Thursday, 17 March 2022

COMPARISON BETWEEN THE VARIOUS METHODS OF WASTE OIL RECOVERY (ENGINE OIL) USING GLACIAL ACETIC ACID AND FORMIC ACID


ABSTRACT

Lubricating oils are viscous liquids used for lubricating moving part of engines and machines. Since lubricating oils are obtained from petroleum – a finite product, and with dwindling production from world oil reserves, the need arises more than ever, to recycle used lubricating oils.

Accordingly, this research work focuses on comparative study of two methods of recycling of used Engine oil using glacial acetic acid and formic acid treatment methods. A recycling process of the used lube oil was carried out which eventually led to comparison of results of the recycled oil with the fresh lube oil using ASTM standards. Tests carried out on the used, fresh and recycled lube oils include: flash point, viscosity at 55°C, specific gravity/density, appearance and pour point. The results show that recycled lubricating oil had the following properties: flash point was 200°C for the acetic and formic acids, as compared with 170°C for untreated oil, Also the pour point of the engine oil using acetic and formic acids are 6°C and 5°C respectively. It has been shown that base oils and oils’ additives are slightly affected by the acetic acid. Upon adding acetic and formic acid to the used oil, two layers were separated, a transparent dark colored oil and a black dark sludge at the bottom of the container. The comparison showed that the recycled oil produced by acetic acid and formic acid treatment showed excellent results in the properties of the oil comparable to the fresh oil.

                              TABLE OF CONTENT

Title page                                                                                                                           i

Certification                                                                                                                       ii

Dedication                                                                                                                          iii

Acknowledgement                                                                                                             iv

Abstract                                                                                                                               v

Table of contents                                                                                                                 vi

CHAPTER ONE

INTRODUCTION                                                                                                             1

Background of Study

Problem Statement

Objective of Study

Justification of Study

Scope of Study

CHAPTER TWO

LITERATURE REVIEW

2.1 Lubricating Oil

2.1.1 Use in vehicle

2.2 Engine Oil

2.2.1 Used Engine Oil

2.2.2 Contamination

2.2.3 Contaminants in used Lubricating Oil

2.2.4 Efeects of Oil Contaminants

2.2.5 Physical and Chemical Properties of used Engine

2.2.6 Impacts of used Lubricating Oil

2.3 Used Oil Recycling and Reuse

2.3.1 Impacts of Used Oil Recycling and Reuse

2.4 Recovery Methods

2.4.1 Solvent Extraction Methods

2.4.2 Membrane Technology

2.4.3  Acid Treatment Process

CHAPTER THREE

MATERIALS AND METHODS

3.1 Materials

3.1.1 Experimenta Materialsl

3.1.2 Equipment used

3.1.3 Reagents

3.2 Methods

3.2.1 Material Preparation

3.2.2 Experimental Procedures

CHAPTER FOUR

RESULTS AND DISCUSSION

4.1 Results

4.2 Discussion

4.2.1 Appearance

4.2.2 Flash Point

4.2.3 Viscosity at 55◦C

4.2.4 Specific gravity

4.2.5 Pour Point

CHAPTER FIVE

CONCLUSION AND RECOMMENDATION 

5.1 Conclusion 

5.2 Recommendation 

References

Appendix/Appendices

CHAPTER ONE

INTRODUCTION

1.1 Background Information

Lubricating oils are viscous liquids used for lubricating moving parts of engines and machines. Lubricating oils are obtained from petroleum finite product and with dwindling production from the world oil reserves, it is essential to recognize that all used oil should be disposed using controlled method disposals. Lubricating oil is used to provide a film between the moving part of machines engines to prevent wear and tear.  This may result in groundwater and soil contamination. Recycling of such contaminated materials will be beneficial in reducing engine oil costs. In addition, it will have a significant positive impact on the environment. The conventional methods of recycling of waste engine oil either requires a high cost technology such as vacuum distillation or the use of toxic materials such as sulfuric acid. These methods also produce contaminating by-products which have highly sulfur levels, especially in the Kurdistan region/Iraq. Lubricant oils have been used primarily for reducing friction between moving parts of various machinery or equipment, minimize material wear, improve the efficiency of equipment /machinery and for fuel and energy savings. Access to lubricants is essential to any modern society and not only does lubrication reduce friction and wear by interposition of a thin liquid film between moving surfaces, but it also removes heat, keeps equipment clean, and prevents corrosion. One of its important applications includes gasoline and diesel engine oil.

Waste lubricating oil refers to the engine oil, transmission oil, hydraulic and cutting oils after use. It is also refers to the degradation of the fresh lubricating components that become contaminated by metals, ash, carbon residue, water, varnish, gums, and other contaminating materials, in addition to asphaltic compounds which result from the bearing surface of the engine. These oils must be changed and removed from the automobile after a few thousand kilometers of driving because of stress from serious deterioration in service. The amount of lubricating oils that is collected annually in Europe and USA is very large, approximately 1.7 to 3.5 million tons. This large amount of waste engine oils has a significant impact on both economical and environmental aspects. They cost millions of dollars to manufacture and represent a high pollutant material when disposed of. If discharged into the land, water or even burnt as a low grade fuel, this may cause serious pollution problems because they release harmful metals and other pollutants into the environment.

As stated earlier, When lubricating oils are used in service, they help to protect rubbing surfaces and promote easier motion of connected parts. In the process, they serve as a medium to remove high build up of temperature on the moving surfaces. Further buildup of temperature degrade the lubricating oils, thus leading to reduction in properties such as: viscosity, specific gravity, etc. Dirts and metal parts worn out from the surfaces are deposited into  the lubricating oils. With increased time of usage, the lubricating oil loses its lubricating properties as a result of over-reduction of desired properties, and thus must be evacuated and a fresh one replaced. It is also vital to note that typical lubricating oil contains 90% base oil, most often petroleum fractions called mineral oils and <10% additives. The chemical breakdown of these additives during use resulted to build up of halogenated hydrocarbons in the oil. Polycyclic Aromatic Hydrocarbons (PAHs) as well as other polycyclic compounds are generated and accumulate in the oil (Wong & Wang, 2015) together with metals from wear and tear of the engine being lubricated (Chuug et al., 20017). These compounds gradually reduces its quality leading to change in its physical and chemical properties and thereby deteriorated (Kamal & Khan, 2013).

 A recommended solution for this issue is the recovery of the lubricating oil from the waste oil. Recycling processes using nontoxic and cost effective materials can be an optimum solution. Acid-clay has been used as a recycling method for used engine oil for a long time. This method has many disadvantages; it also produces large quantity of pollutants, is unable to treat modern multigrade oils and it is difficult to remove asphaltic impurities. Solvent extraction has replaced acid treatment as the method of choice for improving the oxidative stability and viscosity/temperature characteristics of base oils. The solvent selectively dissolves the undesired aromatic components (the extract), leaving the desirable saturated components, especially alkanes, as a separate phase (the raffinate. In one study] a mixture of methyl ethyl ketone (MEK) and 2-propanol was used as an extracting material for recycling used engine oils.

Although the oil resulting from this process is comparable to that produced by the acid-clay method, its cost is high. Expensive solvents and vacuum distillation are required to carry out this method. Recently propane was used as a solvent. Propane is capable of dissolving paraffinic or waxy material and intermediately dissolved oxygenated material.

1.2 Problem Statement

 Large quantities of used engine oil from different sources are disposed as  harmful waste into the environment in rivers and lakes and this creates series of problem as they contaminate fresh water and marine lives. Roughly one gallon of used engine oil would contaminate one million gallon of water including fauna and flora.

1.3 Objective of Study

This research study focuses on the comparative study of treatment methods for used engine oil, and its recovery methods. It addresses recycling of waste engine oils treated using acetic acid. A recycling process was developed which eventually led to comparable results with some of the conventional method.

The specific objectives are as follows;

To ensure that pure oil is gotten from waste engine oil

Assess the recovery capacity of the acetic acid process by characterizing the recovered oil and comparing it with the virgin oil.

To ensure low cost of recycling waste oil.

1.4 Justification of the Study

This research is of great importance to mankind and the academia.The method of waste oil treatment adopted in this research provides a lower cost process in comparison with the conventional methods due to the low cost of the acid and the moderate conditions of the process. The recycled oil obtained by this method has been shown to have potential for reuse as an engine lubricant.

Furthermore this new process of recycling of used engine oil did not emit poisonous gases like sulfur dioxide to the atmosphere. In addition, glacial acetic acid has less of a negative impact on the processing equipment compared with sulfuric acid. Lower amount of additives may be required for the base oil recycled by acetic acid-clay method due its low reactivity with the used oil.

1.5 Scope of the Study

In order to obtain the objectives stated above, spent engine oil has be recycled at low cost this will ensure optimum productivity. Also a comparative analysis of spent engine oil, new engine oil, and the recovered engine oil will be carried out and some parameters such as viscosity, specific gravity, pour point and flash point will be tested for. 

CHAPTER TWO

LITERATURE REVIEW

2.1 Lubricating Oil

   A lubricant is a substance, usually organic, introduced to reduce friction between surfaces in mutual contact, which ultimately reduces the heat generated when the surfaces move. It may also have the function of transmitting forces, transporting foreign particles, or heating or cooling the surfaces. The property of reducing friction is known as lubricity.

Lubricating oil is the very stable, non-volatile and smallest fraction of crude petroleum. As petroleum products are essentially composed of hydrocarbons, lubricating oils have hydrocarbon structures, containing from 20 to 70 carbon atoms per molecule.

The lubricating oil molecules can be divided into three broad groupings i.e. paraffinic, naphthenic and aromatic based on functional group. Paraffinic molecules are predominantly straight chains, tend to be waxy, have a high pour point, good viscosity and better temperature stability. Naphthenic molecules are straight chains with a high proportion of five and to a lesser extent six membered ring structures. They tend to have a low pour point. For this reason they are used as refrigeration oils. They are highly carcinogenic and are little used in engine oil. Aromatics are straight chains with six membered ring benzene structures. In real life applications no sharp distinction exists between these various groupings as many lubricating oil molecules are a combination, to varying degrees, of the different types of hydrocarbons (Yu-Lung & Chun-Chu, 2010).

Lubricating oils are fluids such as engine oils, gear, hydraulic oils, turbine oils, etc., used to reduce friction between moving surfaces. They also serve to remove heat from working parts in machinery created by moving surfaces and provide a protective layer on the metal surfaces to avoid corrosion. They also act as a sealant to fill the microscopic ridges and valleys in any metal surfaces to increase the machinery efficiency. Furthermore, they serve as a cleaning agent to carry away dirt or other debris that may damage the bearings or other parts that are operated in tight tolerance. Debris is removed through the engine oil filter or the transmission filter.

Lubricating oils are usually blended with a number of chemical additives to provide products that last longer and allow the machinery to work better under severe operating conditions.

However, performance of the lubricants deteriorates over time as the additives are chemically changed and the oil becomes contaminated with various unwanted pollutants as a result of many physical and chemical interactions (Dennis, 2010).

There are two basic categories of lubricating oil: mineral and synthetic. Mineral oils are lubricating oils refined from naturally occurring crude oil. Synthetic oils are lubricating oils that are manufactured. Mineral lubricating oils are currently the most commonly used type because of the low cost of extracting the oils from crude oil. Additionally, mineral oils can be manufactured to have a varying viscosity, therefore making them useful in a wide range of applications.

Lubricating oils of different viscosities can be blended together, and it is this ability to blend them that makes some oils so useful. For example, common engine oil is generally a blend of low viscosity oil to allow for easy starting at cool temperatures and a high viscosity oil for better performance at normal running temperatures.

 2.1.1 Use in Vehicles

The use of lubricating oils in vehicles is vital to their operation. When an engine is properly lubricated, it needs to put less work into moving pistons as the pistons glide easily. In the long run, this means that the car is able to operate while using less fuel and run at a lower temperature. Overall, the proper use of lubricating oil in a car improves efficiency and reduces the amount of wear and tear on moving engine parts.

2.2 Engine Oil

Engine oil, or engine lubricant is any of various substances comprising base oils enhanced with various additives, particularly anti-wear additive in addition to detergents, dispersants and, for multi-grade oils, viscosity index improvers. Engine oil is used for lubrication of internal combustion engines. The main function of engine oil is to reduce friction and wear on moving parts and to clean the engine from sludge (one of the functions of dispersants) and varnish (detergents). It also neutralizes acids that originate from fuel and from oxidation of the lubricant (detergents), improves sealing of piston rings, and cools the engine by carrying heat away from moving parts.

2.2.1 Used Engine Oil

This can be referred to as any petroleum -based or synthetic oil that has been used. It could also be referred to as spent oil. During normal use, impurities such as dirt, metal scrapings, water or chemicals can get mixed in with the oil or be generated in it due to thermal degradation or oxidation. Therefore, the oil quality gradually decreases to a level that the used oil should be replaced by a new one. Disposing the used oil off in nature creates an intense dangerous pollution. But by proper recovery and refinement of it, a lot of valuable product can be obtained.

Generally lubricating oil becomes unfit for further use for two main reasons: accumulation of contaminants in the oil and chemical changes in the oil. These effects interfere with the basic properties of lubricating oil which are peculiar for their effective performance during application (Awaja & Pavel, 2016).

2.2.2 Contamination

Engine oil contamination also causes deterioration of the oil. Some of the more common contaminant sources include dirt, sand and dust from the air, soot, unburned fuel in the oil, water from condensation of the combustion process, wear metal particulates that the oil filter cannot trap and hold, corrosion by-products and additive elements that have degraded. In addition dirt, sand and dust can continue to enter the engine and, in addition to creating more wear debris, combine with other contaminants and cause more damage than they would separately.

One of the many by-products of combustion is soot. Soot can be highly abrasive as well as cause filters to become filled and/or plugged in extreme cases. Another contaminant is acidic by-products of combustion, which can produce a highly corrosive mixture and cause corrosion and pitting of internal engine components and additional generation of wear debris. These same acidic solutions can also mix with water inside the engine and form an emulsion that can cause problems with oil filters and passageways (Layzell, 2010).

Yet another source of contamination is fuel. A charge of fuel is rarely 100% burned during the combustion process. This unburned fuel can mix with the oil present in the cylinders. Fuel contamination can also be caused by worn sealing components such as excessive piston ring to cylinder clearances allowing unburned fuel to blow-by the rings.

When motor oil is diluted with fuel the viscosity is lowered. If this reaches extremes of contamination excessive wear and engine damage can take place and may lead to significant deterioration of the different properties of the oil (Chia-Yu, 2014). 

2.2.3 Contaminants in used Lubricating Oil

The main constituents of waste lubricating oils are the base oil, degraded additives, metallic debris, oxidation products and carbon soot. A large number of additives are used to impart performance characteristics to the lubricants. The main additives are antioxidants, detergents, anti-wear elements, metal deactivators, corrosion inhibitors, rust inhibitors, friction modifiers, extreme pressure withstanding elements, antifoaming agents, viscosity index improvers, demulsifying or emulsifying agents and stickiness improver.

During their use, these additives lose their characteristics rendering the lube oil non usable for lubricating purpose. In addition, during their use, the lubricating oils and the metal processing oils pick up fractions of various metals as a result of wearing out of components. The concentration of these impurities depends purely on the application to which the particular oil is put to (Diphare et al., 2013).

Generally, lubricating oil loses its effectiveness during operation due to the presence of certain types of contaminants. These contaminants can be divided into extraneous contaminants and products of oil deterioration.

2.2.4 Effects of  Oil Contaminants

Due to its chemical composition, worldwide dispersion and effects on the environment, used engine oil is considered serious environmental problem. Most current motor-oil lubricants contain petroleum base stocks, which are toxic to the environment and difficult to dispose of after use. Over 40% of the pollution in America's waterways is from used motor oil. Used oil is considered the largest source of oil pollution in the U.S. harbors and waterways, at 1,460 ML (385×106 US gal) per year, mostly from improper disposal. By far the greatest cause of engine oil pollution in oceans comes from rural and urban street-runoff, much of it caused by improper disposal of engine oil. One US gallon (3.8 l) of used oil can generate a 32,000 m2 (8 acres) slick on surface water, threatening fish, waterfowl and other aquatic life. According to the U.S. EPA, films of oil on the surface of water prevent the replenishment of dissolved oxygen, impair photosynthetic processes, and block sunlight. Toxic effects of used oil on freshwater and marine organisms vary, but significant long-term effects have been found at concentrations of 310 ppm in several freshwater fish species and as low as 1 ppm in marine life forms. Engine oil can have an incredibly detrimental effect on the environment, particularly to plants that depend on healthy soil to grow. There are three main ways that motor oil affects the environment. They include;

i.        Contaminating water supply

ii.       Contaminating soil

iii.      Poisoning plants

Used engine oil dumped on land reduces soil productivity. Improperly disposed used oil ends up in landfills, sewers, backyards, or storm drains where soil, groundwater and drinking water may become contaminated.

2.2.5 Physical and Chemical Properties of used Engine Oil

Standard chemical and physical tests are used to evaluate the properties of the oil and the extent of the contaminants in the used automotive oils. These tests involve the following measurements:

(1) Viscosity: viscosity testing can indicate the presence of contamination in used lubricating oil. The oxidation and polymerization products that were dissolved and suspended in the oil cause the increase of oil viscosity. While a decrease in the viscosity of lubricating oil indicates the fuel contamination.

(2) Pour point: pour point is the lowest temperature at which the oil will flow. Low pour point indicates good lubricating oil.

(3) Flash point: flash point is the lowest temperature at which the vapours in air will burn momentarily if ignited by flame or spark. A decrease in flash point indicates contamination by dilution of lubricating oils with unburned fuel. Increasing of flash point indicates evaporation of the light components from the lubricating oil.

(4) Acidity or neutralization number: this is a measure of the amount of alkali required to neutralize one gram of the oil. An increase in acid number indicates the extent in oxidation of lubricating oil.

(5) Ash content: the remaining solid ash, when the oil is completely burned, is a measure of oil purity and indicates contamination with metals.

(6) Carbon or coking test: this evaluates the solid residue obtained when the oil is heated to complete vaporization and it refers to the amount of deposit formed.

(7) Water content: this test is done by distillation and indicates the amount of water emulsified in the oil.

(8) Fuel contaminants: this test indicates the amount of fuel diluting in the lubricating oil during operation (Awaja & Pavel, 2016).

2.2.6 Impacts of used Lubricating Oil

The contaminants in used oil have adverse environmental and health impacts. The presence of degraded additives, contaminants, and by-products of degradation render waste oils more toxic and harmful to health and environment than virgin base oils. If put into storm water drains or sewers, they can affect waterways and coastal waters. When dumped in soil or sent to landfill, they can migrate into ground and surface waters though numerous land treatment processes. In addition, uncontrolled used oils are a threat to plant and animal life, which can further result in economic losses, i.e. recreation and fishing industries. For example, used oil from internal combustion engines generally accumulates a variety of contaminants which increase the oil’s toxicity (Diphare et al., 2013).

Improper use of old oil for a variety of traditional applications results in a variety of environmental and health consequences. Table 2 shows some of the local applications of altered oil, as well as their direct and indirect negative impacts (Nwachukwu et al., 2012).

According to the EPA, one quart of used oil can render one million gallons of water unfit to drink. When used oil enters surface water, oil films will block sunlight, impair  aquatic lives.

These contaminants not only cause issues when they are released into the environment due to poor management, but they can also obstruct used oil recycling. They are also discovered to be concentrated in the waste streams of reprocessing or re-refining operations at times, which can lead to additional disposal issues (Yang, 2008).

2.3 Used Oil Recycling and Reuse

There have been numerous efforts to recycle spent lubricating oils because they are such a valuable resource. Water is removed from used lubricating oil in a dehydration process at "re-refineries." Vacuum distillation separates impurities from spent oil, such as industrial fuel, and the oil is captured. This produces a large amount of oil-filled trash, oil additives and byproducts.

remove other contaminants, the extracted lubricating oil is refined. The oil is refined and then divided into three viscosities for various applications.

For the past four decades, lubricating oil has being reused. In the year 1930, the concept of repurposing leftover lubricating oil was proposed. Used lubricating oils were burned to generate energy at first, and then these oils were treated and re-blended into engine oils. The disposal and recycling of waste oils has become extremely significant as a result of the growing need for environmental protection and stricter environmental legislation. The three basic ways for reusing spent lubricating lubricants are as follows: incineration, reprocessing, and re-refining.

Incineration or combustion of used oil can be used to eliminate it thermally. Only a small amount of used oil is currently burnt due to the economic benefits of recycling it. Incinerated used oil typically contains high levels of harmful pollutants, making recycling impractical or dangerous (Diphare et al., 2013).

Reprocessing technology allows waste oil to be treated and burned in order to recover energy. It entails removing water and particles from old oil so that it can be burned as a fuel to create heat or power industrial processes. Because the oil may only be reused once, this type of recycling is not as preferable as systems that reuse the material.

Nonetheless, it is one of the economically attractive ways of managing used oil providing    valuable energy i.e. about the same as provided by normal heating oil (Chia-Yu, 2008). A litre of used oil re-processed as fuel contains about 8,000 Kcal of energy, which is enough energy to light a 100 W bulb for one day or to operate a 1000W electric heater for 2 hrs. (Nwachukwu et al., 2012). Compared to direct burning, the major advantage from reprocessing used oil is that it improves the burning quality of used oil by removing/reducing some contaminants (Isah, 2013) Used oil can also be re-refined back into base lube oil. Lube oil is a premium substance that can be re-refined and reused again and again. In general, water and dissolved low boiling point organic are removed by atmospheric or moderate vacuum distillation. Lube oil is then recovered using different treatments and/ or unit operations. Light end by-products are commonly used for plant combustion fuels. After further enhanced treatment, the diesel and gas oil fractions can be recovered as high-quality by-products. The asphalt industry can employ the residual streams from distillation as an asphalt flux to make roofing asphalt, paving asphalt, insulating materials, and other asphalt-based goods. Re- refining involves treating used oil to remove impurities so that it can be used as a base stock for new lubricating oil. Rerefining prolongs the life of the oil resource indefinitely. This form of recycling is the preferred option because it closes the recycling loop by reusing the oil to make the same product that it was when it started out, and therefore uses less energy and less virgin oil (Diphare et al., 2013)

2.3.1 Importance of Used Oil Recycling and Reuse

Used oil is unquestionably an important energy source. Oil does not degrade with use; it simply becomes dirty. Utilized oil can be refined into basic lube oil, recycled into fuel oil, or used as a feedstock for the production of petroleum-based products or other commercially valuable products using a variety of ways. Some facts about conserving resources through correct treatment of old oil are available. Refining old oil uses about a third of the energy required to refine crude oil to lubricant quality, and one gallon of re-refined lubricating oil yields the same 2.5 quarts of lubricant oil as 42 gallons of crude oil. As a result, collecting and recycling used oil not only preserves our environment from pollution, but it also saves a valuable resource.

Recycling old oil effectively saves a valuable, non-renewable resource from the standpoint of energy conservation. Only one barrel of crude oil is converted into virgin lube stock for every 70 barrels of crude oil produced. Many oil corporations invest billions of dollars in the exploration, recovery, and refinement of crude oil into high-quality lubricant oil.used oil generated by consumers can be recycled into valuable items like pure lubricating oil over and over again, time and money can be saved significantly. Our natural resources will be preserved, which is even more vital. Because of the huge quantities produced globally, the possibility for direct re-use, reprocessing, and regeneration, and the negative consequences on the environment if not properly managed, treated, or disposed of, the management of spent oil is extremely significant. Recycling used lubricants could have both environmental and financial benefits (Yang, 2008).

2.4 RECOVERY METHODS

The need to treat used engine oil for possible reuse has arisen due to concern for the environment, scarcity, price stability, and increasing dependence on this product for many industrial applications. Various methods of recovering used oil include;

         ·       Solvent Extraction

         ·       Acid/clay treatment method,

         ·       Vacuum Distillation,

         ·        Membrane technology,

         ·       Acetic Acid Treatment

         ·       Formic Acid Treatment

The characteristics of the fresh, used, and treated oil are tested for specific gravity, viscosity index, flash point, pour point and concentrations of heavy metals (aluminum, iron, and lead). 

2.4.1 SOLVENT EXTRACTION METHODS

Solvent extraction has been used to recycle spent oil but has its own disadvantages. The oil produced from this process caused huge loss of solvent, and requires highly skilled operating maintenance. In addition, extraction is conducted at higher pressures (greater than 10 atm.) therefore requires high pressure sealing systems which makes solvent extraction plants expensive to construct (Hopmans, 2014). Later propane extraction was invented.  Propane is capable of dissolving waxy/paraffinic material and intermediately dissolved oxygenated material (www.astm.org.,n.d.). Materials like asphaltenes which contain heavy aromatic compounds are not soluble in the liquid propane. These properties tend to make propane ideal for recycling the waste/used engine oil, but there are many other issues that have to be considered such as propane is hazardous and very flammable therefore it was regarded as a hazardous process (Hamawand,2015).  

2.4.3 MEMBRANE TECHNOLOGY

Another method used for regeneration lubricating oils was membrane technology. Three types of polymer fiber membranes [polyether sulphone (PES), polyvinylidene fluoride PVDF), and polyacrylonitrile (PAN)] were used for recycling the used/waste engine oils.  This process is carried out at 0.1 MPa pressure and 40°C (Martins, 2017) and is a continuous operation which removes metal particles or dusts from used/waste engine oil and also improves the recovered oils liquidity as well as flash point. Despite the above-mentioned advantages, the expensive membranes may get damaged and fouled by large particles (Henry, 2015).

2.4.4 ACID TREATMENT PROCESS

 Acid treatment is one of the popular treatment methods for re-refining used oil. It involves the use of acetic acid or formic acid respectively in the treatment of waste oil. The advantage of using the acetic acid is that it does not react or only reacts slightly with base oils. The recycling process takes place at room temperature or at most 40C. It has been shown that base oils and oils’ additives are slightly affected by the acetic acid.

This process of recycling of used engine oil does not emit poisonous gases like sulfur dioxide to the atmosphere. In addition, glacial acetic acid has less of a negative impact on the processing equipment compared with sulfuric acid used in acid clay treatment process or other treatment processes.


Fig. 2.1 Block diagram of recycling of used engine oil 

CHAPTER THREE

MATERIALS AND METHODS

3.1Materials

3.1.1 Experimental Materials

(i) Used Engine Oil

(ii) Fresh Engine Oil

3.1.2 Equipment Used

        1.     Thermometer

        2.     Solvent extractor

        3.     Round bottom flask

        4.     Measuring cylinder

        5.     Desiccator

        6.      Clock

        7.      Beakers

        8.     Hot plate

         9.     Decanter

3.1.3 Reagents

(i) Acetic Acid

(ii) Distilled water

3.2 Methods

3.2.1 Material Preparation

The used engine oil was collected from various mechanic workshops within the worldbank Housing Estate New Owerri Imo State. The used engine oil collected were used by private and commercial vehicles. All the chemical reagents and solvents used in this project work were of analytical grade, and were used without further purifications.

The regeneration of the used engine oil experiment was carried out at the New Concept Laboratory Obinze. The characterization  of the engine oil was done in the laboratory

3.2.2 Experimental Procedures

i.        Sedimentation /Decantation

At the end of the acid treatment step, the acidic oil will be allowed to settle 24 hours to form sediment at the bottom of the beaker. After this period, the acidic-oil will  properly sediment and decanted into another 500 ml beaker using piece of cloth while the residue (acidic sludge) at the bottom of the beaker is discarded.

ii.       Bleaching

The acidic oil in the beaker is subjected to bleaching. The oil is placed on a regulator hot plate and the temperature was maintained at a temperature of 110°C. 6 wt% of activated bleaching earth is  introduced into the oil and the mixture is continuously stirred for 15 minutes. At the end of the bleaching step, the bleached oil is neutralized.

iii.     Neutralization

The bleached oil is neutralized to adjust the pH of the oil to neutrality. At this step, 4 wt% of the oil of sodium hydroxide was introduced into the bleached oil by taken into consideration the pH of the bleached oil at a given point in time. The bleached oil was neutralized with a continuous manual stirring for 10 minutes. At the end of the bleaching and neutralization steps, the oil is allowed to sediment in the beaker for 24 hours and is decanted into the beaker, while the residue at the bottom of beaker is discarded. 

iv.      Filtration

The sediment oil is finally filtered using a filter cloth and the filtrate is collected in a filtration flask and it is observed to be clear while, the residue (filter cake) will be discarded.

CHAPTER FOUR

RESULTS AND DISCUSSION

4.1 RESULTS

This chapter contains all the results obtained from the experiment carried out in the course of this study. The results of the research which investigates the recycling of used Engine oil and compared with the fresh Engine oil sample using acetic and formic acid treatment have been carefully detailed in Table I. The Table I also includes the results of the various quality tests (appearance, viscosities at 55°C, flash point, specific gravity and pour point) performed using ASTM methods on the lubricating oil products.

 

Table 4.1: Summary of Analysis of Results  

 

Tests

Units

Test Methods

Specifications

Fresh Oil

Used Oil

Acetic Acid Clay Treatment Method

Formic Acid Clay Treatment Method

Appearance

Visual

Bright and Clear

Dark

Dark

Dark

Dark

Dark

Flash Point

(⁰C)

ASTM-D0092

Min.200

220

170

200

200

 Viscosity, 55⁰C

 

(mPa.s)

ASTM-D0445

As Reported

604-610

627

607.15

606.65

 

(Cst mm²/s)

ASTM-D0445

12.5-16.3

13.70

11.42

13.95

14.16

 

(Cst mm²/s)

Calculated

 

134

125

139

138

 

(Mg KOH/g)

ISO 3771

7.00-12

 

11.66

7.23

7.67

Specific Gravity

Kg/m^3

ASTM-D1298

 

0.881

0.8855

0.855

0.877

Pour Point

⁰C

ASTM-D1298

 

4

13

5

6

 

 

 

 

 



 

Fig. 4.1: Effects of recycling used engine oil on its specific gravity

 


Fig. 4.2: Effects of the recycling of used engine oil on its viscosity at 55°C

  


 

Fig. 4.3: Effects of the recycling of used engine oil on its pour point

 

DISCUSSION

4.2 Discussion

The discussion of the results obtained from the recycling experiment was done with emphasis laid on the various basic properties of the oil which includes the appearance, flashpoint, viscosity, specific gravity, density and pour point.

i.         Appearance: This indicates the brightness and clarity of petroleum products. The results of the appearance (Table 1) of the fresh lube oil, used lube oil and the treated lube oil show that the fresh oil have a clear and bright color while the used and the treated lube oil have a dark appearance. The dark appearance of the used lube oil and those from the treated methods were due to their combustion and oxidation at high temperature by the combustion engine for a very long time.

ii.       Flash Point: The flash point of lubricating oil is the lowest temperature where it will evaporate enough fluid or vapor to form a combustible concentration of gas with air that can be ignited spontaneously by a specified flame. In summary, flash point indicates how easily lubricating oil may burn and ignite (Udonne, 2016). The result of the flash point of the fresh lube oil, used lube oil and the treated lube oil above shows that, there was a decrease in the flashpoint for the used lubricating oil which is below the minimum specification of flashpoint for SAE-40 lube oils. The decrease in the flashpoint of the used lube oil was due to contamination of very volatile component. On treating, the volatile components were extracted from the used lube oil. Thereby increasing the flash point above the minimum specification of SAE-40 except the Citric acid clay treatment method.  From the experiment carried out the flash point using acetic  acid  and formic acid treatment is 200°C.

iii.     Viscosity at 55°C: The results (Table 1) of the Kinematic Viscosities (KV) at 40°C using the ASTM-D 0092 Method shows that the used oil sample with Kinematic Viscosity (KV) of  600mPa.s and  using acetic and formic acid we have 606.65mPa.s and 607.15mpa.s. The plot of kinematic viscosities of each of the recycled lube oils (Fig. 2) reveals that they all fell within the required specification range (Brinkman et al., 1981). This shows that at 55°C, the recycled methods still retained the viscosity specification range (604- 610mPa.s) for SAE 50 oils.

 

iv.      Specific gravity/density: The specific gravity of contaminated or used lube oil could be lower or higher than that of its fresh lube oil depending on the type of contaminates in the used oil. If the used lube oil is contaminated by dilution of light oil/volatile component or contaminated due to fuel dilution and/or water originating from fuel combustion in the engine and accidental contamination by rain, its specific gravity will be lower than that of its fresh lube oil (Udonne, 2016). But, on the other hand when the specific gravity of the used oil is greater than that of the fresh lube oil, then the lube oil may have been contaminated by heavy oil or component with a higher carbon atom. The results for the fresh and used lubricating oils are 0.881 and 0.8855, respectively. This shows that the used lube oil may have been contaminated by dilution of light oil. It is also very likely that some of the heavier components of the lube oil had broken down to lighter fractions at the high operating engine temperature. After undergoing different treatments by the various methods, the volatile components were extracted which consequently increased the specific density of the recycled oil obtained using acetic acid is  0.855 and that  of formic acid is 0.877. The plots are shown in Fig. 4.1

 

v.        Pour Point: Pour point is the lowest temperature at which the oil will flow. Low pour point indicates good lubricating oil. From the experiment carried out the

pour point of engine oil using acetic and formic acid is 5°C and 6°C respectively 

CHAPTER FIVE 

CONCLUSION AND RECOMMENDATION 

 5.1 CONCLUSION

This research has shown that used lubricating oil can be effectively recycled using acetic acid treatment and formic acid. The results show that there were contaminants of light oil/ a very volatile components present in the used oil and it was shown that the two methods used removed the volatile contaminants from the used lubricating oil and removed the oil to a quality essentially equivalent to fresh lube oils. Furthermore, this new process of recycling used engine oil does not emit poisonous gases like sulfur dioxide to the atmosphere. It is contemplated that, it will cost less to buy the used oil and it has been proved to yield about 80% while the yield from crude oil is between 5 to 10% (udonne,2015). The recycling of used  oil will greatly decrease the rate at which it has polluted the environment and it will also reduce the demand for lubricant rich crude which is a dwindling and finite resource. In addition, organic acid has less of a negative impact on the processing equipment compared with inorganic acid like sulfuric acid. Lower number of additives may be required for the base oil recycled by acetic acid method due its low reactivity with the used oil. Further research is required in order to take this process to the commercial stage.

5.2 RECOMMENDATIONS

The following strategies are recommended for follow up whilst working on this project:

 

i.        The general public should be sensitized on the danger of the used Engine oil on human health, thus the process of recycling used oil should be encouraged in order to save our environment from indiscriminate disposal of the used lube oil. In addition, Further research is required in order to take this process to the commercial stage.

ii.       As a chemical engineer, I will strongly recommend that the acetic acid treatment method should be encouraged because it is less expensive to operate and it is safe for both equipment’s and labour. Also, to achieve a better result, the regenerated spent engine oil should be heated to a higher temperature before the adsorption process.

 

iii.     However, while few variables have been studied in this research, there are many others that need thorough investigation such as pressure, settling time, mixing speed & time and type & size of adsorbent which have significant effects on the recycled oil qualities. In addition, the aforementioned aspects are important concerning the general characteristics of the treatment and recycling of used oil.

 

iv.     Also, a detailed cost benefit analysis evaluation should be made that will likens the potential benefits of used oil recycling with the expected costs of construction and erection of the scaled-up plant.

 

v.        Further character testing may also be executed to evaluate oxidation stability, thermal stability and foaming character of the recycled oil. Possible practical application of the recovered oil in a real engine system should be experimented on.

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APPENDICES 

Fig. 2.1 Block diagram of recycling of used engine oil

 

Fig 4.2 Effects of recycling used engine oil on its specific gravity

 

Fig. 4.3: Effects of used engine oil on its viscosity at 55◦C

 

 

Fig. 4.4: Effects of used engine oil on its pour point



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