IMPROVEMENTS IN THE. MANUFACTURE OF ACETIC ACID AND ACETATES
Year: 1852

page_text: LETTERS PATENT to Henry Bollmann Condy, of Battersea, in the
County of Surrey, for the Invention of "IMPROVEMENTS IN THE.
MANUFACTURE OF ACETIC ACID AND ACETATES."
Sealed the 21st January 1853, and dated the 26th November 1852.
PROVISIONAL SPECIFICATION left by the said Henry Bollmann.
Condy at the Office of the Commissioners of Patents, with his.
Petition, on the 26th November 1852.
I, HENRY BOLLMANN CONDY, of Battersea, in the County of Surrey,
do hereby declare the nature of the said Invention for "IMPROVEMENTS
IN THE MANUFACTURE OF ACETIC ACID AND ACETATES" to be as follows:-
..This Invention has for its objects, means of purifying crude
acetic acid, and also acetates made with the crude acetic acid, and
consists of applying thereto oxidizing agents, such as bichromate
of potash with sulphuric acid, chlorate of potash, with sulphuric
acid or muriatic acid, or other oxidizing agents acting in a similar
manner; and it also consists of precipitating the impurities, such as tar
and others, by combining them with a base, such as lead, in the state
of a subacetate or acetate with alkali or zinc, in the state of acetate
or sulphate with an alkali, though others may be used, but not, it is

page_text: believed, with such advantage; and the Invention also consists of
employing crude acetic acid in producing acetate of barytes, and
obtaining the acid from that salt by employing another acid for
which the barytes has a stronger affinity, thus obtaining a purifi-
cation of the acetic acid.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Henry Bollmann Condy in the Great Seal
Patent Office on the 25th May 1853.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I,
HENRY BOLLMANN CONDY, of Battersea, in the County of Surrey, send
greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twenty-sixth day of November, in
the year of our Lord One thousand eight hundred and fifty-two, in
the sixteenth year of Her reign, did, for Herself, Her heirs and succes-
sors, give and grant unto me, the said Henry Bollmann Condy, Her
special licence that I, the said Henry Bollmann Condy, my executors,
administrators, and assigns, or such others as I, the said Henry
Bollmann Condy, my executors, administrators, and assigns, should
at any time agree with, and no others, from time to time and at all
times thereafter during the term therein expressed, should and law-
fully might make, use, exercise, and vend, within the United Kingdom
of Great Britain and Ireland, the Channel Islands, and Isle of Man,
an Invention for "IMPROVEMENTS IN THE MANUFACTURE OF ACETIC ACID
AND ACETATES," upon the condition (amongst others) that I, the said
Henry Bollmann Condy, by an instrument in writing under ny hand
and seal, should particularly describe and ascertain the nature of
the said Invention, and in what manner the same was to be per-
formed, and cause the same to be filed in the Great Seal Patent
Office within six calendar months next and immediately after the
date of the said Letters Patent.
NOW KNOW YE, that I, the said Henry Bollmann Condy, do hereby
declare the nature of the said Invention, and in what manner the

page_text: saine is to be performed, to be particularly described and ascertained
in and by the following statement thereof (that is to say):
My Invention has for its object means of purifying crude acetic
acid, and also acetates made with the crude acetic acid, and consists
of applying thereto oxidizing agents, such as bichromate of potash
with sulphuric acic, chlorate of potash with sulphuric acid or muriatic
acid, or other oxidizing agents acting in a similar manner; and
it also consists of precipitating the impurities, such as tar and
others, by combining them with a base, such as lead, in the state of a
subacctate or acetate, with alkali, or zinc in the state of acetate
or sulphate with an alkali, though others may be used, but not,
it is believed, with such advantage; and the Invention also consists
of employing crude acetic acid in producing acetate of barytes, and
obtaining the acid from that salt by employing another acid for
which the barytes has a stronger affinity, thus obtaining a purifi-
cation of the acetic acid. And in order that the Invention may
be most fully understood, and readily carried into effect, I will
proceed to describe the means pursued by me.
The Invention has for its object the purification of impure
empyreumatic acetic acid and of acetates containing such impure
acid; and for this purpose I cause the same to be distilled together
with an oxidizing matter, which will act on the impurities and
cause the acetic acid to distil over pure, or nearly so.
There are
many oxidizing agents suitable for carrying out my Invention,
such as chromic acid, nitric acid, chlorine, and others, with which
chemists are well acquainted; but I believe the three above men-
tioned are best for the purpose, and I prefer to employ in the still
bichromate or chromate of potash, or soda with sulphuric acid in
equivalent quantities, so as to obtain the chromic acid desired in the
process, in place of first obtaining the chromic acid by a separate
process, and then using it for the purpose of my Invention.
In carrying out the Invention, supposing I have a quantity of
rough acetic acid which I am about to purify, I take a small mea-
sure thereof, and I place the same in a small still, together with
about two and a half per cent. of chromate or bichromate of potash
or soda, and ten per cent. of sulphuric acid, and I distil the same,

page_text: and if I find, which will generally be the case, that the acetic acid
does not come over pure, I try a further quantity of the rough
acetic acid with a larger quantity of the oxidizing agents, until I,
by such tests, ascertain the proper quantity of the oxidizing agent
necessary for purifying the particular rough acetic acid I am about
to purify, and having ascertained the proper quantity of the oxidiz-
ing agent to be used, I then proceed to distil on the manufacturing
scale, by causing the whole quantity of the rough acetic acid, or
such quantity as the still will contain, to be distilled together with
the ascertained relative proportion of the oxidizing agent, and by
such means I am enabled by the simple process of distillation
(aided by the oxidizing agents) to obtain from rough and impure
acetic acid colorless and very pure acid free from empyreumatic
flavor. I would state that, although I prefer to use chromic acid
obtained in the process herein described, I do not confine myself
thereto, as other oxidizing agents may be introduced into the still
with rough acetic acid, in the same manner to that above described.
I would remark that I am aware that in some cases oxide of
manganese and sulphuric acid have been before introduced into a
still, when decomposing acetates of lime made with crude acetic
acid; when re-distilling the acid made from such acetates of lime
which oxide of manganese oxidizing the sulphurous acid given off
in the process, and converting it into sulphuric acid, forms sulphate
of manganese; but by such means the impurities and empyreumatic
flavor in the acetate have not been removed by the action of the
oxygen on them.
I mention this fact, in order to state that I do
not claim the introduction of oxidizing agents, except when so
applied as to act on the empyreumatic impurities, and to cause
them to be removed therefrom in the act of distilling, as herein
explained.
Another part of my Invention consists of purifying impure
acetic acid contained in acetates. This may be performed by
means of oxidizing the impurities by treating the solutions of
acetates with oxidizing agents, as above explained. The most effec-
tive agent, however, to be employed being chloride of lime, either
added in solution to the solution of acetate or added to the dried

page_text: acetate in the state of powder, the former method being much pre-
ferred. The chloride of lime on being heated after mixture with
the solution of acetate lime yields oxygen, and oxidizes the empy-
reumatic impurities; the acetate can then be used for making acetic
acid, or any other purpose for which a good acetate is required; or
the object may be accomplished by precipitation by a base in the
manner I will proceed to describe. I take an acetate, which has
been dried, and dissolve it, and I employ a metallic salt, the base of
which is precipitable, or a base which is insoluble in water, such as
hydrated oxide of lead, by which I am enabled to separate the
impurities. The metallic salts which I prefer for the purpose are
subacetate or acetate of lead, with alkali, or alkaline earth, or salts
of zinc, such as acetate or sulphate with an alkali or alkaline earth;
but other metallic salts may be used; not, however, I believe,
with so much advantage as is derived from the use of the salts of
lead, or of zinc above mentioned; and I find that by using metallic
salts as precipitants, that such salts, by yielding their bases, cause
there to be a precipitation of such bases; which carry down in`
combination with them the coloring and impure matters of the
acetate. I prefer to use the hex-acetate of lead at the rate generally
of not more than about five per cent. of the weight of the dry
acetate in the solution, but a less quantity will answer, if the
acetate to be purified be not very impure; and in like manner
neutral acetate of lead may be employed, but it is then necessary to
add immediately afterwards an alkali or alkaline earth, by pre-
ference line mixed with water to the consistence of cream; and in
a similar manner may other metallic salts be used, adding sufficient
thereof to precipitate with the base the impurities in the acetate.
I proceed as follows: -to a solution of acetate of lime or soda,
containing ten per cent. of salts, I add the hex-acetate of lead,
which is first ground into a cream-like thickness, and I add it
gradually so long as it appears to remove color from the solution ;
I then heat up the fluid to about 190° of Fahrenheit; the liquid
portion is then decanted or filtered from the precipitated matters,
and is treated with an alkali or alkaline earth, using lime by pre-

page_text: ference, after which it is allowed to settle, when it may, if desired,
be filtered through animal charcoal; or it may be used as it is in
the manufacture of acetic acid, by decomposing with acid as here-
tofore, or for making acetates by decomposition with other salts, as
is well understood.
Another part of my Invention consists of employing crude
acetic acid. in producing acctate of barytes, and obtaining the
acid from that salt by employing another acid for which the
barytes has a stronger affinity, thus obtaining" a purified acetic
acid.
The manufacture of acetate barytes from impure acetic acid is
thus effected:
The impure acetic acid is poured into a vessel containing native
carbonate bárytes, or sulphide of barium, and the whole then gently
heated to about 90° Fahrenheit; to ensure the acid being saturated,
and to ensure the quickly drawing off the carbonic acid or hydro-
sulphuric acid, it, will be desirable to carry the heat up to. 140°
Fahrenheit. The solution may then be evaporated and crystallized,
dried, and redissolved, and again crystallized, or may be used when
simply dry for the manufacture of acetic acid, by the use of sul-
phuric or nitric or hydrocloric acid, or for the manufacture of
acetates by double decomposition.
Having thus described the nature of my Invention, and the
manner of performing the same, I would have it understood that I
do not confine myself to the details as herein given, so long as
the peculiar character of any part of my Invention be retained.
In witness whereof, I, the said Henry Bollmann Condy, havé
hereunto set my hand and seal this Eighteenth day of May, in
the year of our Lord One thousand eight hundred and fifty-
Witness,
S. CARPMAEL.
HENRY BOLLMANN CONDY. (L. S.)