AndreaBozzo/ceres-open-data-index huggingface dataset:
SUPERCRITICAL FLUID EXTRACTION OF OIL FROM EASTERN OIL SHALES

This paper describes the recovery of oil from eastern oil shales using modifications of the supercritical extraction techniques that were successful in recovering 90 weight percent of the oil from Green River oil shale. In the case of eastern shales as much as 92 weight percent of the oil in the shale was recovered as a liquid product using tetralin and water at a temperature of 400 degrees C. The chemical composition of the oil extracted from a Chattanooga shale is presented. Changes in composition of minerals under supercritical fluid extraction conditions are discussed and related to the overall recovery process.

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RECOVERY OF OIL FROM EASTERN SHALES USING SUPERCRITICAL EXTRACTION TECHNIQUES

This paper describes the recovery of liquid organic matter from eastern shales using modifications of the supercritical extraction techniques that were successful in recovering 90 weight percent of the organic matter from Green River oil shale. In the case of the eastern shales as much as 90 weight percent of the organic matter in the shale was recovered as a liquid product using tetralin and water at a temperature of 400 degrees C. The chemical composition of the extracted organic materials is also discussed.

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HIGH PERFORMANCE LIQUID CHROMATOGRAPHY SEPARATION OF OLEFIN, SATURATE, AND AROMATIC HYDROCARBONS IN HIGH-BOILING DISTILLATES AND RESIDUES OF SHALE OIL

A high performance liquid chromatography method has been developed for the separation of olefin, saturate, and aromatic hydrocarbons found in high-boiling distillates and residues of shale oil and in whole shale oils. The dual-column chromatographic system used silica gel in one column and silica gel coated with silver nitrate in a second column. Separated fractions are analyzed by infrared and carbon-13 nuclear magnetic resonance spectrometry to demonstrate the validity of the separation. The time required for a separation is about two hours. The separations are reproducible, and recovery of material after separation is generally better than 90%. The olefin, saturate, and aromatic fractions obtained from a separation are suitable for further analyses.

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NMR SPECTRA OF PYRIDINES FOUND IN SHALE OIL (EXTENDED ABSTRACT ONLY)

The nuclear magnetic resonance spectra of the alkyl-substituted pyridines found in the tar bases from a hydrocracked crude shale oil are discussed mainly with respect to the chemical shifts, but where possible the coupling constants'are given for individual proton resonances. A determination of the chemical shift of various alkyl groups attached to the pyridine nucleus permits the identification of various alkyl-substituted pyridines where the gross fraction has been partitioned into simple mixtures by gas chromatography.

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IDENTIFICATION OF NOCTYL CYANIDE IN IN SITU SHALE OIL

At the US ERDA's Laramie Energy Research Center, research on the composition of shale oil has been conducted for a number of years. A fraction of shale oil, which had been produced in our Site 4 in situ field experiment, was examined by Infrared, PMR, CMR, and mass spectral techniques and was found to be at least 85% n-Octyl cyanide admixed with alkylnaphthalenes.

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RESULTS OF POST BURN CORING AT GEOKINETICS RETORT 16, UINTAH COUNTY, UTAH

During the summer of 1980, twenty post burn and two unburned coreholes were drilling into retort 16 at the Geokinetics field site in a jointly funded project by the DOE and the US EPA. The purpose of this investigation is to determine the physical, chemical, and mineralogical characteristics of retorted oil shale in a Geokinetics retort. Lithologic description and Fisher assay of the cores indicate that a complex pattern of six distinct zones was created by the process. Zone A is undisturbed rock, zone B has blast fractures, zone C shows slight alteration along fractures, zone D is blackened retorted shale, zone E is pastel colors representing higher temperatures, and zone F melted rock. The boundary of retorted shale is between zones C and D. Many factors control the formation of these zones.

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REVIEW OF 10 AND 150 TON LETC OIL SHALE RETORT PROGRAMS PRIOR TO 1976

For over 30 years the Laramie Energy Technology Center has been actively engaged in oil shale technology research specifically to study various scenarios of oil shale conversion to some type of useable liquid product. One technique which appeared to have significant economic and environmental advantage over others was in situ retorting. Whether "true" or what later evolved and was known as "modified" in situ retorting would apply depended on a number of factors. In either case, successful recovery of substantial quantities of oil from a fractured mass of oil shale depended largely upon permeability, particle size distribution, the degree of control that could be maintained in directing the retorting front and the uniformity of the rate of advance of the front.

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SOME DEGRADATION PRODUCTS OF COLORADO OIL SHALE KEROGEN; KEROGEN CONSTITUTION

The constitution of Colorado oil-shale kerogen was studies by conducting a qualitative organic examination of relatively simple or identifiable degradation products derived from it by degradative chemical action. By this preliminary study it was hoped to provide some qualitative data which would indicate, even though in a highly fragmentary manner, some essential characteristics of its total constitution and structure.

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CORROSION OF ALLOYS FOR TAR SANDS SYSTEMS AND IN SITU GASIFICATION

In situ coal gasification has the potential for making available significant quantities of fossil energy resources which are currently either uneconomical or technologically unfeasible to mine, this significantly increasing this country's recoverable energy reserves. In addition it provides the means of overcoming numerous health, safety, and environmental obstacles to conventional mining, although it contains several potential obstacles of its own, such as ground subsidence and/or water table pollution.

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SOME RESULTS FROM THE SITE 9 IN SITU OIL SHALE EXPERIMENT AT ROCK SPRINGS, WYOMING

An economically feasible method to recover oil from the vast oil shale resources of Wyoming, Colorado, and Utah has long been sought. Until the early 1960's, nearly all work was centered on techniques which mined the shale and recovered oil from the mined shale in aboveground retorts. That approach is useful for only the one-third of oil shale which is high grade and suited for conventional mining techniques. In the early 1960's, Laramie Energy Research Center initiated tests to develop techniques for inducing the permeability necessary for recovery of oil by in situ processing. Successful implementation of in situ recovery will make available the two-thirds of shale oil not suited to conventional mining. Oil produced by in situ recovery can be an economic, environmentally sound contribution to American energy independence.

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EVALUATION OF ROCK SPRINGS SITE 9 IN SITU OIL SHALE RETORTING EXPERIMENT

Results of the first 150 days of operation of an in situ oil shale retorting experiment near Rock Springs, Wyoming, are presented. A zone of oil shale located in the Tipton Member of the Green River Formation was retorted. The target zone was 137 feet deep, 40 feet thick, and assays 21.3 gallons of oil per ton of shale. A section 70-feet square with eight peripheral production wells was hydraulically fractured to produce three horizontal fractures. Slurry-type explosive was forced into the fractures and detonated to produce a bed of oil shale rubble.

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EVALUATION OF AN IN SITU OIL SHALE RETORTING EXPERIMENT IN WYOMING

The results of the first 150 days of operation of an in situ oil shale retorting experiment are presented. A zone of oil shale between 137 feet and 177 feet deep in the Tipton Member of the Green River Formation was retorted. The oil shale averaged 21.3 gallons per ton in the target zone. A section 70-feet square with eight production wells was hydraulically fractured to produce three horizontal fractures. Slurry-type explosive was forced into the fractures and detonated to produce a bed of fractured oil shale.

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CHARACTERIZATION AND TREATMENT OF RETORT WATER FROM IN-SITU OIL SHALE PROCESSING FINAL REPORT

The purpose of this study was to develop the background necessary for identifying processes which might be effective for the treatment of water developed in the in situ retorting of oil shale. In this regard, literature information has been summarized dealing with several aspects of the retort water treatment and disposal problem. The specific information relates to the quantity of the water, its physical and chemical characteristics, and insight developed by other authors concerning possible treatment alternatives.

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INVESTIGATION OF THE GEOKINETICS HORIZONTAL IN SITU OIL SHALE RETORTING PROCESS PHASE III--INITIAL REPORT FOR THE PERIOD NOV.1/1976-JULY 31/1977

Geokinetics, Inc. began full scale work on in-situ oil shale processing during 1971. Extensive planning, design work, and cost analysis was done on a wide variety of in-situ retorting plans under a variety of geologic conditions, in preparation to participate in the Federal Prototype Oil Shale Leasing Program. During 1973 and 1974, a series of tests were designed which were run in above ground steel retorts during 1974 and 1975 to test the concept of a horizontally moving firefront. Encouraged by the results of these tests, in June 1975, Geokinetics moved the test operation into the field and began building and operating a series of small retorts underground. These retorts have been gradually scaled up in size. A total of 15 retorts have been built to date and of these, six have been operated. The size of the retorts has ranged from 66 to 7200 tons. A complete field camp facility has been set up at the field test site to provide full time living quarters and support facilities for the operating personnel. Five hundred barrels of crude shale oil have been produced and shipped to the Platcau refinery at Roosevelt, Utah. Their oil has been blended with conventional crude oil and refined.

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PALEOLIMNOLOGY AND OIL SHALE GENESIS IN GREEN RIVER FORMATION, COLORADO

The Green River Formation was formed from sediments laid down in a series of ancient lake beds of Middle Eocone age in Colorado, Utah, and Wyoming. The formation contains hydrogen-rich organic matter in its oil shales which represent 2 trillion barrels of shale oil in place and it covers an area of 17,000 square miles. The continuous oil shale was formed under a combination of physical, biological, and chemical conditions in a stratified lake. The initial study is aimed to provide evidences in postulating the physical conditions in which appropriate geochemical and sedimentation process could form oil shale. One of the major needs in generating further understanding of the Eocene Green River Formation would be in the investigation of their physical paleolimnology. The lake dynamics provides a critical mechanism for heat transfer, mixing, turbulence, and particle settling. It also affects the productivity of organic material, concentration and decomposition of organic material and ultimately the reaction rate and balance of geochemical processes. The study approach can be a powerful tool to interpret the unique oil shale formation and its distribution.

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GASIFICATION OF GREEN RIVER OIL SHALE KEROGEN

Green river oil shale kerogen when reacted with a sodium tetra-chloroaluminate melt, gasifies efficiently under a low pressure of hydrogen. The function of the tetrachloroaluminate melt is to promote radical formation and rearrangement of aliphatic units through chemical effects in addition to the role the solvent plays as a thermal transfer agent. The mechanism of gasification appears to involve the generation of electron deficient sites, which either undergo bond breakage or rearrange resulting in the formation of low-molecular-weight hydrocarbons, normally gases or near gases at ambient temperatures. The product gases are sufficiently clean that conventional scrubbing techniques may be used and that the process may be operated on a semi-continuous basis.

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OPTIMUM BLASTING IN BEDDED AND JOINTED OIL SHALE FORMATIONS

This report addresses the need for the development of a rational approach to retort blast designs. Specifically it: a) reviews oil shale fragmentation experience to date; b) reviews fragmentations experiments which have been conducted in other jointed rocks; c) based upon a and b proposes some critical oil shale fragmentation experiments which could improve the design base.

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STUDY OF GILSONITE COKER DISTILLATE

The result of this discussion and subsequent correspondence was that the Bureau of Mines agreed to do a small amount of preliminary testing and evaluation of a sample of coker distillate prepared from gilsonite a the university of Utah. Should this study indicate that additional research work would be of interest to the Bureau of Mines, then discussions were to be held relative to establishing a cooperative research project on these materials to be sponsored.

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GAS HYDRATES, ARTIC/OFFSHORE RESEARCH, AND DEEP SOURCE GAS CONTRACTORS REVIEW MEETING

Gas hydrate research, one of the new research efforts in DOE's program on Unconventional Gas Recovery, is focused on the basic sciences related to the formation and dissociation of naturally formed gas hydrate deposits. The research goals are: (1) to determine the extent and nature of the natural gas hydrate resource, and (2) to develop methods to extract it for a future gas supply.

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POST-BURN STUDY OF THE ROCKS SPRINGS, SITE 9 IN SITU RETORTING EXPERIMENT

After completion of the experiment, a post-burn evaluation was made to determine the vertical and horizontal dimensions of the thermal halo and the retorted shale. Post-burn cores were drilled and visually examined, and bitumen or oil samples were analyzed for chemical composition and physical properties to produce analytical data that were analyzed by computerized pattern recognition techniques.

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KEROGEN CONSTITUENTS: REDUCED CHLOROPHYLLIN AS A MODEL FOR THE PRECURSORS OF NITROGENOUS COMPOUNDS IN SHALE OIL

"In evaluating and developing the resource potential of the Nation's vast oil-shale reserves, the U. S. Bureau of Mines has been conducting research in the origins and chemistry of shale oil. As part of this work, the role of plant pigments and their decomposition products as possible precursors of the nitrogenous compounds found in shale oil was investigated. An accurate picture of the origin of the compounds and their compound types may be on aid in analyzing the character of the oil, its suitability as a refinery feedstock, are perhaps its importance as a source of commercially valuable chemical compounds.  The idea that plant pigments may be the origin of nitrogen-containing compounds in shale oil is not new. Mapstone has proposed that the pyrroles found in shale oil result from the pyrolysis of the porphyrins in chlorophyll.  It has been show that kerogen, the organic phase of oil shale, is 45 to 60 percent heterocyclic material.  This work was undertaken to substantiate  Mapstone's proposal and to see if plant pigments could be the origin of the heterocyclic material in kerogen.  Experimentally, a comparison between the nitrogen compounds in a shale-oil light distillate and the nitrogenous compounds found in the pyrolysates of chlorophyll derivatives was made. The similarity, of the compounds found in both the shale oil and chlorophyllin pyralysate indicates that reduced chlorophyll in derivatives are a good model for the portion of kerogen that produces nitrogen compounds upon pyrolysis of oil shale. The present paper describes the preparation and characteristics of the kerogen model and shows that pyrolysis of this model yields pyrroles and products which are comparable to the nitrogenous products of shale oil."

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COMPOSITIONAL VARIATION OF RETORTED SHALE OILS WITH STRATIGRAPHY: WYOMING CORE, NORTHERN GREEN RIVER BASIN

"Current plans for the commercial development of oil shale  resources are designed to obtain the maximum amount of oil from the least amount of shale. Within the United States, the industry would use the thick, rich seams which are reasonably close to the surface in the Green River Formation in the Rocky Mountain region. This formation is made up of four principal basins, the Piceance Creek Basin in Colorado, the Uinta Basin in Utah, and the Green River and Washakie Basins in Wyoming. The construction of mining operations, both surface and subsurface, to support aboveground retorting processes will be designed in such a manner that the thickest seams of rich shale will be used. Modified in situ retorts will be designed to develop the tallest rubble chimneys technically feasible. True in situ retorting sites will be located in those shale seems which are inaccessible to the other technologies and will produce the maximum amount of high quality product oil. Of all the possible variables which can affect the quality of shale oil, the retorting method is by far the most significant. It's also known that shale type can affect  oil quality. A detailed study of Colorado shale oils and  Paraiba Valley (Brazil) shale oils showed significant differences between the two in such characteristics as residuum content, nitrogen content, distribution of nitrogen by boiling range in the oil and hydrocarbon types  Consideration of the quality of the shale from a given location has generally been confined to the variations in yield (gallons of oil per ton of shale) and its mining and retorting properties."

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"PHYSICS OF OIL SHALES A PROGRAM OF THEORETICAL AND  EXPERIMENTAL STUDIES-ANNUAL REPORT (SEPT 21,1981-SEPT 20,1983)"

"The available dielectric data on oil shale materials in the  frequency range (0-1GHz) is analyzed in tens of several empirical dielectric functions proposed earlier in the literature for other materials. The empirical functions involving a distribution of relaxation times represent the data satisfactorily. The implications of these relaxation times with respect to the properties of oil shales are  discussed. Fits of the Lichtenieker's formula to the dielectric data are used to extract the average dielectric constants of Kerogen and the inorganic parts."

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FUNDAMENTAL FACTORS IN ANALYZING AND EVALUATING OIL SHALES

A comparative study of the oil shales in the US will have very little value unless, from the analyses or assays, definite conclusions can be reached as to the quantity and quality of the petroleum substitutes and by-products that may be produced from each shale. The operator of a prospective oil shale plant desires information that will enable him to predict the quantity and quality of oil and other substances that a commercial plant will produce. These data can only be secured through very comprehensive laboratory tests. This chapter brings out those principles of testing which must be recognized and applied in order that reliable data may be obtained and logical conclusions reached.

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GAS COMBUSTION RETORTING PROCESS

In 1944, under the Synthetic Liquid Fuels Act, the Bureau of Mines was directed to supply the scientific engineering, and economic information required for the establishment of an American shale-oil industry. To develop the necessary retorting technology, numerous paper studies of existing processes were made. Also, several field trips were made to obtain information and, where possible, to observe the operation of existing retorting plants. Later several processes were tried at Rifle on a pilot-plant scale. The gas-combustion processes is the result of the development work to date.

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PRELIMINARY FILTRATION STUDY ON CRUDE SHALE OIL FROM RIFLE, COLORADO

"A drum of crude shale oil was secured from the Bureau of Mines Shale Oil Development Plan at Rifle, Colorado for experimental filtration work. This oil is the product from their N-T-U retorting plant. The oil as received contains small percentages of emulsified water and rock dust. Preliminary studies to remove these contaminants by filtration were made. Effect on rate of flow of  temperature and percentage of filter aid was investigated using Hyflo Super-Cel and Celite 503. Increased rates of flow were obtained at the higher filtration temperature,  Rates of 7.9 gals/sq ft/hr with 0.4 per cent Hyflo and 9.0 gals/sq ft/hr with 0.4 per cent Celite 503 were obtained at 900C  In both cases, rock dust and water content were substantially decreased."

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COMPARISON OF SEVERAL SURFACE OIL SHALE PROCESSES COMBINED WITH A MODIFIED IN SITU OIL SHALE PROCESS

"In this study, several surface schemes for using the oil shale by-product of the vertical modified in situ (MIS) process have been combined with a single hypothetical MIS process and evaluated from the standpoint of engineering feasibility. The objective of the study is to identify those processes that are economically attractive when combined with the MIS process. The alternative  process schemes use the energy or products produced from the by-product oil shale to upgrade the liquid and/or gaseous products of the MIS process, or to otherwise enhance it. The by-product oil shale is that which is mined in the construction of the MIS retort void volume and operational accesses. The method of approach selected to meet this objective involves the evaluation of a specific surface process in combination with the MIS process and  the comparison of results with an appropriate base case. The base case is the direct-surface retorting process combined with the MIS process. The candidate alternative surface schemes were limited to those for which a  reasonably complete definition exists and sufficient process data could be discovered or developed for a comparative evaluation. The MIS process has been studied by several different organizations, varying from commercial developers and consortiums to national laboratories. The present developmental status of the process is such that the amount of shale removed in the construction of the MIS retort void volume and the necessary accesses for operation and product recovery can be fairly well defined relative to the amount that can be retorted in situ. However, the control of the operation of the MIS retort is not well understood, and experimental  and theoretical study of the chemical and physical processes continues. It is assumed that the projected retort performance and production  of the MIS process can be achieved. Therefore, study efforts are directed to the coupling of the MIS process with the surface process and its products. It must be noted that the study results are relative: relative economics and relative developmental potential of the various alternative schemes are compared. This is consistent with both the study objective and the present state of the technology. The reported study is a screening evaluation, and the results have use primarily in planning for future research and developmental efforts."

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