Method for producing ultra-pure bis(chlorosulfonyl)imide
US-2024391774-A1 · Nov 28, 2024 · US
US10669232B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10669232-B2 |
| Application number | US-201816485464-A |
| Country | US |
| Kind code | B2 |
| Filing date | May 8, 2018 |
| Priority date | May 11, 2017 |
| Publication date | Jun 2, 2020 |
| Grant date | Jun 2, 2020 |
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Aspects of the invention relate to systems and processes for recovering methanesulfonic acid, in a purified form, from a composition additionally including sulfur trioxide. In accordance with one aspect, the invention provides a process that includes separating a feed stream comprised of hydrocarbons, methanesulfonic acid, sulfur trioxide, and optionally sulfuric acid to produce a light stream comprised of hydrocarbons and a heavy stream comprised of methanesulfonic acid and sulfur trioxide; contacting (e.g., by mixing) the heavy stream with a reactive additive capable of reacting with sulfur trioxide, under conditions effective to cause reaction of the reactive additive with the sulfur trioxide to produce a heavy reaction product having a boiling point higher than the boiling point of methanesulfonic acid; and separating the heavy stream using a distillation column to produce a distillate stream consisting essentially of methanesulfonic acid and a bottoms stream comprising the heavy reaction product.
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The invention claimed is: 1. A process for recovering anhydrous methanesulfonic acid, in a purified form, from a feed stream comprised of hydrocarbon, methanesulfonic acid and sulfur trioxide comprising: separating the feed stream to produce a light stream comprised of hydrocarbons and a heavy stream comprised of methanesulfonic acid and sulfur trioxide; contacting the heavy stream with a reactive additive capable of reacting with sulfur trioxide under conditions effective to cause reaction of the reactive additive with the sulfur trioxide to produce a heavy reaction product having a boiling point higher than the boiling point of sulfur trioxide; and separating the heavy stream using a distillation column to produce a distillate stream consisting essentially of methanesulfonic acid and a bottoms stream comprising the heavy reaction product. 2. The process of claim 1 , wherein separating the heavy stream further comprises recovering a stream consisting essentially of hydrocarbons using a vapor-liquid separator. 3. The process of claim 1 , wherein the step of contacting the heavy stream with the reactive additive further comprises mixing the reactive additive and the heavy stream using at least one mixer. 4. The process of claim 1 , further comprising reacting sulfur trioxide with methane using a reactor to produce the feed stream comprising hydrocarbons, methanesulfonic acid, sulfur trioxide, and optionally sulfuric acid. 5. The process of claim 4 , wherein a peroxide initiator is fed to the reactor. 6. The process of claim 1 , wherein the feed stream further comprises sulfuric acid. 7. The process of claim 1 , wherein the reactive additive is water. 8. The process of claim 1 , wherein the reactive additive is at least one compound selected from the group consisting of alcohols, ethers, alkyl benzenes, and alpha olefins. 9. The process of claim 1 , wherein the distillation column is operated at a pressure of 0,22 mbar to 50 mbar. 10. The process of claim 9 , wherein the distillation column is operated at a pressure of 4 mbar to 30 mbar. 11. The process of claim 10 , wherein the distillation column is operated at a pressure of 6 mbar to 14 mbar. 12. The process of claim 11 , wherein the distillation column is operated at a pressure of 8 mbar to 12 mbar. 13. The process of claim 1 , wherein the distillate stream comprises not more than 500 ppm of sulfuric acid or an equivalent thereof. 14. The process of claim 13 , wherein the distillate stream comprises not more than 400 ppm of sulfuric acid or an equivalent thereof. 15. The process of claim 14 , wherein the distillate stream comprises not more than 300 ppm of sulfuric acid or an equivalent thereof. 16. The process of claim 15 , wherein the distillate stream comprises not more than 150 ppm of sulfuric acid or an equivalent thereof. 17. The process of claim 1 , wherein the distillate stream consists of methanesulfonic acid and less than 50 ppm of impurities. 18. The process of claim 1 , wherein the distillate stream comprises essentially no sulfur trioxide. 19. The process of claim 1 , wherein the distillate stream comprises 60 ppm of sulfur trioxide or less. 20. The process of claim 19 , wherein the distillate stream comprises 40 ppm of sulfur trioxide or less.
containing only one sulfo group · CPC title
Separation; Purification · CPC title
Vacuum distillation (B01D3/12 takes precedence) · CPC title
Flash distillation · CPC title
by reaction with sulfuric acid or sulfur trioxide · CPC title
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