Citric Acid → Sulfosalicylic Acid

Participants

Reaction Conditions

Reaction Steps

25 gms of naphthalene and 25 ml of conc. sulfuric acid were taken into a 250 ml round bottomed flask fitted with a stirrer. The contents of the flask were heated to 80° C. for 120 minutes with constant stirring. A drop of the resulting mass was taken in a beaker and 1 ml water was added to the same with shaking. A clear solution without any naphthalene smell was obtained confirming the completion of sulfonation. Simultaneously, 0.5 gm salicylic acid was taken in a separate beaker and 0.5 ml concentrated sulfuric acid was added with stirring at 25° C. The slurry was left aside with occasional stirring for 3 hrs. The naphthalene sulfonic acid, prepared in flask was allowed to cool down to 60° C. and transferred a reactor fitted with a thermometer, stirrer and a dropping funnel. The mass was stirred continuously for a period of 10 min. while maintaining the temperature at 60° C. with the help of the thermostat. A mixture of 0.2 gm poly acrylic acid, 0.25 gm phthalic acid, 1 gm citric acid and 0.14 gm salicylic acid was dissolved in 10 ml water in a beaker and the same was added to the reaction mass in the reactor through the dropping funnel. The mixture was heated at 65° C. for 20 min. 250 gm of aluminium sulfate was added to the above mass along with 100 ml of water with vigorous stirring. The temperature of the bath was gradually raised to 70° C. and allowed heating to continue for another 60 min. The sulfo salicylic acid which was prepared in the beaker was added to above mass and heating was continued for another 30 minutes. The mixture was transferred to a bucket and pH was raised to 2.5 by adding 60 gms sodium sulfite dissolved in 100 ml water while continuing stirring. The air was passed through the resulting solution for a period of 70 minutes. Slurry was filtered using muslin cloth of pore size 5–10μ. The filtrate was drum dried at 130° C. and the powder stored in a plastic container.

Provenance & Evidence