Improvements in the Manufacture of Nitrate of Ammonia and Sulphates, Chlorides, and Carbonates of Potassium and Sodium.
Year: 1889

page_text: Date of Application, 2nd Feb.,
1889
Complete Specification Left, 2nd Nov., 1889-Accepted, 7th Dec.,
1889
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Nitrate of Ammonia and
Sulphates, Chlorides, and Carbonates of Potassium and Sodium.
I, CARL ROTH, of Charlottenburg, near Berlin, in the Empire of Germany, Chemist,
do hereby declare the nature of this Invention to be as follows:-
The object of this invention is to effect improvements in the manufacture of nitrate
of ammonia and of sulphates chlorides and carbonates of potassium and sodium
from sulphates chlorides or carbonates of ammonia and nitrates of potassium or
sodium also the employment of improved means for effecting the reaction and
separation of the generated products. The conversion of sulphate of ammonia and
nitrate of potassium into nitrate of aminonia and sulphate of potassium has up to the
present only been done by. boiling the aqueous solutions, and the conversion of
chloride of animonia and nitrates of alkalies into nitrate of ammonia and chlorides
of alkalies has been done through direct heating of the dry mixtures of these
substances, according to the following equation :-
SO. (NH), + 2 K NO, = SO, K, + 2 NO, NH,
NH. C+ NO. Na Na Cl+NO, NH..
According to my invention in order to produce nitrate of ammonia and sulphates
chlorides and carbonates of potassium and sodium generally from salts of ammonia
and nitrates of alkalies I treat the salts of ammonia and the nitrates of alkalies with
alcohol or other suitable liquid which has the quality of dissolving the genetrated
nitrate of ammonia and leaving the remaining products of the reaction wholly or
partly undissolved. I take for example 132 parts of sulphate of ammonia and 170
These
parts of nitrate of sodium and I add thereto say 400 parts of alcohol of 95%.
I heat together for some time in a suitable vessel which is connected with a con-
denser by the help of which the quantity of liquid is continuously maintained at the
starting point in the vessel by the re-entry thereinto of the condensed vapourised
liquid or by pressure in an autoclave. The conversion into nitrate of ammonia and
sulphate of sodium of the sulphate of ammonia and nitrate of sodium will take place
so soon as the substances are sufficiently heated and nitrate of ammonia will be
lissolved in the liquid whilst the sulphate of sodium will be left undissolved. The
nitrate of ammonia is afterwards recovered as a residuum by filtration and dis-
tillation.
If water is used instead of alcohol or the like the resulting substances, nitrate of
ammonia and sulphate of sodium will be dissolved in nearly equal proportions and
consequently a separation of them by crystallisation from water is almost impossible
and this is the reason why a practical production of nitrate of ammonia and sulphates
of alkalies from the hereinbefore named raw materials by the help of water has not
to my knowledge received serious attention. I have however discovered that by the
application of acthylalcohol or methylalcohol of different strengths, or, of other
liquids which dissolve the nitrate of ammonia and which take up other products of
reaction only in small proportions or not at all, the separation by crystallisation from
water is avoided. When treating carbonate of ammonia and nitrate of potassium
or sodium it is advisable to effect the heating thereof in a liquid which dissolves
nitrate of ammonia (such as alcohol) in closed vessels to exclude the air for the
purpose of preventing the volatilization of the carbonate of ammonia, or of its
constituents.
After the completion of the reaction the liquid is filtered from the remaining

page_text: undissolved material which consists (according to the kind of the salts of alkali
applied) of sulphate of potassium, sulphate of sodium, chloride of potassium, chloride
of sodium, carbonate of potassium or carbonate of sodium.
After distilling the filtrate a residuum is left consisting of nitrate of ammonia. As
a variation of the process hereinbefore described nitrate of ammonia and the other
products of reaction may be obtained in the following manner. Nitrate of ammonia,
chloride of ammonia or sulphate of ammonia are put into reaction with the nitrates
of alkalies by means of direct heat but precaution is to be taken that the tempera-
ture does not exceed the point at which decomposition of the nitrate of ammonia
takes place. After this the mixed products of the reaction are separated by means of
an agent which dissolves the nitrate of ammonia as before described. If a solution
of the salts in water be present the latter may be evaporated before separating the
said products or the aqueous solution may be mixed with the agent which dissolves
the nitrate of ammonia in which latter case the precipitation of the salts takes place
which by the admixture of water are more or less made soluble in the dissolving
agent. For the purpose of producing and separating the products of the reaction
from the nitrates of alkalies and sulphate, chloride and carbonate of ammonia, I
may employ the following process. Nitrate of potassium or nitrate of sodium may
first be put in reaction with the above mentioned salts of ammonia by any means
until the transformation (according to the nature of the originally employed raw
materials) into chlorides, sulphates or carbonates of alkalies and nitrate of ammonia
has taken place.
The mixture is then transferred into a closed vessel in which superheated steam
or hot air can be introduced by means of a perforated pipe leading to the bottom of
the vessel.
By the action of either of these agents the nitrate of ammonia is made volatile and
therefore can be distilled. The volatilised products when distilled escape from the
vessel by a pipe into a suitable condenser by means of which the evaporated nitrate
of ammonia is finally condensed together with the steam. The temperature of the
superheated steam or air may he regulated in such a manner that the heat of the
contents of the vessel shall not exceed 240° Celsius. If this precaution is not
observed, loss of nitrate of ammonia will be caused by partial decomposition.
The most suitable temperature which effects the distillation of nitrate of ammonia
during the introduction of steam or air is between 150 and 200° Celsius. It is not
at all necessary that in salt mixtures from which the nitrate of ammonia is to be
distilled in the inanner described that nitrate of ammonia should first be in a free or
uncombined state as the steam may be introduced into the vessel containing the
original raw materials (mixed in the required proportions) viz., nitrate of alkalies, with
sulphate, chloride or carbonate of ammonia, in heating which with steam or air the
result is that nitrate of ammonia is first generated and then distilled.
In employing this latter method of generation it is advisable to enclose the
described original materials and to heat them in a vessel of such a construction as
will prevent the contents from volatilising before reaction takes place.
Dated this 2nd day of February 1889.
J. H. JOHNSON & Co.,
A crente
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Nitrate of Ammonia and
Sulphates, Chlorides, and Carbonates of Potassium and Sodium.
1 CARL ROTH of Charlottenburg near Berlin in the Empire of Germany Chemist 5
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:-
The object of this Invention is to effect improvements in the manufacture of nitrate
of ammonia and of sulphates chlorides and carbonates of potassium and sodium from

page_text: sulphates chlorides or carbonates of ammonia and nitrates of potassium or sodium
also the employment of improved means for effecting the reaction and separation of
the generated products. The conversion of sulphate of ammonia and nitrate of
potassium into nitrate of ammonia and sulphate of potassium has heretofore been
accomplished by boiling the aqueous solutions, and the conversion of chloride of
ammonia and nitrates of alkalies into nitrate of ammonia and chlorides of alkalies has
been effected by a direct heating of the dry mixtures of these substances, according
to the following equation :-
According to my Invention in order to produce nitrate of ammonia and sulphates,
chlorides and carbonates of potassium and sodium generally from salts of ammonia
and nitrates of alkalies I heat the salts of ammonia and the nitrates of alkalies with
alcohols or other suitable liquid which have the quality of dissolving the nitrate of
ammonia which is formed and of leaving the remaining products of the reaction,
wholly or partly undissolved. I take for example 132 parts of sulphate of
ammonia and 170 parts of nitrate of sodium and I add thereto say 400 parts of
alcohol preferably methyl alcohol. These I heat together for some time in a reflux
cooler or under pressure in an autoclave or hermetically closed vessel. The conver-
sion into nitrate of ammonia and sulphate of sodium of the sulphate of ammonia and
nitrate of sodium takes place so soon as the substances are sufficiently heated and the
nitrate of ammonia is dissolved in the liquid whilst the sulphate of sodium is left
undissolved. The nitrate of ammonia is afterwards recovered as a residuum by
filtration and distillation.
If water be used instead of alcohol or the like the resulting substances, nitrate of
ammonia and sulphate of sodium are dissolved in nearly equal proportions and con-
sequently a separation of these substances by crystallisation from water is almost
impossible and this is the reason why a practical production of nitrate of ammonia
and sulphates of alkalies from the hereinbefore named raw materials by the help of
water has not to my knowledge received serious attention. I have however discovered
that by the application of aothyl alcohol or methyl alcohols of suitable strengths or of
other like liquids which are capable of dissolving the nitrate of ammonia and which
take up other products of reaction only in small proportions or not at all the separa-.
tion from water by crystallisation can be avoided. When treating carbonate of
ammonia and nitrate of potassium or sodium the heating thereof in a liquid (such as
alcohol) which dissolves nitrate of ammonia is best effected in closed vessels for
the purpose of preventing loss by volatilization of the carbonate of ammonia or of its
constitutents.
After the completion of the reaction the liquid or solution containing the nitrate of
ammonia is filtered from the remaining undissolved material which consists (according
to the kind of the salts of alkali employed) of sulphate of potassium, sulphate of
sodium, chloride of potassium, carbonate of potassium or carbonate of sodium.
It will be understood that the nitrate of ammonia may be separated from the
filtrate either by crystallisation or by evaporating the liquid solvent. It is evident
that the solution must he filtered in a heated condition and that suitable arrange-
ments are to he employed for the filtering operation which will enable the alcohol to
be condensed and recovered so as to avoid waste of this agent-The strength of the
alcohol employed is regulated according to the degree of purity of the nitrate of
ammonia to be obtained.
According to a modification of the process hereinbefore described nitrate of
ammonia and the other products of reaction may be obtained in the following
manner :-Chloride of ammonia or sulphate of ammonia are caused to react with the
nitrates of alkalies by means of heating and melting the dry substances but precaution
is to be taken that the temperature does not reach the point at which decomposition

page_text: of nitrate of ammonia takes place. After this the products of the reaction are
separated by means of an agent such as methyl or ethyl alcohol which dissolves the
nitrato of ammonia and leaves the other salts undissolved as hereinbefore described.
If a solution of the salts in water be present the latter may be evaporated before
separating the said products or the aqueous solution may be mixed with the agent
which dissolves the nitrate of ammonia and precipitates the other salts which are
insoluble in alcohol or the like.
For the purpose of producing and separating the products of the reaction obtained
froin the nitrates of alkalies and sulphates chlorides and carbonates of ammonia, I
employ the following process. Nitrate of potassium or nitrate of sodium may first.
be put in reaction with the above mentioned salts of ammonia by any suitable
means until the transformation (according to the nature of the originally employed raw
materials) into chlorides sulphates or carbonates of alkalies and nitrate of ammonia
has taken place.
The mixture is then transferred into a closed vessel into which superheated steam or
hot air can be introduced by means of a perforated pipe arranged at the bottom of the
vessel.
By the action of either of these agents the nitrate of ammonia is volatilized and
the volatile products are distilled and escape from the vessel through a pipe into a
suitable condensor by means of which the evaporated nitrate of ammonia is finally
condensed together with the steam, when steam employed. The temperature of the
superheated steam or air must be regulated in such a manner that the heat of the
contents of the vessel shall not exceed 240° Celsius. If this precaution is not observed
loss of nitrate of ammonia will be caused by partial decomposition.
The most suitable temperature for effecting the distillation of the nitrate of
ammonia during the introduction of steam or air is between 150 and 200° Celsius..
It is not necessary that in salt mixtures from which the nitrate of ammonia is to be
distilled in the manner described that the nitrate of ammonia should first be in a free
state as the steam may be introduced into the vessel containing the original raw
materials, (mixed in the required proportions) viz.: nitrate of alkalies with sulphate,
chloride or carbonate of ammonia in heating which with steam or air the result is
that nitrate of ammonia is first generated and then distilled.
In employing this latter method of generation, it is advisable to enclose the described
original materials and to heat them in a vessel of such construction as will prevent the
contents from volatilizing before reaction takes place.
Having now particularly described and ascertained the nature of my said
invention and in what manner the same is to be performed I declare that what I
claim is :-
1. Manufacturing nitrate of ammonia and sulphates and chlorides and carbonates
of potassium and sodium by digesting nitrate of potassium or sodium with sulphates
chlorides or carbonates of ammonia in the presence of liquids such as methyl or ethyl
alcohols possessing the property of taking up the nitrate of ammonia formed by the
reaction and leaving the other salts wholly or partly undissolved substantially as
herein before described.
2. Obtaining nitrate of ammonia and sulphates chlorides and carbonates of
potassium and sodium from dry mixtures containing these substances in a free or
uncombined state by extracting the nitrate of ammonia by means of dissolving
agents, such as methyl or ethyl alcohols which take up the nitrate of ammonia and
leave the other salts wholly or partly undissolved substantially as hereinbefore
described.
3. Obtaining nitrate of ammonia and sulphates chlorides and carbonates of potas-
sium aud sodium from concentrated aqueous solutions thereof by treating the said
solutions with methyl or ethyl alcohol or other like agents possessing the property
of precipitating the said sulphates chlorides and carbonates and dissolving the nitrate,
substantially as herein before described.

page_text: 4. Separating nitrate of ammonia from sulphates chlorides and carbonates of
potassium and sodium by the introduction of superheated steam or air into a mixture
of these substances in such manner that the nitrate of ammonia is distilled over in
the current of superheated steam or air and is thus separated from the non-volatile
salts, substantially as hereinbefore described.
Dated the 1st day of November 1880
J. H. JOHNSON & Co.,
Agents.