ABSTRACT This study investigate the production of grease from spent engine oil which was carried out

using different mechanism of recycling process, after which the grea se have been collected from the mechanic dumpsite. Before the treatment take pla ce, the spent engine oil was analyst the level of the deterioration of the oil. The result of the analysis of the spent engine oil was recorded and was compared with that of the fresh spent engine oil, where by the kinematic viscosity at 40C of fresh engine oil was (22-248) and for the spent engine oil it is (111-132), for the kinematic viscosity at 100C is (18.5-22), while that for the refined spen t engine oil is (200) at 40C and the kinematic viscosity at 100C in the refined sp ent engine oil is (18). The test for the viscosity index for the fresh engine oi l is (95) and for the spent engine oil is (99), while the refined spent engine o il is (96.8). After the test have been treated and compared with the fresh engin e oil. This oil is treated with 70% of concentrated of sulphuric acid (H2SO4) in the ratio of 10ml to 1ml. you will observed a distinct separation between the a cidic oil and acidic sludge (acidic oil up and acidic sludge down) whereby the a cidic oil could be dark or brownish in colour. Then treat your acidic oil by cau stic neutralization and extract the mixture of the acidic oil. Therefore, the ne utral spent oil is ready for grease manufacturing. CHAPTER ONE 1.0 INTRODUCTION A lubricants main purpose is to reduce frictional burden that is found in Machine s. Ancient engineers recognized that certain natural oils and fats reduce fricti on and rolling resistance when applied to them. This ancient practice is foundin g the records and indicates that the first lubricants were olive oils or animal fats mixed with various inorganic filters to reduce the friction of rolling ston es over planks and for reducing the frictional force of chariot wheels. (Marcel, 1985). In fact, the first calcium soap grease was a mixture of animal fat(today we them as mixed esters of glycerol), calcium oxide and lime. Frictional heating would cause a chemical reaction between the lime and calcium oxide producing an in sit u saponification action. In even earlier times, spear points were greased to all ow further penetration into wooly mammoth hides. How many times have you seen a Carpenter applying a soap or grease to a nail or screw to reduce. (Marcel, 1985) . Driving friction? Here, we address grease for automotive applications. Any oil t hat is mixed with either organic or inorganic fillers is called grease. Grease i s a semisolid lubricant that stays, put where method of lubrication would fail. Modern grease contains one or more fillers, the base oil, additives, and an opti onal tackifiers, and latter makes the grease sticky and increase adherence. The filler holds the oil in the grease in its interstitial space, but it is the oil in the grease that actually lubricates. The majority of greases on market today are composes of mineral oil blended with a soap thicker. Additives enhance Perfo rmance and protect the grease and lubricated surfaces. Grease has been described as a temperature regulated feeing device, when lubricant film between wearing s urfaces thins, the resulting heat softens the adjacent grease, which expands and releases oil to restore film thickness. In this research grease will be produce by using spent engine oil based on suitable method. The product will be testing their viscosity by using viscometer, to produce qual ity and the best method to produce grease. (Marcel, 1985). 1.1 Problem Statement The major source of water pollution is oil (petroleum and waste lubricants). Mos t Of factories discard their waste into the river and sea and this is the proble m most Developing countries faced today. To rectify this situation we propose to recycle the waste to produce grease. 1.2 Aim The aim of this research is to find the solution that can reduce the water pollu tion, enhances waste management, lessen the demand on our natural resources (cru de oil), and to produce grease from spent engine oil.

1.3 1. 2. 3. 4. he 5. 6. 1.4

Objectives Investigate a better and efficient way of recycling spent engine oil. Determine the level of cleanliness for re-use of treated oil. To produce grease from the recycled spent engine oil. To test the performance of the grease produced by testing viscosity of t product. To compare the quality of grease produced from different kinetics. To enhance waste management.

Scope This project work is required to covered the production of grease from s pent engine oil. 1.5 1. se. 2. 3. 1.6 Significant of Study To create substitute in the raw material used for the production of grea To enhance waste management. To promote entrepreneurship.

Limitation of study Difficulty in getting the appropriate chemical/reagent for the treatment of spent engine oil. Conclusively, the production of grease from spent engine oil will not on ly benefit the environment but also the entrepreneur and the society at large as it is a profitable venture. 1.7 Economic Importance 1. It will reduce the demand on our natural crude oil. 2. It creates job opportunity and adds to our national economic in terms of monetary and standard of living. 3. It enhances waste management through the reduction of indiscriminate di sposal of spent engine oil.

CHAPTER TWO 2.0 LITERATURE REVIEW 2.1 Grease Background Grease is a semi fluid of a fluid lubricant, a thickener, and additives. The flu id lubricant that performs the actual lubrication can be petroleum (mineral) oil , synthetic oil, or vegetable oil. The thickener gives grease its characteristic consistency and is sometimes thought of as a three-dimensional fibrous network or sponge that holds the oil in place. (John, 1981). Common thickeners are soaps and organic or inorganic no soap thickeners. The maj ority of greases on the market are composed of mineral oil blended with a soap t hickener. Additives enhance performance and protect the grease and lubricated su rfaces. Grease has been described as a temperature regulated feeding device, whe n the lubricant Film between wearing surfaces thins, the resulting heat softens the adjacent grease, which expands and releases oil to restore film thickness. ( John, 1981) There has been a need since ancient times for lubricating greases. The Egyptians used mutton fat and beef tallow to reduce axle friction in chariots as far back as 1400 BC. More complex lubricants were tried on ancient axle hubs by mixing f at and lime, but these crude Lubricants were in no way equivalent to the lubrica ting greases of modern times. Good lubricating greases were not available until the development of petroleum-based oils in the late1800 s. Today, there are many different types of lubricating greases, but the basic structure of these grease s is similar. (John, 1981) In general, grease consists of a thickening agent dispersed throughout lubricati ng oil. The thickening agents or gallants include alkali metal soaps, clays, pol

ymers, carbon black, and colloidal silica and aluminum complexes. The lubricatin g oil may be petroleum oil or synthetic oil. The most common type of grease is t he soap-based grease. The soap comes from animal or vegetable fats or fatty acid s, wool grease, rosin or petroleum acids. The lubricating oil is commonly minera l oil from paraffinic, naphthenic or aromatic hydrocarbons. Other components of these greases include unreached fat, fatty acids and alkali, unsaponifiable matt er (including glycerol and fatty alcohols), rosin or wool grease and water. Some of the other additives used in grease are oxidation inhibitors, rust and corros ion inhibitors, color stabilizers, metal passivators, water repellants and visco sity index improvers. In soap greases the metallic soap consists of a long-chain fatty acid neutralized by a metal such as aluminum, barium, calcium, lithium, m agnesium, sodium or strontium. (John, 1981) The fatty acids usually contain 16 to 18 carbon atoms. A common form of soap-bas ed grease uses lithium 12-hydroxystearate as the thickener. To properly thicken the grease the soap must be in the form of fibers of suitable size dispersed thr oughout the lubricating oil. The crystalline fibers are usually in the size rang e of 1 - 100 micrometers with diameters 0.1 to 0.01 of their length. For good sh ear stability the fiber should have a large ratio of length to diameter, and for good oil retention. (John, 1981) The fiber should be as small as possible. Therefore, greases need a mixture of t hese two types of fibers. Also, there must be a balance between the solvency of the fluid and the solubility of the soap to get suitable thickening. Another typ e of thickener that is not soap-based is prepared from clays. The clay, such as Bentonite orattapulgite is reacted with a quaternary amine to change the clay fr om hydrophilic (water-loving) to hydrophobic (water-rejecting) and oleophilics ( attracting oil). Effective thickening is achieved by combining the clay with a p olar activator or dispersant, such as acetone, methanol or ethanol, with small a mounts of water and by delaminating and reducing the platelets to a small size. This process will increase the total surface area of the dispersed clay, this im mobilizes a very high percentage of oil based on the weight of clay. This will t hicken the grease. Other solid additives produce thickened grease by the nature of their fine dispersion throughout the fluid and by their particle-particle int eractions. Solid-additive greases extend the operating temperature range over so ap greases. The solid-type greases do not have a melting point, and their upper temperature limit is that of the oil being used. (John, 1981) 2.2 Properties of Grease Soap thickeners are formed by reacting a metallic hydroxide, or alkali, with a f at, fatty acid, or ester. The type of soap used depends on the grease properties desired. Calcium (lime) soap greases are highly resistant to water, but unstabl e at high temperatures. Sodium soap greases are stable at high temperatures, but wash out in moist conditions. Lithium soap greases resist both heat and moistur e. (John, 1981) A mixed base soap is a combination of soaps, offering some of the advantages of each type. A complex soap is formed by the reaction of an alkali with a high-mol ecular weight fat or fatty acid to form soap, and the simultaneous reaction of t he alkali with a short-chain organic or Inorganic acid to form a metallic salt ( the complexing agent). Complexing agents usually increase the dropping of grease . Lithium, calcium, and sodium greases are common alkalis in complex soap grease s. Non soap thickeners, such as clays, silica gels, carbon black, and various sy nthetic organic materials are also used in grease manufacture. A multipurpose is designed to provide resistance to heat, as well as water, and may contain addit ives to increase load-carrying ability and reduce rust. (John, 1981) 2.3 Grease 1. 2. 3. Grease Grease Manufacturing can be made in either of the standard modes: Batch process Semi-continuous process Continuous process manufacturing entails the following successive steps: reaction, dehydrati

on (removal of water), dispersion and blending. (John, 1981) 2.3.1 Batch Process Batch production is the most common manufacturing method. The steps of manufactu ring include the following. Bulk ingredients are metered or weighed into the pro cessing reactor. For soap-based greases made by saponification (the process of f orming soap by splitting a fat with an alkali), the fatty ingredient, alkali and a portion of the oil are added to the reactor. By heating (300 - 450F) and mixin g, the fat is converted to soap, and the soap is dispersed throughout the mixtur e. This may be done in open kettles or in closed pressure kettles. After complet ion of saponification and dehydration (removal of water), the remaining oil is a dded to the batch to lower the temperature. Next, the grease is milled or homoge nized. (John, 1981) This step of homogenization or milling is very important, because it will produc e a uniform crystal and gel structure that will not change when the grease is us ed. Homogenizing the grease will break down the solid particles or fibers and wi ll disperse the resultant small particles in the liquid. It also breaks up lumps , eliminates graininess and produces a smooth product. Homogenization of certain types of greases will stiffen the grease producing lower penetration value. Hom ogenization can improve texture and brighten greases appearance. In many cases this homogenization process is carried out at temperatures greater than 200F (93C). ( Marcel, 1985). After homogenization, the grease is further cooled, deaerated and packaged. Of c ourse, it is understood that there are many different grease manufacturing metho ds depending on the type of grease and the manufacturer. 2.3.2 Semi-continuous Process Semi-continuous process combines a continuous reactor with one or more batch ket tles. Semi-continuous process entails a continuous tubular reactor producing int o one or more kettles. Here, reaction takes place in the tubular reactor. (Marce l, 1985). 2.3.3 Continuous Process Also for soap based and complex grease only. It is most effective when used for long runs of one product or very similar products. Frequent changes may lead to loss of efficiency and quality. Plants typically consist of all basic grease uni ts: tubular reactor, dehydration and finishing (dispersion and blending). (Marce l, 1985). 2.4 Functions of Grease The function of grease is to remain in contact with and lubricate moving surface s without leaking out under gravity or centrifugal action, or be squeezed out un der pressure. Its major practical requirement is that it retain its properties u nder shear at all temperatures that it is subjected to during use. At the same t ime, grease must be able to flow into the bearing through grease guns and from s pot to spot in the lubricated machinery as needed, but must not add drastically to the power required to operate the machine, mostly at startup. (Boehringer, 19 92). 2.4.1 Functional properties of grease. 1. Functions to minimize leakage and to keep out contaminants. 2. Because of its stability, grease acts to prevent lubricant leakage and a lso to prevent entrance of corrosive contaminants and strange materials. It also acts to keep seals effective (whereas oil would simply seep away). 3. Easier to contain than oil. Oil lubrication can require an expensive sys tem of circulating equipment and complex maintenance devices. In comparison, gre ase is good quality of stiffness, is easily confined with simplified, and less c ostly maintenance devices. 4. Fluid level does not have to be controlled and monitored. 5. Holds solid lubricants in suspension. Finely ground solid lubricants, su ch as molybdenum disulfide and graphite, are mixed with grease in high temperatu re service (over 315 C [99 F]) or in extreme high-pressure applications. Grease holds solids in suspension while solids will settle out of oils. (Boehringer, 19

92) 2.4.2 Applications suitable for Grease Grease and oil are not the same. Grease is used when it is not practical or conv enient to use oil. The lubricant choice for a specific application is determined by matching the machinery design and operating conditions with desired lubrican t characteristics. Grease is generally used for: 1. Machinery that runs from time to time or is in storage for an extended p eriod of time. 2. Because grease remains in place, a lubricating film can instantly form. 3. Machinery that is not easily reached for frequent lubrication. 4. High-quality greases can lubricate isolated or relatively inaccessible c omponents for extended periods of time without frequent replenishing. 5. Machinery operating under extreme conditions such as high temperatures a nd pressures, shock loads, or slow speed under heavy load. 6. Under this situation, grease provides thicker film that is required to p rotect and sufficiently lubricate, whereas oil films can be too thin and can bre ak. (Marcel, 1985). 2.5 Grease Characteristics 2.5.1 Apparent Viscosity At start-up, grease has a resistance to motion, implying a high viscosity. Howev er, as grease is sheared between wearing surfaces and moves faster, its resistan ce to flow reduces. Its viscosity decreases as the rate of shear increases. By c ontrast, oil at constant temperature would have the same viscosity at start-up a s it has when it is moving. (Boehringer, 1992). To differentiate between the viscosity of oil and grease, the viscosity of greas e is referred to as apparent viscosity. Apparent viscosity is the viscosity of a g rease that holds only for the shear rate and temperature at which the viscosity is determined. (Boehringer, 1992). 2.5.2 Bleeding, migration Bleeding is a condition when the liquid lubricant separates from the thickener. It is induced by high temperatures and also occurs during long storage periods. Migration is a form of bleeding that occurs when oil in grease migrates out of t he thickener network under certain conditions. For example, when grease is pumpe d though a pipe in a centralized lubrication system, it may encounter a resistan ce to the flow and form a plug. The oil continues to flow, migrating out of the thickener network. As the oil separates from the grease, thickener concentration increases, and plugging gets worse. If two different greases are in contact, th e oils may migrate from one grease to the other and change the structure of the grease. (Boehringer, 1992). 2.5.3 Consistency, penetration, and National Lubricating Grease Institute (NLG I) Numbers The most important feature of grease is its stiffness or consistency. Grease tha t is too stiff may not feed into areas requiring lubrication, while grease that is too fluid may leak out. Grease consistency depends on the type and amount of thickener used and the viscosity of its base oil. Greases consistency is its resi stance to deformation by an applied force. The measure of consistency is called penetration. Penetration depends on whether the consistency has been changed by handling or working. ASTM D 217 and D1403 methods measure penetration of worked and worked greases. To measure penetration, a cone of given weight is allowed to sink into a grease for 5 seconds at a standard temperature of 25 C (77 F). The de pth, in tenths of a millimeter, to which the cone sinks into the grease, is the penetration. A penetration of 100 would represent solid grease while one of 450 would be semi fluid. The NLGI has established consistency numbers or grade numbe rs, ranging from 000 to 6, corresponding to specified ranges of penetration numb ers. Table 2.1 lists the NLGI grease classifications along with a description of the consistency of each classification. (NLGI, 1999). Table 2.1: NLGI Grease Classification NLGI Number ASTM Worked Penetration Consistency 0.1mm @250C

000 00 0

446-475 Semi-fluid

400-430

Semi-fluid

255-385 Very soft 1 310-340 Soft 2 265-285 Common grease 3 220-250 Semi-hard 4 175-205 Hard 5 130-160 Very hard 6 85-115 Solid (Source: NLGI, 1999) 2.5.4 Corrosion and Rust Resistance This is the ability of grease to protect metal parts from chemical attack. The natural resistance of grease depends upon the thickener type. Corrosion resistan ce Can be enhanced by corrosion and rust inhibitors. 2.5.5 Dropping Point Dropping point is an indicator of the heat resistance of grease. As grease tempe rature rises, penetration increases until the grease liquefies and the desired C onsistency is lost. Dropping point is the temperature at which grease becomes fl uid enough to drip. The dropping point indicates the upper temperature limit at which grease retains its structure, not the maximum temperature at which grease may be used. A few greases have the ability to regain their original structure a fter cooling down from the dropping point. 2.5.6 Evaporation The mineral oil in grease evaporates at temperatures above 177 C (350 F). Excessiv e oil evaporation causes grease to freeze due to increased thickener concentrati on. Therefore, higher evaporation rates require more frequent regarding lubricat ion. (Boehringer, 1992) 2.5.7 Oxidation Stability This is the ability of grease to resist a chemical union with oxygen. The reacti on of grease with oxygen produces insoluble gum, sludges, and lacquer-like deposi ts that cause sluggish operation, increased wear, and reduction of clearances. E xtended high temperature exposure accelerates oxidation in greases. (Boehringer, 1992) 2.5.8 High-Temperature Effects High temperatures damage greases more than they damage oils. Grease, by Its natu re cannot disperse heat by convection like circulating oil. Therefore, with out the ability to transfer away heat, extreme temperatures result in accelerates ox idation or even carbonization where grease hardens or forms a shell. Effective g rease lubrication depends on the grease s consistency. High temperatures bring s oftening and bleeding, causing grease to flow away from needed areas. The minera l oil in grease can flash, burn, or evaporate at temperatures above 177 C (350 F). High temperatures, above 73-79 C (165-175F), can dehydrate certain greases such a s calcium soap grease and cause structural breakdown. The higher evaporation and dehydration rates at high temperatures require more frequent grease replacement . (Boehringer, 1992) 2.5.9 Low-Temperature Effects If the temperature of grease is lower enough, it will become so viscous that it can be classified as hard grease. Pump ability and machinery operation may becom e impossible due to torque limitations and power requirements. The temperature a t which this occurs depends on the shape of the lubricated part and the power be ing supplied to it. As a guideline, the base oils flow point is considered the lo w temperature limit of grease. (Boehringer, 1992)

2.5.10 Texture. Texture is observed when a small sample of grease is pressed between thumb and i ndex finger and slowly drawn apart. Texture can be described as: Brittle: the gr ease ruptures or crumbles when compressed. i. Buttery: the grease separates in short peaks with no visible fibers. ii. Long fiber: the grease stretches or strings out into a single bundle of fibers. iii. Resilient: the grease can withstand moderate compression without permane nt deformation or rupture iv. Short fiber: the grease shows short break off with evidence of fibers. v. Stringy: the grease stretches or strings out into long, fine threads, bu t with no visible evidence of fiber structure. 2.5.11 Water Resistance This is the ability of grease to hold up the effects of water with no change in it stability to lubricate. Soap or water may suspend the oil in the grease, form ing a mixture that can wash away or, to a lesser extent, reduce lubricity by dil uting and changing grease consistency and texture. Rusting becomes a concern if water is allowed to contact iron or steel components. 2.6 Disadvantages of Grease i. Poor cooling. Grease cannot disperse heat by convection like circulating oil ii. Resistance to motion. Grease has more resistance to motion at start-up t han oil, so it is not appropriate for low torque or high speed operation iii. More difficult to handle than oil for dispensing, draining, and refillin g. Also, exact amounts of lubricant cannot be as easily metered. 2.7 Fluid Lubricants Fluid lubricants used to formulate grease are normally petroleum or synthetic oi ls. For petroleum oils in general, naphthenic oils tend to chemically mix better with soaps and additives and form stronger structures than paraffinic oils. Syn thetic oils are higher in first cost but are effective in high-temperature and l ow temperature extremes. With growing environmental concerns, vegetable oils and certain synthetic oils are also being used in applications requiring nontoxic o r biodegradable greases. (Marcel Dekker, 1985) The base oil selected in formulating grease should have the same characteristics as if the equipment is to be lubricated by oil. For instance, lower-viscosity b ase oils are used for grease applications at lower temperatures or high speeds a nd light loads, whereas higher-viscosity base oils are used for higher temperatu res or low speed and heavy load applications. (Boehringer, 1992) 2.8 Soap Thickeners Dispersed in its base fluid, a soap thickener gives grease its physical characte r. Soap thickeners not only provide consistency to grease, they affect desired p roperties such as water and heat resistance and pump ability. They can affect th e amount of an additive, such as a rust inhibitor, required to obtain a desired quality. The soap influences how grease will flow, change shape, and age as it is mechani cally worked and at temperature extremes. Each soap type Brings its own characteristic properties to grease. The principal ingredients in creating soap are a fatty acid and an alkali. Fatty acids can be derived from animal fat such as beef tallow, lard, butter, fish oi l, or from vegetable fat such as olive, castor, soybean, or peanut oils. The mos t common alkalis used are the hydroxides from earth metals such as aluminum, cal cium, lithium, and sodium. Soap is created when a long-carbon-chain fatty acid r eacts with the metal hydroxide. The metal is included into the carbon chain and the resultant compound develops polarity. The polar molecules form a fibrous net work that holds the oil. Thus, a somewhat rigid gel-like material grease is develo ped. Soap concentration can be varied to obtain different grease thicknesses. Fu rthermore, viscosity of the base oil affects thickness as well. Since soap qualities are also determined by the fatty acid from which the soap is prepared, not all greases made from soaps containing the same metals are identical. The n

ame of the soap thickener refers to the metal (calcium, lithium, etc.) from whic h the soap is prepared. From (Weiheim, 2001) 2.9 Additives An additive that mix together to form grease is as surface protecting and effect ively improves the overall performance of grease. Solid lubricants such as molyb denum disulfide and graphite are added to grease in certain applications for hig h temperatures (above 315 C or 599F) and extreme high pressure applications. Incor porating solid additives requires frequent grease changes to prevent accumulatio n of solids in components. (Weiheim, 2001) 2.10 Grease Types 2.10.1 Calcium Grease Calcium or lime grease, the first of the modern production greases, is prepared by reacting mineral oil with fats, fatty acids, a small amount of water, and cal cium hydroxide. The water modifies the soap structure to absorb mineral oil. Bec ause of water evaporation, calcium grease is sensitive to elevated temperatures. It dehydrates at temperatures around 79 C (175 F) at which its structure collapse s, resulting in softening and, eventually, phase separation. Greases with soft c onsistencies can dehydrate at lower temperatures while greases with firm consist encies can lubricate satisfactorily to temperatures around 93 C (200 F). In spite of the temperature limitations, lime grease does not emulsify in water and is ex cellent at resisting Wash out. Also, its manufacturing cost is relatively low. If calcium grease is prepared from 12-Hydroxystearic acid, the result is hydrous (w aterless) grease. Since dehydration is not a concern, anhydrous calcium grease c an be used continuously to a maximum temperature of around 110 C (230 F). Calcium complex grease is prepared by adding the salt calcium acetate. The salt provides the grease with extreme pressure characteristics without using an addit ive .Dropping points greater than 260 C (500 F) can be obtained and the maximum us able temperature increases to approximately 177 C (350 F). With the exception of p oor pump ability in high-pressure centralized systems, where caking and hardenin g sometimes occur calcium complex greases have good all-around characteristics t hat make them desirable multipurpose greases. (Weiheim, 2001) 2.10.1 Sodium Grease Sodium grease was developed for use at higher operating temperatures than the ea rly hydrated calcium greases. Sodium grease can be used at temperatures up to 12 1 C (250 F), but it is soluble in water and readily washes out. Sodium is sometime s mixed with other metal soaps especially calcium, to improve water resistance. Although it has better adhesive properties than calcium grease, the use of sodiu m grease is declining due to its lack of flexibility. It cannot compete with wat er resistant, more heat resistant multipurpose greases. However, it still recomm ended for certain heavy duty applications and well-sealed electric motors. (Weih eim, 2001) 2.10.2 Aluminum Grease Aluminum grease is normally clear and has a somewhat stringy texture, more so wh en produced from high viscosity oils. When heated above 79 C (175 F), this stringi ness increases and produces a rubberlike substance that pulls away from metal su rfaces, reducing lubrication and increasing power consumption. Aluminum grease h as good water resistance, good adhesive properties, and inhibits rust without ad ditives, but it tends to be short-lived. It has excellent inherent oxidation sta bility but relatively poor shear stability and pump ability. Aluminum complex grease has a maximum usable temperature of almost 100C (212 F) hi gher than aluminum soap greases. It has good water and chemical resistance but t ends to have shorter life in high temperature, high speed applications. (Weiheim , 2001) 2.11 Compatibility Greases are considered incompatible when the physical or performance characteris tics of the mixed grease fall below original specifications. In general, greases

with different chemical compositions should not be mixed. Mixing greases of dif ferent thickeners can form a mix that is too firm to provide sufficient lubricat ion or more commonly, a mix that is too soft to stay in place. Combining greases of different base oils can produce a fluid component that will nots provide a continuous lubrication film. Additives can be diluted when greas es with different additives are mixed. Mixed greases may become less resistant t o heat or have lower shear stability. If a new brand of grease must be introduce d, the component part should be disassembled and thoroughly cleaned to remove al l of the old grease. If this is not practical, the new grease should be injected until all traces of the prior product are flushed out. Also, the first grease c hanges should be more frequent than normal Scheduled. (Weiheim, 2001) CHAPTER THREE 3.0 METHODOLOGY 3.1 Materials. The material used in this project includes the following: 1. Spent engine oil 2. aluminum hydroxide 3. calcium hydroxide 4. sodium hydroxide 5. shear butter 6. burner clay 7. distilled water 8. sulphuric acid 3.2 Equipment The equipment used in this project includes the following: 1. Rotary evaporator bath 2. Stirrer 3. Beakers 4. Retort stand 5. Viscometer 6. Thermometer 7. Rotary transducer 8. Rheometer 9. Oven 10. Weighing balance 11. Plastic bowl 12. Aluminum pan 3.3 Overall Methodology The experiments were divided into two sections; 1. The mechanism of recycling spent engine oil, 2. Production of grease from the recycled spent engine oil. 3.3.1 Mechanism of Refining Spent Engine Oil Refining of spent engine oil is the process of regenerating its used substance s o that it can be used again. It is the process involving the removal of the impu rities in the spent oil and bringing it back to the initial state. The choice of method of regenerating base oil is determined by the nature of the spent oil, s ome requires purification from mechanical impurities while others require deep p urification with the use of chemical and physical methods. The physical method i ncludes removal of dirt, sand-metal particles and combustible substance. This include; centrifugation, setting filtrations, distillation etc. Refining th e spent engine oil will only bring back the base oil without additives (Labones, 1990). 3.3.2 Recycling Processes 3.3.3 Acid treatment (Sulphurnation Process) The sample of spent engine oil was dehydrated to be free of moisture at about 10 0C on a hot plate after test has been carried out to know the level of deteriorat ion of the oil. The dehydrated sample of the spent engine oil was mixed with 70%

concentration of Sulphric acid (H2SO4) in the ratio 10ml to 1ml and then heated to 600 C for one hour, and was allowed to settle for six (6) hours so as to enab le the insoluble mater and water remain to settle at the bottom of the beaker. T he treated oil is decanted and sludge formed removed from the beaker. The treate d oil is then contracted with activated carbon, and treated at 2000C 2500C for 2 -3 hours. The treated oil is filtered and allowed to cool. After which, the tre ated oil is analyzed. 3.3.4 Observation. a. The mixture have a distinct separation (acidic oil and sludge {down}). b. The acidic oil could be dark or brownish in color. c. The acidic sludge is highly viscous, dark and thick like a coal tar sett led at the bottom. d. The acidic sludge is highly corrosive therefore handle it should be hand led with care. 3.3.5 Treatment of Acidic Oil a. Take your acidic oil for treatment b. You can neutralize it either by bleaching (lime with or plus bleaching e arth ratio 1:1 with the acidic oil) [15% weight + weight of acidic oil] {15/100 X weight of oil} c. Use that to bleach the acidic oil. d. Calculate a 15% weight of the bleaching earth to that of the weight of t he acidic oil. e. Bleach the acidic oil at 80-1000C. f. Start introducing the bleaching earth at 500C. 3.3.6 Treatment of Acidic Oil by Caustic Neutralization. a. Caustic preparation b. Prepare 3-5N normal solution caustic c. Get a known weight of your acidic oil d. Calculate 25% weight caustic solution to the known weight acidic oil e. Under room temperature with a continuous mixing of the acidic oil in a g lass beaker, gradually introduce your caustic solution into the acidic oil f. You will be introducing the caustic gradually not at once, bit by bit wh ile checking the PH with litmus paper to attain neutrality g. You may not exhaust all the calculated caustic before you attain the end point but in some case it can be possible (Neutral oil). 3.3.7 Extraction of the Mixture of Neutral Oil Extracting Solvent 1. Ethanol 98% purity 2. HO 3. Mix ethanol and HO ratio 1:1 (That is the extract solvent) because H2O is heavier than oil hence it needs 1:2 for easy separation. 4. Maintain the mixture of neutralized oil at 50-60C. 5. The separation in different columns is based on; 6. Remove the solvent and the sulpurnates in the extractor leaving the mois t oil in the extractor. 7. Transfer the moist oil into a beaker. Dry the moist oil at a temperature of 100-110C until moisture is totally removed. You now have your neutral spent o il ready for grease manufacturing. Possible Test on Base i. Viscosity. ii. TAN (Total Acid Number) to make sure that the oil is completely neutrali zed. iii. Moisture content. iv. Moisture causes emulsification that can contaminate the reaction of grea se.

Experimental Analysis 3.4 Treatment of spent engine oil with activated clay 3.4.1 Clay Preparation. Brownish-red clay was used and apparatus used include jars, sieve conical flask, bowls, oven, distilled water. 3.4.2 Method i. The clay sample was grounded and then make into slurry in distilled wate r. ii. Impurities such as sand and stone settled at the bottom. Then were get ri d off by decanting iii. The slurry was kept in an oven at temperature of 1100C to be dried up. iv. The dried clay was grounded into very fine particles and sieved to a mes h of 0.5 mm using test sieve on a mechanical shaker. 3.4.3 Clay Activation Apparatus: Aluminum pan, plastic bowl, oven, burner clay, distilled water. 3.4.4 Method: i. 200g of clay (after dirt, sand and stone have been removed) was made int o slurry with distilled water of about 80cm3. ii. 50-60cm3 of acid in 0.35 mole/cm3 concentration was added to the slurry made. iii. The slurry into aluminum pan and left for one hour at temperature betwee n 90-100C. iv. After the time duration, the mixture was washed with distilled water in order to remove any excess acid. The pH of washing water was monitored until it was found to be neutral. v. The washed clay mixture was dried in an oven for one hour and grounded i nto powdery form. (Oboh, 1991). 3.5 Purification Process of Spent Engine Oil The spent engine oil was purified using activated clay. The activated clay was g rounded and mixed with the spent engine oil that has been already heated for abo ut 5 min, the mixture was stir together thoroughly with the aid of electric stir rer. The mixture was kept till the following day so that there will be some chem ical reaction between the spent oil and the activated clay. The impurities in th e spent engine oil, had already settled the following day with the clay particle s then the oil was sieve with the aid of cloth. 3.6 Production of Grease The experiments were carried out according to the standard procedure outline in section. The experiments were divided into two parts. The first part was to prepa re the samples of grease by using refined spent engine oil as base oil instead o f petroleum oil. The Second part of the experiment involved analyzing the product by d etermines the viscosity of the grease using viscometer. Figure 3.1 shows the out line of the overall. Methodology where Experiment Work 1 was producing grease from used lubricant, 3 different type of soap is used in this experiment. For the Experiment Work 2 whe re the product dropping point and viscosity was analyzed. Then the comprehensive discussion was carried out on the viscosity of the grease, to know and analyzed the quality of the Grease product.

Figure 3.1: Outline of Overall Methodology 3.6.1 Experimental Methodology 3.6.2 Production of Grease 1. Spent engine oil was collect from dumped site. 2. Tests were carried out on the spent engine oil to test the level of dete rioration and impurities. 3. The spent engine oil was sieved to remove suspended particles, dirt, met al chips and impurities treated and analyzed (table 1). 4. For the production of grease, three (3) different known weights of metal lic hydroxide was used. 5. These metallic hydroxide was mixed with shear butter in the proportion o f 15% and 85% by mass at room temperature. 6. Three different soap ratios were used in 10%, 20%, and 30% by volume mix ed with base oil for each of soap. 7. Base oil and soap (thickener) mixture were heated up to 200oC using the rotary evaporator bath. At the same time, the mixture was stirred to improve the mixing efficiency. 8. The mixture was heated for 1 hour, and then was cooled down to get the pr oduct.

Figure 3.2: Block diagram Production of grease Process Flow CHAPTER FOUR 4.0 RESULT AND DISCUSSION OF RESULT 4.1 Result Table 4.1 Analysis carried out on the sample of engine oil Test Fresh engine oil Spent engine oil Refined spent oil Kinematics Viscosity at 400C 22 - 248 111 - 132 200 Kinematics Viscosity at 1000C 18.5 - 22 17.83 18 Viscosity index 95 99 96.8 Flash point 246 230 239 Pour point -12 -10 -12 TBN (MgKOH)/g 4.8 % Sulphated mass 1.2 4.5 2.9 Specific gravity 0.899 0.928 0.920 (Source: Experimental, 2012) Table 4.2 table 4.1 Analysis carried out on grease produced from spent engine oil in of treatment, sulphurnation) Results 184 19.64g 0.92g/cm3 1000C None

(Method Test method Types of test Temperature D3941 Flash point 1000C D874 Sulphated ash 1000C SI Density 200C D95 Moisture content D445

Viscosity 1000C 18.2mm2/sec Basis sample received and tested, product shows the following characteristics; P hysical state; Semi solid. PH; No data available. Color; Characteristics. Solubility; Insoluble in water. The stability of the results is within specification. (Source: Experimental, 2012) Table 4.3 Test Analysis % % % % Analysis showing sample of clay before and after activation. Activated clay Sample Inactivated clay 88.66 3.40 5.31 90.02 6.79 42.22 3.04

Moisture content Ash content Fe0 loss on ignition

43.87

(Source: Experimental, 2012) Table4.4 Analysis of grease produced from spent engine oil in table 4.2 (Method of treatment, activated clay treatment) Type of test Temperature Res Flash point Sulphated ash Density Dropping point Moisture content Viscosity 20C 100C 100C 100C 100C 20C

Test method ult D3941 146 D874 21.08g SI 6.899g/cm EF 308 D95 None D445 18.08mm/sec

Basis sample received and tested, product shows the following characteristics; P hysical state; Semi solid. PH; No data available. Color; Characteristics. Solubility; Insoluble in water. The stability of the results is within specification. (Source: Experimental, 2012) 4.4 Discussion of Results From the research carried out it was discovered that when 25 liters of spent oil was recycled appropriately, 10liters of lubricating oil was obtained from the p rocess and when 50liters of spent oil was recycled 20liters of lubricating oil w as obtained from the process whereas 220liters of crude oil would be required to produce the same 10liters of oil and 440liters of crude oil would be required t o produce the same 20liters of lubricating oil. The kinematics viscosity of the spent engine oil at 100 C was analyzed to be 17.8 3; recycled spent engine oil was also analyzed to be 18.0 which are close to the standard (18.5-22). The experiment shows that the recycled spent engine have so me certain degrees of lubricating properties which is suitable for the productio n of grease. However, grease produced from these method of treatment of spent engine oil (Aci d clay treatment) gives a better performance except were additives may be needed to improve the quality of the grease. Other parameters were also tested which g ives close values to the ASTM Standard test for grease.

CHAPTER FIVE 5.0 CONCLUSIONS AND RECOMMENDATIONS 5.1 Conclusions The recycling process has shown from research, the possibility of obtaining good quality base oils from spent engine oils. The cost of recycling (of spent engin e oil) is relatively low compared to its production from crude oil as the number of purification stage involved is reduced. The base oil from the process can be converted into valuable end product for the manufacturing processes of grease a nd can be marketed. The returns from these transactions could cover the cost of buying the necessary chemical and maintain the recycling plant and therefore mak e the process potentially profitable. In recent times, many marketers of lubrica nt have had to import base oil to blend lube products. Although, the refinery in Kaduna produces this raw material, there are periods when the vacuum distillati on units breakdown and production is suspended. In the wake of such events, lubr icant prices shoot up as marketers buy at higher rate from importation. If only many of these companies can invest in settling up plants that would recycle used oil, it is believe that the scarcity of base oils would be reduced. Finally, th e practice of recycling spent engine oil offers a lasting solution to pollution problems caused by waste oil. 5.2 Recommendations Since the petroleum prices increases each year, using the recycled spent engine oil is the best solution to produce grease in the low cost at the same time; it will enhance waste management and promote Entrepreneurship Development. It is al so strongly recommended that more research should be done on the treatment proce sses of spe4nt engine oil to enhance its suitability of been used as base oil in the production of grease. REFERENCES Ademola, B and Luxembourg, M. (2001). A new Approach to Caustic treatment of Was te Lubricants, Waste Treatment and Utilization. Journals of Engineering Technolo gy, (2): 43-47. Aliyu, T. O. (2002). Preliminary Study on the Recycling of Used Lubrication oil. Macmillan Publisher, Nigeria. 9-14. Billet, M. (1999). Institute Lubrication. Pergamon Limited, London. PP 234 -239. Boehringer (1992): Manufacture and Application of Lubricating Greases, (New York : Reinhold Publishing). Brussels, S. and Luxembourg, R. (2001). Recycling of used Mineral Oil.Journals o f Mechanical Engineering and Processing Technology, 8(12):67-81. Cock, V. R. (1998). Laboratory Handbook for Mineral Oil and Organic Oil Analysis . Academy Press, London. 111-113. Harry, M. F. (2005). Standard Handbook of Hazardous Waste and Disposal. McGraw-h ill Book Company, New York.782-793. Holdridge, D.A. (1966). Re-adsorption of heavy metal cations of clay minerals.Pr oc. 2nd Int. Clay Conf. Heller, L.; and Weiss, A. (Eds.).Arranged by CIPEA, Jeru salem, Israel, 20-24 June 1966, pp. 341-9, Israel University Press, Israel Progr am for Scientific Translations. Institute of Petroleum. (1987). Idumeh, J. (2000). Lubecon Laboratory Handbook for Engine Oil Analysis.Lubecon B lending Company, Ilorin.3-11. Jilner D. A. (1997).Method for Analysis and testing of Petroleum Relatedproducts .Journals of Materials Processing Technology. 7(4): 15-21. John A,( 1981): European Patent Office 0072184 B1; Jonathan, T. (1993). Introduction to Environment Studies, 3rd Edition Saunder Co llege Publisher, New York.23-41. Labones, J.A. (1990). Use of local clay as decolorizing agent for vegetable oils . J. Mining Geol. 26: 121-31. Marcel Dekker, (1985). Lubricating Grease Guide, Kansas City: National Lubricat ing Grease Institute.

Methods for analysis and testing of petroleum products, vol. 4. Wiley, London, E ngland, pp.150-261, 99-103. NLGI lubricant grease guide 4th ed. Feb, (1999). Oboh, A.O.; and Aworh, O.C. (1991). Bleaching performance of selected acid-activ ated Nigerian clays on some common pre-bleach crude palm oil feedstocks. Nigeria n Food J. 9: 20-25. WeiheimWikey VCH,( 2001): Process Bulletin. www.lubricatingrease.com