S. W.

, ANDERSON & G, C, KAAR,

PROCESS OF PRODUCING LEAD NITRATE SOLUTIONS,
APPLICATION FILED DEC, 27, 1912.
1,083,911. Patented Jan, 13, 1914,

LEAD Rs CoNG. HNo.

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ATTORWEY
 UNITED STATES PATENT OFFICE.
SAMUEL. W. ANDERSON AND GROVER. C. KAAR, OF SPOKANE, WASHINGTON.
PROCESS OF PRODUCING LEAD-NITRATE SOLUTIONS.

1,083,911. Specification of Letters Patent. Patented Jan. 13, 1914.

Application filed December 27, 1912. Serial No. 738,940.
To all whom it may concern: silicious sediment and is purified by means
Be it known that we, SAMUEL W. ANDER of alkalis such as sodium carbonate or so
SON and GROVER C. KAAR, citizens of the dium hydroxid. The precipitating or puri
United States, residing at Spokane, in the fying agent is added in two instalments so 60
5 county of Spokane, State of Washington, that the iron is completely precipitated as
have invented certain new and useful Im hydroxid and none or but little of the lead
provements in Processes of Producing Lead precipitated. There results a lead nitrate
Nitrate Solutions, of which the following is solution which is relatively pure and which
a specification. can be used directly for the production of 65
O This invention relates to the production of lead pigments. From this lead nitrate solu
lead pigments from lead nitrate solutions tion the lead is precipitated in an insoluble
obtained by the action of dilute nitric acid form. This insoluble form may be that of
on lead sulfid ores; and it comprises a proc the lead chromate or the basic lead car
ess of obtaining such pigments wherein the bonate. In either case the precipitating 70
5 filtrates resulting from the precipitation of agent in solution is added to the lead nitrate
such pigments are used repeatedly for pur solution and the insoluble lead compound
poses of diluting the concentrated nitric acid thus precipitated. . This precipitate is fil
to furnish the necessary dilute acid for dis tered, the filtrate separated from the pre
solving the lead ore; it further comprises cipitate, the precipitate washed, and then 75
20 a process of precipitating lead from lead taken to the drier for drying. The wash
nitrate solutions by a precipitant such as water resulting from the washing of the pre
sodium chromate, or a mixture of sodium cipitate consists of a dilute solution of so
hydroxid and carbonate, in which the wash dium nitrate and, in making the chromate,
water used for washing the precipitate is nitric acid. It is too dilute for evapora 30
25 returned and used repeatedly for dissolving tion and recovery of the nitrate contained
the solid precipitant and forming the pre in it. We have found, however, that it can
cipitating solution used in precipitating the be used advantageously for dissolving the
lead; and it further comprises combinations solid precipitant, being thus returned to
of these two processes; all as more fully the reaction, repeatedly, until its concentra 85
30 hereinafter set forth and as claimed. tion has been sufficiently increased to make
In our companion application Serial Num its evaporation economically possible.
ber 738,939 of even date we have described The filtrate resulting from the filtration
and claimed a process of dissolving lead sul of the lead precipitate is a dilute solution of
fid ores by means of dilute nitric acid toform sodium nitrate, but much stronger however, 90
35 lead nitrate solutions, and of purifying such than that of the wash water. If the lead
solutions from accompanying iron nitrate chromate has been precipitated by sodium
and other impurities to give a pure or rela bichromate, nitric acid is also present. We
tively pure lead nitrate solution. This proc have found that this filtrate can with ad
ess, it is not deemed necessary to describe in vantage be returned to the process and used 95
40 detail here, reference being had to said ap in diluting the concentrated nitric acid to
plication for a more extended description give the 7% solution used in dissolving the
of the same, but the process described briefly lead ore. The concentration of the filtrate
is as follows: Concentrated nitric acid is can be thus gradually increased until it be
diluted with dilute nitric acid or a dilute comes sufficiently concentrated to make its 00
45 solution of sodium nitrate to give a seven evaporation profitable. Moreover the pres
per cent. by weight nitric acid solution. ence of the sodium nitrate in the dilute acid
This solution is used at a temperature of used for dissolving the ore is advantageous
from 150 to 165° F. to dissolve lead sulfid since it increases very materially the con
ores to form lead nitrate solutions, hydro centration of the nitrate ions in such acid 105
50 gen sulfid being formed during the reactionand thus makes the acid more effective
and reacting with part of the nitric acid to without the presence of an excess of nitric
set free sulfur and oxids of nitrogen. These aClO.
oxids of nitrogen are recovered and may be The series of reactions taking place in the
used in part for diluting the concentrated. complete process of the present invention
55 nitric acid. The lead nitrate solution so
10
and in the novel cycles of it are shown dia
obtained is separated from the sulfur and | grammatically on the accompanying draw
 2 1,083,911
ing. In this illustration the concentrated and washing of these precipitates are those 50
nitric acid diluted with the filtrate contain already referred to. Whether sodium bi
ing a small amount of sodium nitrate is chromate or a mixture of sodium carbonate
used as a 7% nitric acid solution to dissolve and hydoxid is used there results a dilute
the lead ore. The impure lead nitrate so solution of sodium nitrate, and also nitric
lution is purified, precipitated, and filtered, acid in the case of the bichromate, from the 55
the filtrate obtained being that referred to interaction of the lead nitrate and the solu
for diluting the concentrated acid. The ble sodium salt.
precipitate is washed and taken to the drier In the filtrate from the lead chromate.
10 solid
and the wash water used for dissolving the
precipitant and thus form the precipi
there is also present more or less nitric acid;
but in such a dilute condition that its re 60
tating solution. It will of course be under covery directly would be unprofitable.
stood that only so much of the wash water Moreover, in recovering the sodium nitrate
and filtrate can be returned to the process contained in the solution this nitric acid
15 as are necessary; and that a greater or less would need to be first neutralized and thus
amount may be removed continuously or lost; whereas by returning the whole fil 65
intermittently as the concentration ap trate to the original nitric acid solution it
proaches that at which evaporation and re not only serves to dilute the concentrated
covery of the sodium nitrate is profitable. acid, but is itself used over again and thus
20 theIfbasic
the lead is precipitated in the form of
carbonate there is used as a pre
saved. Usually, after being used over two
or three times its concentration is such that 70
cipitating agent a solution containing so it can be profitably, evaporated and the so
dium carbonate and hydroxid in such pro dium nitrate thus recovered. This sodium
portions that the resulting precipitate will nitrate can be used for the production of
25 have the composition of white lead cor the concentrated nitric acid by treating the 75
roded by the old Dutch process. If the same with sulfuric acid.
lead is precipitated as chromate a solution We claim:- e
of sodium bichroirate is used. The follow 1. A method of preparing a solution of
ing equations illustrate these reactions. nitrate of lead which comprises digesting :
30
For basic carbonate. crude lead sulfid with a solution containing
about 7% of nitric acid, together with a 80
nitrate of an alkali metal.
2. A method of preparing a solution of
For normal chromate.
nitrate of lead which comprises digesting
35 crude lead sulfid with a solution contain
II. 2Pb(NO)--NaCrO.--H,O= ing about 7% of nitric acid, together with 85
2PbCrO+2NaNO+2HNO, purifying a nitrate of an alkali metal, and thereafter
said solution from compounds
In either case sufficient of the precipitat of the heavy metals, other than lead, by the
40 ing agent is added to throw down all of the addition of successive Small quantities of
lead in the form of the insoluble precipi an alkali. 90
tate. - The precipitate after filtering is In testimony whereof we affix our signa
washed and may be then taken to the drier tures in presence of two witnesses.
for removing its accompanying water. The SAMUEL W. ANDERSON. . .
45 pigments are thus obtained in a pure and S. GROWER C. KAAR.
dry form starting with the ore itself and
without first smelting the ore and convert Witnesses:
ing it into metallic lead. The filtrates and L. L. WESTFALL,
wash waters resulting from the filtering WILLIAM H. KAYE.