Process for removal of sulphur from raw methanol

Patent metadata

Field	Value
Publication number	US-10160706-B2
Application number	US-201415027967-A
Country	US
Kind code	B2
Filing date	Oct 13, 2014
Priority date	Oct 11, 2013
Publication date	Dec 25, 2018
Grant date	Dec 25, 2018

Abstract

A method for purifying raw methanol containing sulfur compounds, wherein the method comprises the step of washing raw methanol with a non-polar organic solvent.

First claim

The invention claimed is:

1. A method for purifying a composition comprising methanol and sulfurous compounds obtained as a by-product in a Kraft or sulfate process of pulp production in a pulp mill, the method comprises a step of:
washing the composition comprising methanol and sulfurous compounds with a non-polar organic solvent to extract sulfurous compounds, wherein the non-polar organic solvent is a solvent comprising at least 60 wt. % alkanes and/or cyclo-alkanes having a carbon number of 14 or higher, and/or wherein the non-polar organic solvent comprises at least 10 wt. % triglycerides which are liquid at temperatures of less than 40° C.;
wherein the non-polar organic solvent has a boiling point higher than 100° C. but lower than 600° C. and a viscosity at 40° C. of not more than 100 cSt.

2. The method according to claim 1 , wherein the non-polar organic solvent comprises less than 2.5 wt. % polycyclic aromatic hydrocarbons.

3. The method according to claim 1 , wherein the non-polar organic solvent is a mixture of hydrocarbons.

4. The method according to claim 3 , wherein the non-polar organic solvent is selected from the group consisting of white mineral oil, mineral oil, and mixtures thereof.

5. The method according to claim 1 , wherein the density at 25° C. of the non-polar organic solvent is in the range 0.80 to 0.90 g/cm 3 ; or wherein the density at 25° C. of the non-polar organic solvent is in the range 0.91 to 1.20 g/cm 3 .

6. The method according to claim 1 , wherein the method further comprises a step of diluting the composition comprising methanol and sulfurous compounds with water before being washed with the non-polar organic solvent, the methanol content in the composition comprising methanol and sulfurous compounds before being diluted being at least 65 wt. %, wherein the water content of the diluted aqueous composition comprising methanol and sulfurous compounds and the non-polar organic solvent are selected such that their difference in density at 25° C. is at least 0.01 g/ml.

7. The method according to claim 6 , wherein the diluted aqueous methanol phase has higher density than the non-polar organic solvent.

8. The method according to claim 6 , further comprising a step of separating turpentine before washing the diluted aqueous methanol.

9. The method according to claim 1 , wherein the methanol to non-polar organic solvent volume ratio is 1:0.75 to 1:5.

10. The method according to claim 1 , wherein the washing is performed at a temperature of 15 to 60° C.

11. The method according to claim 1 , wherein the non-polar organic solvent is regenerated by steam stripping, and re-used as non-polar organic solvent in the washing step.

12. The method according to claim 1 , wherein the composition comprising methanol and sulfurous compounds is acidified and precipitated salts are removed before washing the composition comprising methanol and sulfurous compounds with a non-polar organic solvent, and wherein the method further comprises a step of separating turpentine after the composition comprising methanol and sulfurous compounds has been acidified.

13. The method according to claim 12 , further comprising a step of distilling the methanol subsequently to having been acidified, wherein the distillation is performed in a manner such that volatile sulfurous compounds firstly are distilled off and then methanol.

14. The method according to claim 12 , wherein the amount of hydrogen sulfide, methyl mercaptan, and dimethyl sulfide, being more volatile than methanol, are reduced by distillation prior to acidifying the methanol.

15. The method according to claim 1 , wherein the process further comprises a step of separating hydrogen sulfide and methyl mercaptan prior to the washing step.

16. The method according to claim 1 , wherein the content of water, acetone, and ethanol in the washed methanol is reduced by distillation in three steps after the wash with the non-polar organic solvent.

17. A method of purifying raw methanol from a Kraft or sulfate process of pulp production in a pulp mill, the raw methanol comprising sulfurous compounds and nitrogenous compounds, the method comprising steps of:
acidifying the raw methanol to form precipitations;
removing the precipitations;
optionally at least partly removing turpentine;
optionally distilling sulfurous contaminants;
distilling the acidified methanol from which precipitations have been removed to obtain distilled methanol composition;
diluting the distilled methanol composition with water to obtain a diluted methanol composition;
optionally removing turpentine from the diluted methanol composition;
washing the diluted methanol composition with a non-polar organic solvent to extract sulfurous compounds, wherein the non-polar organic solvent is a solvent comprising at least 60 wt. % alkanes and/or cyclo-alkanes having a carbon number of 14 or higher, and/or wherein the non-polar organic solvent comprises at least 10 wt. % triglycerides which are liquid at temperatures of less than 40° C., wherein the non-polar organic solvent has a boiling point higher than 100° C. but lower than 600° C. and a viscosity at 40° C. of not more than 100 cSt; and
removing acetone, water and/or ethanol by one or several distillation steps.

18. The method according to claim 17 , further comprising a step of re-generating non-polar organic solvent by steam stripping and subsequently re-using the re-generated non-polar organic solvent in washing the diluted methanol composition.

Assignees

• Andritz Oy

Inventors

• Warnqvist Jan
• Olsson Släger Johan
• Eliasson Anders

Classifications

• B01D11/0492

  Applications, solvents used · CPC title

• C07C27/34

  by extraction · CPC title

• C07C29/88

  by treatment giving rise to a chemical modification of at least one compound (chemisorption C07C29/76) · CPC title

• D21C11/0007

  Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for (volatile compounds obtained by decomposition of spent liquors in order to regenerate them D21C11/125; compounds obtained by fractionating the liquors in order to regenerate them D21C11/0042) · CPC title

• C07C31/04

  Methanol · CPC title