0a. so, 1928.

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1,689,547.

TRI'-SODIUM PHOSPHATE.

Filed Aug. 8, 1925

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1,689,547

Patented Oct. 30, 1928.

UNITED STATES PATENT OFFICE. ,

JOHN R. CABOTHEBS, 0F ANNISTON, ALABAMA, ASSIGLIOB TO FEDERAL PHOSPHOBUS

COMPANY, OF BIRMINGHAM, ALABAMA, A COBIOP'ATION OF ALABAMA.

METHOD FOR MAKING TERI-SODIUM PHOSPHATE.

Application ?led August a, 1925. Serial m3. mass.

This invention relates to a method for by the chemical formula Na,PO.12H,O,

from which an inspection shows there is

making tri-sodium-phosphate, especially present
approximatel 57% water of crystaladapted to the use of concentrated phos

phoric acid.
5

I ,

lization. I proceed by adding sodium car

strong phosphoric acid simul

The object is td provide a method which bonate and
in a mixingtank, where vdi-sodium
requires less e uipment and is therefore less taneously
phosphate is formed. By strong phos
costly, and w ich at the same time, has

acid I mean an acid of such concen

greater e?iciency than existing methods phoric
tration
that it will not be necessary to em~
which are adapted to the use, of dilute phos

ploy any evaporation step in my process,

the water with the phosphoricacid, the
With these and other objects in view, the but
di-sodium
phosphate ?lter press water, and
invention consists in the novel details of a
that necessary to dissolve the caustic soda"
method embodying features of construcw will
provide enough to supply the water of
tion and combination of equipment consti
16 tuting my invention, more fully disclosed crystallization in the product. This acid 70
and particularly set forth in the appended may range from 50% to 75% HsPO? de
pendiInIg on operatingconditions, and while
,PO, may be continuously used pro
Referring to the accompanying drawing, 50%
vided
the
di-sodiuin ?lter press water be re
forming part of this speci cation, the appas
20 ratus comprises an acid tank 1 containing duced in proportion to the additional water
strong phosphoric acid, which is neutralized added by such acid, it is preferable to employ
by the addition of sodium carbonate to di acid of higher concentrations. The phos
sodium phosphate solution in mixing tank phoric acid and sodium carbonate are added
2, from which the solution passes through until di-sodium phosphate is formed, having,

10 phoric acid.

claims.

25 ?lter 3 into the receiving and mixing tank 4, in case iron tanks are used, a slight excess of
where caustic soda solution is added from sodium carbonate. Where acid resistant
dissolving tank 5.' After thoroughly mix-' tanks are used no excess of sodium carbonate
ing the resultant tri-sodium phosphate solu is needed. The chemical reaction is repre
tion in tank 4 it is assed through ?lter 6 and sented by the following equation:
30-,into receiving ta ,7, from which it ?ows
through crystallizers 8 which may have arti
?cial coolers 81 if desired. From the crystal-
lizers the crystals and a portion of the mother The solution is heated approximately 100
liquor pass into the centrifuge 9 where the ' C. by a heating coil 14 to expel all dissolved
35 crystals are de-watered. The mother liquor carbonic acid (00,) and to coagulate the
passes from the centrifuge 9 into the sump precipitate of iron, aluminum, calcium or
tank 10 and thence is returned by pump 11 magnesium phosphates, which will form if
to mixing tank 2 or'4, according to opera these impurities be present. In case this so
tion requirements, while the crystals pass lution is higher than 1.30-1.36 speci?c grav
40 ?rst through dryer 12" and then through ity at 85 0., wash water or mother liquor 95
be added to reduce the speci?c grav
cooler 13, after which they may be shipped should
as dried or screened crystals in any well ity to that mentioned. From the mixing
known manner. The elements of the, fore tank 2 the di-sodium phosphate solution
going apparatus are conveniently illus-\ passes through a ?lter of any standard type
45 trated as they constitute severally standard to remove the precipitate from the solution. 100
The clear solution of di-sodium phosphate
equipment.
1
In order that the operation of my method is then mixed with a caustic soda solution to
carried out in my apparatus may be clearly form tri-sodium phosphate. This reaction

understood and practiced by those skilled in is represented by the following equation:

50 the art, I will outline the procedure in NaJIPO, 121L120 +NaOH=

volved. In the production of tri-sodium phos

phate a large percentage of the compound

'

106

Na3PO,,.12H2O+H,O

is water which is present as water of crystals Caustic soda solution may be prepared by

lization. The compound is represented dissolving solid caustic, or commercial caus

1,689,547

tie solution may be used. The strength of

the solution may be varied, but if made from
solid caustic a solution containing approxi

mately 70-72% NaOH is preferred. Since

Having thus described my invention, what

claim as new and desire to secure by Let
ters Patent, is :

_
rocess for the

_ l. The hereindescribed

commercial caustic soda solution contains production of tri-sodium p osphate, whlch 70"
only approximately 50% NaOH, this may consists in subjecting sodium carbonate to
not be used exclusively; however, a mixture the action of phosphoric acid having more
of solid caustic dissolved in the commercial, than 50% HsPO4 to form di-sodium phos
solution may be' satisfactorily used. The phate, then adding su?icient caustic soda to
10 tri-sodium phos hate solution is then ?ltered
convert said dil-sodium phosphate into tri .75
in any standar ?lter to remove solid mat
ter introduced b the caustic, as well as an

precipitate whic

'ay result from the addi

tion of caustic so a to the di-sodium phos

phate solution. In the addition of caustic

soda, su?lcient is added until titration with
half normal acid of a sample of the solution
being causticized, shows a relation of the
end point of phenolphthalein and the end
points of phenolphthalein and methyl or

20

an e

sodium phosphate, substantially as de

scribed.

2. The hereindescribed process for the

production of tri-sodium' phosphate, which

consists in subjecting sodium carbonate to
the action of stron phosphoric acid havingv
more than 50% ,PO, to form .di-sodium

phosphate, then removing all solid matter,

then adding caustic soda to convert said d1
sodium phosphate to tri-sodium phosphate,

varying between 0.53 and 0.56, arrived substantially as described.

. at by dividin the reading from the phenol

phthalein en point, by t e sum of the phe

3. The hereindescribed

rocess for the

production of tri-sodium osphate, which

nolphthalein and methyl orange end points. consists in subjecting sodlum carbonate in

This relation of titrations is a simple and

to the action of strong ghosphoric
quick means of controlling the addition of solution,
acid having more than 50% HSP ,, to form
caustic. After causticizing, the solution. di-sodium phosphate, then remov'
all
should have a speci?c gravity from 1.36'to solid matter, then adding caustic so a so
1.40 at 85 C. for best operation. After ?l lution to convert said di-sodium phosphate
tration, the solution is run into any suitable into tri-sodium phosphate, then cooling said
crystallizing uipment. The use of a con tri-sodium- phosphate solution until crystals
tinuous. 'crysta izer is referred, as thereb of tri-sodium phosphate form, substantially

30

a continuous feed and 'scharge is obtaine . as described.

It is desirable to add a certain percentage of

mother liquor, from

4. The hereindescribed
revious crystalliza production
of tri-sodium

rocess for the

osphate, which

100

tions, to aid in suspen in the crystals and consists in subjecting a sodium carbonate so
to facilitate han/dling. g.lhe quantity of - lution
to the action of stron phosphoric
mother liquor added Wlll vary depending on acid to ,form a di-sodium phospiate
solution

operating conditions at the time, .andsthe

approximately 1.33 speci?c gravity at 85
only means of judging is the fact that crys- - of
(1., t en'removing all so id matter, then add
tals produced are of the size desired, and in? caustic soda solution to convert said di
hand e readily in the crystallizer. From the so ium phosphate into tri-sodium phos

(0

crystallizer, the crystals pass into a centri

_fuge where they are d'e-watered before pass

15 mg to the dryer. '

. "

ince the I melting point of tri-sodium

phate, then cooling said tri-s'odium phos

phosphate form, thenseparatin said crys

105

phate solution until crystals of tri-sodium

'110

tals from the accompanying s?ution', sub

phos hate is very' ow, it is necessary to stantially
as described.
avoiw overheating and either melting or
5. The hereindescribed rocess for the ,

partly de-hydrating the crystals. _ In order

of tri-sodium osphate, which
that the dried crystals may be .in the best production
consists in subjecting SOdluIII carbonate to 115
physical condition, it is preferable that they the action of stron phosphoric acid to form
passed through a cooler aftenthe dryer, 1a di-sodium phosg ate solution of approxi~ I

that they may be at atmospheric tempera mately 1.33 speci c gravity at 85 0., then
ture when stored or packed.
55
The solution, elimlnated from the. crys removing all solid matter therefrom, then
" tals in the centrifu e, ?ows to a sump tank adding caustic soda solution to convert said
di-sodium phosphate into tri-sodium phos
from w ere it may
e returned by pump 11, phate in a solution of ap roximately 1.38
4 as conditions of pper speci?c gravity at 85 _C., t en cooling said
[nation require._
'~ $By the use of strong phosphoric acid and tri~sodium phosphate solution until crystals
the apparatus as described, I am enabled to of tri-sodium (phosphate are formed, then
separatingso1sai
"cr?stals from the accom
roduce .tri-sodium phosphate more ef panying
ution, t on d in said 0 stals

- to mixing tank 2 or

.cientlyv and less expensively than otherwise, substantially as described.y g

ry
,
"smce the expensive evaporation step em
6.
The
hereindescribed
continuous
.proc
ployed in\ common practice is eliminated.
ess of 'producing tri-sodium phosphate crys

120

meme-7v

3'

talsg which consists in producing a. tri- and returning the mother liquor to the tri
sodium phosphate solution from strong acid, sodium phosphate solution, substantially as
continuously feeding" such tri-sodium phos- described.

phete solution having an approximate spe~

In testimony whereof I al?x my signa

ci?o gravity of 1.36 to 1.410v at 85 vG. to a ture.

crystallizer, and continuously Withdrawing

crystals of tri-sodium phosphate therefrom,

JOHN N. CAROTHERS.