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Pre-Conc Treatment of Tar Sand Project Proper

Pre-Conc Treatment of Tar Sand Project Proper

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PRE-CONCENTRATION TREATMENT OF ONDO TAR SAND RESIDUE FOR RUTILE RECOVERY

By

OJO Adedayo Adeyinka (MME/2003/036)

A THESIS SUBMITTED TO THE DEPARTMENT OF MATERIALS SCIENCE AND ENGINEERING, FACULTY OF TECHNOLOGY, OBAFEMI AWOLOWO UNIVERSITY, ILE-IFE, OSUN STATE, NIGERIA.

IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE AWARD OF BACHELOR OF SCIENCE (B.Sc HONS) DEGREE IN MATERIALS ENGINEERING

FEBRUARY 2010

CERTIFICATION I certify that this research was carried out by OJO Adedayo Adeyinka of the department of Materials Science and Engineering, Obafemi Awolowo University, Ile-Ife, Osun state, Nigeria under my supervision.

______________ Dr. L.E. Umoru Head of Department

_________________ Engineer A.A. Adeleke Project Supervisor

______________ Date

_______________ Date

DEDICATION I dedicate this work to the glory of God Almighty, who made it possible despite all odds and challenges, for me to bring this work to completion. Also to my parents Mr. and Mrs. OJO, for the grand opportunity given to me to run this degree programme and all the support they offered me both financially and morally. To my beautiful sisters, family friends and well wishers; thank you all and God Bless.

ACKNOWLEDGEMENT My profound gratitude goes to my supervisor, Engr. A.A. Adeleke whose ideas, advice, literature and moral support were pivotal in bringing this research to successful completion. I will also use this opportunity to thank the members of staff of the department’s Metallurgical Testing Laboratory, most especially Mr. Olaoye. My appreciation also goes to my very good friend and project partner, Oladokun Babajide for his dedication and selfless efforts during the course of this work, God bless you. Also to my colleagues, Yahaya, Sanusi, Adeniran, thank you for your support. My special thanks and recognition goes to my parents for their immense financial contribution to the execution of this research, and also to my favorite uncle, Dotun Somoye for his contributions. God shall surely reward you all greatly. To almighty God, who made all things possible, I shall always remain grateful to you. God Bless. OJO, A.A February, 2010

ABSTRACT
Ondo tar sand has been shown in literatures to contain appreciable content of rutile for which Nigeria has no known large deposits. This research was therefore designed to recover substantial proportion of rutile from Ondo tar sand. The sand residue of the Ondo tar sand was subjected to particle size analysis, composition analysis, and gravity pre-concentration using shaking table, dense medium separation and leaching treatment. This research was used to determine the liberation size of rutile in the tar sand residue and provide process parameters to effectively pre-concentrate the sand residue for rutile recovery. Rutile is an important raw material used in paints, plastics, rubber, ceramics, high quality paper as well as other vast applications. The successful recovery of high grade rutile from Ondo tar sand will provide a reliable source of good grade TiO2 for various industrial applications, especially the local paint industry; thus, reducing dependence on imports and boosting our foreign exchange earnings.

.....................................................................................................2 DEDICATION....................................................................................................................4 ABSTRACT.11 Leaching Treatment..................8 CHAPTER ONE...36 2.....21 2......................................................................... 7 LIST OF FIGURES............................................................................15 2..........9 Dense Media Separation (DMS)................................................34 2...................................................................................................... 3 ACKNOWLEDGEMENT..................5 Nigerian Tar Sands............. 6 LIST OF TABLES..................................38 3..................... 29 2...................................33 2................................................................................9 1...................................................................................................................................................8 Rutile.......................................................14 2................9..........................1 Derivation of equation to obtain the required Density from the mixture of two liquids............................................................ 9 CHAPTER TWO.............3 Determination of most potent reagent.....2.......................................................................TABLE OF CONTENTS PRE-CONCENTRATION TREATMENT OF ONDO TAR SAND.....................1 Background............................................................... 13 Definition of Tar Sand.....3 Composition of Tar Sand ..............................................................................................................................................................................................................................................2 Origin of Tar Sand ..................................1 Materials.....................................................36 CHAPTER THREE.............................................................................................................................................. 27 2............1 CERTIFICATION..............................10 Shaking Tabling ..................................................................................................38 3..........................................................................................................................................4 Microstructure of Tar Sands ......................................................................................................42 ......................................5 TABLE OF CONTENTS............................................. .................................6 Mineral and Metal Content of Tar Sand ...7 Identification and Analysis of tar and sand valuable mineral and metal content..............................................................................17 2....................................................................19 2................................25 2............................................

...........53 CHAPTER FIVE..............52 4................................................................................................................................43 CHAPTER FOUR................1 Results....5 Determination of optimal reagent concentration............................ 56 LIST OF TABLES Table 2...................3..................2...........54 5................................................2: Determination of Contact Time for Highest Recovery Table 4..... 55 REFERENCES..................52 4..3: Specific gravity of some heavy liquids Table 4...................................................... Nigeria Table 2.................3: Determination of Leaching Efficiency Using Sodium Hydroxide Table 4............47 4................................2: Specific gravity of some Oxides Table 2...................4 Determination of optimal leaching time ........................... 47 4............................42 3.4: Analysis of Bitumen and Sand Residue Recovery from Tar Sand ....................2.............................. 54 5...............................1: Determination of Suitable Leaching Reagent Table 4......................................................................2 Discussion of Results..........2..................43 3..............6 Sieve Analysis Ondo Tar sand Residue.............2 Effect of Sodium Hydroxide in Recovery of Bitumen and Sand Residue...............2 Recommendations...................................................1 Recovery of Heavy Bitumen and Sand Residue from Tar Sand............1: Comparative Analysis of Tar Sand Samples Collected in Ondo State.1 Conclusion.......2...............................................................2............................................................................

2: Simplified Diagram of Hot Water Recovery Process Figure 4.5 Sieve Analysis of Tar Sand Residue Table 4.1: Microstructure of Tar Sand Figure 2.Table 4.1: Sieve Shaker Figure 3.2: Raw rutile sample Figure 3.3: A graph showing the weight of Bitumen and Sand residue recovery .6: Mineralogical Composition of Ondo Tar Rich Sand residue LIST OF FIGURES Figure 2.2: A graph showing the weight of sodium hydroxide against sand tailings Figure 4.1: A graph of recovery of bitumen and sand tailings against contact time Figure 4.

convectional crude petroleum has enjoyed a monopoly of the energy scene. valuable minerals and metals in varying proportions.1 Background Over the years. Madagascar.CHAPTER ONE INTRODUCTION 1. recovery of “synthetic crude” and other minerals from tar sands takes on a new significance. Although exceedingly rich in oil. Russia. United states and Nigeria to mention but a few. often referred to as bituminous sand or oil sands occur in various parts of the world including Canada. development of . Tar sand deposits. As the demand for energy begins to be on the rise the world over and as production and distribution problems of all fuels became pronounced. Venezuela.

can add to the much desired flexibility of Nigeria’s present and future petrochemical industry. Tar sands are water wetted or . The bitumen in tar sands cannot be pumped from the ground in its natural state. protection for electric cable. 1984). The technology of mining tar sand in a most unfavourable climatic condition has been mastered and plants are in full operation for converting extracted bitumen to synthetic crude and a subsequent refining to conventional refining products (Allen and Stanford.such deposits has been slow. inaccessibility of the deposits. usually using strip mining or open pit techniques. Slow development has been attributed to technical problems associated with production and processing. The bituminous materials. The sulphur content of Nigeria tar sand constitutes a potential source of elemental sulphur for sulphuric and superphosphate fertilizer production plants (Adegoke et al. 1973). apart from the production of crude oil. which is then refined into oil. Tar sands can be mined and processed to extract the oil-rich bitumen. this general picture has taken significance turn over the last 15 years. however. In the particular case of Canada. in other cases. instead tar sand deposits are mined. Tar sand reserves in Ondo state alone is estimated to be about 31billion metric tonnes. The estimate is about 35-45 billion barrels of heavy oil trapped in tar sand deposits in Ondo State alone. Other industrial applications include production of anticorrosive coatings. 1980). There are few instances in earlier years where saturated sand was mined for use as paving material and limited amounts of heavy oil were extracted and turned into more or less conventional-type petroleum products. Tar sand deposit can be mined by the use of open-pit method (for thicker over-burden) or by the use of in-situ method (hot water process). 1980). Russia and Venezuela (Adegoke et al. or the oil is extracted by underground heating with additional upgrading. bonder adhesives and brake lining to mention a few. It is estimated that the Nigeria tar sand is the fourth largest in the world after Canada. with more reserves in Ogun and Delta States (Wood.

Rutile is one of the most common titanium minerals. It is also associated with quartz. 1983). ranging from 25 to 35 percent. Rutile is brownish red and other shades. The tar sand with 5-10 wt% of bitumen is designated to be good or medium grade. and minerals. With several means of analysis. extraction techniques for the tar sand are different (Carrigy. The clays consist of kaolinite. This study is aimed at the preconcentration treatment of Ondo tar sand residue for Rutile recovery. with small amounts of feldspar. ilmenite. the tar sands are transported to an extraction plant. different component and distribution of minerals and metals existing in Nigeria tar sand is revealed. present as grains. It has a . 1996). sometimes up to 10%. along with the other titanium mineral.hydrocarbon wetted. the oil sands in this deposit have great diversity in their composition and properties (Shaw et al. schist. Heavy minerals such as titanium-bearing minerals. such as the liquid medium which is in contact with the mineral particles of the tar sand. Titanium. Generally. occurring in gneiss. where a hot or cold water process separates the bitumen from sand. mica. Nickel and Zircon of economic importance have also been revealed in tar sands. 1996). As a result of this. water. 1960). Rutile is a major mineral source of the element titanium. bitumen and some mineral accessories. It has long been established that tar sand tailings greatly concentrate these minerals. granite. illite and chlorite in different ratios. Tar sands are frequently characterized by their mineralogy. it is common in beach sand deposits. the predominant mineral is quartz. As a secondary mineral. Consequently. but not black. After mining. Basically. hematite and feldspar. water. Vanadium. Minerals in several tar sand tailings (clay fraction) are very similar with little variation in composition (Ignasiak et al. limestone and dolomite. Rutile is typically about 60% titanium and 40% oxygen. It can have some iron present. mica flakes and clays (Shaw et al. tar sand is composed of sand. Tar sand deposits are diverse and contain varying amounts and sizes of mineral components in ores from various zones. The tar sands also have varying porosity.

a metallic luster and a pale brown streak. . Conduct dense media separation. shaking tabling and leaching treatment of the sand residue to concentrate TiO2 and determining the most suitable method. ii.3 Scope The research involves the development of a process flow sheet for the efficient recovery of rutile from Ondo tar sand residue.hardness of 6.mine-engineer. To produce rutile of improved grade for titanium oxide production. It fractures unevenly. Melting point is 1825°C (www. Pre-concentration of Ondo tar sand residue for rutile recovery. iii. to determine the oxide composition. Chemical and instrumental analysis of raw and treated samples. Chemical and instrumental analysis of raw and treated samples of the tar sand residue using the XRFS.6 (on the mohs hardness scale). Pre-concentration of tar sand residue using Shaking tabling. Its crystals are prismatic. iii. i.2. Extraction of bitumen content from the tar sand and subsequent collection of the sand residue. specific gravity of 4. The objectives include the following. The scope of this work includes. to subconchoidal. i. DMS and leaching treatment.com). 1. 1.18 to 5.2 Aim and Objectives The aim of the research is to obtain rutile from Ondo tar sand residue. iv. ii. vertically striated or furrowed.

4 Justification for the Research Research on the pre-concentration of Ondo tar sand residue for the recovery of rutile has not been reported in literatures. Sieve analysis of tar sand residue. thus reducing dependence on imports and conserving our foreign exchange earnings.iv. Since the raw tar sand is readily available in commercial quantities. the successful recovery of high grade rutile from it will provide an essential input for the local paint industry. considering the vast uses and economic importance of rutile. 1. CHAPTER TWO LITERATURE REVIEW . The success of this research poses to be an economic breakthrough.

oil sands are low in hydrogen). There is also a high carbon-tohydrogen molecule count (i. sand or sandstone saturated with bitumen. Tar sands is a common term for what are more accurately called bituminous sands. tar-like substance must be upgraded with an injection of hydrogen or by the removal of some of the carbon before it can be processed. water. Tar sand . connate water and heavy oil bitumen. a dark. Because of its glue like consistency. bitumen. The diluents used for blending is less viscous and often a byproduct of natural gas. and 5% water. black. This thick. Typically. The material is a naturally occurring mixture of sand or clay. Tar sand. Tar sand products are sold in two forms: as a raw bitumen that must be blended with a diluents (becoming a bit-blend) for transport and as a synthetic crude oil (SCO) after being upgraded to constitute light crude. and extra heavy crude oil or bitumen which is found in significant amounts. 10% silt and clay. The bitumen has high density. Tar sands (also called oil sands) are mixtures of organic matter. Tar sand. sand or sandstone saturated with bitumen a dark. and asphalt like oil. Once extracted and refined. bitumen is too viscous (thick) to extract from the ground by conventional production techniques. Bitumen consists of a mixture of hydrocarbons chemical compounds containing hydrogen and carbon and small amounts of other compounds.e. e. composed mainly of mineral matter. a natural gas condensate. a “heavy oil” that cannot be recovered by ordinary petroleum production methods. and asphalt like oil. but also commonly referred to as oil sands or extra heavy oil. and water that can either be mined or extracted in-situ using thermal recovery techniques. high viscosity. Bitumen may be of variable hardness and volatility. oil sands contain about 75% inorganic matter.g.Definition of Tar Sand Tar sand is a naturally occurring hydrocarbon described as black mass of solid aggregate. 10% bitumen. The organic constituent of tar sand is bitumen. bitumen can be used as fuel and as a raw material in the chemical industry (Adegoke et al. ranging from crude oil to asphalt. quartz sand. and is largely soluble in carbon disulphide. and high metal concentration. 1980).

000 to 40. Upon separation from the mineral components of the tar sand. it is pertinent to mention that oil bearing stones have to be mined and specifically processed to recover contained minerals (Fine Tailings Fundamentals Consortium. The uncertainty centres on whether the source rocks are Mississippian (320-355 million years ago) or of Jurassic age (145-205million years ago). 1996). geologies have not yet agreed on how the oil got into the sand. 2. The first stages in the creation of the oil sands were in principle similar to the origination of conventional oil. bitumen is high viscous material with viscosity between 5. heat and pressure combined with a reservoir for the oil to accumulate. However. The age of the source rocks for the oil found in the Alberta oils sands deposits is still a matter of uncertainty. The presence of organic material. it requires chemical alteration (called upgrading) to make it fluid enough for transportation by pipeline and it makes it suitable as refinery feedstock. or perhaps a combination of the two (National Energy Board. 1995). bacterial removed most of the oxygen and . 2005). 1980). With time the remains of marine organisms formed organic material in the depressions in the pre-historic seabed. millions of years ago. on extraction. bacteria. provided the right circumstances for the creation of oil (Alberta Community Development. 2000).000 poises at 600F. However. due to its viscosity. thus its final product is termed synthetic crude oil (Adegoke et al. The tar sands deposits are the remains of marine life inhabiting an ancient ocean. On the formation of tar sand. washed by water forming dunes of all shapes and description (Shaw. which covered what today is Alberta. bitumen has many useful applications and also can be refined into valuable commodities.2 Origin of Tar Sand Most tar sand are form oil bearing sand by evaporation of more volatile components which results in great loss of fluidity. During the creation of the oil. These sands were at the shore of a sea. such as oil.is generally granular. blown by wind.

2000). The microbial action preferentially decomposed the lighter hydrocarbon molecules. leaving the more complex heavy molecules. 1995 the output of the world’s only . For similar reasons the concentration of heavy minerals such as vanadium. gold and silver also increased. heavy minerals and sulphur behind. As a result. World reserves of tar sands contain an estimated 3. Heat and pressure caused by layer upon layer of rock and silt accumulating over time. thus forming the present tar sands. The equivalent sands became primary collector of the generated oil and provided the main channel for migration. nickel. It has been estimated that prior to biodegradation. Decomposition by microscopic organism led to a reorganization of their carbon and hydrogen bonds to form hydrocarbons or oil (Wood. It is the later stages of development that differ the creation of the tar sands form that of the creation of conventional oil deposits. 1984). One of these deposits.nitrogen leaving primarily hydrogen and carbon molecules. transforming them into bitumen (National Energy Board. located near Fort McMurray along the lower Athabasca River.5 trillion barrels of bitumen. The characteristics of the bitumen and reservoir properties of the oil sands are in large part a function of the degree of biodegradation that took place.58 trillion barrels of bitumen. The world’s largest tar sand deposits are located in the province of Alberta. somewhat pressure-cooked the organic material. Tar sands represent a potentially vast supply of energy. magnetite. and then migrated long distances north into the existing sand deposits. the oil was mixed with fine particles of clay and other minerals such as various metals and sulphur. the original volume of oil in the tar sands was two to three times as large as it is today. Canada. left behind by ancient river beds. the specific gravity and sulphur content of the crude oil increased. The lighter oils that remained in the sands deposits were then subjected to biodegradation by microbes. contains an estimated 919 billion barrels of bitumen the largest known deposit of crude oil in the world. For the creation of the tar sands. The generated oil was probably sourced in the deeper portions of in pre-Cretaceous formations due to pressure from the formation of the Rocky Mountains. and contain a total of about 2.

zirconium. along with minor amounts of other minerals. The United States contains about 40 billion barrels of bitumen located in about 550 tar sand deposits. silt and clay. However. a typical composition is: . The explorers could not have predicted that this resource would be one of the largest in the world. tourmaline and pyrite. Within Asia. of the 2. and 10 billion barrels in South America. it covers approximately 46 800 square kilometres (Fine Tailing Fundamental Consortium. including titanium. With the decline of conventional oil reserves.5 trillion barrels of bitumen located in Alberta. located in Fort McMurray.2trillion barrels (88 percent) may be unrecoverable with current mining methods. 1995). 1995). amounted to one-quarter of Canada’s crude oil production.commercial bitumen plants. Tar sands are present in smaller amounts on other continents: 30 billion barrels in Asia. The Canadian oil sands deposits have been well known since the first European explorers discovered bitumen seeping nom the banks of the Athabasca River. excluding Russia. Of the estimated total. 60 billion barrels are recoverable using surface mining techniques. water and bitumen. this percentage has inevitably grown. China has about 10 billion barrels of bitumen. Tar sand deposits in Russia contain an estimated 760 billion barrels of bitumen. some 2. Most of these deposits are located in the Volga-Urals basin and in north eastern Siberia. By 1988. 2. the Athabasca oil sands were providing more than 15 percent of Canada’s oil requirement (Fine Tailings Fundamental Consortium.3 Composition of Tar Sand The tar sands deposits are composed primarily of quartz sand. this resource will prove to have increasing economic importance in Canada’s petroleum future. A significant amount of these bitumen reserves occur in consolidated (naturally cemented) sandstone in Utah. The Athabasca region represents the biggest oils sands deposit in Alberta with an estimated in-place reserve of 89 billion barrels of bitumen. Although there can be considerable variation. Consequently.

Average crude oils contain about 84 percent (by weight) carbon. In order to transport bitumen to refineries equipped to process it. each sand grain is surrounded by an envelope or film of water about 10 nanometres thick. 14 percent hydrogen. 1982). 0. The average composition of Alberta’s bitumen is 83. tar-like substance that pours extremely slowly. that is.94 percent oxygen. and a viscosity at room temperature typically greater than 50.36 percent nitrogen and 4. nickel and iron. bitumen contained in the tar sands is characterized by high densities. and the rock is said to be “waterwet”. oxygen. A key aspect of the tar sand reservoirs is the presence of bound formation water. with this inorganic portion composed 90 percent of quartz sand. which surrounds the individual sand grains as layer. high amounts of sulphur and a high ratio of carbon to hydrogen molecules. very high viscosities. high metal concentration. 0. With a density range of 1970 to 1015 kilograms per cubic meter (8-140API).2 percent carbon. • • 3 to 5 percent water. bitumen must first be blended with a diluent. 1 to 3 percent sulphur and minor amounts of nitrogen. to met pipeline specification for density and viscosity. black. with bitumen saturation varying between zero and 18 percent by weight. along with trace amounts of heavy metals such as vanadium. 10. 10 to 12 percent bitumen. commonly referred to as condensate.8 percent sulphur. In comparison to conventional crude oils.000 centipose.4 percent hydrogen. bitumen is a thick. The bitumen is trapped within the pore space of the rock itself. This is similar to most conventional oil reservoirs. The presence of the water layer around the grains enables the bitumen to be recovered more easily since the bonding forces between the bitumen and water are much weaker than those between the water and the sand grains (Takamura. metals and salts. .• 75 to 80 percent inorganic material.

Cottrell proposed a model for the microstructure of tar sands of interactions between water. Nigerian reserves are at about 40billion barrels which occur in parts of Ondo. ii. Before the commencement of commercial bitumen separation operations in 1967. It sticky and easily flows out of the soil. iii. each containing over 15billion barrels of bitumen. This reserve contains about 7000 billion tones of bitumen. with the bitumen and water making the balance. He concluded that a water film of uniform thickness surrounds the . and former Soviet Union. it was found with considerable regularity that the bitumen and water total about 12-17wt% of the rich tar sand. 1982). The target deposit is in the Athabasca area in the Province of Alberta Canada. In fact. 1972). 1980) 2. Tar sands are sand deposit impregnated with dense viscous petroleum. Reserves of tar sand.Tar sands generally are categorized into three grades: i.4 Microstructure of Tar Sands Takamura has summarized the evolution of the microstructure model of oil sands (Takamura. Mineral matter content is also found to be 78%. Romania. is rich in hydrocarbon and darker with oil content of about 12-17 wt% while the lean tar sands or low grades contain between 3-6 wt% of oil. bitumen and mineral particles. it is not all that rich in hydrocarbon. Tar sand deposits are widely distributed throughout the world often in the same geographical area as conventional petroleum (Codd. This corresponds to a tar sand mixture of roughly 83wt% sand. The rich tar sand. Albania. The outcrop The rich tar sand The lean tar sand The outcrop contains the highest oil content (about 35%). also known as the high grade. Ogun and Edo States (Adegoke et al. Venezuela. had been located in the United State.

10-15 percent of the pore space is occupied by formation water. at the contact points between the sand grains (Takamura. with the voids between the individual sand grains. Consequently.4 ppm) than the richer ores. with a thickness below 25 nm. .sand grains while clay particles are suspended within the water phase. In this concept the sand grains occupy approximately 65 percent of the total pore volume. while the remainder is occupied by bitumen. 1982). Cottrell’s earlier hypothesis suggested that the clay minerals are suspended in the water layer. Takamura has developed a more refined structural model takes other factors into consideration. the proposed models are only applicable to highgrade tar sands. the water film is surrounded by a bitumen layer. Moreover. Low-grade oil sands contain more fines (4. In this updated model. It was shown that water exists as pendulum rings. While the clay particles adhere directly to the sand grain surfaces. all the sand grains are in direct contact with one another. In high grade tar sands. These fine particles exist between the coarse sand particles as clusters saturated with water. Also. an increase in fines content results in increase in this so-called formation water. These updated models assume that the thickness of the water film is uniform.

the first attempt at commercial exploitation was by the defunct Nigeria Bitumen Corporation. The basin was formed during the early cretaceous by extensive block fauthing of basement complex during the geological events which led to the opening of the Atlantic Ocean. In Nigeria.Figure 2. According to Adegoke et al (1980). between 1908 and 1914. The Ondo State tar sands occur in the eastern margin of the Dahomey basin. This extends from the Ghana-Ivory Coast boundary.1: Microstructure of Tar Sand 2. The Nigerian tar sands can be . the crude has migrated up-deep into near surface losing. coastal sedimentary basin. Ogun and Edo States. through Togo and Benin Republic to Western Nigeria. in the process.5 Nigerian Tar Sands Nigerian tar sand deposit is known to occur in part of Ondo. its volatile component thus forming the highly viscous bitumen.

i. and low grade called the lean tar sand. iv. The over burdened thickness of the deposit is general considered shallow. ii. However. the average thickness of pay is estimate at about 20m (65. has been postulated for the Nigerian deposit only because it is similarly amenable to the hot water process. ranging from about 0. Higher Sand Porosity Low Content Clay and Fines Less Lean Tar Sand Higher Bitumen No External Stress Absence of Basal Aquifer Less Basal-Gas Less Sulphur and Heavy Metal vii.5m to 13m with an average of 6m. the outcrop. the Nigeria variety exhibits the following characteristics. the high grade called the rich tar sand. vi.categorized. the Niger tar sands have some potential for easy development namely: i. viii. the Nigerian rich tar sands deposits constitute a potential reserve of over 78million barrels of bitumen. similar to that of Athabasca.6ft) with a mean hydrocarbon content of about 112. with limited modifications. 1923). v. into three grades. according to Wood (1984). iii. Based on an average bitumen content of 15% by weight. Compared to the Athabasca tar sands. Amenability to gravity drainage . it is pertinent to mention that the water wet structure. As a result of these characteristics and advantages. The tar sand reserves have been conservatively estimated to be more than 40billion barrels (Clark. Bitumen reserve in the south-western area of Nigeria is tentatively estimated at about 15billion barrels.miles). The total area of possible bitumen coverage is estimated at about 189 sq.km (73 sq. The similarities in the Athabasca and Nigeria tar (oil) sands imply that process technology applied in the former can be adopted for the later.

as well as steam injection because of the good reservoir properties while the surface and near-surface occurrences would be won by open cast mining. iii. 1984). more of Nigeria tar sand can be recovered by surface mining. The differences between the Nigeria tar sand and the Athabasca tar sand includes: i. which is a more expensive process. . ii. whereas only about 3% of the Athabasca tar sand can be obtained by surface mining with the rest recoverable by insitu process. The Nigeria tar sand deposit had very low clay content ranging from 2%-7% with an average of 5%.ii. Potential for steam assistance (SAG-D) Amenable to open-pit mining It could be concluded that the Okitipupa tar sand. The Ondo State bitumen deposit. The over-burdened Nigeria tar sand is smaller compared to that of Athabasca i. when encountered in the sub-surface would be amenable to gravity drainage. was found to be better in road surfacing than its Athabasca equivalent (Wood. This low clay content is a great advantage since it means that there could be less environmental problem to cope with during oil extraction than has been the case with Alberta.e. iii. tested by a German construction company Longed Rhugas (L/R) process in 1972.

600 42.000 ND 41.3 19.900 42.1: Comparative Analysis of Tar Sand Samples Collected in Ondo State. Sample Ramsbottom Carbon % weight Asphaltene % weight 23.TABLE 2.300 42.200 18.3 10.700 Nigeria A Nigeria B Nigeria C Nigeria D Nigeria 56.8 12.4 10.2 21.30 Athabasca 10.1 32.300 42.200 18. Nigeria.1 .2 Heat of combustion BTU/BL 18.0 18.300 ND 17.2 9.300 18.7 7.2 23.

mica flakes and clays (Shaw et al. It has long been known that the tar sand tailings greatly concentrate these minerals. Generally.2. It is clear that Tar sands deposits are diverse and contain varying amounts and sizes of mineral components in ores from the various zones. sometimes referred to as connate water. the predominant mineral is quartz.6 Mineral and Metal Content of Tar Sand Tar sands are frequently characterized by their mineralogy. 1996). They heavy metals concentration in the tar sands samples is consistent with concentration. Minerals in several Tar sands tailing (clay fraction) are very similar with little variation in composition (Ignasiak et al.08wt %). The tar sands also have varying porosity. about 70wt% of the Ti02 and 63wt% of the Zr02 are concentrated in the sand fraction. The Nigeria tar sand samples contains the varying amounts of Ti02 (0..008 wt% zircon. ranging from 25 to 35 percent. Ironbearing minerals are known to occur in the tar sand Ells (1926) made comments on this occurrence. However other minerals are also contained in tar sands. titanium. with small amounts of feldspar. the bitumen of such water wet tar sands is not in direct physical contact with the mineral particles but rather forms a relatively thin film which surrounds the water envelope around the mineral particles. Generally. nickel and zircon. The bitumen-free mineral sand deposit also contains only 0. present as grains. In addition. vanadium. such as by the liquid medium which is contact with the mineral particles of the tar sand. The clays consist of kaolinite illite and chlorite in different ratios. tar sands are frequently characterized by their richness or the amount of bitumen they contain and the quality thereof. Siderite is considered indicative of littoral shallow-water strata containing abundant . The water wet tar sands such as the tar sand deposits generally found in the Ondo State deposit of Nigeria comprise mineral particles surrounded by an envelope of water. On average.4wt %) and Zr02 (0.06 wt% Ti02 and 0. The Nigeria Tar sands has been known to have striking similarities with the Canadian tar sand which has been confirmed to have the following valuable heavy minerals such as titanium-bearing minerals. 1983).

Twelve elements: K. . 1455oC.organic material. impregnated by extremely viscous oil. and chromium fall into the category of refractory metal – metals with high melting temperature. and P were detected and their concentrations. white quartz and formation about 50 – 80m thick with a net thickness of about 20m saturated with tar. and correlation determined. The Athabasca oil sands consist of uncemented quartz sand. enrichment factors. It is a clearly washed. Elements such as vanadium. sulphur is stored or shipped to market while the nitrogen as ammonia and the fuel gas produced as a by-product are used as energy source throughout the plant. Very high enrichment factors were obtained for Cu. They also occur in coarse-grained at tar sands in the lower part of the tar sand formation. As. Zn. The investigation studies focus on the distribution and composition of minerals. Seventy-six per cent of the variation in the oil content of these sediments is related to the median diameter and to the percentage of clay-size material (less than 2 microns). 1910oC. Their melting temperature is as listed in order of listing above: 1668oC. V. with minor amounts of smectite which appears to be inter-layered. kaolinite and illite are dominant through much of the sequence. titanium. Ti. and clay. and 1907oC respectively. Mn. silt. The Athabasca sand which has been reported to be similar to Nigeria tar sand is a Precambrian formation on Lake Athabasca. and As. Ca. nickel. There is abundance of siderite-cemented beds in the upper part of the tar sand formation and in the basal sands. “Total reflection Xray fluorescence (TXRF) analytical technique was used to determine the elemental composition of south western Nigeria oil sand. Cu. Cr. Fe. The relative abundance of these varies little thought most of the core. Ni. The tar sand minerals are identified in groups. In the Athabasca tar sands the major clay mineral contributor with this structural characteristics is kaolinite. Zn.

it is often found on fluorite. The effect can be observed only in darkness.g. Some minerals emit a bright. apatite. zeolites are not scratched by steel. You may observe the following phenomena: a. The lattice defects are always due to radioactive radiation which had hit the crystal since its formation. classical wet analysis plays an important role in many other analytical applications including identification and analysis of valuable minerals and metals in tar sand. Such boiling melt points to minerals of the zeolite group. zircon. . and diamond in specimens from different outcrops. often coloured light when heated below redness.2. Only materials with a low melting point fuse in the closed tube. In addition to more conventional titration analysis.7 Identification and Analysis of tar and sand valuable mineral and metal content The classical wet analysis was developed and widely used in the 19th century. The method usually relies on chemical reactions between the material being used. It is caused by the healing of lattice defects on heating. c. also termed wet chemical analysis. Minerals containing liquid inclusions may snap and explode owing to the evolution of steam during heating. Classical wet analysis may be used to “empire” a traditional instrumental approach for accuracy. e. no wet separation process is employed (Wood. Change in the condition or appearance of the assay The formation of gases which collect in the tube The formation of sublimates or condensed liquids on the cold walls of the tube. milky quartz. 1984). They can be distinguished by their hardness. calcite. (T >> 300oC). quartz. The tar sand residue is used directly. This phenomenon is called ‘Decrepitation’. consists of those analytical techniques that use no mechanical or electronic instruments other than a balance. Sometimes they break up into very fine powder or dust. This effect is called thermo luminescence. b. Classical analysis. or to crystal hydrates.

XRF is for the most part capable of yielding satisfactory results when carried out by highly trained personnel. This rearrangement of electrons is associated with the emission of X-rays characteristic (in terms of energy) or the given atom. – But minerals may also change colour after heating. X-ray Fluorescence (DRT) spectroscopy is a non destructive qualitative and quantitative analytical used to determine the chemical composition of samples. During interaction with samples. especially zircons. According to the present invention there is provided a method for determining the mineral and metal composition of a sample from x-ray data obtained by subjecting a pellet of the tar sand sample to x-ray energy in an X-ray fluorescence spectrometer. The collected data gives precision and data of known minerals to determine the mineral and metal composition of the sample.Sometimes the colour of mineral changes due to the healing of lattice defects on moderate heating. This reaction occurs only at higher temperatures (e. owing to decomposition. Energy dispersive x-ray emitted to determine the chemical composition for many type of material. it will etch the glass. This process is referred to as emission of fluorescent X-rays (fluorescent yield). This phenomenon originates when incident radiation knocks out an electron from the innermost shell of an atom creating a vacancy. primary X-rays emitted from a sealed radioisotope source are utilized to irradiate samples. The atom is excited and releases its surplus energy almost instantly by filling the vacancy with an electron from one of the higher energy shells. source X-rays may either undergo scattering (dominating process) or absorption by sample atoms in a process known as the photoelectric effect (absorption coefficient).g. The overall efficiency of the fluorescence process is . topaz) The present technique used in the industry is X-ray fluorescence analysis or “XRF”. Sometimes minerals containing fluorine as well as OH-groups cause hydrofluoric acid HF to form. In a source excited DRF analysis. Such bleaching is a common procedure used in treating raw gemstones. The atoms in the samples are excited by x-ray emitted from XRF-tube or radioisotope. gives an acid reaction to pH-paper and has a pungent odour. mostly from dark colours to lighter ones.

Norway. Rutile occurs as an accessory in many rock types. 2.referred to as excitation efficiency and is proportional to the product of the absorption coefficient and the fluorescent yield. It has a hardness of 6.18 to 5. occurring in gneiss. but not black. It can have some iron present.com).mine-engineer. • • It can be sued for a wide range of elements. As a secondary mineral. hematite and feldspar. Melting point is 1825°C (www. a metallic luster and a pale brown streak. chiefly in Switzerland. schist. ilmenite. from sodium to uranium. specific gravity of 4. granite.2. ranging from plutonic to metamorphic rocks. It is also associated with quartz. limestone and dolomite. Its crystals are prismatic. in Brazil it often occurs as inclusions in clear quartz crystals (rutilated quartz). Rutile is typically about 60% titanium and 40% oxygen.8 Rutile Rutile is a major mineral source of the element titanium. along with the other titanium mineral. Large crystals have been found in some granite pegmatites. and even as a detrital material in sediments and placers because of its resistance to weathering. It fractures unevenly. Rutile is commonly . Rutile is one of the most common titanium minerals.6 (on the mohs hardness scale). sometimes up to 10%. Brazil. Rutile is brownish red and other shades. The features and uses include: • Most accurate. mica. to subconchoidal. most economic and simple analytical methods for determination of the chemical composition of many type of material. vertically striated or furrowed. it is common in beach sand deposits. Detection limits at the sub-ppm level and can measure concentration up to 100% easily and simultaneously. Rutile is found in igneous and metamorphic rocks. and parts of the United States.

org).mine-engineer. increasing to approx. In groups of acicular crystals it is frequently seen penetrating quartz as in the "fléches d'amour" from Grisons. The reserves.wikipedia. In 2005 the Republic of Sierra Leone in West Africa had a production capacity of 23% of the world's annual rutile supply. . it is marketed as an ore of titanium. are estimated at 259 million tons. Venezuela. Rutile can also be extracted from tar sand deposits. Slow development has been attributed to technical problems associated with production and processing and in other cases. Although exceedingly rich in oil. valuable minerals and metals in varying proportions.2: Raw rutile sample (Source: www.com) Figure 2. often referred to as bituminous sand or oil sand occurs in various parts of the world including Canada.com) Rutile is mined in Norway and is widespread in the Alps. (www.. Russia. Mexico.en. According to Oladapo (2008) tar sand deposits. inaccessibility of the deposit.S. United states and Nigeria to mention but a few. development of such deposits has been slow. and elsewhere. the southern U.com. lasting for about 19 years.associated with apatite in high-temperature veins.mineral.galleries. In sufficient quantities. (www. Switzerland. 30% in 2008. Madagascar.answers.

non-corrosive metal are aerospace. Venezuela. Reserves of tar sand. titanium.Tar sand deposits are widely distributed throughout the world often in the same geographical area as conventional petroleum (Codd. flux coatings and finally as mineral specimens and gemstones on the precious stone market. The titanium dioxide pigment is extracted directly from rutile. It replaced lead as the most common paint pigment used in the manufacture of paint. It has been long known that the tar sand tailings greatly concentrate these minerals. vanadium. This is done by calcining a mixture of rutile. nickel and zircon. about 70 wt% of the TiO2 and 16 wt% of the ZrO2 are concentrated in the sand fraction. sports. 1983). This reserve contains about 700 billion tones of bitumen. 1972). and medicine.008 wt % Zircon.06 wt % TiO2 and 0. the production of titanium metal.08wt %). The bitumen-free mineral sand deposit also contains only 0. and the former Soviet Union. The Nigeria tar sand has been known to have striking similarities with the Canadian tar sand which has been confirmed to have the allowing valuable heavy minerals such as titanium-bearing minerals. Ogun and Edo states (Adegoke et al. high strength. automobiles. had been located in the United States. which contains 92 – 96 % TiO2. its main use is in paint as a paint pigment. both to preserve fruits and vegetables and to remove pollution. each containing over 15billion barrels of bitumen. Still. The target deposit is in the Athabasca area in the province of Alberta. 1980). Canada. and it is used to treat the air. Nigeria reserves are at about 40 billion barrels which occur in parts of Ondo. The most important of these by far is for the production of titanium dioxide white pigment. Major uses of this lightweight. Minerals in several tar sand tailings are very similar with little variation in composition (Ignasiak et al. Other uses include a coating for tiles. The Nigeria tar sand samples contains varying amount of TiO2 (0. rutile is used for four main purposes. Today. . On the average. coke and chlorine to form gaseous titanium tetrachloride (TiCl4).4 wt %) and ZrO2 (0. These include the production of titanium dioxide pigment. Romania.

. This process is known as the Chloride process. Today. it improves their welding qualities and corrosion resistance. as when combined with carbon. or as a lightweight metal for aircraft and spacecraft components. fabric.S. The metal became valued for its high strength.g. During the 1950’s titanium began to come into use as a structural material. of which the most commercially important is rutile. toothpaste. sun cream) due to its ability to reflect ultra violet light (Andrew. and even some foods (e. These days titanium dioxide white pigment is used in paints and plastics. It is then reheated to a gas and mixed with hot oxygen to form very fine crystalline rutile (raw white pigment). light weight and corrosion resistance and thus its use increased rapidly.TiO2(s) [impure] + C(s) + 2Cl2(g) TiCl4 (g) + CO2(g) The titanium tetrachloride is then condensed to a liquid and the impurities separated as solids.g. ceramics (e. titanium metal is used to form surgical pieces such as heart pacemakers. turmeric). stimulated initially by aircraft applications.g. which involves chlorinating rutile to titanium tetrachloride (as in the pigment process) and then reducing it to a titanium sponge using molten magnesium. Titanium is produced by the Kroll process.A) and Ti-oxide (in Britain). It is also used in sun screening products (e. TiCl4(g) + O2 (g) TiO2(s) + 2Cl2(g) The displaced chlorine gas can be recycled and thus is a catalyst. About 92 % of the world’s titanium minerals are used to make titanium dioxide pigment and the three largest manufactures of it are Du Pont (in France). rubber. cosmetics. Millennium (in the U. soap. in the manufacture of stainless and heat-resistant steels. porcelain). high quality paper. artificial limbs and joints. false teeth. 2001). It is also used as an alloying metal. Titanium is the fourth most abundant metallic element in the earth’s crust and occurs primarily as an oxide ore.

i. n(SiO2) – n(TiO2) lie in a stable state. Only 3 % of the world’s titanium minerals are used to make titanium metal (Andrew. 2001) Improved electric welding rods are produced by the use of coatings containing rutile. This is because at high temperatures and pressures. or the sink and float process. the rejection of gangue prior to grinding or final liberation. the golden needles of rutile. Rutilated quartz is formed when rutile and quartz crystals are cooled together from high temperatures. sapphire and other gemstones. tourmaline.e. Here. As the temperature cools and the pressure eases. Heavy liquids of suitable . each arrangement being individual. 2. These inclusions can produce effects such as cats’ eyes and asterisms (stars). In principle it is the simplest of all gravity processes and has long been a standard laboratory method for separating minerals of different specific gravity. is applied to the pre-concentration of minerals. One of the most common types of stone produced by inclusions of golden rutile is called rutilated quartz.TiO2(s) [impure] + C(s) + 2Cl2(g) TiCl4(g) + 2Mg(l) TiCl4(g) + CO2(g) Ti(s) + 2MgCl2(g) Finally.9 Dense Media Separation (DMS) The Dense Medium Separation also known as the heavy medium separation (HMS). a semi-precious stone. This is due to the fact that it stabilizes the electronic arc and reduces the viscosity of the slag formed during welding. ruby. the sponge is consolidated into ingots in an electric furnace. are arranged in clear quartz in what are sometimes breathtaking patterns. Rutile is of major importance to the gemstone market in the form of microscopic inclusions in quartz. the two separate with rutile crystals being trapped inside the quartz. called Venus hairs.

1994) . while those denser than it sink. liquids covering a range of densities in incremental steps are prepared and the representative sample of crushed tar sand is introduced into the liquid of highest density. until all the densities are exhausted. (1) Also.density are used. (2) Substituting for Vm in (2) Dm (V0 + V1) = D0V0 + D1V1 The formula takes the form.9. then placed in the next liquid of lower density. DmVm = D0V0 + D1V1 …………………. In this method. whose float product is then transferred to the next liquid of lower density. Given. The float products from the liquid of highest density are removed and washed. Tottle. evaluating the performance of an existing plant (Yaro et al..1 Derivation of equation to obtain the required Density from the mixture of two liquids. 2. Dm = D0V0 + D1V1 V0 + V1 Where Dm – density of the mixture D0 – density of liquid 1 D1 – density of liquid 2 V0 – volume of liquid 1 V1 – volume of liquid 2 (C. Usually the results of the heavy liquid tests are used in producing theoretical washability. 2003). Vm = V0 + V1 …………………………. so that those minerals lighter than the liquid float..R.

2 3.4– 4.3: Specific gravity of some heavy liquids Liquid Bromoform Choloroform Tetrabromoethane Carbontetrachloride Di-iodomethane Specific Gravity 2.0 4.34 4.51 2.7 Table 2.65 3.2: Specific gravity of some Oxides Oxide SiO2 (Silica) Al2O3 (Alumina) Fe2O3 (Haematite) TiO2 (Rutile) MgO (Calcined Magnesite) Fe3O4 (Magnetite) Na2O (Di-Sodium oxide) K2O (Potassium oxide) CaO (Lime) MnO (Manganese II oxide) Specific Gravity 2.9 – 4.0 – 6.65 5.58 3.96 1.48 2.30 3.30 .89 1.Table 2.5 2.5 – 6.1 5.

denser particles riding highest towards the concentrate launder at the far end. this mechanism is utilized in the shaking-table concentrator which is perhaps the most metallurgically efficient form of gravity concentrator being used to treat the smaller. is introduced at the feed box and is distributed along.. the smaller. which causes the mineral particles to “crawl” along the deck parallel to the direction of motion. The shaking table consists of a slightly inclined deck. wash water is distributed along the balance of the balance of the feed side from the launder. While the larger lighter particles are washed into the tailings launder.11 Leaching Treatment This is a method for upgrading a concentrate of tar sands bitumen containing fine mineral matter and optionally coarse mineral matter in which solvent-diluted bitumen is contacted for a short time in a riser with hot attrition-resistant substantially catalytically inert acid-resistant fluidizable particles. due to the flowing film of water. a flowing film of water effectively separates coarse light particles from small dense particles. most . a high-grade concentrate and a middling fraction. The net effect is that the particles move diagonally across the deck from the feed end. force due to the table motion and that. The table is then vibrated longitudinally by the mechanism. and to produce finished concentrates from the products of other forms of gravity system. on to which feed. which are. The minerals are thus subjected to two forces. at right angles to it. 2. at about 25% solids by weight. causing a selective vaporization of the lighter high hydrogen content components of the bitumen. and since the effect of the flowing film depends on the size and density of the particles. which runs along the length of the table. An adjustable splitter at the concentrate is often used to separate the product into two fractions. more difficult flow streams. using a slow forward stroke and a rapid return. The preferred particles are composed of silica-alumina.10 Shaking Tabling In this method. they will fan out on the table.2.

Reagan (op. The metals may be separated from the leachate and purified in separate processing steps and can be sold as by-products. The leachate to be used is ammonium nitrate at temperatures in excess of about 88° C. so most processes capable of reducing CaO and TiO2 to the desired levels will also reduce iron to levels below about 1.5%. is contacted with a solution of acid to remove the deposit of mineral matter and deposited metals without decomposing the particles of contact material. The contact material. The heated particles of contact material are reintroduced into the riser for further contact with incoming diluted bitumen charge (Reagan and Bartholic. . with deposit. Fine mineral matter in the bitumen feed also deposits on the fluidized particles instead of being carried over with the vaporized hydrocarbon product. CaO and TiO2 contents of up to about 3% can be tolerated. 1989) A variety of acid leach procedures may be used to remove the ashes deposited mineral matter from the withdrawn contact material samples.preferably a mixture of mullite and crystalline silica or mullite. A portion of the heavier asphaltenes and most of the components which contain metals. crystalline silica and an acidresistant form of alumina. which is usually satisfactory. The presently preferred process uses a high temperature mineral acid leach to remove deposited mineral matter and metals from the substrate material followed by filtration to separate the metalscontaining solution from the contact material. Typically.cit) further explained that ‘the preferred acid leach procedures’ will remove at least about 40% by weight of the calcium oxide present of the surface of the materials. Iron oxide is easily removed. sulfur and nitrogen remain on the attrition-resistant fluidizable particles.

i. They were then placed on a large placed on a large plastic sheet on a laboratory bench and thoroughly mixed using the coning and quartering method. Thermometer . Equipment / Facilities used include: The following equipment will be required for the work. which is not noticeably associated with the sand.CHAPTER THREE MATERIALS AND METHODS 3. After sampling in the field. The naturally occurring tar sand of Ondo State deposit was found to occur in two forms on site. the tar sand was placed in large plastic bags. Bitumen seepage from well (plain bitumen). A large deposit of tar sand is found occurring in this region. and it occurs as a semi-solid substance which is very black in colour. Magnetic stirring hot plate iii. The sample was collected in from a well located in Gbelejulooda village in Irele Local Government area of Ondo State. The choice of this location was guided by the availability of plain bitumen in the zone coupled with the accessibility. Nigeria.1 Materials The basic raw material used in this work was lumps of Bituminous Tar sand obtained from Ondo State. Oven ii. 2. namely: 1. Seepage and outcrops of bitumen impregnated sands (tar sands) from which bitumen and the sand residue can be extracted by suitable processes.

The reagent used for optimal recovery of bitumen and tar sand residue is Sodium hydroxide (wetting agent). Benzene. Nitric acid iii Ammonium nitrate iv. Hammer ix. Hydrochloric acid v. XRFS – machine v. Glass beakers vii. Chloroform ii. Chemicals used include: i. Stirrer. Chisel x. Vibrating screen vii. Distilled water vi. Electric Cooker xii.iv. Steam bath xi. Electronic weighing balance vi. All the materials and equipment were available at the Department of Materials .

which came in lumps of black mass. Ile –Ife and the Centre for Energy research Development (CERD) OAU.1 Sample Preparation The tar-rich sand.Science and Engineering. Smaller sizes less than 9. The tar-rich sand was then dried in an oven at a temperature of about 110˚C. was properly homogenized in a mortar by means of pounding with an iron rod. Obafemi Awolowo University. Screening was conducted for both dry and wet samples which served as a process of classification. Still smaller sizes were obtained by crushing and grinding. . The classified sample was weighed on the electronic balance. The resulting mass gave a properly blended mixture and a finer surface.2 Methods 3. and the samples were weighed on a sensitive electronic balance. 3. Both the oversized and undersized among the crushed samples were screened with various meshes using the vibrating screen. The prepared tar sand sample was then placed in a 600 ml beaker for the hot water extraction.2.4 mm (3/8 inch) where obtained by crushing the lumps with the use of hammer and chisel with a little addition of water.

after which a finer and cleaner sand residue was obtained. The addition of the Sodium hydroxide aids the optimal recovery of bitumen and tar sand residue. A beaker was filled with distilled water and heated to a temperature of about 75˚C. the temperature was measured with the aid of a Thermometer.2. Pellets of Sodium hydroxide were fed into the beaker to obtain an aqueous solution.2 Hot water extraction (Bitumen and Sand Residue separation) The basic method commonly used for tar sand analysis is the hot water extraction process to determine the bitumen. water and sand content. The sand residue was then poured into a container and allowed to dry at room temperature. Sodium hydroxide which acts as a wetting agent was added to maintain a pH of around 8. The hot water extraction process for primary extraction of bitumen from tar sands is used to clean up the bitumen for further processing.2. The stirrer agitates the mixture. but diluted bitumen. which has a combined heating and stirring effect. Water and mineral with any unrecovered bitumen removed from the froth constitute an additional tailing stream. The stream of middlings was carefully scavenged for recovery of incremental amounts of bitumen. The remaining mixture is decanted to fully separate the softened lumps of tar sand (bitumen and sand) from the tar sand residue. The resulting residue still contained tiny lumps of bitumen which was dissolved using benzene. A lump of the tar sand was weighed and placed in the mixture which was heated on the magnetic stirring hot plate.3. . after which it was further dried on the electric cooker at a temperature of about 90-95˚C. and the combined effect of hot water and agitation releases bitumen from the tar sand and causes tiny air bubbles to get attached to the bitumen droplets that float to the top of the plastic container where the bitumen is skimmed off. The hot water extraction yielded an oily product of essentially pure.

30mins and 45mins. that that float to the top of the beaker where bitumen was skimmed off. 2g of tar sand was placed in a 250ml beaker.3.2. 1g of tar sand and 25ml of distilled water in the beaker with varying extraction time. Benzene and toluene were used to dissolve some traces of bitumen in the tailings and it was later filtered. 3.3 Determination of most potent reagent The basic method commonly used for tar sand analysis was the hot water extraction process to determine the bitumen. 1g of tar sand was placed in a 250ml beaker.1g of leaching reagents. sodium hydroxide and hot water was done.4 Determination of optimal leaching time The time efficiency was carried out using 0. The remaining softened lump of tar sand in the mixture (consisting of sand and bitumen) was removed into a beaker and weighed. 15mins. The determination of most potent reagent was carried out for both sodium hydroxide and sodium carbonate. Different contact time was used for leaching starting from 5mins. sodium hydroxide and hot water was done. 25ml of distilled water was added to it with 0. The solution was allowed to cool. Continuous heating of the mixture of the tar sand. The solution was allowed to cool.1g of leaching reagent. 10mins.2. A magnetic stirrer hotplate was used which agitate the reagent and the tar sand simultaneously. The combined effect of hot water and agitation releases bitumen from tar sand and causes tiny air bubbles to get attached to the bitumen droplets. and tar sand residue was obtained. 25ml of distilled water was added to it with 0. settle and . The remaining softened lump of tar sand in the mixture (consisting of sand and bitumen) was removed into a beaker and weighed. Continuous heating of the mixture of the tar sand.1g of Na0H. The combined effect of hot water and agitation releases bitumen from tar sand and causes tiny air bubbles to get attached to the bitumen droplets. water and sand content. A Stuart scientific magnetic stirrer hotplate was used which agitate the reagent and the tar sand simultaneously. that that float to the top of the beaker where bitumen was skimmed off. settle and decantation process was used to separate the tailings.

The retained particles in each of the sieves were then weighed separately.decantation process was used to separate the tailings. The combined effect of hot water and agitation releases bitumen from tar sand and causes tiny air bubbles to get attached to the bitumen droplets.1g of tar sand was placed in a 250ml beaker. 25ml of distilled water was added to it with a contact time of 15mins and varied leaching reagent.2. sodium hydroxide and hot water was done. . and the sand residue was obtained.6 Sieve Analysis Ondo Tar sand Residue Sieve analysis was carried out on the tar sand residue to obtain finer particles of sizes less than 150 µm. 125 µm.5 Determination of optimal reagent concentration The optimal reagent concentration was carried out using hot water extraction method. The sizes of sieves used are 150 µm. settle and decantation process was used to separate the tailings. Continuous heating of the mixture of the tar sand. The remaining softened lump of tar sand in the mixture (consisting of sand and bitumen) was removed into a beaker and weighed. that that float to the top of the beaker where bitumen was skimmed off. and the residue was sand recovery. 106 µm and 63 µm. 3. Benzene and toluene was used to dissolve some traces of bitumen in the tailings and it was later filtered. 3. Benzene and toluene was used to dissolve some traces of bitumen in the tailings and it was later filtered.2. A Stuart scientific magnetic stirrer hotplate was used which agitate the reagent and the tar sand simultaneously. The electrically operated sieve shaker was used to conduct the analysis for 30 mins. The solution was allowed to cool.

1: Sieve Shaker.Figure 3. 3.7 Determination of the mineral content of Ondo Tar sand residue .2.

rays at characteristic energies when bombarded by a high energy X-ray source. In as source-excited analysis. which emit X. Inductively Coupled Plasma Spectroscopy (ICPS) and Neutron Activation Analysis (NAA). This spectroscopic technique is carried out on metallic elements (such as the sample to be obtained). fast and cost effective. Furthermore. The technique to be used is the X-ray fluorescence spectroscopy (XRFS) in an attempt to determine the oxide composition of the tar sand residue as well as the quantity. XRF has the advantage of being non destructive. This comprises of the qualitative analysis which will be used to identify the substances in the sample and a quantitative analysis which is an attempt to determine the quantity or concentration of a specific substance in the sample. The XRF spectroscopy is widely used for the qualitative and quantitative elemental analysis of the bituminous rich tar sand. source X-rays may either undergo scattering (dominating process) or absorption by sample atoms in a process known as the photo electric effect (absorption coefficient). it provides a fairly uniform detection limit across large portion of the periodic table and is applicable to a wide range of concentrations. The XRF was used to determine the chemical composition of the sample.Chemical Analysis involves body of procedures and techniques used to identify and quantify the chemical composition of a sample of a substance. . The composition of the rich tar sand was displayed on the monitor in the form of a graph illustrating different minerals present with their amount and proportions. such as Atomic Absorption Spectroscopy (AAS). During the interaction with samples. primary X-rays emitted from a sealed radioisotope source were utilized to irradiate samples. Compared to other techniques. from a 100% to few parts per million (ppm) and percentage weight. multi-elemental.

2: Simplified Diagram of Hot Water Recovery Process (Merchant and Westhoff. 1985) .Figure 3.

40 31.7 Table 4. Table 4.3 98.60 Overall Recovery (%) 60.0 60.4 84.70 Weight of Sand Tailings (%) 27.80 40.10 41.40 Overall Recovery (%) 66.08 Weight of bitumen Recovered (%) 26.60 Table 4.1g NaOH) Leach Contact Time (mins) 5 10 15 30 45 Bitumen Recovery (%) 52.20 47.00 34.60 44.20 68.60 .1 Results The results of the analysis are presented in the following tables. 0.3: Determination of Leaching Efficiency Using Sodium Hydroxide NaOH (g) 0.1: Determination of Suitable Leaching Reagent (Using 2g Tar sand) Leaching reagent Sodium Carbonate Sodium Hydroxide Contact time (mins) 15 15 Bitumen recovery (%) 20.20 40.15 88.4 72.CHAPTER FOUR RESULTS AND DISCUSSION 4.30 Sand Tailings (%) 13.30 31.60 21.90 50.20 31.95 48.2: Determination of Contact Time for Highest Recovery (1g Tar sand.00 Sand Tailings (%) 39.06 0.20 Overall Recovery (%) 53.

....20 ..3 Contact time (mins) 30 .1 Table 4..2 Weight of Sand Residue (g) 3.4....40 47.60 49...10 98.4 Analysis of Bitumen and Sand Residue Recovery from Tar Sand using the Hot Water Extraction Process (Bulk Extraction) Weight of Tar Sand (g) 10 Weight of Bitumen Recovered (g) 4.80 50.12 0..20 97.0.10 0...14 50..40 97..10 47...80 47...

22 Table 4.86 10.20 30 50 70 8.5 20. @30mins) Size of Sieve (µm) 150 125 106 63 <<63 Weight of Sand Residue Retained (g) 11.50 11.8 1.6: Mineralogical Composition of Ondo Tar Rich Sand residue Mineral Composition Weight (%) .5 Sieve Analysis of Tar Sand Residue (30g.3 6.5 7.6 2.52 5.5 22.5 15 21.5 40 45 50 50 Table 4.

0.5 2 0.1 .3 – 0.0.43 0.05 .01 0.1: A graph of recovery of bitumen and sand tailings against contact time .02 0.Zircon (Zirconium silicate) Ilmentite Rutile Mica Siderite Magnetite Kaolinite Quartz Silimanite 0.1 0.9 0.01 4 Fig 4.

2: A graph showing the weight of sodium hydroxide against sand tailings. Fig 4.Fig 4.3: A graph showing the weight of Bitumen and Sand residue recovery .

However.2. as shown in Table 4.1 Recovery of Heavy Bitumen and Sand Residue from Tar Sand The process used in separating the bituminous content of the tar sand from the sand residue was effective in obtaining a good grade of both bitumen and tar sand. The results of the hot water extraction process can be used to analyse the varying weights of tar sand samples treated. and chemical reactions leading to the separation of bitumen from the sand tailings.4. the effect of which increases the probability of collision and adhesion of the particles. mass and heat transfer. it can be observed that the recovery of bitumen decreased on extracting larger samples of the tar sand. From the table. there is an increase in the recovery of sand residue when .2 Discussion of Results 4. The process also involves agitation of the reacting particles. The hot water extraction is a process which objective is to effectively separate bitumen from mineral particles which are heavily present in the tar sand residue. The process involves mixing.4.

15% respectively. it can be seen that the 15mins contact time yielded the second highest bitumen recovery of 50.2 Effect of Sodium Hydroxide in Recovery of Bitumen and Sand Residue Tar sand samples were leached with sodium hydroxide and sodium carbonate in separate experiments. The overall recoveries of sodium hydroxide and sodium carbonate are 88. The leaching of the tar sand with sodium hydroxide produced bitumen recovery of 48.45% greater than that of sodium carbonate. while the highest recovery of tailings was at 15mins contact.00% and 40.95% bitumen and 39. while the overall recovery with sodium hydroxide is 28.20% sand residue. From these results. These results show that leaching with sodium hydroxide yielded higher bitumen and sand tailings recoveries. 4. The low recovery of 13.00% sand residue.05%. it can be deduced that sodium hydroxide reacts more actively with tar sand to liberate the bitumen from the sand admixture with more sand residue obtained.40%) occurred with 5mins leach time.40% for bitumen and sand residue was obtained at 15mins leach contact time.1. while that of sodium carbonate produced 20. The determination of bitumen and sand residue recovery by the leach contact time is presented in table 4. The results of the treatment are presented in table 4.60% and 60. The overall recovery of 98. The recovery of bitumen with sodium hydroxide exceeds that of sodium carbonate by 27. .2.2.treating larger samples in the solution of sodium hydroxide.60% with the highest sand tailings recovery of 47. and it is normally used to optimize bitumen recovery.60% for sand tailings at 5mins contact time may be due to high tailing loss during sedimentation and decantation coupled with a poor liberation from the bituminous tar sand. The role of NaOH is to produce natural surfactants from the bitumen. From these results. The 15mins contact time may thus be preferable as it not only indicates pure bitumen but also produces a large amount of sand tailings from which a useful mineral like TiO2 can be recovered.80%. The optimal recovery of tar sand residue is obtained when 70g of tar sand is used. The results shows that the highest recovery of bitumen (52.

CHAPTER FIVE CONCLUSION AND RECOMMENDATIONS 5. and Magnetite. The Ondo tar sand exhibits the following characteristics. Addition of NaOH below the optimum required for extraction decreases the effectiveness of the froth. The recoverable valuable minerals from the tar sand residue are in minute quantities. From table 4. The . and the sand residue can be further processed to recover valuable minerals like Rutile. the optimal bitumen recovery from tar sand in aqueous sodium hydroxide is reached at 0.1g NaOH with 50. Sodium hydroxide was found to be a more effective leaching reagent for the successful recovery of bitumen and sand residue from the Ondo tar sand. to functionally predict bitumen and sand residue recovery from tar sands. less lean tars. Zircon.It can be shown from table 4.1 Conclusion The Ondo tar sand is a natural resource that will provide significant development in a few years to come if properly explored. higher sand porosity.3 that sodium hydroxide added in excess of the optimum causes the free natural surfactants concentrations to exceed their optimum levels thereby reducing bitumen separation efficiency. The relationship between primary bitumen recovery and process aid (NaOH addition) for a given tar sand varies with tar sand composition and forms a partial means for categorizing tar sands. This research work shows that bitumen can be successfully recovered from tar sands. Bitumen can be effectively recovered through the hot water extraction.3.60% of bitumen recovered. Extensive quantitative analyses of the mineralogical aspects of tar sand could lead to the identification of mineral characteristics. which liberates the mineral rich sand residue. low clay content. heavy metals and higher bitumen content. low sulphur content.

The successful recovery of rutile for paint making will reduce the dependence on imports and increases the economy’s Gross Domestic Product (GDP). . iii. This would be beneficial to plant operations. 5. Literatures have also shown that rutile is present in varying composition of tar sand residue and is of very high economic importance. However. Follow-up analysis by experts in the field of minerals extraction and processing. there is very little information in literatures on the recovery of rutile from tar sand residue. the successful recovery of rutile from tar sand residue was not achieved because of the unavailability of chemicals to concentrate the rutile content of the sand. Further research work could focus on understanding the association between bitumen recovery and heavy metals recovery from tar sands.significance of TiO2 (rutile) as a raw material in Titanium dioxide pigment. the following recommendations are made: i. Government and private establishments should explore the opportunities available in the successful extraction of valuable minerals and metals present in tar sands. ii. iv. production of titanium metal and gemstones. Also. therefore further research is expected to be carried out.2 Recommendations From the results obtained in this investigation. and lead to improved recovery of bitumen and other minerals. as well as its presence in Ondo tar sand has been discussed.

(1960). Oil Sands Fundamental Consortium c/o Oil Sands Research Division of Alberta Energy.oilsandsdiscovery. Geological Survey Open-File Report 76-381. http://www. 27 p. University of Ife. Alberta Community Development (2005). vol.R.com. P. . (2001). “Oil sands facies. ultra-fines and tailings”.S. Oil Sands Discovery Center. ‘Uses of rutile’. Mineralogy of tar sand in the upper part of the Green River Formation in the eastern Utah Basin.google.L. Utah: U. (1980).REFERENCES Adegoke.A.. Geological Consultancy Unit.1 – Geology and Reserves estimate: Unpublished Proprietary Report. Report No: ER-1332-95S. J. www. Geotechnical investigation of Ondo State Bituminous Sands.com [2005-03-31] Alberta Energy and Utilities Board (AEUB) Andrew. Allen and Stanford (1973). O. Carrigy.

17. Free patents online. (1979).. The Canadian Institute of Mining and Metallurgy. Cuddy. 257-374. Pearson.13. ‘Microscopic structure of Athabasca Oil sand’. (1996) “Geology of Canadian Oil sands”. .com. (1994). (1984). Oladapo. 6th ed. The Science and Practice of Heavy minerals processing. The Canadian Journal of Chemical Engineering. The Future of Heavy Crude and Tar Sands. pp 295-300.. vol. “Hot-water Separation of Alberta Bituminous Sand”. UNITAR. USA. AOSTRA. G. (1926). (2008). Encyclopedia of Metallurgical and Materials Engineering.Sc Thesis: Department of Materials Science and Engineering. Tottle.T. A. Ignasiak. Syncrude Canada private communications Ltd. M. America Chemical Society. Osun State.. T. Ells.F. (1983). (1998).A. K. M.R.. Shaw. B.K. 60. Process for Upgrading tar and bitumen’. 639-675. Cambridge University Press.A.B Bartholic (1989). OAU. 538-545. ‘Investigation of the Mineral and Metal Content of the Ondo Bitumen Rich Tar Sand’. O. Ile-Ife.Clark. Edmonton. Reagan W. C.J and D.E.

. and Abubakar. S. Federal University of Technology. Y. Elemental composition of rutile from south-western Nigeria using X-ray techniques. R. Wikipedia – The free encyclopedia (en.com. A. Siyanbola.nation master. Yaro. Unpublished report. T. I. Minna. Nuclear Instruments and methods in Physics Research Section B: Beam Interactions with Materials and Atoms. 2005. Funtua. . Adetunji. O.wikipedia. 240-245. A. (2003).org. Fasasi. O. M. 215. www.W.A.org). Afolabi . pp. January 2004. Issues 1-2. Minerals Processing Research unit. Adesiyan. S. I. A.wikipedia.M. ‘Determination of the liberation size of Manganese deposit using heavy sink-float method’. Vol. en.

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