Process of Refining Crude Mineral Oils and their Distillates. Page: 1 of 5
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FELIX C. THIELE, OF NEW ORLEANS, LOUISIANA, ASSIGNOR OFTHREE-
FIFTHS TO JOHN FINKE AND JOHN M. PARKER, OF SAME PLACE.
PROCESS OF REFINING CRUDE MINERAL OILS AND THEIR DISTILLATES.
SPECIFICATION orming part of Letters Patent No. 683,354, dated September 24, 1901.
Application filed May 23, 1901, Serial No. 61,645, No srecimen''
To all whom? ?, imay concern: else but hydrated aromatic hydrocarbons,
Be it known that I, FELIX C. THIELE, a (Beilstein, Organie Chemistry, Vol. III, 1890,
citizen of the United States, residing at New page 279,) their presence has been long sus-
Orleans, in the parish of Orleans, State of pected in crude oils; but their successful 45
Louisiana,have invented certain new and use- separation from the crude oil direct was first
ful Improvements in Processes of Refining effected by me.
Crude Mineral Oils and Their Distillates, of The process is capable of use upon oils of
which the following is a specification. different characters and their distillates.
This invention relates to a process for One method of using the process with crude 5o
refining crude mineral oils and their distil- oil not having a specific gravity higher than
lates. 0.835 is to mix with the oil from .5 to 1. per
The process herein described is especially cent., by weight, of nitric acid of specific
designed to further the purification of refrac- gravity 1.42. The oil or its distillates is agi-
tory crude mineral oils, such as are found in tated with the acid for about half an hour 55
the Trenton limestone formation, present in and then set at rest. When completely set-
Canada and several States in the United tied, the water which has separated out at
States, and particularly the oils discovered of the bottom of the vessel is withdrawn. The
late in the Southern States, as Texas, Lonisi- acid almost combines completely with certain
ana, California, Mississippi, and others, the compounds in the oil, and the following re- 6o
foregoingbeinghereinafterreferredtoingen- actions can be observed during the above
eral as oils of the Lima type. It has for an treatment. The first noticeable action of the
object to manufacture marketable products acid on the oil is the discharge of sulfurous
from these crude oils, and consequently in- acid. The formation of sulfurous acid from
crease the value of the natural products. the oil is partly due to the oxidation of the 65
Terpenes (ClOHiG) and polyterpenes (C10H16) sulfureted hydrogen in the oil and partly due
have been found in almost every crude min- to the elimination of one atom of sulfur in
oral oil, and they exist in the oils in different the shape of SO2 from the organic sulfur con-
forms. One of them is asphaltum, (a mix- pounds in the oil. These sulfur compounds
ture of sulfureted polyterpenes,) present in contain a nucleus (CS) and must be regarded 70
all crude mineral oils found on the Western as derivatives of the trithio carbonic acid,
Hemisphere. It can be readily detected by probably its esters, as in distilling sulfur-
treating the crude oil with tetrachlorid of tin bearing oils very often the odor of allyl-al-
(see Thiele, American Chemical Journal, cohol is observed. A further confirmation
Vol. XXII, No. 6, December, 1899) and was of the above results is found in the fact that 75
found with certaintyby me in Texas crude oils, oils treated according to the herein-described
Lima (Ohio) oil, and Canada oil, (Petrolia dis- process yield on distillation bisulfid of car-
trict ) A further confirmation of the occur- bon (CS2) in the light distillates, which can
rence of terpenes and polyterpenes in crude only have been formed by the primary de-
oils may be found in a paper by Charles F. struction of the higher sulfids into the lower 8o
Mabery, Journal Franklin Inst iute, Vol. sulfids by the nitric acid. The following
CXL, page 1, 1896. As terpenes are nothing equation expresses this reaction:
CS s/H, + 2INO, = CS2 + SO, + 2CH6OH + (NO)2
Tiithiochally Nitic acid Bisulfid of carbon Sulfuious acid Allyl-alcohol Nitiogen dioxid
The second reaction of the nitric acid on
the oil is the formation of nitriles and nitrolic
85 acids in the oil.
The third and fourth reactions observed in
the action of nitric acid on the oil is the elimi-
nation of asphaltum and terpene compounds,
also of certain aromatic hydrocarbons, which
settle as a very viscous tar on the bottom of 90
the vessel. In order to fit the thus-treated
oils for distillation, it is necessary to remove
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Thiele, Felix C. Process of Refining Crude Mineral Oils and their Distillates., patent, September 24, 1901; [Washington D.C.]. (texashistory.unt.edu/ark:/67531/metapth515000/m1/1/: accessed February 22, 2019), University of North Texas Libraries, The Portal to Texas History, texashistory.unt.edu; crediting UNT Libraries Government Documents Department.