Process for purifying alkanesulfonic acids

Patent metadata

Field	Value
Publication number	US-10577312-B2
Application number	US-201615774847-A
Country	US
Kind code	B2
Filing date	Nov 8, 2016
Priority date	Nov 10, 2015
Publication date	Mar 3, 2020
Grant date	Mar 3, 2020

Abstract

A process comprising: (a) distilling a melt comprising crude alkanesulfonic acid to completely or partly remove low boilers, wherein the low boilers are drawn off at the top of a distillation column or of a one-stage evaporation apparatus and a material stream comprising alkanesulfonic acid, high boilers and residual low boilers is withdrawn at the bottom of the distillation column or of the one-stage evaporation apparatus, (b) sending the stream comprising alkanesulfonic acid, high boilers and residual low boilers into a melt crystallization as the starting melt to obtain crystals formed from the alkanesulfonic acid, hydrates of the alkanesulfonic acid or a mixture of both suspended in mother liquor, (c) performing a solid-liquid separation to remove the crystals from the mother liquor, and (d) optionally washing the crystals to remove mother liquor adhering to the crystals.

First claim

The invention claimed is:

1. A process for purifying an alkanesulfonic acid, the process comprising:
(a) distilling a melt comprising crude alkanesulfonic acid to completely or partly remove low boilers, wherein the low boilers are drawn off at a top of a distillation column or a one-stage evaporation apparatus and a material stream comprising alkanesulfonic acid, high boilers and residual low boilers is withdrawn at a bottom of the distillation column or the one-stage evaporation apparatus,
(b) sending the material stream into a melt crystallization as a starting melt to form crystals of the alkanesulfonic acid, of hydrates of the alkanesulfonic acid or of a mixture of both the alkanesulfonic acid and the hydrates of the alkanesulfonic acid suspended in mother liquor,
(c) performing a solid-liquid separation to remove the crystals from the mother liquor, and
(d) optionally washing the crystals to remove mother liquor adhering to the crystals.

2. The process according to claim 1 ,
wherein the mother liquor after removal of the crystals and/or the mother liquor generated is/are at least partly recycled into the melt crystallization or into (a).

3. The process according to claim 1 ,
wherein the mother liquor after removal of the crystals and/or the mother liquor generated is/are at least partly sent into a high boilers removal to remove high boilers from the mother liquor.

4. The process according to claim 3 ,
wherein the mother liquor after removal of the high boilers is recycled into (a).

5. The process according to claim 3 ,
wherein the mother liquor after removal of the high boilers is partially condensed and a condensed portion of the mother liquor is recycled into (a) and an uncondensed portion of the mother liquor is discharged from the process as low boilers.

6. The process according to claim 4 , wherein the material stream withdrawn from (a) is cooled before being sent to the melt crystallization and the mother liquor which is recycled into (a) is heated.

7. The process according to claim 6 ,
wherein heat from the material stream is transferred to the mother liquor.

8. The process according to claim 1 ,
wherein the alkanesulfonic acid is methanesulfonic acid.

9. The process according to claim 1 ,
wherein the low boilers comprise water or sulfur trioxide.

10. The process according to claim 1 ,
wherein the material stream sent to the melt crystallization comprises in addition to water or sulfur trioxide not more than 6 wt % of further impurities based on a total mass of the material stream.

11. The process according to claim 1 ,
wherein the melt crystallization is carried out at a temperature of from −15° C. to 19° C.

12. The process according to claim 1 ,
wherein the material stream comprises at least 76 mol % of alkanesulfonic acid based on a total amount of alkanesulfonic acid and water in the material stream.

13. The process according to claim 12 ,
wherein the melt crystallization is carried out at a temperature of from −10° C. to 19° C.

14. The process according to claim 1 ,
wherein the material stream comprises at least 87 mol % of alkanesulfonic acid based on a total amount of alkanesulfonic acid and sulfur trioxide in the material stream.

15. The process according to claim 14 ,
wherein the melt crystallization is carried out at a temperature of from −10° C. to 19° C.

16. The process according to claim 1 ,
wherein the material stream comprises 31 to 75 mol % of alkanesulfonic acid based on a total amount of alkanesulfonic acid and water in the material stream.

17. The process according to claim 16 ,
wherein the melt crystallization is carried out at a temperature of from −15° C. to 12° C.

18. The process according to claim 1 ,
wherein the optionally washing comprises washing the crystals with molten crystallizate.

19. The process according to claim 18 ,
wherein the molten crystallizate for washing the crystals has a temperature of from 0.1° C. to 15° C. above a solidification temperature of an alkanesulfonic-acid-containing crystallizate.

20. The process according to claim 7 ,
wherein the melt crystallization is a suspension crystallization or a layer crystallization.

Assignees

• Basf Se

Inventors

• Spielmann Jan
• Koch Michael
• Wortmann Juergen
• Ruether Feelly
• Weiguny Sabine
• Borgmeier Frieder

Classifications

• B01D9/0004

  cooling by heat exchange (by evaporation of components of the mixture to be separated B01D9/0013; refrigeration machines F25B) · CPC title

• C07C309/01

  Sulfonic acids · CPC title

• C07C303/44 Primary

  Separation; Purification · CPC title

• B01D2009/0086

  Processes or apparatus therefor · CPC title

• B01D9/0045

  Washing of crystals, e.g. in wash columns · CPC title