MANUFACTURING OF OXYCHLORIDE OF LEAD
Year: 1860

page_text: LETTERS PATENT to Jane Ann Herbert, of Guildford, in the County
...of Surrey, Widow, for the Invention of "MANUFACTURING OF OXYCHLORIDE
OF LEAD." A communication from abroad by Ludwig Brumleu, of New
York, in the United States of America.
Sealed the 29th May 1860, and dated the 21st March 1860.
COMPLETE SPECIFICATION filed by the said Jane Ann Herbert at the
Office of the Commissioners of Patents, with her Petition and Declaration,
on the 21st March 1860, pursuant to the 9th Section of the Patent Law
Amendment Act, 1852.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JANE
ANN HERBERT, of Guildford, in the County of Surrey, Widow, send greeting.
WHEREAS I am in possession of an Invention for "MANUFACTURING
OF OXYCHLORIDE OF LEAD," and have petitioned Her Majesty to grant unto
me, my executors, administrators, and assigns, Her Royal Letters Patent
for the same, and have made solemn declaration that it has been com-
municated to me from abroad by Ludwig Brumleu, of New York, in the
United States of America.
NOW KNOW YE that I, the said Jane Ann Herbert, do hereby declare that
the following Complete Specification, under my hand and seal, fully describes
and ascertains the nature of the said Invention, and in what manner the same is
to be performed, in and by the following statement thereof (that is to say):-
To enable others skilled in the art to understand my Invention for the manu-

page_text: facture of white oxychloride of lead, I will describe the same. The process of
making white oxychloride of lead has to be divided into two preparatory
operations; first, the chloride of lead; second, the oxychloride of lead.
The process of making oxychloride of lead is based upon the fact, that
chloride of lead and subacetate of lead decompose each other, and alter
their respective proportions, so that the chloride of lead is formed into the
oxychloride of lead by combining with the superabundant oxyd of lead con-
tained in the subacetate of lead, and the subacetate of lead is formed into the
acetate of lead.
To facilitate the process of making acetate of lead and subacetate of lead,
metallic lead is melted and passed through a perforated vessel or sieve into
water, forming a fine lead wire; by which process the metallic lead is divided
into as much surface as possible to be exposed to the action of the acid and
the atmosphere, as hereafter described. In this state the lead wire is placed
into tubs about five feet diameter and two feet deep, arranged in tiers, so that
liquid in the upper tier empties by a faucet into the second tier, thence into the
third tier, and thence into a separate vessel for further treatment. These tubs
containing the lead wire are then filled full with diluted acetic acid, or a weak
solution of sugar of lead. The acetic acid may be of a strength that one
ounce will neutralize twenty grains of carbonade of potash, or the sugar of
lead in solution of about one hundred pounds in two hundred gallons of water.
After the acetic acid, or the solution of sugar of lead, has remained on the
lead wire contained in the upper tier of tubs for a few minutes, it is then
drawn off on to the lead wire in the second tier of tubs, and retained a few
minutes; then it is drawn off on to the lead wire in the third tier of tubs, and
retained a few minutes, and thence drawn off into a separate vessel for further
use. Thus, after the action of the acetic acid, or the solution of sugar of lead,
the lead wire contained in said tubs is fully exposed to the action of the
atmosphere, causing the lead wire to oxydize on its surface, and forming a crust
of white oxyd of lead on said lead wire. Then by refilling said tubs with acetic
acid, as before stated, the said oxyd of lead formed on the surface of the lead
wire will be rapidly dissolved; the acetic acid may then be drawn off as quick
as possible. By which process the remaining lead wire in said tubs will be
exposed to the action of the atmosphere and oxydize, causing the formation of
white oxyd of lead. The same process may be repeated until all the lead wire
contained in said tubs is reduced or formed into white oxyd of lead. The tubs
may then be refilled with new lead wire, &c., and the same process continued
over and over again.
To perform this process expeditiously, it is obvious in the first place, to

page_text: .
obtain as much surface as possible by dividing the metallic lead into wire to
facilitate the action of the acetic acid on said lead wire. Then the acetic acid
is drawn off rapidly to allow the action of the atmosphère on the lead wire, in
order to facilitate the formation of white oxyd of lead, as before described.
When the metallic lead, by the aforesaid process, has been prepared and
deposited in said tubs, the process of making oxychloride of lead is divided
into two branches.
First, to make acetate of lead for the formation of the chloride of lead,
is thus performed:-A portion of said tubs containing the lead wire are
filled with acetic acid, which after remaining a few minutes acetate of. lead is
formed and is drawn off, as before described, into a separate vessel to be
treated with muriatic acid under continued agitation in said vessel. The
muriatic acid during said process will combine with the lead contained in the
acetate of lead, forming chloride of lead, which will settle to the bottom of
said vessel, leaving the vinegar or acetic acid nearly free, which may be then
drawn off ready to be used over and over again for a similar process, leaving
the chloride of lead to be used for the production or the formation of
oxychloride of lead, as hereafter described in the second process.
Second, to make subacetate of lead for the formation of oxychloride of lead
is thus performed:-The second division of said tubs containing lead wire, and
intended for this process, are then filled with liquid acetate of lead, and reduced
to a strong subacetate of lead, and then drawn off into a separate vessel, and there
under continued agitation the said chloride of lead is introduced into the sub-
acetate of lead. During this process the chloride of lead will combine with the
oxyd of lead contained in the subacetate of lead, and will form white oxy-
chloride of lead until the subacetate of lead will be returned into acetate of lead,
which is then drawn off, and may be used over and over again on lead wire in
said tubs, forming subacetate of lead to be used for making oxychloride of lead,
as herein-before described, until by waste or loss the acetate of lead is reduced,
and has then to be replaced with fresh acetic acid, or acetate of lead. The
acetate of lead may be tested with litmus paper at any time during said process.
The oxychloride of lead thus produced will then settle to the bottom of said
vessel, and may then be prepared for use by washing, drying, and packing for
market.
The oxychloride of lead may also be made by introducing muriatic acid
directly into subacetate of lead as long as the liquid is kept below neutral;
but the very instant that said subacetate of lead becomes acetate of lead, a
mere chloride is precipitated; therefore this process has to be conducted with
great care.

page_text: The subacetate of lead may also be made by dissolving litharge in acetic
acid, and many other alterations or modifications from the foregoing description
may be introduced without departing from the spirit of my Invention; nor is
it possible to give the exact proportions, because the materials used always
vary in quality. The number and size of the tubs in each tier or division, &c.,
may be increased or diminished in size to suit the locality or the idea of the
manufacturer, &c.
What I claim as my Invention, and desire to secure by Letters Patent,
are as follows:-
First, that chloride of lead and subacetate of lead will decompose each
other, and cause the formation of oxychloride of lead and acetate of lead.
Second, the whole rotary process as set forth in the foregoing description
for the purpose of manufacturing oxychloride of lead from chloride of lead and
subacetate of lead, leaving the liquid free to be used over and over again for
the same purpose.
Third, the manufacture of oxychloride of lead in any manner performed by
decomposition of subacetate of lead, by chloride of lead, or muriatic acid.
In witness whereof, I, the said Jane Ann Herbert, have hereunto set my
hand and seal, this Twenty-first day of March, in the year of our
Lord One thousand eight hundred and sixty.
JANE ANN HERBERT. (L.S.)