Year: 1886

page_text: Date of Application, 27th Aug., 1886.
Complete Left, 26th May, 1887.
Complete Accepted, 28th June, 1887.
RESERVI
I ALEXANDER NIKIFOROFF of Chika, near Moscow, in the Empire of Russia,
Engineer do hereby declare the nature of this invention to be as follows:-
The tar obtained from naphtha or naphtha residues resulting from the manufacture of
gas contains hydrocarbons of the aromatic series C" H2-6, anthracene and naphthaline,
the same as are contained in coal tar.
In distilling naphtha or naphtha residues according to my invention I obtain,
besides other products, about fifteen per cent of benzol and about 0.5 per cent of
anthracene.
To obtain aromatic hydrocarbons, naphtha or naphtha residues are subjected to two
processes. The first process has for object to obtain as large a quantity as possible of
hydrocarbons boiling from 0° to 200° cent. and having a specific gravity of about
0,800 to 0,810. The second process has for object to transform the said hydrocarbons
into hydrocarbons C H-6, sp. gr. 0,870.
The product boiling at a temperature of from 200° to 300° cent. contains naphtha-
line and other matters. From the remaining matter which boils at a temperature
above 300° cont. anthracene is obtained which can be extracted by the ordinary
moans.
To obtain hydrocarbons boiling from 0° to 200° cent. and having a specific gravity
of 0,800 to 0,810 naphtha or naphtha residues are subjected to a slow decomposition
by means of repeated distillations in cylindrical retorts. The retorts are provided
with corresponding condensers and receivers. The stream of naphtha or naphtha

page_text: residues and the temperature of the retorts should be such as to produce not more
than fifteen per cent of gas and the remainder should pass into the receiver in the
form of tar.
From the tar AI thus produced I then extract by distillation all the liquid which
boils at from 0° to 200° cent. -B I. A rosidue is obtained which boils only at a
temperature above 200° cent. - CI. The residue CI is subjected to a second distilla-
tion when and under the same conditions is produced tar A 2, from which is distilled
all that boils from 0° to 200° cent. and then there will remain a residue C2. About
thirty per cent of hydrocarbons boiling from 0° to 200° cent. can be obtained from
the naphtha or naphtha residues treated. The number of distillations are from 4 to 6.
The second process consists in the distillation of the hydrocarbons obtained as above
and boiling at from 0° to 200° in the retorts at a certain pressure and temperature.
The temperature of the retorts and the pressure must be such as will produce not less
than soventy per cent of tar having a specific gravity of not less than 1.00.
From the tar produced are distilled the hydrocarbons boiling at from 80° to 135°
and the product will have a specific gravity of 0,870 representing in itself hydro-
carbons H-8. About fifty per cent of such hydrocarbons can be thus obtained.
The product obtained is refined by a second distillation and treatment with sulphuric
acid and soda. On treating it with nitric acid it produces from 130 to 140 per cent
of nitro-product with a specific gravity of 1.19. On reduction the nitro-product gives
from 55 to 60 per cent. of aniline oil boiling at from 180° to 200° and with a specific
gravity of 1,014.
From the residue of tar above 135° anthracene and naphthaline are obtained.
In the second distillation the process can be effected in cylindrical or in other shaped
retorts observing the conditions by which the most advantageous pressure can be
made at a certain temperature and flow of the products. I have found that the best
result is obtained if the hydrocarbons boiling at from 0° to 200° cent. are divided for
the second distillation into two parts viz.: those boiling at from 0° to 140° and
higher and then to redistil them again separately.
The results produced will be:-about 12 per cent of benzol boiling at from 80°
to 135° cent. sp. gr. 0.870
and a residue consisting of a mixture of different hydrocarbons some of which can be
used for the manufacture of lubricating oils.
By distilling naphtha or naphtha residues in any suitable manner a part of the
hydrocarbons contained therein which boils at a low temperature will be carried away
by the gas produced, thereby increasing its lighting qualities. Low boiling hydro-
carbons carried away by the gas are dissolved in hydrocarbons boiling at above 170°
cent. For the collection of these hydrocarbons from the gas obtained in producing
benzol the gas is passed through a scrubber or washer.
For this purpose into the scrubber, instead of water, are admitted hydrocarbons
boiling at a temperature above 170°. In experimenting I have obtained about four
per cent of hydrocarbons boiling from 0° to 140° cent. from the naphtha or naphtha
residues taken. Their specific gravity is equal to 0,825. By employing my process
of transforming them into the aromatic series, about two per cent of hydrocarbons is
obtained boiling at from 80° to 135° cent. and with a sp. gr. of 0,870.
My invention is based on the theory of producing firstly, easily transformable
hydrocarbons with a grouping of elements capable of being transformed into a more
solid group, viz: into the aromatic group. These hydrocarbons at the pressure and
temperature obtained by a second distillation of the tar boiling at from 0° to 200°
cent. produce benzol from which aniline oil can be prepared.
Up to the present time it has not been possible to produce benzol commercially
from naphtha. I am aware that it has been proposed to produce benzol in retorts

page_text: charged with coke, copper filings or platinised coke, but as each charging of the
retorts, besides increasing the cost of the production is quite impracticable owing to
the stopping up of the retorts, such method of producing benzol has not answered.
By distillation of the products boiling at from 0° to 200° cent at a pressure and a
certain temperature as above described coke detaches itself in the retorts which up to
the present has not occurred in the distillation of naphtha or naphtha residues for gas.
The benzol produced is that product which is known in commerce as 50 per cent.
Benzol. It boils at a temperature of from 80° to 135° cent. and produces the aniline
oil of commerce.
Dated the 27th day of Angnet 1886

page_text: I, ALEXANDER NIKIFOROFF, of Chimka, near Moscow, in the Empire of Russia,
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:-
-
The tar obtained from naphtha or naphtha residues resulting from the manufacture
of gas contains hydrocarbons of the aromatic series C H2-6, anthracene and
naphthaline, the same as are contained in coal tar.
In distilling naphtha or naphtha residues according to my invention I obtain
besides other products about fifteen per cent. of benzol and about 0.5 per cent of
anthracene.
To obtain aromatic hydrocarbons, naphtha or naphtha residues are subject to two
processes. The first process has for object to obtain as large a quantity as possible
of hydrocarbons boiling from 0° to 200° Cent., and having a specific gravity of
about 0,800 to 0,810. The second process has for object to transform the said
hydrocarbons into hydrocarbons C H2-, sp. gr. 0,870.
The product boiling at a temperature of from 200° to 300° Cent. contains
naphthaline and other matters. From the remaining matter which boils at a
temperature above 300° Cent. anthracene is obtained which can be extracted by the
ordinary means.
To obtain hydrocarbons boiling from 0° to 200° Cent., and having a specific gravity
of 0,800 to 0,510 naphtha or naphtha residues are subjected to a slow decomposition
by incans of repeated distillations in cylindrical retorts. The retorts are provided
with corresponding condensers and receivers. The stream of naphtha or naphtha
residues and the temperature of the retorts should be such as to produce not more
than fifteen per cent. of gas and the remainder should pass into the receiver in the
form of tar.
-
From the tar Al thus produced I then extract by distillation all the liquid which
boils at from 0° to 200° Cent - BI. A residue is obtained which boils only at a
temperature above 200° Cent CI. The residue C1 is subjected to a second
distillation, when, and under the same conditions, is produced tar A 2, from which is
distilled all that boils from 0° to 200° Cent and then there will remain a residue C 2.
About thirty per cent of hydrocarbons boiling from 0° to 200° Cent. can be obtained
from the naphtha or naphtha residues treated. The number of distillations are
from 4 to 6.

page_text: The second process consists in the distillation of the hydrocarbons obtained as above
and boiling at from 0° to 200° in the retorts at a certain pressure and temperature.
The temperature of the retorts and the pressure must be such as will produce not
less than seventy per cent of tar having a specific gravity of not less than 1.00.
From the tar produced are distilled the hydrocarbons boiling at from 80° to 135°
and the product will have a specific gravity of 0,870 representing in itself hydro-
carbons H-8. About fifty per cent of such hydrocarbons can be thus obtained.
The product obtained is refined by a second distillation and treatment with sulphuric
acid and soda. On treating it with nitric acid it produces from 130 to 140 per cent
of nitro-product with a specific gravity of 1,19. On reduction, the nitro-product
gives from 55 to 60 per cent of aniline oil boiling at from 180° to 200° and with a
specific gravity of 1,014.
From the residue of tar above 135° anthracene and naphthaline are obtained.
In the second distillation the process can be effected in cylindrical or in other
shaped retorts observing the conditions by which the most advantageous pressure can
be made at a certain temperature and flow of the products. I have found that the
best result is obtained if the hydrocarbons boiling at from 0° to 200° (Jent. are divided
for the second distillation into two parts viz:-those boiling at from 0° to 1.40° and
higher and then to ro-distil thom again separately.
The results produced will be about 12 per cent of benzol boiling at from 80° to
1350 Cent en Com 0470
and a residue consisting of a mixture of different hydrocarbons some of which can be
used for the manufacture of lubricating oils.
By distilling naphtha or naphtha residues in any suitable manner a part of the
hydrocarbons contained therein which boils at a low temperature will be carried away
by the gas produced, thereby increasing its lighting qualities. Low boiling hydro-
carbons carried away by the gas are dissolved in hydrocarbons boiling at above
170° Cont. For the collection of these hydrocarbons from the gas obtained in
producing benzol, the gas is passed through a scrubber or washer.
For this purpose into the scrubber, instead of water, are admitted hydrocarbons
boiling at a temperature above 170°. In experimenting I have obtained about four
per cent of hydrocarbons boiling at from 0° to 140° Cent. from the naphtha or naphtha
residues taken. Their specific gravity is equal to 0,825. By employing my process
of transforming them into the aromatic series, about two per cent of hydrocarbons is
obtained boiling at from 80° to 135° Cent. and with a sp. gr. of 0,870.
My invention is based on the theory of producing firstly, easily transformable
hydrocarbons with a grouping of elements capable of being transformed into a more
solid group viz: into the aromatic group. These hydrocarbons at the pressure and
temperature obtained by a second distillation of the tar boiling at from 0° to 200° Cent.
produce benzol from which aniline oil can be prepared.
Up to the present time it has not been possible to produce benzol commercially from
naphtha. I am aware that it has been proposed to produce benzol in retorts charged
with coke, copper filings, or platinised coke, but as each charging of the retorts,
besides increasing the cost of the production, is quite impracticable owing to the
stopping up of the retorts, such method of producing benzol has not answered.
By distillation of the products boiling at from 0° to 200° Cent. at a pressure and a
certain temperature as above described coke detaches itself in the retorts which up to
to the present has not occurred in the distillation of naphtha or naphtha residues
for gas.
The benzol produced is that product which is known in commerce as 50 per cent,
Benzol. It boils at a temperature of from 80° to 135° Cent. and produces the aniline
oil of commerce.

page_text: 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 :-
The manufacture or production of benzol, anthracene, naphthaline and other products
from naphtha and naphtha residues by first slowly decomposing naphtha or naphtha
residues in cylindrical retorts at a low temperature so as to produce as large a quantity
as possible of hydrocarbons boiling at a temperature of from 0° to 200° Cent. and then
submitting the said hydrocarbons to a second distillation by which they are trans-
formed into aromatic hydrocarbons C H¼-6 (benzol) the residues being then
treated in known manners in order to produce anthracene, naphthaline and other
products substantially as hereinbefore described.