A Process for Manufacturing Diethyl-ether.
Year: 1899

page_text: Date of Application, 10th July, 1899
Cominiato CanniAnntinn loft Rth An= 1000
Accented 10th wulu 1000
A Process for Manufacturing Diethyl-ether.
I, GEORGE HILLARD BENJAMIN, of 45, Broadway, New York, United States
of America, Engineer, do hereby declare the nature of this invention to be as
follows:-
:―
My invention relates to a process for manufacturing diethyl-ether, CH¸—0—
CH, and consists essentially in mixing ethylene, CH, and oxygen and hydrogen
in a nascent state, or in the form of a highly heated vapor, H₂O, with sulphuric
acid, H₂SO, and then subjecting to the heat necessary to produce the distillation
of the ether. Or preferably instead of mixing the substance mentioned, I may
start with hydrogen-ethyl-sulphate, C,H,SO, and to this I add ethylene, CH,
and oxygen and hydrogen in a nascent state, or in the form of a highly heated
vapor HO.
The object of my invention is to decrease the cost of producing diethyl-ether,
by bringing about a chemical combination of the elements necessary to form
diethyl-ether, without first producing alcohol.
To carry my invention into effect I proceed as follows:
The ethylene or the hydrogen-ethyl-sulphate may be produced by any means
known to chemists.
'
In practice I prefer to produce the ethylene by subjecting acetylene C₂H.,
(derived from the decomposition of calcium carbide, CaC, by water) to the
action of nascent liydrogen, and the hydrogen-ethyl-sulphate by subjecting the
ethylene produced as described to the action of sulphuric acid.
Where hydrogen-ethyl-sulphate is employed CH.SO. I add the required
quantity of ethylene, CH, and the required quantity of hydrogen and oxygen.
The hydrogen and oxygen are preferably in a nascent condition. Or, I may
use water, HO, in the form of steam or super heated steam.
The reactions are indicated by the following formula:
C₂H HSO + C₂H + HO
=
CH - O – CąH +H,SO,
Where ethylene is employed, I proceed by first saturating a quantity of sulphuric
with the required amount of ethylene C.H.. and the required quantity
acid H SO
C₂HHSO̟ + C₂H + H₂O = C¿H¸ − ( − C¿H¸ + H₂SO,
-
Where ethylene is employed, I proceed by first saturating a quantity of sulphuric
acid, HSO with the required amount of ethylene CH and the required quantity
of hydrogen and oxygen in a nascent state, or water H₂O, in a vaporized form,
and as distillation is accomplished adding the required quantity of ethylene, C.H.
Any suitable apparatus may be employed to carry out the above processes. The
distillation is preferably accomplished by means of a steam coil. The distilled
ether, in the form of gas, may be condensed to a liquid form by any suitable
condensing apparatus. The required quantity of the different materials may be
readily calculated.
The nascent hydrogen and oxygen to be introduced into the mixture of
hydrogen-ethyl-sulphate, ethylene and water, may be obtained by electrolyzing
the water by passing a current of electricity through it; the oxygen being set
free at the positive pole, and hydrogen at the negative.
In practice I consider it preferable to collect the gases generated at the respective
poles, and then discharge them separately into the mixture. I take this course
to avoid the possibility of forming an explosive mixture in the vessel.

page_text: Instead of electrolyzing, the water to produce nascent hydrogen and oxygen, I
may introduce these gases in their combined form, H₂O, as a vapor, such as highly
heated steam.
The above described process may be made continuous or intermittent as desired.
The character of the apparatusi employed will in some measure depend upon
whether hydrogen-ethyl-sulphate or ethylene is employed, and also upon whether
the hydrogen and oxygen is introduced in the form of water, or these gases in
a nascent condition.
I do not wish to limit myself. 'in any wise to any particular apparatus, and
hence I have shown none. However, it will be within the knowledge of any
chemist to arrange a suitable apparatus for carrying the described process into
anot
A Frocess for manufacturing Diethyl-ether.
I, GEORGE HILLARD BENJAMIN, of 45, Broadway, New York, United States
of America, Engineer, 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:-
==
My invention relates to a process of manufacturing diethyl-ether C₂H¸—0——
CH, and consists essentially in subjecting hydrogen-ethyl-sulphate; CH.HSO
to the aotion of heat, and at the same time introducing into the hydrogen-ethyl-
sulphate the required quantity of ethylene, CH, and hydrogen, H, and oxygen; 0.
The object of my 'invention is to decrease the cost of producing pure diethyl-
ether, by bringing about a chemical combination of the 'elements necessary to
form diethyl-ether without employing alcohol, or producing alcohol in 'the
process.
To carry my invention into effect I proceed as follows:-
.P
To a definite quantity of hydrogen-ethyl-sulphate, CH,HSO, for instance five
hundred (500) pounds, contained in a suitable vessel to which sufficient heat is
applied, I add ethylene, CII, and hydrogen H, and oxygen 0,, in the form of a
mixed gas or gases and allow the gas or gases in sufficient quantity to bubble
up into the hydrogen-ethyl-sulphate. As these gases. How into the hydrogen-
ethyl-sulphate they combine with it and owing to the influence of the heat
applied to the mixture, distill over as diethyl ether in the form of a gas, which
gas may be condensed to a liquid form by any suitable condensing apparatus.
The distillation of di-ethyl ether will continue from the mixture until the
hydrogen-ethyl-sulphate is exhausted and its place taken by the product remain-
ing after the distillation, i.c. sulphuric acid, which may be again used to form
hydrogen-ethyl-sulpliate.
The temperature at which distillation will take place can readily be determined
by experiment but I have found it to be between 140° and 160° Fah.
The required quantity of hydrogen-ethyl-sulphate, ethylene, hydrogen and
oxygen can readily be calculated by, and the reactions taking place in the process
are indicated by the following formula:

page_text: known to chemists, but preferably that described in British Patent No. 17,159,.
dated August 9th, 1898, and granted to Frederic R. Coudert Jr.
The hydrogen and oxygen may be obtained by any process known to chemists,
but preferably by electrolyzing water by passing a current of electricity through
it, as by this means these elements are obtained in the required proportions,
hydrogen H, and oxygen O, and in a state or condition in which they are more
active than if obtained by chemical means.
In practice I consider it preferable to collect the gases generated, at the
respective poles and then discharge them separately into the mixture. I take
this course in order to avoid the possibility of forming an explosive mixture in
the vessel.
Instead of forming the hydrogen and oxygen external to the mixture, I may
add these gases in their combined form, ie, in the form of steam, preferably
highly heated steam, of a temperature above 2120 (the higher the temperature
the quicker the disassociation of the gases) or, I may add water to a mixture of
hydrogen-ethyl-sulphate and ethylene, and then electrically decompose the water
by passing an electric current through the mixture, in which case the hydrogen
and oxygen will be set free in a nascent condition.
I do not wish to limit myself to any special apparatus for carrying out my
improved process, and hence I have shown none. However, it will be within the
knowledge of any chemist to arrange a suitable apparatus for carrying the
described process into effect.
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. The herein described process of manufacturing diethyl-ether, which consists
in subjecting a mixture of hydrogen-ethyl-sulphate, ethylene, and hydrogen and
oxygen to the action of heat."
2. The herein described process of manufacturing diethyl-ether, which consists
in subjecting a mixture of hydrogen-ethyl-sulphate, ethylene and water to the
action of an electric current, whereby the water is decomposed into hydrogen and
oxygen, and at the same time subjecting the mixture of hydrogen-ethyl-sulphate,
and hydrogen and oxygen so formed, to the action of lieat.
14. 1941 ..
A 1000
HERBERT HADDAN & Co.,
Agents to the Applicant,
18, Buckingham Street, Strand, London, W.C.