A solution of SOz (212 g) in methanol (636 g) and a solution
of sodium formate (120g) in water (106g) are simultaneously
added (50 % of each solution in 15 min and the rest within
7.5 min) to a suspension of sodium formate (1 20 g), NaOH(solid)
(9Og), water (382g), and methanol (402g) in a 2-1 glass
flask fitted with a stirrer and two entry tubes; the temperature
is kept at 67°C during the addition. After cooling to 60°C,
the solid material is filtered off, washed with methanol, and
dried. In this way, 211 g of a crystalline product is obtained
which consists of Na2S2O5.NaOOCH (94.5 %), Na2S2O4
(2.3 %), Na2SO3 (3.0 %), and Na2S2O3 (0.2 %); the yield of
Na2S205.NaOOCH is 46.7 % based on SO2. |