Year: 1895

page_text: Date of Application, 12th Oct., 1895
Complete Specification Left, 26th June, 1896-Accepted, 10th Oct., 1896
I mix, intimately in the form of a very fine powder, biborate of soda and
hydrochlorate of animonia, the following are the best proportions :-
Biborate of soda
-
Hydrochlorate of ammonia -
-
100 parts.
150 "}
It is obvious that these proportions may be varied according to the degree of
purity of the material used. I may also use borate of soda or borate of potash
instead of biborate of soda. The mixture is calcined in a closed vessel of platinum,
earthenware or other refractory substance. The calcination should take place at a
red heat and be carried on for about an hour.
When the calcination is terminated the apparatus is taken to pieces and there is
removed therefrom a mass of a greyish white color, porous and honeycombed or
hollowed out which is an impure mixture of BN + NaCl (nitride of boron and
chloride of sodium). This product is first pulverised and then placed in contact
with boiling water to which a slight quantity of hydrochloric acid has been added
in order to separate the insoluble nitride of boron from the chloride of sodium, this
operation being performed in a horizontal cask provided with blades and forming a
kind of churn. The insoluble nitride of boron is separated from this liquid by a
filtering press and the chloride of sodium is recuperated by evaporation.
2. MANUFACTURE OF THE CYANIDES.
I use some of the nitride of boron obtained as above, say about
Carbonate of potash about
-
-
50 parts.
-
Carbon black or any other product containing a large quantity
of carbon about
250
"
30 "
It is obvious that these proportions may be varied according to the degree of
purity of the products used. The whole is thoroughly mixed after having been
previously pulverized. When ferro-cyanides are required iron filings are subsequently
ade in the proportion of about 10 per cert, of the mass. This mixture is placed
in a cylinder to which a rotary motion is imparted, so that it turns in a medium
which raises it to a dark red heat in the course of one hour or thereabouts, the
I use some of the nitride of boron obtained as above, say about
Carbonate of potash about
-
Carbon black or any other product containing a large quantity
of carbon about
-
50 parts.
250
"2
-
30
"
It is obvious that these proportions may be varied according to the degree of
purity of the products used. The whole is thoroughly mixed after having been
previously pulverized. When ferro-cyanides are required iron filings are subsequently
adde in the proportion of about 10 per cert, of the mass. This mixture is placed
in a cylinder to which a rotary motion is imparted, so that it turns in a medium
which raises it to a dark red heat in the course of one hour or thereabouts, the

page_text: material being subsequently removed and consisting chiefly of borate of potash
and cyanide of potassium. The following formula shows the reactions which take
place
-
This mass is then dissolved in boiling water in a washing cask or tub similar to
that above mentioned wherein it is allowed to remain for some time, being then
allowed to crystallize in suitable basins after the liquid has been suitably
concentrated.
The product obtained in this second operation may be likewise treated by alcohol
which dissolves the cyanides but allows the insoluble biborates to be deposited.
The advantages of my invention as regards manufacture are important since
1 can manufacture cyanides directly without having recourse to the provious
manufacture of ferro-cyanides. It may likewise be worthy of notice that the
quantity of cyanide obtained by my process considerably exconds that obtained by
means of the animal stuff or material generally used. I may add that in my
process a considerable economy is realise on the cast price, as the matter used is
nearly entirely recuperated, such as the biborates which may be used again through
the various stages of the manufacture of nitride of boron. Moreover I gather a
considerable quantity of chloride of sodium or of potassium according to whichover
of these salts 1 use, which chloride is nearly pure and can be sold in commerce.
Dated 12th October 1895.
Improvements in the Manufacture of Alkaline Cyanides,
Ferro-oyanides, and their Derivatives.
I, GEORGE CLEMENT DOWNING of & Quality Court London England Patent Agent
a communication from abroad by Jean René Moïse, Paris, Chemist, do hereby
declare the nature of said invention and in what manner the same is to he
performed, to be particularly described and ascertained in and by the following
statement :-
This invention has for its object to provide a substitute for the industrial
processes hitherto used for the manufacture of alkaline cyanides, ferro-cyanides and
their derivatives.
My improved process is divided into two parts:
1. The manufacture of nitride of boron for the production of cyanides.
2. The manufacture of cyanides.
To manufacture nitride of boron. I make an intimate mixture of biborate of soda
and hydrochlorate of amunonia, ground to a very fine powder.
The following are advantageous proportions:
:―
Biborate of soda
Hydrochlorate of ammonia
-
-
100 parts.
150 "
It is obvious that I may vary these proportions according to the degree of
purity of the substances used. I inay also use borate of soda or borate of potash.
The mixture is calcined in a closed vessel of graphite, stonewaro
or other
refractory material, provided with a receiver for collecting in a condensing chamber
the parts of the hydrochlorate of ammonia which are volatilized at the com-
mencement of the reaction. The hydrochlorate thus collected in the condensing
chamber is used again in a new operation.

page_text: I treat the product of the second operation with alcohol, which dissolves the
cyanides and leaves the insoluble biborates. This operation is carried on by an
apparatus for complete extraction. When I require to manufacture ferro-cyanides,
I add to the mixture either before, or preferably after its calcination, about 10 per cent.
of its own weight of iron filings or shavings. The separation of the ferro-cyanides
and of the borates is carried out by fractional cristallisation the latter being much
more soluble.
The advantages of my invention are obvious as regards manufacture, since
I manufacture cyanides directly without resorting previously to the manufacture of
ferro-cyanides, it is also important to state that the quantity of cyanide obtained by
my process is more than double the quantity obtained by means of the animal
matter hitherto used.
Also by my process a great economy is realized over the cost
price, as the substances used are almost entirely recovered, such as the biborates,
which may be used again in the manufacture of nitride of boron. Moreover
I collect a considerable quantity of chloride of sodium or of potassium (according
as one or the other salt is used) which chloride is almost in a pure state and can be
readily sold in commerce. It must be well understood that besides the use of the
apparatus before mentioned, I may use any other suitable apparatus for the aforesaid
manufacture.
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. A process for the direct manufacture of alkaline cyanides, and their derivatives,
without previously manufacturing ferro-cyanides, this process being characterized by
the use of nitride of boron, produced by the action of hydrochlorato of ammonia

page_text: upon boron salts, in a refractory vessel heated to redness, the portion of the hydro-
chlorate which is not converted into nitride being recovered in a condensing chamber,
and the separation of this nitride of boron and of the equally utilizable chlorides,
being effected by treatment with boiling water, to which a small quantity of hydro-
chloric acid is added, and subsequently by filtration, in order to manufacture cyanides
directly by converting an intimate mixture of powdered nitride of boron, alkalino
carbonate, and carbon, under the action of a dark red heat, into a combination of
cyanides and borates separated by treatment with alcohol, substantially as
hereinbefore described.
2. The direct manufacture of ferro-cyanides by the process above claimed, while
adding iron filings or scrapings, before or after the fusion of the indicated mixture
of nitride of boron, alkaline carbonate and carbon, the ferro-cyanides being separated
from the more soluble borates by fractional cristallisation substantially as hereinbefore
described.