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Diammonium hydrogen phosphate → Tricalcium Phosphate

HRID 477758
Notes
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Reaction equation

HRID 477758 reaction equation
[N+]([O-])([O-])=O.[Ca+2:5].[N+]([O-])([O-])=O.O.N.[P:12]([O-:16])([O-:15])([OH:14])=[O:13].[NH4+].[NH4+]>O>[P:12]([O-:16])([O-:15])([O-:14])=[O:13].[Ca+2:5].[P:12]([O-:16])([O-:15])([O-:14])=[O:13].[Ca+2:5].[Ca+2:5]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 24540Diammonium hydrogen phosphateHCID 24963Calcium nitrate2×HCID 12896473Azane;hydrate2×HCID 178435178HCID 178435178, compound

Product 1

HCID 24456Tricalcium Phosphate

Reagents, catalysts & solvents 1

HCID 962
Water
Solvent
4×

Conditions

Temperature
80 °C

Procedure

In 7.1 l. of distilled water there was dissolved 2500 g of commercially available calcium nitrate [Ca(No3)2. 4H2O], and 7.9 l. of 28% ammonia water was slowly added to the resultant solution. The thus obtained solution was then diluted with 3 1. l. of distilled water. Separately therefrom, 840 g of commercially available ammonium hydrogen-phosphate [NH4)2HPO4 ] was dissolved in 10 l. of distilled water. 4.8 l. of 28% ammonia water and 10 l. of distilled water were then added to this solution. While keeping the former calcium nitrate aqueous solution at 20° C., the latter ammonium hydrogenphosphate aqueous solution (20° C.) was added dropwise thereto with stirring to effect reaction therebetween. After completion of the dropwise addition, the mixture described above was heated to 80° C. and maintained for 20 minutes under reflux, while continuing stirring. After cooling, the reaction mixture was allowed to settle for 2 days. Subsequently, the solution was dehydrated (2000 g) with a centrifugal dehydrator equipped with a polypropylene-made filter cloth (1000 mesh) and washed with distilled water until the system showed no alkaline property. The thus obtained calcium phosphate filtered cake was dried and then ground into powders in a mortar. The powders were passed through a sieve of 140 mesh to give 920 g of calcium phosphate powders. The calcium phosphate powders were packed in 18 pieces of polyurethane foam "Everlightscott Filter" (HR-20; cell number, 17-25 cells/25 mm; porosity, 97%) manufactured by Bridgestone Corporation, which were then each inserted in a respective rubber form as in Example 1. Three pieces each in a group were pressed with a rubber press under 6 levels of pressure as shown in Table 1. They were put in an electric furnace and calcined for 2 hours at 1100° C., after elevating the temperature to 1100° C.

Workup

  1. additionThe thus obtained solution was then diluted with 3 1
  2. customat 20° C.
  3. customreaction
  4. additionAfter completion of the dropwise addition
  5. temperaturemaintained for 20 minutes
  6. temperatureunder reflux
  7. stirringwhile continuing stirring
  8. temperatureAfter cooling
  9. filtrationmade filter cloth (1000 mesh)
  10. washwashed with distilled water until the system
  11. dry with materialThe thus obtained calcium phosphate filtered cake was dried

Sources & evidence

ORD record
ord-e3076b04655a4184a3c8065608cc7b05
Source dataset
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04889833

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes