HRID1375297

反应详情

EQUATION

反应方程式

HRID 1375297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. additionwas added
  2. waitThe slurry was left aside
  3. stirringwith occasional stirring for 3 hrs
  4. temperatureto cool down to 60° C.
  5. customfitted with a thermometer, stirrer and a dropping funnel
  6. stirringThe mass was stirred continuously for a period of 10 min.
  7. temperaturewhile maintaining the temperature at 60° C. with the help of the thermostat
  8. additionthe same was added to the reaction mass in the reactor through the dropping funnel
  9. temperatureThe mixture was heated at 65° C. for 20 min
  10. temperatureThe temperature of the bath was gradually raised to 70° C.
  11. temperatureallowed heating
  12. additionwas added to above mass
  13. temperatureheating
  14. waitwas continued for another 30 minutes
  15. temperaturewas raised to 2.5
  16. stirringwhile continuing stirring
  17. waitThe air was passed through the resulting solution for a period of 70 minutes
  18. filtrationSlurry was filtered
  19. customdried at 130° C.