Improvements in the Manufacture of Nitrate of Ammonium and of a Resulting Bye-product.
Year: 1889

page_text: Date of Application, 28th May, 1839
Complete Specification Left, 26th Feb., 1890-Accepted, 12th Aor., 1890
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Nitrate of Ammonium and of
a Resulting Bye-product.
I CHARLES ANTHONY BURGHARDT of 35 Fountain Street in the City of Manchester
Analytical Chemist, do hereby declare the nature of this Invention to be as
follows:-
My Invention relates to the manufacture of ammonium nitrate and has for its
object to facilitate the production of such salt and to lessen the cost of the same. I
produce the said salt by a reaction between nitrate of lead and ammonium sulphate
whereby I obtain ammonium nitrate and also sulphate of lead as a bye-product.
When carrying my Invention into effect I dissolve in separate vessels ammonium
sulphate and nitrate of lead using as small a quantity of water in each case as would
be suitably convenient. The amount of nitrate of lead should be proportioned to the
amount of ammonium sulphate so as to be chemically equivalent to the same. I mix
the two solutions and agitate the same when a double decomposition of the two salts
quickly takes place. The nitric acid leaves the lead and displaces the sulphuric acid
in the ammonium sulphate thus by combining with the ammonium forming ammonium
nitrate whilst the liberated sulphuric acid enters into combination with the lead and
forms the compound known as sulphate of lead. The sulphate of lead is permitted to
subside as a precipitate and the supernatant liquid which is a solution of ammoniumi
nitrate is drawn off. I concentrate this solution until the crystallising point of
ammonium nitrate is reached and allow the salt to separate by crystallisation as in
ordinary chemical processes. I drain or dry the salt in any suitable manner. The
sulphate of lead precipitate is well washed taking care to dissolve as little as possible
of the salt. To lessen the tendency of the washing water to dissolve the said sulphate
a little free sulphuric acid or a proportion of ammonium sulphate may be added to
such water. The washings may be utilised wholly or partially in the preparation of
the solution of ammonium sulphate for mixture with the nitrate of lead solution as
aforesaid.
The bye product which I obtain by my process is sulphate of lead of fine quality
which may be used as a pigment or be reduced to the metallic state or be otherwise
utilised.
1 1
050
1000
DUTTON & FULTON,
1, St. James Square, Manchester, Agents.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Nitrate of Ammonium and of
a Resulting Bye-product.
I CHARLES ANTHONY BURGHARDT of 35 Fountain Street in the City of Manchester
Analytical Chemist do hereby declare the nature of this Invention and in what
manner the same is to be performed to be particularly described and ascertained in
and by the following statement :-
My Invention relates to the manufacture of Ammonium Nitrate and has for its
object to facilitate the production of such salt and to lessen the cost of the same. I
produce the said salt by a re-action between lead nitrate and ammonium sulphate
whereby 1 obtain ammonium nitrate and also lead sulphate as a bye product. When
carrying my Invention into effect I dissolve in separate vessels ammonium sulphate
and lead nitrate using as small a quantity of water in each case as would be suitably
convenient. The amount of lead nitrate should be proportioned to the amount of
ammonium sulphate so as to be chemically equivalent to the same. I mix the two
e4d. 1

page_text: solutions and agitate the same when a double decomposition of the two salts quickly
takes place. The nitric acid leaves the lead and displaces the sulphuric acid in the
aminonium sulphate thus by combining with the ammonium forming ammonium
nitrate whilst the liberated sulphuric acid enters into combination with the lead and
forms the compound known as lead sulphate or sulphate of lead. The lead sulphate is
permitted to subside as a precipitate and the supernatant liquid which is a solution of
ammonium nitrate is drawn off. To produce 100 tons of ammonium nitrate about
206 tons of lead nitrate and 82 tons of ammonium sulphate are required, but I
prefer to test the resultant to ascertain whether or not the two salts are in the required
equivalent proportions.
For this purpose I take two portions of the ammonium nitrate solution and add to
one portion a few drops of ammonium sulphate solution. If a white precipitate of
lead sulphate results sufficient ammonium sulphate has not been used and therefore a
further quantity of a solution of that salt should be added carefully to the bulk of the
solution of ammonium nitrate until a sample remains clear after the addition of
ammonium sulphate solution. To the other sample portion I add a few drops of lead
nitrate solution when a slight precipitate will be formed if a sufficient quantity of
ammonium sulphate has been used but if the sample solution remains clear more
of the last named salt must be added carefully as aforesaid. If a fixed quantity of
sample solution be taken for each test and a testing solution of fixed strength be
used and be added to the sample solution in the same proportion for all the tests the
results will be more useful for comparison and more instructive to the operator who
will be able to see at once whether or not the result of the operation has been
satisfactory. When a satisfactory re-action has been obtained the clear supernatant
liquid is syphoned off or run off or withdrawn by suitable means from the precipitated
lead sulphate. After the bulk of the clear liquid has been drawn off the liquid
remaining in company with the precipitate may be separated by the aid of a filter
press. I have found that a sinall quantity of lead sulphate dissolves in the ammonium
nitrate solution. This may be removed by means of ammonium bi-carbonate.
Previous to the treatment with this salt the solution may be concentrated to reduce
its bulk. To the solution add ammonium bi-carbonate in the proportion of one
part for each one and three tenth parts of metallic lead contained in the solution. The
mixture is then well stirred or agitated with or without the use of heat. The lead is
thrown down as an insoluble precipitate in the form of basic lead carbonate. The
clear solution of ammonium nitrate is then concentrated to the crystallising point and
kept for some time at a temperature of about 110° Centigrade. The fused mass whilst
still fluid may be run into kegs or other packages or receptacles and by remaining
solid therein will be protected to some extent from deliquescent action. The sulphate
of lead precipitate is well washed taking care to dissolve as little as possible of the
salt. To lessen the tendency of the washing water to dissolve the said sulphate a
little free sulphuric acid or a proportion of ammonia sulphate may be added to such
water. The washings may be utilised wholly or partially in the preparation of the
solution of ammonium sulphate for mixture with the nitrate of lead solution as
aforesaid. The bye product which I obtain by my process is sulphate of lead of fine
quality which may be used as a pigment or be treated with potassium bichromate or
sodium bichromate to produce chrome yellow or be otherwise utilised.
Having now particularly described and ascertained the nature of my said Inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
:-
1) The process for the production of ammonium nitrate substantially as set forth.
2) The production of ammonium nitrate by a re-action between ammonium sulphate
and lead nitrate and the recovery as a bye-product of lead sulphate.
Dated thin 95th J
J
T1
DUTTON & FULTON,
1, St. James Square, Manchester, Agents.