Method for isolating concentrated paraffin sulfonic acids
View Patent ↗The invention relates to a method for isolating concentrated paraffin sulfonic acids from reaction mixtures that are produced during the sulfoxidation of n-paraffins, from which a major part of the sulfuric acid and the paraffin was removed by phase separation and which contain, in addition to the free paraffin sulfonic acids, n-paraffins, water and optionally minor amounts of sulfuric acids. The method according to the invention is characterized by removing paraffin and optionally residual water by vacuum distillation. The paraffin sulfonic acids obtained by distillation have a content of more than 85% by weight of the active substance. The material is pale, odorless and low in sulfuric acid and paraffin.
1. A method for isolating concentrated paraffin sulfonic acids from reaction mixtures that are produced during the sulfoxidation of n-paraffins, from which a major part of the sulfuric acid and the paraffin has been removed by phase separation and which comprise, in addition to the free paraffin sulfonic acids, also n-paraffins, water and optionally small amounts of sulfuric acid, comprising the step of removing paraffin and optionally residual water from the reaction mixture by vacuum distillation, wherein the vacuum distillation is carried out at a pressure from 10 −3 mbar to 1 mbar.
2. The method as claimed in claim 1 , wherein the starting material for the vacuum distillation consists of 10 to 50% paraffin sulfonic acids, 30 to 70% n-paraffins, 0 to 40% water and 0 to 5% sulfuric acid.
3. The method as claimed in claim 1 , wherein the starting material for the vacuum distillation consists of 12 to 40% paraffin sulfonic acids, 40 to 60% n-paraffins, 15 to 40% water and 0 to 3% sulfuric acid.
4. The method as claimed in claim 1 , wherein the vacuum distillation is carried out at a temperature from 50 to 150° C.
5. The method as claimed in claim 1 , wherein the vacuum distillation is carried out at a temperature from 80 to 120° C.
6. The method as claimed in claim 1 , wherein the vacuum distillation is carried out at a pressure from 10 −2 mbar to 0.1 mbar.
7. The method as claimed in claim 1 , wherein the vacuum distillation is carried out in a thin-film evaporator.
8. The method as claimed in claim 1 , wherein the vacuum distillation is carried out in a short-path evaporator.
9. The method as claimed in claim 1 , wherein the starting material is dewatered prior to the vacuum distillation.
10. The method as claimed in claim 1 , wherein the sulfuric acid in the starting material is neutralized with alkaline earth metal salts prior to the vacuum distillation and the alkaline earth metal sulfates that are produced are separated off from the starting material.