Sulfuric Acid → 2-Methylbenzenesulfonic acid hydrate

Participants

Reaction Conditions

Reaction Steps

Reference Example 1. 6 mol Of toluene were added dropwise over a period of 1 hour to a mixture of 3.75 mol sulfuric acid and 2.25 mol fuming sulfuric acid at a mixture temperature of 45 to 60° C. The reaction mixture was heated for another 30 minutes at 45° C., which gave toluenesulfonic acid monohydrate. A mixture of 1 mol trichlorosilane and 6.6 molitoluene was added dropwise to this over a period of 5 hours at 30° C., and the reaction mixture was heated for another 30 minutes at 45° C. After the solution was allowed to cool and separate, the toluenesulfonic acid layer (at the bottom) was removed, after which the top layer was washed with a suitable amount of sulfuric acid/water (50/50 weight ratio), then with a suitable amount of sulfuric acid/water (25/75 weight ratio), and then with pure water in order to remove the acid contained in the top layer. Azeotropic dehydration was then performed for 1 hour in order to remove the water completely. The toluene solution obtained in this manner was put under reduced pressure with a vacuum pump at 60° C. to remove the toluene, which gave a hydrogen silsesquioxane resin whose main skeleton consisted of siloxane units described by formula HSiO3/2. This hydrogen silsesquioxane resin had a number average molecular weight of 1650, and the ratio of the weight average molecular weight/number average molecular weight was 19.4.

Provenance & Evidence