Patented Apr.

16, 1935 1,998,182

UNITED starts PATET OFFI€E '

7 I 1,998,122

rnonn'c'rroN or or SODIUM PHOSPHATE

Francis M. Anable, Chicago Heights, and George
Klein, Chicago, 11L, assignors to Victor Chem
ical Works, a corporation of Illinois
No Drawing. Application July 16, 1932,
Serial No. 623,008
17 Claims. (oi. 23-107)
This invention relates to a method of prepar rapid by increase in temperature, and it is, there
ing pure anhydrous di-sodium phosphate. fore, preferred to boil the solution in ‘order to
In preparing anhydrous di-sodium phosphate save time. However, at lower temperatures com
from phosphoric acid and sodium carbonate lete elimination of the impurities may be $8
and/or some other alkaline sodium compound cured by allowing a longer period for precipita- 5
such as caustic soda or tri-sodium phosphate, the tion. ‘
ordinary steps of ?ltration plus evaporation to For example, a 52° Bé. solution (as measured
dryness, following the neutralization reaction, at‘ 80° C.) showed complete absence of iron and
no not result in- a di-sodium phosphate which aluminum after two hours of boiling (106° C.).
10 will produce-an entirely clear Water solution. A similar solution agitated at 100° C. required 10
This is due chie?y to impurities such as silica approximately six hours for complete removal of
and iron and aluminum compounds which are. the impurities. It is preferred to agitate the so
water insoluble in the ?nal product, but which lution in order to hasten the precipitation.
are not precipitated. and removed by the preced Diminution in the gravity of the solution be
15 ing ?ltration. low 52-54° Be. results in a decrease in the rate 15
According to the present invention a 31113513311“. of precipitation. For example, solutions treated
tially pure di-sodium phosphate may be pre under identical conditions as to pH showed a
pared from phosphoric acid, preferably 00116911‘? freedom from iron and aluminum impurities
trate‘d phosphoric acid such as is produced by after two hours of boiling where the Be’. grav
20 a volatilization process, for example, by the blast ity was 53°, whereas a solution having a Be. grav- 20
furnace or electric furnace methodsby carefully‘ ity of 435° still showed traces of impurities after
controlling the conditions at the end point of the nine hours of boiling. Solutions having a Be.
reaction and then maintaining the solution un gravity below. 40° (as measured at 80° C.) do not
der such conditions until the impurities ‘have appear to completely precipitate impurities when
precipitated out. For example, concentrated treated by this. method. ‘ 25
phosphoric acid is mixed with soda ash or caustic After a sample ?ltrate shows no iron or alumi
soda or both, and water added, if necessary, su?i num upon test, the impurities may be removed
cient to produce a Be. gravity of preferably from the main body of liquid, for example, by
52-540 (as measured at 80° C.). It is preferred ?ltering, and the solution then evaporated to
to use soda ash for the ?rst part of the neutraliza dryness in the desired manner, as, for example, “
tion and caustic soda or tri-sodium phosphate for spray or ?lm drying of any type. ,
the ?nal neutralization. A further improvement may be accomplished
For example, by the use of tri-sodium phosphate for the ?nal
7094 lbs. ‘75% phosphoric acid neutralization of the phosphoric acid. It has
5460 lbs. soda ash been discovered that by using tri-sodium phos
340 lbs. caustic soda, or phate instead of caustic soda, the silica remain
2400 lbs. tri-sodium phosphate ing in the di-sodium phosphate is practically all
in soluble form, whereas With caustic soda a con
give a solution of the proper proportions. siderably greater portion of the silica appears in
40 The pi-I of the mixture is adjusted so that the 40
the ?nal product in insoluble form.
pI-I of a diluted sample will be approximately A water solution of di-sodium phosphate pro
8.90, say from 8.85 to 9.0ii, preferably 8.85 to 8.95, duced in the above manner is practically perfect,
when measured after diluting 10 cc. of the 53-5Ll° the amount of insoluble material being in the
Be. solution with 50 cc. of water where the origi neighborhood of .002 to .01 %, and consisting es- 45
nal solution has a higher or lower concentration, sentially of hydrated silica. By proceeding in
the dilution is varied to give the same ultimate
accordance with this invention, it has been dis
concentration. The reaction mixture is then
covered that practically all of the silica in the
heated, preferably to 100° C. or above, and agi
tated until a test of the ?ltered solution shows no final product is rendered soluble.
trace of iron or aluminum impurities, for ex The foregoing detailed description has been
ample, as shown by the ammonium acetate test. given for clearness of understanding only, and
It is evident that in the above process the phos no unnecessary limitations should be understood
phoric acid may be replaced by mono-sodium therefrom, but the appended claims should be
phosphate. construed as broadly as permissible, in view of
Precipitation of the impurities is rendered more the prior art. 55
 2 1,998,182
We claim: ‘ 10. The method as set forth in claim '7, in
1. The method of purifying di-sodium phos which the solution is agitated.
phate containing iron and aluminum impurities 11. The method as set forth in claim '7, in
which comprises producing a solution compris which the solution is heated to a temperature
ing di-sodium phosphate of a Bé. gravity in ex not substantially less than 100° C.
cess of 40° as measured at 80° C., maintaining a 12. The method as set forth in claim '7, in
pH therein such that on dilution of a sample to which said solution is boiled.
a dilution corresponding to the addition of 5 13. The method of producing a pure anhydrous
parts of water to a 52°-54° Baumé solution, the di-sodium phosphate from components contain
diluted sample has a pH of 8.85-9.00, heating the ing iron and aluminum impurities, which com 10
solution until said iron and aluminum impuri prises: producing a solution comprising disodium
ties are completely precipitated, removing said phosphate of a Bé. gravity in excess of 40° as
solution from said precipitated impurities, and measured at 80° C., maintaining a pH therein such
removing the di-sodium phosphate from said so that on dilution of a sample to a dilution corre
lution. sponding to the addition of 5 parts of water to a 15
2. The method as set forth in claim 1, in which 52°-54° Baumé solution, the diluted sample has
the pH of the sample is approximately 8.9. a pH of 8.85-9.00, heating the solution until said
3. The method as set forth in claim 1, in which iron and aluminum impurities are completely pre
said solution is maintained at a Bé. gravity of cipitated, removing said solution from said pre
20 52-54°. cipitated impurities, and evaporating the water 20
4. The method as set forth in claim 1, in which from said solution.
the solution is agitated. 14. In the method of producing puri?ed di
5. The method as set forth in claim 1, in which sodium phosphate which comprises producing a
the solution is heated to a temperature not sub solution of disodium phosphate by reaction of an
stantially less than 100° C. acid phosphate with an alkaline sodium compound
6. The method as set forth in claim 1, in which and heating the completed reaction mixture at a
the solution is boiled. Baumé gravity in excess of 40° as measured at
'7. The method of purifying iron and alumi 80° C. and at a pH, as measured after diluting the
num-containing di-sodium phosphate produced reaction mixture to a dilution equivalent to that
by the use of phosphoric acid made by a vola obtained by diluting a 52°-54° Bé. solution with 5
tilization process which comprises producing a parts of water, of 8.85-9.00, until the iron and
solution comprising di-sodium phosphate of a aluminum impurities have been completely pre
Bé. gravity in excess of 40° ‘as measured at 80° C., cipitated, the step which comprises completing
maintaining a pH therein such that on dilution the neutralization of the acid phosphate by the
of a sample to a dilution corresponding to the addition of trisodium phosphate.
addition of 5 parts of Water to a 52°-54° Baumé 15. The method as set forth in claim 14 in
solution, the diluted sample has a pH of which the acid phosphate is ?rst partially neu
8.85-9.00, heating the solution until said iron and tralized with sodium carbonate.
aluminum impurities are completely precipi ' 16. The method as set forth in claim 14 in which
40 tated, removing said solution from said precipi the acid phosphate is phosphoric acid. 40
tated impurities and removing the puri?ed cli 17. The method as set forth in claim 14 in which
sodium phosphate from said solution. the acid phosphate is phosphoric acid, and in
8. The method as set forth in claim 7, in which which the phosphoric acid is preliminarily partly
the pH of the sample is approximately 8.9. neutralized with sodium carbonate.
45 9. The method as set forth in claim '7, in which
said solution is maintained at a Bé. gravity of FRANCIS M. ANABLE.
52-54". GEORGE KLEIN.