IMPROVEMENTS IN THE PRODUCTION OF COLCOTHAR OR JEWELLERS' ROUGE (FERRIC OXIDE), AND CUPRIC CHLORIDE
Year: 1879

page_text: LETTERS PATENT to Juan Francisco Nepomuceno Macay, of Charapotó, in the
Republic of Ecuador, South America, and at present of York Place, Baker
- Street, in the County of Middlesex, for the Invention of "IMPROVEMENTS IN
THE PRODUCTION OF COLCOTHAR OR JEWELLERS' ROUGE (FERRIC OXIDE), AND
CUPRIC CHLORIDE.”
'Sealed the 9th January 1880, and dated the 17th October 1879.
PROVISIONAL SPECIFICATION left by the said Juan Francisco Nepomuceno
Macay at the Office of the Commissioners of Patents on the 17th October
1879.
JUAN FRANCISCO NEPOMUCENO MACAY, of Charapotó, in the Republic of Ecuador,
South America, and at present of York Place, Baker Street, in the County of
Middlesex. "IMPROVEMENTS IN THE PRODUCTION OF COLCOTHAR OR JEWELLERS'
ROUGE (FERRIC OXIDE), AND CUPRIC CHLORIDE."
My Invention relates to the production of ferric oxide (Fe,, O,), variously known
in commerce as colcothar, crocus, martis, or jewellers' rouge, and of cupric chloride
(Cu Cl). One method of my Invention consists in boiling with access of air in a
solution of chloride of sodium (Na CI) a certain proportion of cupric oxychloride
(Cu Cl₂ 3 Cu O, OH₁), and of ferrous or ferric sulphate (Fe SO, 7 OH₂), or (Fе, 3
SO). The iron is oxidised at the expense of the oxygen of the copper salt, and
of the air, and is precipitated in the form of ferric oxide, leaving cupric chloride
(Cu Cl₂) and sulphate of sodium (Na, SO, 10 OH₂) in solution. In carrying out
this process in practice I proceed as follows:-Certain proportions of chloride of
sodium in solution, ferrous sulphate, and cupric oxychloride are placed together in
a wooden vat, or other suitable vessel, and boiled, with free access of air, until the
ferric oxide is thrown down as a pale yellowish-red flocculent precipitate, which
assumes a deeper red color by continuing the boiling about a quarter of an hour
longer. The following is the chemical reaction:—
2 Cu Cl, 3 Cu O. 4 OH, + 12 Na Cl + 6 Fe SO, 7 OH, +30 + 54 OH₂
8 Cu Cl, 6 Na, SO, 10 OH, +3 Fе, O, + 44 OH₂.
After all the insoluble cupric oxy-chloride has been converted into cupric chloride
(Cu Cl) and the iron precipitated as ferric oxide, the cupric chloride is separated
by filtration, and the residue offeric oxide is well washed first with water, and,
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page_text: lastly with acidulated water, in order to free the ferric oxide from any salt of
copper. The iron peroxide is then calcined in the usual way to bring it to the
desired color.
Another process of my Invention consists in boiling, with access of air, a solution
of ferrous chloride (Fe C₁₂) with a certain proportion of cupric oxy-chloride.
I proceed as follows:-I boil together in an open wooden vat, or other suitable
vessel, ferrous chloride in solution and cupric oxy-chloride in certain proportions,
whereupon cupric chloride is formed and ferric oxide precipitated, the chemical
reaction being as follows:-
6 Fe Cl₂+2 Cu Cl₂. 3 Cu O. 4 OH₂ + 30 === 3 Fe, O, +8 Cu Cl₂,
The cupric chloride is filtered off, and the ferric oxide is washed and calcined as
in the process first described.
In either process when absolute purity of the products is required there must be
& slight excess of the cupric oxychloride or of the ferrous salt, as the case may be.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent. filed by
the said Juan Francisco Nepomuceno Macay in the Great Seal Patent Office
on the 17th April 1880.
JUAN FRANCISCO NEPOMUCENO MACAY, of Charapotó, in the Republic of Ecuador,
South America, and at. present of York Place, Baker Street, in the County of
Middlesex. "IMPROVEMENTS IN THE PRODUCTION OF COLCOTHAR OR JEWELLERS'
ROUGE (FERRIC OXIDE), AND CUPRIC CHLORIDE."
My Invention relates to the production at one operation of ferric oxide (Fe, O,),
variously known in commerce as colcothar, crocus martis, or jewellers' rouge, and
of cupric chloride (Cu Cl₂).
One method of carrying my Invention into effect consists in digesting or boiling
in a solution of chloride of sodium (Na Cl), with access of air, a certain proportion
of cupric oxychloride (Cu Cl, 3 Cu O. 4 OH), and of ferrous or ferric sulphate
(Fe SO 7 OH), or (Fe, 3 SO). The chemical reactions produced take place in
the following manner:-
The sulphuric acid and oxygen of the ferrous or ferric sulphate combine with
the sodium of the chloride of sodium, forming sulphate of oxide of sodium, ¿.e.,
sulphate of soda, thus liberating the chlorine; the chlorine in the nascent state
combines with the iron of the ferrous or ferric sulphate, thereby forming ferrous
chloride; and, lastly, by the mutual reaction of the ferrous chloride thus formed,
and the cupric oxychloride, the oxygen of the copper salt is exchanged for the
chlorine of the ferrous salt, thereby producing cupric chloride (Cu Cl₂) and ferrous
oxide which by the action of the oxygen of the atmosphere is converted into ferric
oxide.
In carrying out this process in practice I prefer to use ferrous sulphate, and I
proceed as follows:-Chloride of sodium in solution, ferrous sulphate, and cupric
oxychloride in the following proportions, viz. :-
Cupric oxychloride
Chloride of sodium
Ferrous sulphate
-
1 part by weight estimated in the crystallised form.
17
0.70
"
"
"
"
"
"
are digested or boiled together in a wooden, or other suitable vessel, with free
access of air, until the ferric oxide is thrown down as a pale-yellowish red flocculent
precipitate which assumes a deeper red color and a state of aggregation more
suitable for the purpose for which it is required by continuing the boiling. The
following is the chemical reaction:-
=
2 Cu Cl, 3 Cu O. 4 OH, + 12 Na Cl + 6 Fe SO. 7 OH₂ + 3 O + 5+ OH₂ =
8 Cu Cl, +6 Na₂ SO₁. 10 OH₂ + 3 Fе, O, + 44 OH₂.
After all the insoluble cupric oxychloride has been converted into cupric chloride
(Cu Cl₂) and the iron precipitated as ferric oxide, the cupric chloride is or may be
separated by filtration, and the residue of ferric oxide is or may be well washed,
first with water, and lastly with acidulated water, in order to free the ferric oxide
from any salt of
copper. The iron peroxide may then, if necessary, be calcined in the
usual way to bring it to the desired color.
Another mode of carrying out my Invention consists in starting with a solution
of ferrous chloride already formed, instead of forming it in the process, and boiling
this solution, with access of air, with a certain proportion of cupric oxychloride. I
proceed as follows:-I boil together in an open wooden vat, or other suitable
vessel, the solution of ferrous chloride and cupric oxychloride in the following
proportions, viz. :—
Solution of ferrous chloride, equivalent to 1·1 part by weight of the salt in the
crystallised form.
Cupric oxychloride
10 part by weight
whereupon cupric chloride is formed and ferric oxide precipitated, the chemical
reaction being as follows :-

page_text: The cupric chloride is filtered off, and the ferric oxide may be washed and
calcined as in the mode first described. In either case when absolute purity of
the products is required there must be a slight excess of the cupric oxychloride or
of the ferrous salt, as the case may be.
Having described the nature of my Invention and the manner of performing the
same I declare that what I claim as my Invention to be protected by the herein-
before in part recited Letters Patent is,―
1st. The production at one operation of ferric oxide (Fe, Os) and cupric chloride
(Cu Cl₂) from ferrous or ferric sulphate, chloride of sodium, and cupric oxychloride,
substantially as described in the first mode herein specified.
2nd. The production at one operation of ferric oxide (Fe, Os) and cupric chloride
(Cu Cl₂) by the mutual reaction of cupric oxychloride and ferrous chloride, substan-
tially as described in the second mode herein specified.
In witness whereof, I, the said Juan Francisco Nepomuceno Macay, have
hereunto set my hand and seal, this Twelfth day of April, in the year of our
Lord One thousand eight hundred and eighty.