Dehydration processes of Mg (H
2PO
4) 
2·2H
2O and Ca (H
2PO
4) 2·H
2O in the presence of 85% H
3PO
4 were studied under a reduced pressure of 50mmHg at 180°C or 250°C. Some properties of the products; MgH
2P
2O
7, Mg (PO
3) 
2, CaH
2P
2O
7, and γ-Ca (PO
3) 
2, Obtained under the optimal conditions in these reactions were examined by means of measurements of density and surface area, and electron micrography. On each dehydration, two kinds of mixtures (phosphate : H
3PO
4= 10 : 20 and 10 : 1 in mixing ratio of g) were used.
The slurry mixtures of Mg (H
2PO
4) 2· 2H
2O with H
3PO
4 and Ca (H
2PO
4) 
2·H
2O with H
3PO
4, at a mixing ratio of 10 : 20, were heated at 180°C for 40h and at 250°C for 8h, respectively.
The dehydration processes proceeded along the following routes : 
1) Mg (H
2PO
4) 
2· 2H
2O→ Mg (H
2PO
4) 
2→MgH
2P
2O
7→Mg (PO
3) 
22) Ca (H
2PO
4) 
2·H
2O→ [Ca (H
2PO
4) 
2] →CaH
2P
2O
7→γ-Ca (PO
3) 
2.
In route (2) Ca (H
2PO
4) 
2 was not detected because the dehydration of Ca (H
2PO
4) 
2·H
2O to CaH
2P
2O
7proceeded rapidly.
In the case of powder-like mixtures in a mixing ratio of 10 : 1, the process of the Mg (H
2PO
4) 
2·2H
2O-H
3PO
4 system was the same as route (1), but the final stage of the Ca (H
2PO
4) 
2·H
2O-H
3PO
4 system differed from that of route (2) : 
3) CaH
2P
2O
7→ Ca
2HP
3O
10+amorphous→γ-Ca (PO
3) 
2.
It was found that these reactions in the presence of phosphoric acid occurred at lower temperatures than those in air or under reduced pressure.
MgH
2P
2O
7, Mg (PO
3) 
2, CaH
2P
2O
7, and γ-Ca (PO
3) 
2, obtained in this experiment had better crystallinity and more uniform grain size than those obtained by heating in air.
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