Improvements in the Manufacture or Separation of Ammonium Nitrate and Sulphate or Chloride of Sodium and of Potassium.
Year: 1890

page_text: Date of Application, 16th Jan., 1890
Complete Specification Left, 7th Oct., 1890-Accepted, 8th Nov., 1890
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture or Separation of Ammonium
Nitrate and Sulphate or Chloride of Sodium and of Potassium.
I CARL ROTH of Charlottenburg in the Empire of Germany Chemist do hereby
declare the nature of this invention to be as follows:-
:-
According to this invention equivalent quantities of sulphate of ammonium and
either nitrate of potassium or nitrate of sodium may be either heated together in a
watery solution or melted together in a dry state below the temperature at which
decomposition of ammonium nitrate takes place the result being as is well known
that ammonium nitrate and a sulphate of the alkali employed are produced. I
effect the separation of the said products by means of thermal moment or force 1
have discovered that watery solutions of ammonium nitrate at a temperature above
110° Celsius (one hundred and ten degrees of Celsius) lose their power of dissolving
sulphate of potassium or sulphate of sodium in proportion as the solvent becomes
volatilized owing to the heat and in the same degree as the temperature advances
to the point at which all the water is driven off I have further discovered that molten
ammonium nitrate (free of water) is capable of dissolving traces only of alkaline
sulphates.
If the heating be carried above 110° Celsius until all, or practically all, of the
water is driven off or yet higher until the temperature at which ammonium nitrate
begins to be decomposed is nearly reached or if equivalent quantities of sulphate of
ammonium and nitrate of potassium or of sodium are heated together without the
"presence of water and the temperature of the melt be maintained under ordinary
pressure of the air for say an hour or thereabouts at preferably between 160° and
200° Celsius (one hundred and sixty and two hundred degrees Celsius) or at the
corresponding degrees of temperature in presence of increased or diminished pressure
or in absence of the pressure of the air the liquid ammonium nitrate will lie above
the alkaline sulphate which sinks to the bottom of the vessel in a solid form and it
will be easy to separate the ammonium nitrate from the alkaline sulphate for example
by siphoning, or by means of a heated hydro-extractor or by any means suited to the
separation of liquified crystal masses from a solid residuum. If during the reaction
water be present it is necessary to drive it off either by heating to above 110° Celsius
under the ordinary pressure of the air or to the corresponding degrees of heat under
diminished pressure or vacuum to such an extent that it shall not have the power
of dissolving the alkaline sulphate to an extent prejudicial to the purpose which the
resulting ammonium nitrate is to serve.
As a solution consisting of equal parts of ammonium nitrate and water under
ordinary or atmospheric pressure boils at about 110 degrees Celsius and at this
temperature is capable of absorbing 15 per cent. or thereabouts of sulphate of sodium
or 10 per cent. or thereabouts of sulphate of potassium this degree of temperature is
the lowest admissible limit taking into consideration the fact that for some manu-
facturing purposes nitrate of ammonium containing the abovenamed percentage of
the alkaline sulphates is capable of being used.
The enrichment in nitrate of ammonium of the liquid above the solid product due
to the increasing separation of the alkaline sulphate is in proportion to the increase
of temperature above 110 degrees Celsius and attains its maximum when the
temperature at which ammonium nitrate decomposes (i.e. above 200 degrees Celsius)
is nearly reached the liquid then shewing only traces of alkaline sulphate.
Similarly chloride of ammonium and the alkaline nitrates can be used to produce
ammonium nitrate as the chloralkalies formed in the reaction (K Cl and Na CI.)
are also difficultly soluble in a highly concentrated solution of ammonium nitrato or

page_text: in molten ammonium nitrate but owing to the higher price chloride of ammonium
does not offer the same economical advantages as are incidental to the use of
sulphate of ammonium.
Dated this 16th dox of Tanu 1800
J. H. JOHNSON & Co.,
47, Lincoln's Inn Fields, Agents.
COMPLETE SPECIFICATION.
Improvements in the Manufacture or Separation of Ammonium
Nitrate and Sulphate or Chloride of Sodium and of Potassium.
I, CARL ROTH of Charlottenburg in the Empire of Germany Chemist do hereby
declare the nature of my said invention and in what manner the same is to be
performed to be particularly described and ascertained in and by the following
statement:
According to this invention equivalent quantities of sulphate of ammonium and
either nitrate of potassium or nitrate of sodium may be either heated together in a
watery solution or melted together in a dry state below the temperature at which
decomposition of ammonium nitrate takes place the result being as is well known
that ammonium nitrate and a sulphate of the alkali employed are produced. I effect
the separation of the said products by means of thermal effect as hereinafter
described. I have discovered that watery solutions of ammonium nitrate at a
temperature above 110° Celcius (one hundred and ten degrees of Celcius) lose their
power of dissolving sulphate of potassium or sulphate of sodium in proportion as the
solvent becomes volatilized owing to the heat and in the same degree as the
temperature advances to the point at which all the water is driven off. I have further
discovered that molten ammonium nitrate (free of water) is capable of dissolving
traces only of alkaline sulphates.
If the heating be carried above 110° Celcius until all or practically all of the
water is driven off or yet higher until the temperature at which ammonium nitrate
begins to be decomposed is nearly reached or if equivalent quantities of sulphate of
ammonium and nitrate of potassium or of sodium are heated together without the
presence of water and the temperature of the melt be maintained under ordinary
pressure of the air for say an hour or thereabouts at preferably between 160° and
200° Celcius (one hundred and sixty and two hundred degrees Celcius) or at the
corresponding degrees of temperature in presence of increased or diminished pressure
or in absence of the pressure of the air the liquid ammonium nitrate will lie above
the alkaline sulphate which sinks to the bottom of the vessel in a solid form and it
will be easy to separate the ammonium nitrate from the alkaline sulphate for example
by siphoning or by means of a heated hydro-extractor or by any means suited to the
separation of liquified crystal masses from a solid residuum. If during the reaction
water be present it is necessary to drive it off either by heating to above 110° Celcius
under the ordinary pressure of the air or to the corresponding degrees of heat under
.diminished pressure or vacuum to such an extent that it shall not have the power
of dissolving the alkaline sulphate to an extent prejudicial to the purpose which
the resulting ammonium nitrate is to serve.
As a solution consisting of equal parts of ammonium nitrate and water under
ordinary atmospheric pressure boils at about 110° Celcius and at this temperature is
capable of absorbing 15 per cent. or thereabouts of sulphate of sodium or 10 per cent.
or thereabouts of sulphate of potassium this degree of temperature is the lowest
admissible limit taking into consideration the fact that for some manufacturing
purposes nitrate of ammonium containing the abovenamed percentage of the alkaline
sulphates is capable of being used.
The enrichment in nitrate of ammonium of the liquid above the solid product due
to the increasing separation of the alkaline sulphate is in proportion to the increase
of temperature above 110° Celcius and attains its maximum when the temperature at

page_text: which ammonium nitrate decomposes (i.e. above 200° Celcius) is nearly reached the
liquid then shewing only traces of alkaline sulphate.
Similarly chloride of ammonium and the alkaline nitrates can be used to produce
ammonium nitrate as the chlory alkalies formed in the reaction (K Cl and Na Cl)
are also difficultly soluble in a highly concentrated solution of ammonium nitrate or
in molten ammonium nitrate but owing to the higher price chloride of ammonium
does not offer the same economical advantages as are incidental to the use of sulphate
of ammonium.
Having now particularly described and ascertained the nature of this inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
In the manufacture or separation of ammonium nitrate and sulphate or chloride of
sodium or sulphate or chloride of potassium the treatment under thermal condition's
substantially as hereinbefore explained.
Dated this 6th day of Ortahan 1000
J. H. JOHNSON & Co.,
47, Lincoln's Inn Fields, London, W.C., Agents.