Improvement in the Manufacture of Asphaltum.
Year: 1892

page_text: Date of Application, 16th Feb., 1892-Accepted, 19th Mar., 1892
COMPLETE SPECIFICATION.
Improvement in the Manufacture of Asphaltum.
I, JESSE ADAMS DUBBS, Chemist residing at 95 Lincoln Avenue, in Allegheny,
in the County of Allegheny, State of Pennsylvania, and United States of America,
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 invention described herein relates to the manufacture of asphaltum from
crude petroleum or petroleum residuum, and under the term residuum I include all
heavy products which remain in the still after distillation, whether the distillation
be effected with or without the aid of steam, such as tar, cylinder stock, heavy
oils, etc., and in general terms the invention consists in the combination, when
subjected to heat, of the crude petroleum or petroleum residuum with sulphur, all
as more fully hereinafter described and claimed.
When using Pennsylvania or Lima crude oils, or crude oils similar thereto
containing paraffine or paraffine compounds, the crude oil is subjected to distillation
or evaporation until the paraffine or its compounds which seem to prevent the
combination of the sulphur with the oil, are driven off. The charge in the still is
then reduced about two hundred degrees in temperature, and a proper amount of
sulphur is placed in the still with the cooled residuum. The amount of sulphur
added is about one pound to each gallon of the residuum, though this amount of
sulphur will vary slightly with the character of the asphaltum required, and also
the specific gravity of the residuum. Heat is again applied and the contents of
the still raised to a temperature a little below the point of distillation, and maintained
at this temperature for from two to six hours, more or less, dependent upon the
grade of asphaltum desired.
When using previously formed residuum, such as has been allowed to become
entirely cool, the entire amount of sulphur may be charged into the still together
with such residuum. But I prefer to charge in with the residuum only about 20
to 25% of the total charge of sulphur, and then heat the mixture until traces of
sulphuretted hydrogen (HS) are developed. Firing is then stopped, and 40
to 50% of the entire charge of sulphur is added. Heat is again applied and
continued for from three to five hours, when the remainder of the sulphur is added
and the heat continued until the resultant product will have the desired hardness,
which can be determined by samples taken from the still. The heat to which the
charge is subjected should be a little below the point of distillation. While the
entire amount of sulphur may be added at the beginning of the operation, as above
stated, I find that a more cohesive product is made by adding it at different stages
in the operation.
When my process is carried on as a continuation of the distilling operation, the
sulphur may be charged into the still with the crude petroleum, but no such
combination as is required with the sulphur will be formed, when Pennsylvania or
Lima crude oils are employed, until the paraffine or its compounds have been
removed, as the paraffine and its compounds prevent the chemical combination of
the oil and sulphur, which remains as an inert matter until the distillation has been
carried on to such an extent that the charge in the still will, as heretofore stated,
become viscid when cooled.
Some crude petroleum such as those as are found in Wyoming and other parts of
the country, do not seem to contain the constituents which are in the case of the
Pennsylvania and Lima oils, preventive of the combination of the sulphur with the
crude oils. Hence in working with such crude oils, a suitable quantity of the crude
oil is charged into a suitable still together with twenty to twenty-five per cent.

page_text: (20 to 25%) of the entire amount of sulphur designed to be employed and heat
applied until slight traces of sulphuretted hydrogen are developed. The firing is
then stopped and forty to fifty per cent. (40 to 50%) of the total amount of sulphur
is added, when firing is resumed, and the heat maintained at a point slightly below
the temperature of distillation for from three to five hours, when the remainder of 5
the sulphur is added and the heat continued until the asphaltum has been reduced
to the required hardness. In this case as the others heretofore described, sulphur
is added in about the proportion of one pound for each gallon of the crude oil.
The product of this process is jet black and very close grained, and somewhat
pliable at ordinary temperature. But this pliability when undesirable can be over- 1
come by adding thereto about ten per cent. (10%) of sand or other silicious
material, the addition of such material rendering the asphaltum hard and rigid.
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. The method herein described of manufacturing asphaltum consisting in
subjecting crude petroleum or residuum thereof and sulphur mingled together in
suitable proportions to a sufficient heat to effect the combination of said substances,
substantially as set forth.
2. The method herein described of manufacturing asphaltum, consisting in:
subjecting crude petroleum or residuum thereof and sulphur to a suitable heat,
reducing such heat, charging in an additional amount of sulphur, again subjecting
the entire charge to a further heat, adding more sulphur and continuing the heat
until the product has attained the desired degree of hardness, substantially as set
forth.
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Witnesses-
DARWIN S. WOLCOTT.
E. NEWELL.
JESSE ADAMS DUBBS.