Process for oxidizing one or more thiol compounds and subsequent separation in a single vessel
US-10435362-B2 · Oct 8, 2019 · US
US10780398B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10780398-B2 |
| Application number | US-201815907388-A |
| Country | US |
| Kind code | B2 |
| Filing date | Feb 28, 2018 |
| Priority date | Mar 1, 2017 |
| Publication date | Sep 22, 2020 |
| Grant date | Sep 22, 2020 |
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The present invention relates to the field of extraction of sulphur-containing compounds such as mercaptans, COS, H 2 S or CS 2 from a hydrocarbon cut. This selective extraction is carried out by bringing the hydrocarbon cut in the liquid phase into contact with an alkaline solution, for example caustic soda. The process in accordance with the invention is an improved process for the regeneration of alkaline solution which can be used to reduce the quantity of alkaline solution necessary in the regeneration section.
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The invention claimed is: 1. A process for the regeneration of a spent alkaline solution from a unit for the extraction of sulphur-containing compounds from a hydrocarbon cut, comprising: a) sending the spent alkaline solution to an oxidation reactor ( 4 ) in which it is brought into contact with an oxidizing agent ( 5 ) and a catalyst ( 3 ), and optionally with a hydrocarbon cut, said spent alkaline solution having been heated to a temperature in the range of 40° C. to 50° C., and in which the rise in temperature is controlled by cooling by using a cooled partially regenerated alkaline solution, b) sending effluents from the oxidation reactor ( 4 ) to a separator ( 8 ) from which a hydrocarbon phase which is rich in disulphides ( 10 ) and a partially regenerated alkaline solution ( 11 ) are extracted, and c) cooling the partially regenerated alkaline solution ( 11 ) obtained from step b) to a temperature of 45° C. or less to obtain the cooled partially regenerated alkaline solution, wherein the cooled partially regenerated alkaline solution is supplied directly to said oxidation reactor at one or more points. 2. The process for the regeneration of a spent alkaline solution from a unit for the extraction of sulphur-containing compounds from a hydrocarbon cut as claimed in claim 1 , further comprising: d) dividing the cooled partially regenerated alkaline solution ( 15 ) obtained from c) into two streams: a first stream ( 22 a ) is sent to the oxidation reactor ( 4 ) and serves as the cooled partially regenerated alkaline solution supplied directly to said oxidation reactor, and a second stream ( 22 b ). 3. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , further comprising adding fresh alkaline solution to the partially regenerated alkaline solution. 4. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the one or more points for the introduction of the cooled partially regenerated alkaline solution into the oxidation reactor ( 4 ) are provided with a distribution means or a mixing means. 5. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the one or more points for the introduction of the cooled partially regenerated alkaline solution into the oxidation reactor ( 4 ) are positioned in a manner such as to allow the rise in temperature of said oxidation reactor to be controlled. 6. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the catalyst in the oxidation reactor ( 4 ) is a cobalt or vanadium phthalocyanin catalyst. 7. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the catalyst in the oxidation reactor is added to the alkaline solution at an inlet to the oxidation reactor in a manner such as to obtain a concentration of catalyst in the alkaline solution in the range of 10 to 1000 ppm by weight. 8. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the oxidation reactor ( 4 ) further comprises a supplemental cooling means ( 23 ). 9. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the cooled partially regenerated alkaline solution ( 15 ) is further cooled by at least 5° C. before being returned to the oxidation reactor ( 4 ). 10. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the hydrocarbon cut treated in the unit for extraction of sulphur-containing compounds comprises methane or kerosene. 11. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the one or more points for the introduction of the cooled partially regenerated alkaline solution into the oxidation reactor ( 4 ) are provided with a distributor or a mixer; and/or the oxidation reactor ( 4 ) further comprises a supplemental cooler ( 23 ); and/or the cooling of the partially regenerated alkaline solution ( 11 ) obtained from the separator is by a heat exchanger. 12. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the catalyst in the oxidation reactor is added to the alkaline solution at an inlet to the oxidation reactor in a manner such as to obtain a concentration of catalyst in the alkaline solution in the range of 10 to 500 ppm by weight. 13. The process for the regeneration of a spent alkaline solution as claimed in claim 1 , in which the rise in temperature in a) is controlled by cooling by the cooled partially regenerated alkaline solution having a temperature of 35° C. or less. 14. A facility for the regeneration of a spent alkaline solution from a unit for the extraction of sulphur-containing compounds from a hydrocarbon cut, comprising: heating equipment ( 2 ) for heating the spent alkaline solution before it is introduced into the oxidation reactor to a temperature of 40° C. to 50° C., an oxidation reactor ( 4 ) in which the spent alkaline solution is brought into contact with an oxidizing agent ( 5 ) and a catalyst ( 3 ), a separator ( 8 ) supplied with an effluent obtained from the oxidation reactor ( 4 ), from which a hydrocarbon phase which is rich in disulphides ( 10 ) and a partially regenerated alkaline solution are extracted, and a cooling means ( 14 ) for cooling the partially regenerated alkaline solution ( 11 ) obtained from the separator to a temperature of 45° C. or less forming a cooled partially regenerated alkaline solution, a conduit for injecting a portion of the cooled partially regenerated alkaline solution directly into the oxidation reactor ( 4 ) at one or more points, which cools to control a rise in the temperature of said reactor. 15. The facility for the regeneration of a spent alkaline solution as claimed in claim 14 , further comprising a fresh alkaline solution supply. 16. The facility for the regeneration of a spent alkaline solution in claim 14 , in which the conduit for injecting the excess alkaline solution directly into the oxidation reactor ( 4 ) is supplied with the cooled partially regenerated solution ( 22 a ) obtained by dividing the cooled partially regenerated alkaline solution ( 15 ) into two streams: a first stream ( 22 a ) which is the cooled partially regenerated alkaline solution returned to the oxidation reactor ( 4 ), and a second stream ( 22 b ). 17. The facility for the regeneration of a spent alkaline solution as claimed in claim 16 , in which a supplemental cooling means is present to cool the cooled partially regenerated alkaline solution to a temperature which is at least 5° C. lower than that of the cooled partially regenerated alkaline solution ( 15 ). 18. The facility for the regeneration of a spent alkaline solution as claimed in claim 16 , in which a supplemental heat exchanger or circulating reflux or jacket around the reactor is present. 19. The facility for the regeneration of a spent alkaline solution as claimed in claim 14 , in which the oxidation reactor ( 4 ) comprises a supplemental cooling means ( 23 ). 20. A process for the regeneration of a spent alkaline solution from a unit for the extraction of sulphur-containing compounds from a hydrocarbon cut, comprising: a) sending the spent alkaline solution to an oxidation reactor ( 4 ) in which it is brought into contact with an oxidizing agent ( 5 ) and a catalyst ( 3 ), and optionally with a hydrocarbon cut, said spent alkaline solution having been heated to a temperature in t
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