HRID426538

反应详情

EQUATION

反应方程式

HRID 426538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of oxalic acid consisting of 138.7 grams of oxalic acid dihydrate dissolved in 200 mL water was warmed to 60° C. and treated with 316 grams of urea phosphate made from wet-process phosphoric acid made from calcined North Carolina phosphate rock. The urea phosphate was added gradually over a 10-minute period with stirring while maintaining the temperature at 55°-60° C. Stirring and heating (at 60°-70° C.) was continued for 20 minutes. The hot mixture was filtered, and the clear, pale green filtrate was cooled to 5° C. and refiltered. The second filtrate weighed 377.2 grams, and it contained 32.1 percent P2O5, 1.82 percent N, 1.3 percent oxalic acid, 0.04 percent Al, 0.11 percent Fe, 0.08 percent Mg, and SO4. This corresponds to removal of 74 to 80 percent of the Al, Fe, Mg, F, and SO4 impurities originally present in the phosphoric acid used to make the urea phosphate. The urea oxalate filter cake from the first filtration was washed with about 200 mL of cold water and then dried, yielding 112.7 grams of urea oxalate containing 0.03 percent P2O5, 26.4 percent nitrogen, and 43.3 percent oxalic acid (theoretical composition of urea oxalate is 26.95 percent nitrogen and 42.86 percent oxalic acid). X-ray diffraction analysis showed that it was homogeneous as urea oxalate. The wash from the urea oxalate (first filter cake) weighed 220.0 grams, and it contained 5.6 percent P2O5, 1.17 percent N, and 2.3 percent oxalic acid. The second filtration yielded 66.0 grams of dried, unwashed crystals which contained 5.0 percent P2O5, 20.9 percent N, and 47.8 percent oxalic acid.

WORKUP

后处理

  1. temperaturewhile maintaining the temperature at 55°-60° C
  2. stirringStirring
  3. temperatureheating (at 60°-70° C.)
  4. filtrationThe hot mixture was filtered
  5. temperaturethe clear, pale green filtrate was cooled to 5° C.
  6. customThis corresponds to removal of 74 to 80 percent of the Al, Fe, Mg, F, and SO4 impurities originally present in the phosphoric acid
  7. filtrationThe urea oxalate filter cake
  8. filtrationfrom the first filtration
  9. washwas washed with about 200 mL of cold water
  10. customdried