UNITED STATES PATENT OFFICE.

JOHN P. WALKER, OF ROLLA, MISSOURI.

PROCESS OF MAKING PRECIPITATED BARIUM SULFATE.
1,040,594. Specification of Letters Patent.
IPatented Oct. 8, 1912.
NoDrawing, Application filed August 17, 1911. Serial No. 644,629.
To all whom it may concern. The tank and its contents are then heated
Be it known that I, JoHN P. WALKER, to a desired temperature and, as a result,
a citizen of the United States of America, the barytes and sulfuric acid produce a ba
residing at Rolla, in the county of Phelps lytic and sulfuric acid solution in which 8)
and State of Missouri, have invented certain such substances as silica settle to the bottom
new and useful Improvements in Processes of the primary tank, leaving the main body
of Making Precipitated Barium Sulfate, of of the solution free of such foreign sub
which description.
exact the following is a full, clear, and stances.
O My invention relates to a process of mak The next step in my process consists in
ing precipitated barium sulfate of a high Withdrawing the barytic and sulfuric acid
degree of purity, very finely divided, and Solution in any suitable manner from the
especially adapted for such uses as paints, primary tank and introducing it into a sec
enamels, wallpapers, and writing papers. ondary tank in which it mixes with water
5 The generally known and common method and by reason of which mixture there is com 70
of making precipitated barium sulfate is as plete precipitation of all of the barium in the
follows: Mineral barytes is first mixed with Solution as precipitated barium sulfate. The
fine coal and heated to a high degree of quantity of Water with which the barytic
temperature in a crucible, retort, or rotary and sulfuric acid solution is mixed in the
20 furnace, with the result that the barium sulSecondary tank must be sufficient to cause
fate in the mineral is reduced to barium complete separation of the barium from the 75
sulfid. The barium sulfid is then subjected Sulfuric acid and its precipitation as barium
Sulfate, and experiments have determined
to the action of hydrochloric acid, with re that
sultant reaction of the barium sulfid and the the most satisfactory results are ob
25 production of a solution of barium chlorid. tained when the volume of water utilized is 80
in the neighborhood of fifty per cent. (50%)
Then, to complete the process, sulfuric acid of the volume of the solution mixed there
is added to the barium chlorid solution, and with. The water is preferably placed in the
the desired precipitated barium sulfate is
obtained. Secondary tank before the barytic and sul
30 The process just described is an expensive furic acid solution is delivered thereinto, but 85
one, owing to the high heat necessary to the reverse course may in some instances be
redice the barium sulfate to barium sulfid, followed; or, in some instances, the water
the necessity for the use of an expensive re and solution may be delivered into the sec
agent-hydrochloric acid-and the con ondary tank at the same time. I may here
recite it as my belief that the reaction of 90
sumption of large quantities of sulfuric acid sulfuric
required for the carrying out of the process. water on acid on mineral barytes and of
the barytic and sulfuric acid solu
It is the object of my invention to provide tion is one indicated substantially by the
a process by which precipitated barium sul following example:
fate may be produced much less expensively
40 than by the process I have described. While BaSO-HSO, Ba(HSO), 95
it contemplates the employment of sulfuric In the foregoing example, the action of
acid as a solvent, it provides for the saving the sulfuric acid on the mineral barytes is
or recovery of the greatest percentage of the shown
sulfuric acid, this being one of the main arrow, by
45 economical and
the compound following the upper
the result of the reaction when 100
features in my process. the barytic sulfuric acid solution is mixed
In carrying out my process, I pursue the with the water is shown by the compounds
following steps: The mineral barytes from preceding the lower
which the precipitated barium sulfate is to is given to indicate aarrow. This example
50 be derived is first crushed to a requisite de my process, since it shows that economy
point of
no
in
sulfuric
gree of fineness and placed in a primary acid is used up or lost in the action on the 105
tank, of suitable construction, that is capa pure mineral barytes, but is liberated com
ble of resisting the action of strong sulfuric pletely from the and
compound by the use of the
acid. In this tank, I place strong sulfuric water employed the consequent precipi
55 acid, preferably of a strength above E. tation of the barium sulfate on one hand O
six per cent. (96%), and preferably of suffi and only the dilution of the sulfuric acid on
cient quantity to cover the crushed mineral. the other hand. The only chemical loss of
2 1,040,594
acid is that resulting from the action of the that I claim the use of the process when 60
employed in making precipitated barium
acid on impurities that, may be present in sulfate in the manner described, and which
the mineral barytes, such, for instance, as may afterward be employed in a suitable
iron and alumina. manner in making “lithopone'.
The next step in my process consists in 65
the removal of the diluted sulfuric acid from I1. claim:--The process of making precipitated ba
the secondary tank to permit access to the rium sulfate, which consists in subjecting
precipitated barium sulfate at the bottom of
the tank. The precipitated barium sulfate mineral barytes to the action of strong sul
may then, if it is desired to render it free of sulfuric acidthereby
furic acid, producing a barytic and 70
acid, be washed with water and, if neces ing the barium sulfateand solution, then precipitat
sary to remove all traces of free acid, an diluting the solution with water.solution
in such by
alkaline wash may be employed. After 2. The process of making precipitated ba. . . .
such washing, the precipitated barium Sul rium sulfate, which consists in subjecting
fate may be dried before being placed on mineral barytes to the action of sulfuric 75
the market; or it may be sold in a moist acid of a strength above ninety-six per
state when it is to be used in the manufac
ture of paper, it being most desirable that cent, thereby producing a barytic and sul
, the barium sulfate should not be dried be the barium solution,
furic acid and then precipitating
sulfate in such solution by dilut 80
foreAsitpreviously
enters intomentioned,
the manufacture
one ofofthepaper.
eco ing3.the solution with water.
nomical features of my process is that it rium sulfate, The process of making precipitated ba
provides for the sulfuric acid utilized in mineral baryteswhich to the
consists in subjecting
action of strong sul
carrying out the process being recovered furic acid, thereby producing
and reused. The dilute acid solution that sulfuric acid solution, heating asaid barytic and 85
is separated from the barium sulfate in the and then precipitating the bariumsolution,
secondary tank may be readily concentrated solution by diluting the solution with inwater. the
by any usual or ordinary process suitable 4. The process of making precipitated ba
for such concentration until the acid is of rium sulfate, which consists in subjecting
the desired strength for re-using in carrying barytes to the action of strong sul 90
out my process, or of a strength that will mineral furic acid in a suitable receptacle, then re
render it salable for other uses. -
My process may be used in the manufac moving to
said solution to another receptacle
separate it from matter foreign to the
ture of a paint material known commer
baytic and
cially as “lithopone'; and, if I desire to ited in said vessel, Sulfuric acid elements, depos
and then causing precipi 95.
make “lithopone” by my process, I may not tation of the barium in the solution by di
wash all sulfuric acid from the precipitated
barium sulfate, but leave sufficient to form luting the Solution with Water.
the soluble sulfate of zinc upon the addi rium stilfate, which consistsprecipitated
5. The process of making
in
ba-.
subjecting
tion of the required amount of zinc. The mineral barytes to the action of strong sul 100
zinc may be added in the form of oxid, the furic acid, thereby, producing a barytic and
contents of the tank agitated, and hydrogen sulfuric acid solution, then precipitating the
Sulfid gas passed until the zinc is changed barium sulfate in such solution by diluting.
to Zinc sulfid; or I may add instead of the the solution with water, and then with
oxid of zinc any salt of zinc or metallic drawing the diluted sulfuric acid from the 05
Zinc, or suitable material containing zinc,
and pass hydrogen sulfid gas; or I may add precipitated
6. The barium
process of sulfate. precipitated ba
making
Some excess Zinc oxid; that is, zinc oxid in rium sulfate, which consists in subjecting
excess of that which is precipitated as sulfid. crushed or finely divided mineral barytes to
When the current of gas is shut off, allow action of strong sulfuric acid, thereby 10
ing the contents of the tank to settle, the the producing a barytic and sulfuric acid solu
Zinc sulfid and barium sulfate will settle in tion,
an intimate state of mixture and may be re fate inandsuch then precipitating the barium sul
solution by diluting the solu
moved from the tank, dried and sold
“lithopone”, or in the production of “lith as tion with water. JOHN P. WALKER.
opone’. In the presence of -
My process being usable as specified in HENRY CIMo,
making paint material such as is known as W. D. JoNES.
“lithopone”, I desire it to be understood