Patented Nov. 8, 1927.

1,648,656
UNITED STATES PATENT OFFICE.
HERBERT H. MEYERS, OF PITTSBURGH, PENINSYLVANIA, ASSIGNOR TO ARMOUR FER
TILIZER WORKS, OF CHICAGO, ILLINOIS, A CORPORATION of NEw JERSEY.
MANUFACTURE OF DISODIUM PHOSPHATE.
NoDrawing. Application filed January 14, 1927. Serial No. 161,241.
Disodium phosphate as it at present uni tains no sodium pyrophosphate, unless it is
versally appears on the market is in the Subsequently heated to increase still further
form of a white, pure, crystallized solid the P.O., content, when it also may contain
containing twelve molecules of Water of mere traces of sodium pyrophosphate.
is crystallization, its formula being This product may be prepared pure, or, 60.
NaHPO,12HO, in many cases, it may be satisfactorily
placed on the market containing impurities
which shows, therefore, that it contains only present in the phosphoric acid, which are
about 19.9% P.O. in many instances harmless for the pur
0 If it be attempted to increase the P.O. poses to which the disodium phosphate is 65
percentage of such solid by driving off water
of E. there is always the danger putThein general commerce.
of forming a certain proportion of sodium rial is preparedmethod by which this mate
by my improved and novel
pyrophosphate (NaPO), which is for process is as follows:
15 many purposes not as desirable as the diso Phosphoric acid of as great concentration 70
dium orthophosphate. as will permit of mixing in the required
The reason for the formation of this solid amount of Soda ash is used, the actual con
is that some of the water of combination is centration varying with the purity and tem
driven off at the same time as water of crys perature of the phosphoric acid, but, in any
20 tallization is driven off by heating, and, in case, it will contain considerably less water 75
fact, the formation of sodium pyrophos than is necessary to form the
phate starts at slightly over 98 centigrade, NaHPO,12HO
and, so far as is known, no one has suc
ceeded in preparing, by heating, a dehy and to this concentrated phosphoric acid
25 drated disodium orthophosphate without at
the same time producing at least traces of . there is added, in the form of a powder or 80
dust, the required amount of soda ash to
the pyro salt. .. ..
The usual process of preparing disodium form which
the disodium salt, and the mixture,
forms a hot mass of rather high vis
orthophosphate cosity, and, in case the acid contains a cer
30
(NaHPO.12HO) tain amount of impurities which precipitate, 85
is a rather thick slurry, is thoroughly stirred
is to treat dilute phosphoric acid, either so that the reaction is completed.
pure or impure, which contains a sufficient This hot mass is then run into pans, where,
excess of water, with sodium carbonate in after standing awhile, as it cools it crys
35 the right proportion to produce the diso tallizes into a solid mass, which may be go
dium salt, whereupon this solution is fil somewhat porous due to the presence of
tered, if necessary, to remove solid impuri CO, generated by the reaction of the acid
ties, and then the and soda ash.
NaPO.12HO There may also be present some undecom
posed soda ash, if a little excess of this is p5
is allowed to crystalize out in various crys employed, or the reaction has not quite been
tallizing devices, the crystals being washed completed.
and then filtered off and dried, whereupon Such solidified mass is thereupon removed
there is obtained the ordinary disodium
45 phosphate of commerce containing but from the pans, or it may be loosened from
19.9% P.O. the pans while it is somewhat hot to make 100
its removal easy, and it is then ground into
This pantentee has prepared a disodium any size particles it is desired to make, by
phosphate in a very simple manner, which any of the usual methods and apparatus for
contains very materially more PO content grinding.
50 than the
This improved and novel process of pro- 105
NaPO.12HO, ducing disodium phosphate has a number of
marked advantages, since it gives a higher
as it contains less water of crystallization, salt content than the usual method em
and in some cases practically no water of ployed, it is cheaper to prepare and fur
55 crystallization, and at the same time it con nishes a material which is not necessarily 10
 1,648,656

pure, where a pure product is not required, treatment, these impurities are of no con
hence obviating the necessity of removing sequence, and the commercial acid may be
impurities, and consequently cheapening the used to advantage.
process. The product is, therefore, a disodium
5. In this way a salt can be prepared con phosphate containing less than twelve mole 70
taining any desired amount of PO above cules of water of crystallization and which
19.9% up to 40% and over, and if it is actu may have present in it the impurities present
ally desired to make the pure, anhydrous in the materials from which it is prepared;
salt containing 50% PO, this original and the process by which such material is 75
10 \product may be completely dehydrated by produced is the treatment of phosphoric acid
R just as in the usual method, in which of such concentration that in combination
case there probably will be present a mere with the required amount of soda ash and
trace of the pyrophosphate. subsequent cooling, it will set to a solid mass
The preferred method of preparing the which can be disintegrated and shipped for 80
15 salt referred to is as follows: use in the industries, the concentration of
A charge consisting of twelve hundred the acid varying considerably, depending on
parts by weight of commercial phosphoric the product which it is desired to produce,
acid of about 60° Baumé, such as is shipped in regard to the content of PO, and the de
ordinarily in commerce, containing about 53 gree of purity required. 85
20 to 54% by weight of PO, is introduced into I claim:
a wooden stirring tank provided with a pad 1. In the process of making disodium
dile, and to this is added a slight amount of phosphate, mixing together phosphoric acid,
water, say, between two hundred and four a sodium salt of an acid more volatile than
hundred parts by weight, depending on what phosphoric acid, and less water than is neces 90
25 analysis of the final product is desired, and sary to form
then, with constant stirring, one thousand NaHPO,12H.O,
parts by weight of soda ash are added
This mass is then thoroughly stirred, there and permitting the product to cool and
is a considerable evolution of CO, and the harden.
30 precipitation of the impurities in the phos 2. In the process of making disodium 95
phoric acid occurs. phosphate, mixing together phosphoric acid,
Such mass becomes hot and thickens con soda ash, and less water than is necessary
siderably, so that in order to assure that all to form
of the lumps are well broken up, the charge
is discharged, continuously through a small and cooling NaHPO,12HO,
the product in a pan.
100
E. mill such as is used in the paint in 3. In the process of making disodium
ustry, and is delivered directly into an iron
pan, in which it is allowed to cool off and phosphate, mixing together phosphoric acid,
a sodium salt of an acid more volatile than
become crystallized.
40 It is well, however, for the sake of ease phosphoric acid, and less water than is neces 105
and facility in removing it from the pan, to sary to form
loosen it somewhat from the bottom while NaHPO,12HO,
the mass is still slightly soft, and upon such cooling the product in a pan, and loosening
removal, in the form of hard, crystallized
45 material, it is introduced into a cage mill it from the pan during the cooling operation.
or hammer mill and ground to whatever phosphate, 4. In the process of making disodium O
fineness is desired. mixing together phosphoric acid,
In this way, a product is economically soda ash, and less water than is necessary
produced containing between 30% and 40% to form
50 POs, depending upon the amount of water NaHPO,12H.O, 15
added to the phosphoric acid at the start. cooling the product in a pan, loosening it
The product may contain a slight de from the pan during the cooling operation,
ficiency of sodium below that required to and grinding the cooled product.
form the disodium salt, or it may contain 5. In the process of making disodium
55 an excess of Soda ash to any degree pre phosphate, mixing together approximately 20
ferred, but this depends on the use to which 1200 parts by weight of commercial phos
the product is to be put and affects in no phoric acid of about 60° Baumé and contain
way the principle of the method of prepara ing in the neighborhood of 53% by weight of
60
tion. - -
POs, about 200 to 400 parts by weight of
If pure phosphoric acid has been used to Water, and approximately 1000 parts by 125
EE this salt, the analysis, of course, will Weight of soda ash, and cooling the result.
be higher than if the product contains the ing product.
impurities originally present in commercial 6. In the process of making disodium
phosphoric acid, but, for many of the uses phosphate, mixing together approximately
of disodium phosphate, such as boiler-water 1200 parts by Weight of commercial phos. 130
 1,648,656
phoric acid of about 60° Baumé and contain ing in the neighborhood of 53% by weight of
ing in the neighborhood of 53% by weight of PO, about 200 to 400 parts by weight of
PO about 200 to 400 parts by weight of water, and approximately 1000 parts by 15
water, and approximately 1000 parts by weight of soda ash, passing the resulting
5 weight of soda ash, discharging the mass mass through a paste mill and discharging
continuously through a paste mill, and de
livering it into a pan for cooling and crys itloosening
tallization.
into a pan for cooling and crystallization,
the mass from such pan while it
is still slightly
7. In the process of making disodium crystallized material soft, and grinding the hard 20
10 phosphate, mixing together approximately In witness whereoftoI have the required fineness.
hereunto set my
i200 parts by weight of commercial phos hand.
phoric acid of about 60° Baumé and contain HERBERT H. MEYERS.