Reaction #1960514

ord-ce48b94063434b299fe829cf92d08c00

Reaction equation

[Zn]
Zn
O=P([O-])([O-])[O-].[Zn]
Zn phosphate
O.O.O.O.O.O.O=[N+]([O-])[O-].O=[N+]([O-])[O-].[Zn+2]
zinc nitrate hexahydrate
O.O.O.O.O.O.O=[N+]([O-])[O-].O=[N+]([O-])[O-].[Zn+2]
zinc nitrate hexahydrate
C(C[*:2])[*:1]
polyethylene
O=P([O-])([O-])[O-].O=P([O-])([O-])[O-].[Zn+2].[Zn+2].[Zn+2]
Zinc Phosphate

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.DISTILLATIONAn aqueous solution of 8.51 g 50 wt % H3PO2 in 8.00 g distilled water
  2. 2
    Otherwas prepared
  3. 3
    Otherproceeded giving a homogeneous solution once the sample
  4. 4
    TemperatureFurther warming of this solution to >25° C. on a hotplate
  5. 5
    workup.WAITabated somewhat for a period of five minutes
  6. 6
    Othervigorously resumed finally resulting in the formation of a mass of moist white solid
  7. 7
    Otherused as a reaction vessel
  8. 8
    Temperatureto cool to room temperature

Procedure

An aqueous solution of 8.51 g 50 wt % H3PO2 in 8.00 g distilled water was prepared as described in Example 1. To this solution was added 28.78 g zinc nitrate hexahydrate salt, Zn(NO3)2.6H2O (ACS reagent, Aldrich Chemical Co., Inc. #22, 873-7, CAS #10196-18-6), equivalent to 21.97 wt % Zn. The molar ratio of Zn/phosphate in this mixture was 3/2 and the equivalent solids level [as Zn3(PO4)2] was 27.5 wt %. Endothermic dissolution of the zinc nitrate hexahydrate proceeded giving a homogeneous solution once the sample warmed to room temperature. Further warming of this solution to >25° C. on a hotplate initiated a reaction in which the solution vigorously evolved red-brown acrid fumes of NOx (g). The reaction continued for approximately 10 minutes while the sample remained a clear, colorless solution, abated somewhat for a period of five minutes, then vigorously resumed finally resulting in the formation of a mass of moist white solid, some of which was very adherent to the walls of the Pyrex beaker used as a reaction vessel. The hot solid was allowed to cool to room temperature and was stored in a polyethylene vial.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08303976B2uspto-grants-2012_11