FIVE HUNDRED grams of technical _p_-toluenesulfonyl chloride are ground
in a mortar to break up all lumps. Three liters of water are placed
in a 12-l. crock provided with a large brass stirrer and a tube
for passing steam directly into the liquid. Dry steam is passed
into the water until the temperature reaches 70'0. The steam is then
shut off and 400 g. of zinc dust (90 to 100 per cent pure) is added.
The sulfonyl chloride is then added in small portions by means
of a porcelain spoon. The addition takes about ten minutes.
The temperature rises to about 80'0. Stirring is continued
for ten minutes after the last of the chloride has been added.
Steam is then passed into the mixture until the temperature
reaches 90'0. If it is heated any hotter, bumping takes place.
The steam is shut off, and 250 cc. of 12 _N_. sodium hydroxide
solution is added. Finely powdered sodium carbonate is then
added in 50-g. portions until the mixture is strongly alkaline.
The mixture froths considerably, but this causes no trouble unless
too small a crock is used. The stirrer is loosened and the crock
is removed. The mixture is filtered by suction in a large funnel.
The filtrate has a volume of about 4.5 l. The cake of unchanged
zinc dust and zinc compounds is transferred to a 3-l. battery jar
and placed under the stirrer, and the latter is clamped in place.
Water (750 cc.) is added, the stirrer is started, and steam
is passed in until the mixture starts to froth too violently.
The steam is then shut off, but the stirring is continued
for ten minutes. The mixture is filtered and the filtrate
is added to the main solution in a large evaporating dish.
The liquid is evaporated over a large burner to a volume of about
1 l., or until a considerable crust forms around the edges.
The mixture is then cooled. Large, flat, transparent crystals separate.
The thoroughly cooled mixture is filtered by suction,
and the crystals are air-dried until efflorescence just starts.
They are then bottled. The product is CH3C6H4SO2Na<.>2H2O. Yield 360 g.
(64 per cent of the theoretical amount). Careful acidification
of the mother liquor with dilute hydrochloric acid yields 15 g.
of the free sulfinic acid.