S, PEACOCK,

PROCESS OF MAKING DI-AMMONIUM PHOSPHAE,

APPLICATION FILED SEPT, 2, 1909,
995,898, Patented June 20, 1911.

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1NWENTOR
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 UNITED STATES PATENT OFFICE.
SAMUEL PEACOCK, OF CHICAGO, ILLINOIS, ASSIGNOR. To AMERICAN CYANAMID
COMPANY, OF NEW YORK, N. Y., A CORPORATION OF MAINE.
PROCESS OF MAKINGDI-AMMONIUM PHosPHATE.
995,898. Specification of Letters Patent. Patented June 20, 1911.
Application filed September 2, 1909. Serial No. 515,805.
To all whom it may concern: The unabsorbed gases may be led out of the
Be it known that, I, SAMUEL PEACOCR, a top of the tower 2, by ineans of the pipe
citizen of the United States, residing at 9, through a second cooling means 10, and
Chicago, in the county of Cook and State of into a second tower 11, provided with a cir 60
5 Illinois, have invented certain new and use- culating pump 12, and cooling means 13 for
ful Improvements in Processes of Making the phosphoric acid solution. As many
IDi-annonium, Phosphate from Ammonia towers, cooling coils and pumps may be emi
and IPhosphoric Acid; and I do hereby de-ployed as desired, and the final unabsorbed
clare the following to be a full, clear, and gases may be permitted to escape from the
O exact description of the invention, such as last tower by means of the fle 15. The 65
will enable other's skilled in the art to which cuits
it appertains to make and use the same.
valvedin pipe 16 connects all the pump cir
order that should one tower become
This invention relates to a process for mak- unduly heated, a cooler solution may at once
ing secondary or di-ammonium phosphate, be supplied from another tower. The cir
:5 (NH), HPO, from ammonia and phos-culation of the phosphoric acid solution is 70
phoric acid; and has for its object to pro- continued until a measured quantity of phos
duce a simple and comparatively cheap proc- phoric acid has neutralized an equivalent
ess for making in a single operation, sub- quantity of ammonia, for the formation of
stantially pure commercial secondary an- Secondary ammonium phosphate. The total 75
monium phosphate, that is more uniform solution from the absorption system is then
and constant in composition than the prod- drawn
ulcts now ordinarily sold.
from the tank 18, and evaporated at,
O a few degrees below, SOo C. to the density
To this end the invention consists in the of crystallization in a vacuum pan using a
novel steps and combinations of steps con- vacuum not exceeding 350 millimeters of 80
stituting my process, more fully hereinafter mercury. The specific gravity of the solu
disclosed, and particularly pointed out in tion and therefore the size of the crystals to
the claims. . ." be obtained will be determined by the use to
Referring to the accompanying drawing which the salt is to be put. Generally,
forming a part of this specification, in which speaking, for commercial purposes large
the figure is a diagrammatic view of an ap- crystals are desired and these may be pro
O
paratus embodying the principles of my in-duced by employing relatively weaker solu
vention 1 represents any suitables cooling tions, thereby causing a slow formation of
means for the ammonia gases which enter the crystals. If a higher specific gravity of
the absorption system. the solution is employed, the crystals are
5 In order to produce secondary or di-am- precipitated faster but are smaller. The 90
monium phosphate free of the primary or purpose of thus concentrating the product
mono-ammonium phosphate, by direct com- to the density of crystallization is therefore
bination of a solution of phosphoric acid to effect a separation of the di-ammonium
and cooled ammonia gas, it is necessary to phosphate, in that Solid form which is most
40 keep the temperature of the solution below desirable for commerce. Further, it will be 95
80 degrees centigrade. This I accomplish observed by keeping the temperature at or
by passing the ammonia gases, previously below 80° C. that no mono-ammonium phos
cooled by means of the coil 1 through the phate or tri-ammonium phosphate is formed
pipe 3, into the tower 2, provided with any in the liquor, which would not be the case
45 suitable cooling means as the coils 4. The if the solution was permitted to rise to say 100
phosphoric acid may be placed initially in 10° above or fall to say 20° below 80° C.
the tanks 18, and after the operation has it, therefore, follows since no mono-am
ibeen started the phosphoric acid solution 5 monium phosphate nor tri-ammonium phos
from the discharge of the absorption tower phate is present in the liquor, that the crystal
5. 2, is forced by means of the pump 6 continu- produced are entirely free from the sai
ously through any suitable cooling means 7, other salts which would not be the casei
and through the valved pipe 8, back to the these said salts were allowed in the firs
top of the tower 2, where it may be passed place to form in the solution. In othe
over the cooling coils 4, and there absorb the words, it is evident that it would be impos.
55 ammonia gases entering through the pipe 3. sible to precipitate di-ammonium phosphate 113.
 g 995,898

in the presence
carrying of other
down some saltsother
of said without
salts also
ad react in the presence of water, the tempera
mixed with the said di-ammonium phos ture of which is maintained at a point too
phate. low to permit the formation of the primary 55
5
As is well known, ammonium salts are sold Salt; in passing the unabsorbed gases into a
On a guaranteed percentage of ammonia, and second chamber and causing them to react in
are subject to strict State laws. If the com the presence of water; and in constantly cir
mercial product is not of a uniform chemical culating the water solutions through said
composition the appraisement is governed by chambers and in suitably concentrating the 60
O
the ammonia content (NH) of the lowest solution thus formed under a pressure below
grade salt the product contains. Therefore that of the atmosphere, substantially as de
scribed.
it is of great commercial importance to pro 4. The process of producing di-ammonium
duce the secondary salts as free as possible phosphate substantially free from mono 65
from the primary salts.
Of course it will be understood that those ammonium phosphate which consists in pass
ing ammonia and phosphoric acid fumes into
skilled in the art may vary the details of a suitable chamber, in causing the same to
my process without departing from the spirit react in the presence of water the tempera
thereof, and therefore I do not wish to be ture of which is maintained through cool 70
20 limited to the exact minor features set forth, ing means at a point too low to permit the
except as may be required by the claims.
What T claim is:-- formation of the primary salt; in passing the
1. The process of producing di-ammoni unabsorbed gases into a second chamber and
um phosphate (NH), HPO, substantially causing them to react in the presence of
free from mono-ammonium phosphate water; in passing the solution containing the 75
NIH, HPO, which consists in passing am secondary salt from the second chamber into
monia and phosphoric acid into a suitable the first; and in constantly circulating the
chamber; and in causing the same to react water Solutions through said chambers and
in the presence of water at a temperature too in Suitably concentrating the solution thus
low to permit the formation of the primary formed under a pressure below that of the 80
30 salt and in suitably concentrating the solu atmosphere, substantially as described.
tion thus formed under a pressure below that 5. The process of producing di-ammonium
phosphate substantially free from mono
of the atmosphere, substantially as described. ammonium phosphate which consists in pass
2. The process of producing di-ammonium ing ammonia and phosphoric acid fumes 85
35
phosphate substantially free from mono through a series of chambers; in circulating
ammonium phosphate, which consists in water solutions of ammonium phosphate
passing animonia and phosphoric acid into through said chambers; in maintaining the
a suitable chamber; in causing the same to temperature in the first chamber at a point
react in the presence of water at a tempera too low to permit the primary salt to form; 90
ture too low to permit the formation of the
40. primary salt; in passing the unabsorbed in passing the solution from the other cham
bers into said first mentioned chamber and
gases into a second chamber and there caus in suitably concentrating the solution thus
ing them to react in the presence of water; formed under a pressure below that of the
and in passing the Solution from said second atmosphere; and in recovering the secondary 95
chamber into said first chamber and in suit
45 ably concentrating the solution thus formed salt thus produced, substantially as de
scribed.
under a pressure below that of the atmos . In testimony whereof, I affix my signa
phere, substantially as described. ture, in presence of two witnesses,
3. The process of producing di-ammonium
phosphate substantially free from mono SAMUEL PEACOCK.
50
ammonium phosphate which consists in pass Witnesses:
ing ammonia and phosphoric acid fumes into T. A. WITHERSPoon,
a suitable chamber; in causing the same to GEO. B. PITTs,