반응 #347590

ord-68d7b1406c054d5dbd629c149f4f5994

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타This solution was evaporated to dryness over a period of 30 minutes
  2. 2
    온도The solid was then heated at 195°-220° C. for 10 minutes
  3. 3
    기타removed from the heat
  4. 4
    온도to cool
  5. 5
    온도The solid was then heated at 230°-245° C. for 10 minutes
  6. 6
    기타removed from the heat
  7. 7
    온도to cool
  8. 8
    온도Finally, the solid was heated at 230°-245° C. for 10-15 minutes
  9. 9
    기타removed from the
  10. 10
    온도heat
  11. 11
    workup.ADDITIONa solution of 8.0 g of sodium hydroxide in 12 ml of water was added over 5 minutes

실험 절차

A solution of 2.1 g (0.01 moles) of citric acid monohydrate (Formula weight 210) and 0.32 g (0.0028 moles) hexanediamine was added to 19.6 g (0.2 mole) maleic anhydride which had been dissolved in 40 ml water at 80°-95° C., and finally 30 g of 30% aqueous solution of ammonium hydroxide (0.22 mol NH3) was added. This solution was evaporated to dryness over a period of 30 minutes. The solid was then heated at 195°-220° C. for 10 minutes, removed from the heat, allowed to cool and broken up with a spatula. The solid was then heated at 230°-245° C. for 10 minutes, removed from the heat, allowed to cool and broken up with a spatula. Finally, the solid was heated at 230°-245° C. for 10-15 minutes, removed from the heat and allowed to cool to room temperature. The resulting water insoluble polymer was slurried in 40.0 ml of water and a solution of 8.0 g of sodium hydroxide in 12 ml of water was added over 5 minutes. The solution was stirred for 10-20 minutes to give a clear red-brown solution, pH 10-11.0 of a copolymer of polyaspartic acid, citric acid and hexanediamine. The tests for CaSO4, Example 3, and CaCO3 (below) were run and the result are recorded in Table 2.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05527863uspto-grants-1996_06