventors: Menzel, Johannes
• Primary Examiner(s): Robinson, Renee E
• Assistant Examiner(s): PILCHER, JONATHAN L
• Application Number:
  US13/580,904
• Publication Number:
  US 20130098245A1
• Time in Patent Office: 2,040 Days
• US Class Current: 1/1
• CPC Class Codes: B01D 1/14 with heated gases or vapours or liquids in contact with the liquid
• CPC Class Codes: B01D 2252/204 Amines
• CPC Class Codes: B01D 3/14 Fractional distillation or use of a fractionation or rectification column
• CPC Class Codes: B01D 3/143 by two or more of a fractionation, separation or rectification step
• CPC Class Codes: B01D 3/148 in combination with at least one evaporator
• CPC Class Codes: B01D 3/38 Steam distillation
• CPC Class Codes: B01D 53/1425 Regeneration of liquid absorbents

Abstract

Process for removal of salts thermally non-regenerable in a temperature range from 0° C. to 200° C., from organic solvents in an aqueous solution by evaporation, the normal boiling point of organic solvents being higher than that of water, and by enriching the organic constituents existing in the solvent as well as the heat stable salts existing therein in a liquid phase forming by evaporation of water and a portion of the organic constituents of a first vessel, and discharging an evolving vaporous phase from the first vessel. In particular, the liquid phase formed in the first vessel is passed into a second vessel, water in vaporous and/or liquid form being passed into the second vessel, water and another portion of the organic constituents contained in the solvent being evaporated and forming a vaporous phase which is discharged from the second vessel, the heat stable salts being enriched in concentration in the liquid phase forming in the second vessel, and wherein a partial stream of the liquid phase formed in the second vessel is discharged from the second vessel.

Claims

1. A process for removal of heat stable salts thermally non-regenerable in a temperature range from 0°

C. to 200°

C. from organic solvents in an aqueous solution by evaporation comprising steps of;

(a) placing an aqueous solution containing organic solvents with a normal boiling point being higher than that of water and heat stable salts forming a liquid phase into a first vessel and evaporating water in the first vessel,

(b) passing the liquid phase containing the organic solvents and the heat stable salts from the first vessel into a second vessel,

(c) passing water in vaporous form, liquid form, or both into the second vessel,

(d) evaporating water and a portion of the organic solvents as a vaporous phase and discharging the vaporous phase from the second vessel,

(e) enriching the heat stable salts in concentration in a remaining liquid phase of the second vessel, and,

(f) discharging a partial stream of the remaining liquid phase from the second vessel.

2. The process according to claim 1 further comprising steps of determining a concentration of the heat stable salts of the liquid phase formed in the first vessel, and passing the liquid phase of the first vessel into the second vessel as soon as the concentration of the heat stable salts of the liquid phase to be carried over has reached a maximally admissible concentration at which the heat stable salts are soluble in the liquid phase.

3. The process according to claim 2 further comprising steps of passing the liquid phase of the first vessel into the second vessel as soon as the concentration of the heat stable salts in the liquid phase is 5 to 35% by wt., 5 to 25% by wt., 5 to 15% by wt., or 8 to 12% by wt.

4. The process according to claim 1 further comprising steps of determining the salt concentration of the liquid phase formed in the second vessel, and discharging a partial stream of the liquid phase from the second vessel as soon as the concentration of the heat stable salts of the liquid phase to be discharged has reached a maximally admissible concentration at which the heat stable salts are soluble in the liquid phase.

5. The process according to claim 4 further comprising a step of discharging a partial stream of the liquid phase from the second vessel as soon as the concentration of the heat stable salts in the liquid phase is 25 to 65% by wt., 40 to 65% by wt., 45 to 65% by wt., or 55 to 65% by wt.

6. The process according to claim 1 further comprising a step of externally heating, cooling, or both the first vessel, the second vessel, or both.

7. The process according to claim 1, wherein step (c) is carried out before step (b).

8. The process according to claim 1 further comprising a step of producing a concentrated salt solution depleted in organic constituents as wastewater that encompasses the liquid phase formed in the second vessel.

9. The process according to claim 1 further comprising a step of supplying a partial stream of a main circulating stream of an industrial plant encompassing organic solvent(s) burdened with heat stable salts to the first vessel.

10. The process according to claim 1 further comprising a step of returning the vaporous phases of the first vessel, the second vessel, or both formed by evaporation into a main circulating stream of an industrial plant.

11. The process according to claim 1 further comprising steps of:

(h) continuously passing the liquid phase formed in the first vessel into the second vessel,

(i) continuously passing water in vaporous form, liquid form, or both into the second vessel,

(j) controlling supply of heat, discharge of heat, or both,

(k) continuously evaporating water and portions of the organic solvents contained as a vaporous phase,

(l) discharging the vaporous phase from the second vessel,

(m) enriching the heat stable salts in concentration in the liquid phase forming in the second vessel,

(n) continuously discharging a partial stream of the liquid phase formed in the second vessel from the second vessel as a wastewater stream which encompasses a concentrated salt solution depleted in the organic solvents, and

(o) returning vaporous phases of the first vessel, the second vessel, or both which are formed by evaporation into a main process stream of an industrial plant.

12. The process according to claim 1 further comprising a step of supplying a strong base to the first vessel, the second vessel, or both.

13. The process according to claim 1 further comprising a step of removing CO₂, H₂S, HCN, mercaptans, or a combination thereof from flue gases.