Phosphoric Acid → Zirconium phosphate

HRID 586102Notes

Reaction equation

HRID 586102 reaction equation
S([O-])([O-])(=O)=O.[Zr+4:6].S([O-])([O-])(=O)=O.[P].[OH:13][P:14]([OH:17])([OH:16])=[O:15].[OH-].[Na+]>O>[P:14]([O-:17])([O-:16])([O-:15])=[O:13].[Zr+4:6].[P:14]([O-:17])([O-:16])([O-:15])=[O:13].[P:14]([O-:17])([O-:16])([O-:15])=[O:13].[P:14]([O-:17])([O-:16])([O-:15])=[O:13].[Zr+4:6].[Zr+4:6]

Participants

6

Reactant 4

HCID 1004Phosphoric AcidHCID 14798Sodium HydroxideHCID 26793Zirconium(IV) sulfateHCID 5462309Phosphorus2×

Product 1

HCID 160986Zirconium phosphate

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
160 °C

Procedure

Amorphous zirconium phosphate was prepared in all the examples. In this example the material was prepared according to the following procedure. In the first stage, a slurry containing 440 g of basic zirconium sulfate (40% ZrO2) (MEI, HCP PP142A), with a predetermined particle size distribution ranging from 50 to 60 microns, in a phosphorus-containing solution was made. The phosphorus-containing solution had the following composition: 3.3 kg of water, 402 g of 75 wt % H3PO4, 380 g of 30 wt % NaOH and 45 g of Na4SiO4. The slurry was transferred into an autoclave, sealed and heated at 160° C. for 3 hours under constant stirring. The resulting product of conversion was filtered, washed with 0.5 kg of water and re-slurried in 2 L of 1 M H2SO4. The zirconium phosphate slurry in sulfuric acid was heated to the boiling point and kept at this temperature for 1 hour. After cooling down, the zirconium phosphate was filtered, washed with 0.5 kg of water and re-slurried in 1 L of water. To the ZrP suspension a 30 wt % NaOH solution was added gradually for 30 to 40 minutes to raise the pH to 7.0. Then, the zirconium phosphate was filtered, washed with 1 kg of water and dried at 150° C. for 12 hours in air.

Workup

  1. additioncontaining solution
  2. customsealed
  3. filtrationThe resulting product of conversion was filtered
  4. washwashed with 0.5 kg of water and re-slurried in 2 L of 1 M H2SO4
  5. temperatureThe zirconium phosphate slurry in sulfuric acid was heated to the boiling point
  6. temperatureAfter cooling down
  7. filtrationthe zirconium phosphate was filtered
  8. washwashed with 0.5 kg of water and re-slurried in 1 L of water
  9. additionTo the ZrP suspension a 30 wt % NaOH solution was added gradually for 30 to 40 minutes
  10. temperatureto raise the pH to 7.0
  11. filtrationThen, the zirconium phosphate was filtered
  12. washwashed with 1 kg of water
  13. customdried at 150° C. for 12 hours in air

Sources & evidence

ORD record
ord-af0dffba1f8943f9a75bf4c5009644c5
Source dataset
uspto-grants-2005_08
Patent number
US06936175B2

Reaction notes

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