Method for preparing monosodium sulfosuccinate
A technology of dimethyl sulfosuccinate monosodium salt and dimethyl sulfosuccinate monosodium is applied in the field of preparing sulfosuccinate monosodium salt, and can solve the problem that the reaction raw material sulfur dioxide is difficult to buy, sulfonic acid Succinic acid is expensive, unfavorable for industrial production and other problems, and achieves the effects of low cost, short reaction period and mild reaction conditions
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Embodiment 1
[0022] Add 9.2 g dimethyl sulfosuccinate monosodium salt in the there-necked flask, and add 25 ml of water in the bottle, stir to make the solid dissolve completely, add 3.56 g sodium hydroxide in the above solution; Carry out hydrolysis reaction at 25 ℃ for 10 hours; then add 2.4 ml of concentrated sulfuric acid to the above-mentioned hydrolyzed reaction solution, and after the reaction is completed, evaporate the solvent under reduced pressure to obtain a white solid; add 25 ml of methanol to the above-mentioned white solid, And the resulting solution was heated to 60°C, filtered under reduced pressure while hot to remove insoluble matter, and the obtained mother liquor was evaporated to dryness to obtain 3.9 g of white solid with a molar yield of 47%. 1 H-NMR (D 2 O, 500 MHz): d = 2.95 (dd, 1H), 3.14 (dd, 1H), 4.25 (dd, 1H).
Embodiment 2
[0024] Add 9.2 g dimethyl sulfosuccinate monosodium salt in the there-necked flask, and add 25 ml of water in the bottle, stir to make the solid dissolve completely, add 3.56 g sodium hydroxide in the above solution; Carry out the hydrolysis reaction at 55°C for 6 hours; then add 2.4 ml of concentrated sulfuric acid to the above-mentioned hydrolyzed reaction solution, and evaporate the solvent under reduced pressure after the reaction is completed to obtain a white solid; add 25 ml of methanol to the above-mentioned white solid, The temperature of the formed solution was raised to 60°C, and the insoluble matter was removed by suction filtration under reduced pressure while it was hot, and the obtained mother liquor was evaporated to dryness to obtain 4.2 g of white solid with a molar yield of 56%. 1 H-NMR (D 2 O, 500 MHz): d =2.95 (dd, 1H), 3.14 (dd, 1H), 4.25 (dd, 1H).
Embodiment 3
[0026] Add 9.2 g dimethyl sulfosuccinate monosodium salt in the there-necked flask, and add 25 ml of water in the bottle, stir to make the solid dissolve completely, add 3.56 g sodium hydroxide in the above solution; The hydrolysis reaction was carried out at 55°C for 6 hours; then 2.4 ml of concentrated sulfuric acid was added to the above-mentioned hydrolyzed reaction solution, and after the reaction was completed, the solvent was evaporated under reduced pressure to obtain a white solid; 25 ml of 90% methanol, and the temperature of the formed solution was raised to 60°C, while it was hot, it was suction-filtered under reduced pressure to remove insoluble matter, and the obtained mother liquor was evaporated to dryness to obtain 5.2 g of a white solid with a molar yield of 70%. 1 H-NMR (D 2 O, 500 MHz): d =2.95 (dd, 1H), 3.14 (dd, 1H), 4.25 (dd, 1H).
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