Method and apparatus for removing H.sub.2 S from a process gas and recovering sulfur

• US 5,122,351 A
• Filed: 12/20/1990
• Issued: 06/16/1992
• Est. Priority Date: 12/20/1990
• Status: Expired due to Term

• Current Assignee: Merichem Company
• Original Assignee: ARI Technologies, Inc.
• Inventors: Hardison, Leslie C.
• Primary Examiner(s): Straub, Gary P.
• Assistant Examiner(s): Vanoy, Timothy C.
• Application Number:
  US07/630,826
• Time in Patent Office: 544 Days
• Field of Search: 423/140, 423/141, 423/154, 423/242 A, 423/242 R, 423/236, 423/563, 423/567 A, 423/567 R, 423/578, 423/574 L, 423/220, 23/293 S, 201/12, 159/47.3
• US Class Current: 423/220
• CPC Class Codes: B01D 53/52 Hydrogen sulfide
• CPC Class Codes: C01B 17/05 by wet processes

Abstract

A catalytic polyvalent metal redox solution can be recovered and re-used in a catalytic polyvalent metal redox solution H₂ S-removal, sulfur production process by interposing a closed loop evaporator/condenser process and apparatus in the sulfur washing/filtering/recovery process and apparatus so that wash water used to purify the sulfur, and any polyvalent metal redox solution recovered from the sulfur melter are fed to an evaporator to concentrate the redox solution to a concentration capable of effective absorption of H₂ S, and the water evaporated in the evaporator is condensed as pure water for use in washing and/or filtering the recovered sulfur.

Claims

1. In a process for removing H₂ S and recovering sulfur from an H₂ S-containing process gas wherein the sulfur is melting in a sulfur melting device for separation of sulfur from water including:

intimately contacting the process gas with an aqueous polyvalent metal redox solution to absorb the H₂ S into the polyvalent metal redox solution, while simultaneously forming a reduced polyvalent metal redox solution, and subsequently oxidizing the reduced polyvalent metal redox solution sufficiently to regenerate the polyvalent metal redox solution, to form an oxygenated polyvalent metal redox solution capable of again absorbing H₂ S from said process gas, and to convert dissolved H₂ S to elemental sulfur, including the steps of;

separating the elemental sulfur from a majority of the polyvalent metal redox solution; and

washing the polyvalent metal redox solution from the sulfur with wash water;

the improvement comprising;

recovering the wash water and polyvalent metal redox solution removed from the sulfur for recycle to the process;

introducing the recovered wash water and the polyvalent metal redox solution removed from the sulfur to an evaporator, to evaporate sufficient wash water therefrom such that the polyvalent metal redox solution remaining in the evaporator is sufficiently concentrated for further absorption of H₂ S from the process gas, and removing the evaporated water from the evaporator;

condensing the evaporated water removed from the evaporator as pure condensed water;

using the pure condensed water as said wash water for washing the elemental sulfur;

recovering the polyvalent metal redox solution from the evaporator; and

recycling the recovered polyvalent metal redox solution for further absorption of H₂ S from the process gas.

2. A process as defined in claim 1 further including the steps of:

adding pure condensed wash water to the washed sulfur to form a slurry of washed sulfur, and water;

conveying the slurry to the sulfur melting device;

heating the slurry in the sulfur melting device to a temperature sufficient to melt the sulfur in the slurry to form a high purity molten sulfur, and a mixture of water and polyvalent metal redox solution, and

conveying the mixture of water and polyvalent metal redox solution to the evaporator for separate recovery of wash water and polyvalent metal redox solution, each for re-use in the process.

3. A process as defined in claim 2 wherein the sulfur is washed on a water-pervious conveyor belt including the step of applying vacuum suction under the belt for drawing the wash water and polyvalent metal redox solution through the sulfur.

4. A process as defined in claim 3 further including adding a portion of the water condensed from the evaporator to the washed sulfur to form the slurry of washed sulfur, water and polyvalent metal redox solution.

5. A process as defined in claim 1 wherein the polyvalent metal redox solution includes a redox catalyst, and wherein dissolved salts in the polyvalent metal redox solution are crystallized in the evaporator upon concentration of the redox solution as substantially catalyst free solid crystals.

6. A process as defined in claim 5 wherein the crystals formed in the evaporator comprise a metal sulfate.

7. A process as defined in claim 6 wherein the metal sulfate is principally sodium sulfate.

8. A process as defined in claim 5 wherein the crystals formed in the evaporator are principally potassium bicarbonate.

9. A process as defined in claim 7 further including the step of recovering the sodium sulfate.

10. In an apparatus for effecting mass transfer of a liquid reagent sequentially with two different gases in a separate mass transfer zone for each gas without permitting both gases to contact the same portion of the liquid simultaneously, including a first mass transfer zone for mass transfer between a liquid reagent and a sulfur-containing gas into the first mass transfer zone;

a second mass transfer zone in liquid, but not vapor, communication with the first mass transfer zone;

means for directing the liquid reagent from the first mass transfer zone into the second mass transfer zone;

means for directing a second gas into the second mass transfer zone for intimate contact and mass transfer therebetween;

including

means for recovering sulfur from the first or second mass transfer zone;

means for separating the recovered sulfur from the liquid reagent; and

means for washing the sulfur;

the improvement comprising;

means for recovering sulfur wash water and liquid reagent from the sulfur;

means for separating a portion of the sulfur wash water, in non-contaminated form, from the liquid reagent; and

means for recycling the separated wash water to the sulfur washing means.

11. In an apparatus as defined in claim 10 further including means for recycling the liquid reagent, after separation of a portion of the sulfur wash water, back to the first or second mass transfer zone for recover of sulfur.

12. In an apparatus as defined in claim 11 wherein the means for separating the recovered sulfur from the liquid reagent includes a liquid-porous filter, and wherein the means for recovering wash water and liquid reagent further includes liquid receiving means disposed on a down stream side of the filter for recovering wash water and liquid reagent.

13. In an apparatus as defined in claim 12 wherein the means for separating a portion of the sulfur wash water from the liquid reagent comprises an evaporator adapted to vaporize a portion of the wash water from the liquid reagent, and means to condense the evaporated wash water, outside of said evaporator, for use in washing said recovered sulfur.

14. In an apparatus as defined in claim 10 further including means for slurrying the recovered and washed sulfur with water.

15. In an apparatus as defined in claim 10 wherein the means for separating the recovered sulfur from the liquid reagent comprises a sulfur melting device.

16. In an apparatus as defined in claim 15 further including means for recovering water and liquid reagent from the sulfur melting device;

and means for introducing the recovered water and liquid reagent recovered from the melting device into the evaporator.

17. In an apparatus as defined in claim 12 wherein the means for recovering the sulfur wash water and liquid reagent includes a water-pervious conveyor belt including vacuum suction means disposed beneath the belt.

18. In a method as defined in claim 10 further including means for evaporating a portion of the wash water in the liquid reagent recovered from the sulfur washing means;

and means for condensing the evaporated water for use in washing the sulfur.