Reaction #1375809

ord-e818cb7f3e9446be87f4df68f2020468

Conditions

Temperature
140°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONwere charged
  2. 2
    workup.ADDITIONThe reaction mix
  3. 3
    Otherto evolve at about 130° C
  4. 4
    TemperatureThe temperature was slowly raised to 150° C
  5. 5
    Otherthe remaining ammonia was removed
  6. 6
    OtherProduct yield
  7. 7
    Otherat 25° C.
  8. 8
    workup.DISTILLATIONfurther purified by vacuum distillation

Procedure

In a suitable reactor equipped with agitation and a reflux condenser, 465 parts by weight of urea and 798 parts by weight of diethylenetriamine were charged. The reaction mix was slowly heated to 140° C. Ammonia started to evolve at about 130° C. The temperature was slowly raised to 150° C. As the evolution of ammonia subsided, vacuum was applied and the remaining ammonia was removed. Product yield was approximately 1000 parts by weight. The product had a viscosity of 6000 cps at 25° C. and an MEQ/g of 6.5. (MEQ=milliequivalent weight). Gel phase analysis of the product showed approximately 95% purity. The product can be used as is or further purified by vacuum distillation. The major impurity is unreacted diethylenetriamine.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05746946uspto-grants-1998_05