Reaktion #347590

Reaktionsgleichung

ammonium hydroxide

citric acid monohydrate

hexanediamine

maleic anhydride

→

hexanediamine

citric acid

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle