INDUSTRIAL ATTACHMENT REPORT

BY

DONGONDA ZVIKOMBORERO

FACULTY: ENGINEERING

DEPARTMENT: CHEMICAL ENGINEERING

STUDENT NUMBER: N0188161W

COMPANY NAME: VERIFY ENGINEERING

INDUSTRIAL SUPERVISOR: ENG T. GOTOZA

ACADEMIC SUPERVISOR: MR L. L MGUNI

ACADEMIC YEAR: 2021/22

This report was submitted in partial fulfilment of the requirements of the Bachelor of
Engineering (Honours) Degree in Chemical Engineering.

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DEDICATION

I dedicate this report to myself for being strong and not giving up in working through all the
harsh conditions and high temperature sections, my family for their love and never ending
support, fellow interns and Verify Engineering staff for they were the impulse behind my
positive determination and their immense support. The experience gave me more motivation
and the diversity of engineering applications in the production industry.

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ACKNOWLEDGEMENTS

I would like to thank my industrial supervisor Eng T. Gotoza for not only mentoring me but
also for giving me guidance with experience for the hands-on job and application of my
knowledge from the institution. I appreciate the help that I got from all section heads and
artisans that I worked with for they gave me a chance to learn and give ideas on problem
solving.

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ABSTRACT

This report provides a concise and vivid account of the student’s experience gained during the
time spent on Verify Engineering premises, 25 km from Mutare CBD in Manicaland. It is
intended to establish that this experience meets the objectives of Bachelor of Engineering
Honours Degree Chemical Engineering. Verify Engineering is a production company which
specialises in producing high grade industrial and medical gases with qualities that conform to
Good Manufacturing Practices and Medical Control Authority Zimbabwe guidelines.
Cryogenic distillation method is used for producing nitrogen and oxygen in a fractionating
column. Verify Engineering is also working on completing installations on the Acetylene plant
and other projects include Coal-to-Fertilizer and Silicon Nanoparticle project. In this report,
familiarization of the machines and equipment used in the production of industrial and medical
gases from the initial production stage to the point where the gaseous and liquid products are
filled is covered. Also, the maintenance measures taken to keep the machines’ efficiency at
optimum levels and activities carried by the student is covered.

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TABLE OF CONTENTS

DEDICATION I

ACKNOWLEDGEMENTS II

ABSTRACT III

LIST OF FIGURES VII

LIST OF TABLES IX

LIST OF ABBREVIATIONS X

CHAPTER 1: INTRODUCTORY CHAPTER 1

1.1 INTRODUCTION 1
1.2 COMPANY BACKGROUND 1
1.3 COMPANY LOCATION 1
1.5 MISSION 2
1.6 CORE VALUES 2
1.7 ORGANISATIONAL STRUCTURE 3
1.7 PRODUCT AND MARKET 3
1.8 TRAINING PROGRAM 4

CHAPTER 2: DEPARTMENTS/ SERVICES DESCRIPTION 5

2.1 INTRODUCTION 5
2.2 SHEQ 5
2.2.1 ROUTINE TASKS 5
2.3 CLINIC 5
2.4 ADMINISTRATION 6
2.4.1 ROUTINE TASKS 6
2.4.2 NON-ROUTINE TASKS 6
2.5 LOGISTICS 6
2.5.1 ROUTINE TASKS 6
2.6 FINANCE 7
2.6.1 ROUTINE TASKS 7
2.7 ICT 7

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2.7.1 ROUTINE TASKS 7
2.8 ELECTRICAL AND INSTRUMENTS 8
2.8.1 ROUTINE TASK 8
2.9 CIVILS AND DRAWING 8
2.10 MECHANICAL 8
2.11 CHEMICAL SERVICES 9
2.11.1 ROUTINE TASKS 9
2.12 PRODUCTION 9
2.12.1 ROUTINE TASKS 9

CHAPTER 3: PROCESS DESCRIPTION 10

3.1 INTRODUCTION 10
3.2 BLOCK FLOW DIAGRAM 10
3.3 RAW MATERIAL AND QUALITY 11
3.4 PROCESS DESCRIPTION 12
3.4.1 AIR COMPRESSION 12
3.4.2 THE PROCESS SKID (AIR COOLING AND PURIFICATION) 12
3.4.3 AIR COOLING 13
3.4.4 CRYOGENIC FRACTIONAL DISTILLATION 13
3.5 FILLING STATION 14
3.6 PROCESS PARAMETERS, MONITORING AND CONTROL 14

CHAPTER 4: ACETYLENE PRODUCTION 15

4.1 INTRODUCTION 15
4.2 RAW MATERIALS 15
4.2.1 WATER 16
4.2.2 CALCIUM CARBIDE 16
4.3 UNIT OPERATIONS 16
4.3.1 REACTION INSIDE THE CALCIUM CARBIDE GENERATOR 16
4.3.2 COOLER CONDENSER 17
4.3.3 LOW PRESSURE DRIER 17
4.3.4 AMMONIA SCRUBBER 18

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4.3.5 ACETYLENE COMPRESSOR 18
4.3.6 HIGH PRESSURE DRIER 18
4.4 FILLING STATION 18
4.5 PROCESS PARAMETER, MONITORING AND CONTROL 18
4.6 SAFETY PRECAUTIONS AND MEASURES 19

CHAPTER 5: EQUIPMENT DESCRIPTION AND PRODUCT STORAGE 20

5.1 INTRODUCTION 20
5.2 COMPRESSOR 20
5.3 HEAT EXCHANGER 21
5.4 PROCESS SKID 21
5.5 COLD BOX 22
5.6 EXPANSION ENGINE 23
5.7 LIQUID OXYGEN PUMP 24
5.8 COOLING TOWER 25
5.9 CYLINDER VESSELS 25
5.10 PRODUCT STORAGE 26
5.10.1 GOX 26
5.10.2 LOX 27
5.10.3 LIN AND GAN 27

CHAPTER 6: INTERNSHIP ACTIVITIES 28

6.1 INTRODUCTION 28
6.2 RESEARCH ON MODIFICATION OF COAL TAR USING SINPS 28
6.2.1 THE DESTRUCTIVE DISTILLATION OF COAL 28
6.2.2 METHODS FOR COAL TAR MODIFICATION 28
6.2.2.1 ADDITION OF POLYVINYL CHLORIDE (PVC) 29
6.2.2.2 PREPARATION OF LOW TEMPERATURE COAL TAR ASPHALT 29
6.2.2.3 ADDITION OF SILICON NANOPARTICLES (SINPS) 29
6.3 STANDARD OPERATING PROCEDURE 31
6.3.1 SOP FOR LOX EXPORT FROM BATCH TANK TO MAIN STORAGE TANK 32
6.4 FACTORY PERFOMANCE REPORT 32

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6.5 CYLINDER STORAGE 33
6.6 PLANT OPERATION 33
6.7 OTHER ACTIVITIES 33

CHAPTER 7: CONCLUSION AND RECOMMENDATION 34

7.1 INTRODUCTION 34
7.2 CONCLUSION 34
7.3 RECOMMENDATIONS 34

REFERENCES 36

APPENDIX 37

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LIST OF FIGURES

Fig 1.1: Verify Engineering’ organisational structure……………………………………..3

Fig 3.1: ASU block flow diagram…………………………………………………………10
Fig 3.2: Process flow diagram for ASU…………………………………………………...11
Fig 3.3: Industrial oxygen cylinders connected to the manifold…………………………..14
Fig 4.1: BFD for acetylene production………………………………………………….....15
Fig 4.2: PFD for VE’s acetylene plant……………………………………………………..17
Fig 5.1: Kirloskar type four-stage compressor……………………………………………..20
Fig 5.2: ASU process skid………………………………………………………………….21
Fig 5.3: The cold box……………………………………………………………………….22
Fig 5.4: Unit 1 expansion engine…………………………………………………………...23
Fig 5.5: RTF circular cooling tower………………………………………………………..24
Fig 6.1: BFD for production of SINPs……………………………………………………..29

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LIST OF TABLES

Table 1.1: Training program………………………………………………….4

Table 3.1: Components of air and abundance………………………………..12
Table 5.1: Color-codes for cylinders…………………………………………25
Table 5.2: Cylinder size and capacity………………………………………...26
Table 6.1: Comparison of coal tar modification methods…………………....30

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LIST OF ABBREVIATIONS

ASU Air separation unit

BFD Block flow diagram
GAN Gaseous nitrogen
GOX Gaseous oxygen
ID Inner diameter
LIN Liquid nitrogen
LOX Liquid nitrogen
MSB Molecular sieve battery
SHEQ Safety health environment and quality
VE Verify engineering

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 CHAPTER 1: INTRODUCTORY CHAPTER

1.1 INTRODUCTION

The author of this report served as a process engineering intern at Verify Engineering. The
whole purpose of this training was to cognize the student on the working environment,
adamantly expose her to an industrial setup and present to her, a platform to practise various
requisite skills and attitude of process engineers. The author provides an in-depth
understanding of the Oxygen plants at Verify Engineering and the content of this report serves
to relate several aspects of the plant with which the author interacted during her industrial work.
From routine task to non-routine tasks, down to numerical plant specifics and specifications.
This chapter gives and insight on the company background, geographical location, vision,
mission statement and its core values. It also covers the organisational structure, company’s
line of business as well as the products handled at large.

1.2 COMPANY BACKGROUND

Verify Engineering (Pvt) Ltd is a grant aided wholly Government owned private limited
company, formed in April 2005 and is under the patronage of the Ministry of Higher and
Tertiary Education, Science and Technology Development. At establishment, the company was
mandated to implement the Coal-to-Liquid Fuels and Chemicals project. It has now been given
an extended mandate which is in line with the vision of the Ministry to focus on heritage-based
science and technology innovations in order to help turn around the country’s economic
fortunes. Verify Engineering is a vehicle that aims at contributing to the broader national
industrialization agenda through commercialization of various technologies.

1.3 COMPANY LOCATION

Verify Engineering is located on the Feruka plot about 25km West of Mutare CBD.

1.4 VISION STATEMENT

Industrialisation through heritage based Science and Technology Development by year 2025
and to be the supreme producer and supplier of gases and related products in Africa.

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1.5 MISSION

‘Through our valued and innovative employees, we shall a customer centric engagement
process to create permanent links and business specific technological solutions for wealth
creation by availing superior, safe and environmentally friendly gases related products and
services which enhance perceptions and above all return on investment to our valued
shareholders’

1.6 CORE VALUES

Safety The safety of our customers, stakeholders and employees is our priority.
Innovation Creativity is a key pillar to the successful implementation of VE
Projects.
Integrity The organisation and individual employees commit to be morally
astute, honest and upright in all transactions.
Engagement Committed to interaction and exchange of ideas with our stakeholders
in order to generate valuable solutions.
Accountability We commit ourselves to account for our activities, accept responsibility
for them and disclose results in a transparent manner.

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1.7 ORGANISATIONAL STRUCTURE

Ministry of Higher & Tertiary

Education, Science &Technology
Development

Board of Directors

Chief Executive Officer

General Manager Technical Audit & Company Secretary

Technical Services Administration Quality Assurance &Legal Corporate Commercial Director
Manager Manager Affairs VE Gases

Engineering
Manager Site Administrator Internal Audit Marketing & Sales
Production Plant Officer Manager

Electrical &
Instruments Site Administrator Production
Manager SHEQ Officer Manager
Mine Site

Technical Services
Manager Finance & IT
Manager

Chemical Services
Manager

Production
Manager

Mining Manager

Fig 1.1: Verify Engineering’s organisational structure

1.7 PRODUCT AND MARKET

Our final products are liquid oxygen, gaseous oxygen, liquid nitrogen and gaseous nitrogen
depending on the plant’s production mode and we sell these to Hospitals, food processing and
cattle breeding industry and steel making industries. Acetylene is another product that will soon
be on the market once the plant has been commissioned.

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1.8 TRAINING PROGRAM

The student’s industrial experience was made easy by the industrial supervisor, through
management, who prepared an all-encompassing training program.

Table 1.1: Training Program

Section Period (weeks)

Department familiarisation 2
Process Description(ASU & Acetylene plant) 2
Water supply system 1
Process air compression 2
Process air purification(process skid) 2
Air separation (cold box) 2
Product storage 2
Product dispatch 2
Management training 2
Projects and plant maintenance Whole period
Reports and presentations Whole period

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 CHAPTER 2: DEPARTMENTS/ SERVICES DESCRIPTION

2.1 INTRODUCTION

The sole purpose of this chapter is to familiarise the reader with all of Verify Engineering’s
departments and how they inter-link to fulfil the company’s vision and achieve its goals.

2.2 SHEQ

This department is responsible for giving daily SHEQ training to employees before resuming
plant operations. Issues out hazard identification and risk assessment forms to be done on a
daily basis before beginning work. It is mandatory that the SHEQ personnel deal with all issues
regarding safety and health of workers. Initiates buying of protective personal clothing (PPC)
based on the PPC matrix, a document (preparation still in progress) which matches the job
description and the PPC required and risks likely to occur and ensures that workers comply
with the safety and health regulations as required.

2.2.1 Routine tasks

 Plant visits
 Product quality control if the plant is running. (Works together with the chemical
services department to ensure that the required expectations are met)
 Update workers on new regulations if there any
 Filing of incidents and accidents and also recording in the FG1 register as required by
NSSA
 Investigates causes of incidents and accidents that take occur at the workplace.
SHEQ department also reviews on the standard working conditions and operations to see if
they concur with the Standard Association of Zimbabwe.

2.3 CLINIC

This department works hand in hand with SHEQ to ensure that workers are physically, mentally
and psychologically fit for work. Manages health complaints and deals with emergent treatment
of injuries by addressing what they can deal with at a local level. Prescribes medication to
workers and refer them to other hospitals but due to the absence of the license they are not

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allowed to dispense drugs to patients. Maintaining ethics yields respect from co-workers hence
medical duties are subject to confidentiality.

2.4 ADMINISTRATION

The administration department is responsible for overseeing that all other departments follow
the standard operation procedures adopted by the owner of the company. It is the duty of the
administrator to supervise other staff and delegate responsibilities.
2.4.1 Routine tasks
 Ensures that all paperwork is well kept and up to date i.e. leave forms, contract forms
etc.
 Keep records and reports up to date
 Hiring of new staff
 Distribution of payslips to workers.
2.4.2 Non-routine tasks
 Arrange and schedule meetings or events for the company.

2.5 LOGISTICS

Due to space limitation on Feruka grounds, the logistics team share the same office with the
administration team. The main duty of this department is to ensure that each department has
the materials required to make progress. The logistics department is responsible for managing
the outgoing and incoming of goods, tracking product delivery to depots and making sure that
they are delivered. They also plan delivery timetables, manages the ordering and packaging of
goods.
2.5.1 Routine Tasks

 Carry out quotations for required goods

 Keeps records of goods in store
 Provision of PPC to workers and ensuring that they sign for it.

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2.6 FINANCE

This department is responsible for receiving funds of the organisation and mobilising them on
behalf of other departments. All issues involving funds is accounted for by the Finance
department and since Verify Engineering uses government funds, accountability is their main
responsibility. When a request has been made for certain goods and the quotations have been
done by the logistics department, the finance crew then carries out an analysis of those
quotations, verifies and approve the quotations followed by goods purchasing. Also responsible
for keeping customer’s purchase orders and abiding to the rules that govern the purchase orders.
In case the customer fails to purchase some of the goods mentioned in the purchase order, the
supplier is rightfully in a position to sue the customer and the opposite is true if the supplier
fails to provide some of the goods as per the purchase order.

2.6.1 Routine tasks

 Prepares sales schedule

 Checks quotations and approves quotations
 Making payments for Canteen and Indian groceries
 Keeps the petty cash book up to date
 Entering goods records in the goods received voucher (GRV)
 Keeping records of power consumption at the plant.

2.7 ICT

This department focuses on maintenance of computer systems, hardware and software

included. It is their responsibility to monitor network services, keep in touch with our network
service provider, Powertel, and report to them if there are challenges faced. Communication
with Powertel is very vital in order to keep the network up and running and eliminate problems
if there are any.
2.7.1 Routine tasks

 Configuration of emails to persons

 Keeps the asset register for ICT equipment up to date
 Carry out graphic design tasks assigned to him

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  Prepares performance reports, weekly and monthly reports for the department
 Keeps records of the internet downtime log-sheet
 Connects staff to the internet.

2.8 ELECTRICAL AND INSTRUMENTS

It is mandatory for this department to ensure availability of required electrical appliances in

other departments. Raise awareness of the hazards associated with the use of electrical gadgets
especially in the plant. This team also does installation of electrical equipment, instruments and
maintenance of faulty equipment together with calibration of instruments.

2.8.1 Routine task

 Switching breakers for plant start-up

 Substation maintenance (Weeding) and ensuring no unauthorised personnel enters
 Hourly logging of solar power exportation to the main grid
 Calibration of instruments and maintenance.

2.9 CIVILS AND DRAWING

This department deals with solving the civil needs of workers through site visits, assessment
and site establishment in order to provide habitable infrastructure. Their sole responsibility is
to design plans for construction of factory, buildings and plants by starting with drawing plans
of where the plant will be sited, considering various factors such as proximity to water sources
and pipeline positioning. It is their duty to make sure that large and heavy equipment such as
the cold box, compressor units are properly mount on to the ground and also note that the
vibration of one unit does not affect the next unit. Maintenance of infrastructure and roads is
also a duty for this department and upon request, members of this department are expected to
produce drawings.

2.10 MECHANICAL

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System maintenance of equipment in relation to mechanics is the duty of the mechanical
department. Servicing of equipment and repair is also their responsibility hence there are no
routine tasks for this department because they deal with every problem as it rises.

2.11 CHEMICAL SERVICES

The chemical department deals with quality control, quality assurance, research and
development.

2.11.1 Routine Tasks

 Testing for oxygen purity and quality

 Keeping records of purity tests
 Keeping track of oxygen shelf life.
Non-routine tasks include preparation of chemicals when they are needed, carrying out research
and development when instructed to by the management.

2.12 PRODUCTION

The production team is responsible for monitoring and operating the plants, ensuring smooth
flow of air from the point it is sucked into the compressor to the moment where oxygen reaches
the filling station. This department is made up of plant operators and process engineers capable
of dealing with problems as they arise during plan operation.

2.12.1 Routine tasks

 Monitoring of valves and gauges.

 Maintenance of process parameters.
 Use online analysers to check if operating specifications are met.
 Daily recording of plant performance.
 House-keeping of the plant to avoid silly incidents caused by misplacement of tools and
equipment.

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 CHAPTER 3: PROCESS DESCRIPTION

3.1 INTRODUCTION

This chapter gives a comprehensive outline of VE Air Separation Unit (ASU) from raw
material acquisition to the final products. A detailed description of the stages involved in ASU
is given as well as the block flow diagram and the process flow diagrams to provide a vivid
understanding of the unit operations and equipment used.

3.2 BLOCK FLOW DIAGRAM

The Block flow diagram summarises the unit operations that occur in the ASU.

Atmospheric air Air Compression

Process Skid
(Air Cooling and
purification)

Air Cooling

Nitrogen to Skid

Fractional Gaseous Product to

Distillation of Air Filling Station

Fig 3.1: ASU block flow diagram

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Fig 3.2: Process flow diagram for ASU

3.3 RAW MATERIAL AND QUALITY

The only raw material used by ASU is atmospheric air at room temperature and pressure and
the table below summarises the components found in air and their respective abundance.

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Table 3.1: Components of air and abundance

Component Abundance (%)

Oxygen 20.9
Nitrogen 78
Carbon Dioxide 0.04
Rare Gases <0.01
Carbon Monoxide Trace
Ammonia Trace

3.4 PROCESS DESCRIPTION

The ASU produces liquid oxygen and nitrogen, gaseous oxygen and nitrogen through fractional
distillation of air. During operation, process air undergoes a number of unit operations i.e. air
compression, air purification, air cooling and fractional distillation.

3.4.1 Air Compression

Atmospheric air is drawn into the dust filter for removal of impurities such as dust, leaves and
any other smaller particles. Air is compressed in a four-stage compressor. Suction valves
located below compressor number 1 suck air from the dust filter into the compressor where it
is compressed to about 1.2 bars. The discharge valves discharge air from compressor 1 into
the shell and tube heat exchanger, heat exchange is effectively achieved by a counter-current
flow between air and water. Air flows inside copper tubes whilst water is inside the shell of the
heat exchanger. There’s a subsequent increase in pressure from 1.2 bars in compressor 1 as air
is compressed to about 45 bars in compressor 4 and the size of compressor decreases following
number of stages. From stages one to three, each contain a heat exchanger for cooling of air
and a moisture absorber is installed on each stage for removal of moisture from process air.
From the fourth stage process air flows to the process skid made up of the after-cooler, cascade
cooler, chilling unit, moisture separator, oil absorber and molecular sieve battery.

3.4.2 The Process Skid (Air Cooling and Purification)

Hot process air from compressor enters the after-cooler wrapped inside copper coils to prevent
it from mixing with water. Inside the moisture separator, moisture is removed from process
air using gravity to force moisture to settle at the bottom and the condensed moisture is drained
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once in an hour. Process air flows into the cascade cooler filled water, dry nitrogen is bubbled
into water to become wet gas thereby simultaneously cooling the water in the tank and process
air inside the copper coils. Process air is passed through an oil absorber packed with alumina
balls where oil carried in the air is removed by absorption to prevent damage to sieves. Carbon
dioxide, hydrocarbons and moisture are removed from air inside the molecular sieve batteries
to prevent choking of the heat exchangers inside the cold box. The driers operate one at a time
to allow regeneration of the one drier as the other one is under operation. Dry air is filtered
inside the dust filter prior entry to the cold box. The air is further cooled through special coils
in the chilling unit which equalizes the temperature after the molecular sieve drier before
process air enters the cold box.

3.4.3 Air cooling

Compressed air with a temperature range of 100c-200c free from moisture and carbon dioxide
enters the cold box. Inside the first heat exchanger, process air inside copper coils is cooled to
about -1000c by outgoing oxygen inside copper coils and nitrogen in the shell. The cooling
agents flow in a direction counter current to the direction of flow of process air. 60% of this
cooled air flows directly to the expansion engine at a pressure of about 45 bars where it is
expanded during the downward stroke of the piston and discharged during the upward stroke
through the outlet valve at a pressure of 5.5 bars. The remaining 40% passes on to the second
heat exchanger where it is cooled to about -1700c and it flows to the expansion valve, V3, where
it is expanded when the valve is slightly opened. Process air leaving expansion valve is around
5.5 bars and it combines with process air from the expansion engine inside the sub-cooler
before entering the fractionating column.

3.4.4 Cryogenic Fractional distillation

Process air entering the lower column partly condenses into liquid and falls at the bottom of
the column (rich liquid), nitrogen which is more volatile rises to the top of the lower column
where it is cooled and collected inside the condenser pockets(poor liquid). The rich liquid flows
into the middle of the upper column where nitrogen evaporates leaving oxygen. The poor liquid
enters the top of the column and as if flows it is contacted with evaporating oxygen thus
condensing and nitrogen turns into a gas as it is more volatile. Gaseous nitrogen is piped out
from the top of the column through heat exchangers. Liquid oxygen at the bottom is carried to

13
the LOX pump from which it is compressed and again passed through the heat exchangers to
the filling station.

3.5 FILLING STATION

This is the place where oxygen and nitrogen cylinders are filled. Liquid oxygen is withdrawn
from the condenser and it flows to the pump where it is compressed automatically into a gas.

Fig 3.3: Industrial oxygen cylinders connected to the filling manifold

For filling, the cylinder are carried to the filling station where they’re connected to the manifold
as shown above.

3.6 PROCESS PARAMETERS, MONITORING AND CONTROL

Operational parameters need to be within optimum hence a number of valves and sensors are
monitored and adjusted accordingly in order to maintain process parameters. Pressure gauges
and liquid level gauges have to be calibrated periodically to obtain true readings. On each plant,
an operator is stationed and their duty is to monitor operational parameters, take down readings
and record them in log-sheets.

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 CHAPTER 4: ACETYLENE PRODUCTION

4.1 INTRODUCTION

In this chapter, VE’s acetylene production process is covered, details of the raw materials used
and their acquisitions are also given. Bearing in mind that acetylene gas is a highly flammable
gas with a garlic-like odour when its concentration is between 2.5%-100% in air, it is important
to keep acetylene out of air and vice versa. The stages used in acetylene production are outlined
as well as a block flow diagram.

Low pressure
Cooler condenser
drier

Generator Purifier
Water

Granulated calcium
carbide
Ammonia
scrubber
Acetylene to filling
station

Acetylene High pressure

compressor drier

Fig 4.1: BFD for Acetylene production

4.2 RAW MATERIALS

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4.2.1 Water

Verify Engineering uses Pungwe water supplied by Mutare city council. It draws this water
from Mutare Prison which is about 10 kilometres away from Feruka site straight into a reservoir
with a capacity of 200 000 litres. This reservoir feeds water to the Air Separation Unit,
Acetylene plant and the ablution block. Pressure of water ranges between 1.6 to 2.2bars. The
water used on the plant is of the city council’s grade and currently there are no water treatment
schemes implemented on site for effective removal of hard elements and other impurities. If
by any chance the water quality is deemed inappropriate for use, the Quality Assurance
department is responsible for taking corrective action.

4.2.2 Calcium Carbide

Granulated calcium carbide used is imported from overseas.

4.3 UNIT OPERATIONS

4.3.1 Reaction inside the calcium carbide generator

The acetylene plant at Verify Engineering uses the calcium carbide generator method to
produce acetylene which is quite a simple method in which calcium carbide reacts
exothermically with water producing acetylene and lime. Since the reaction generates a lot of
heat, this heat needs to be eliminated to stop acetylene from exploding. This chemical reaction
process involves variations that require either addition of calcium carbide to water or water is
added to calcium carbide. Both processes are known as wet processes because excess water is
used for containing heat of the reaction. The equation below summarises the reaction.

CaC2 (s) + 2H2O (l) Ca (OH)2 (aq) + C2H2 (g) ΔH = - 32.5 kcals ….(1)

The generator is filled with water up to a maximum of 6000L and is provided with two valves
to check high and low level positions. Calcium carbide is charged into an air tight hopper at
the ground level then it is lifted by a chain pulley and transferred to a hopper permanently
mounted at the top. Calcium carbide reacts with water producing acetylene and lime.

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Fig 4.2: PFD for VE’s Acetylene plant

The process flow diagram above gives a pictorial view of the acetylene plant and when coupled
together with an insight of the process description helps the reader understand

4.3.2 Cooler condenser

Acetylene gas leaving the generator is hot and laden with moisture and other impurities. The
condenser cools the gas thereby condensing the excessive moisture. Cooling water is circulated
on the shell side from bottom to top and acetylene gas on the tube side from top to bottom. The
condensate is collected at the bottom and is drained periodically.

4.3.3 Low pressure drier

This is a vertical cylinder vessel charged with anhydrous calcium chloride. This absorbs the
gas moisture. The gas leaving the drier should not be entirely dry as further purification is
dependent on the wetness of the gas. After the low pressure drier the product is purified by
removal of hydrogen and phosgene.

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4.3.4 Ammonia Scrubber

From the purifier acetylene is passed on to the ammonia scrubber which has a level gauge and
water make up line to keep water level maintained at all times. Acetylene gas is bubbled into
the vessel so that water soluble impurities like ammonia will be scrubbed

4.3.5 Acetylene compressor

This is a 3 stage compressor operating at 393 rpm and has cooling pipes immersed in water to
prevent pressurized acetylene contact with air and to continuously cool the components.

4.3.6 High pressure drier

It acts the same way as the low pressure drier except that it consists of 3 columns. Moisture is
collected at the bottom and is drained periodically.

4.4 FILLING STATION

The acetylene gas filling manifold consists of two headers, each having provision for fitting 60
cylinders at a time. Each header is individually fitted with two non-return valves. One flash
back arrestor, gauge and manual isolation valve.

4.5 PROCESS PARAMETER, MONITORING AND CONTROL

The temperature of the generator can be maintained by proper control of the carbide and
cooling water fed to the generator. 10.0 L/kg of carbide will maintain the temperature constant.
This can be monitored by the water controls and the number of hoppers of carbide being fed.
If the temperature is continuously below the set point, some acetylene will remain dissolved in
the water and may be discharged through the drain leading to lower yield so an optimum
temperature of 65°C shall be maintained. The temperature is maintained by an ON/OFF screw
feed and a high temperature alarm is used to alert extremes in temperature. Liquid level in the
generator needs a close control, if the level is above normal, water overflows to the carbide
hoppers and can cause an explosion. At the same time, the space required for gas generation
inside the generator reduces and the yield of gas will increase. Similarly, if the level is below
normal, the temperature of the generator is bound to increase rapidly. The level is controlled
by a level controller mounted at one end of the generator. The calcium carbide should be kept
dry at all times and not exposed to air to avoid extraction of air to form acetylene.

18
4.6 SAFETY PRECAUTIONS AND MEASURES

 Plant operators and any personnel with access to the plant must wear the relevant
protective clothing before entering the plant.
 The use of any naked flame, sparking devices or open electric wiring within the plant
room is prohibited to minimize risk of initiating a massive explosion.
 The use of silver for brazing in the plant area and metal containing more than 70%
copper should be avoided.

19
 CHAPTER 5: EQUIPMENT DESCRIPTION AND PRODUCT STORAGE

5.1 INTRODUCTION

This chapter gives a detailed explanation of the equipment that the student mastered in the ASU
for manufacturing LOX, GOX, LIN and GIN. The equipment are defined and their function is
also mentioned in this chapter, product storage is also covered in this section.

5.2 COMPRESSOR

The two types of compressors used by VE are Kiloskar and Super Freeze both of which are 4-
stage centrifugal compressors with the former being more efficient. Since each compressor is
made of a combination of cast steel and mild steel, these compressors each weigh about 1.5
tonnes hence they’re properly mount onto the steel mesh-reinforced concrete slab to withstand
high pressure exerted on the slab by the compressor.

Fig 5.1: Kirloskar type four-stage compressor

The figure above shows a compressor with a dust filter into which air is withdrawn from the
atmosphere through a suction air filter which has a high rotating fan pulling the air inwards.

20
Air is compressed inside these 4-stage compressor which subsequently increase in pressure
from stage 1 to the last as compressor size decreases and there exists inter-stage coolers (heat
exchangers) between the compression stages. These centrifugal compressors are capable of
holding 1000 m3/hr of air and a 475 HP electric motor converts electrical energy into
mechanical energy to drive the compressors.

5.3 HEAT EXCHANGER

Shell and tube heat exchangers are the common heat exchangers used by VE for cooling
process air together with cooling towers for cooling water. The outer casing of the heat
exchangers is made of mild steel and the tubes running inside it are made of copper. Inside
these vessel, water on the shell side flows counter current to process air on the tube side thereby
achieving efficient cooling of process air.

5.4 PROCESS SKID

The skid is made up of a number of units which include the after cooler, moisture separator,
cascade cooler, chilling unit, oil absorber and molecular sieve battery as shown below.

Fig 5.2: ASU process skid

The after cooler is a cylindrical vessel which has a supply pipe and a return pipe which brings
water into the after cooler. The cascade cooler is a cubical vessel with inter-connected pipe

21
coils submerged in water. In order to achieve effective removal of oil from process air, the oil
absorber is packed with alumina balls which are removed and changed every 6-12 months.

Each vessel of the MSB is filled with 1.5mm molecular sieves, type 13-X and activated alumina
material for efficient absorption of carbon dioxide, hydrocarbons and water vapour. MSB can
handle air quantity up-to 2000m3/hr and the absorbing capacity of MSB drops rapidly if process
air is warm. The molecular sieves should be replaced if they become powder, if they get
contaminated by oil or if they lose their absorption capacity. As one MSB is under operation
for 10 hours the other will undergo regeneration for the exact time. Regeneration of MSB is
achieved by passing hot nitrogen through the sieves, this is done to release the captured
impurities from the molecular sieves in preparation for the next operation.

5.5 COLD BOX

Fig 5.3: The Cold Box

The cold box shown in Fig 5.3 has primary functions which include housing all cryogenic
equipment and its piping from outside atmosphere and heat loads, providing a vacuum
environment and provide control and access to the equipment located inside it. The cold box
inner casing is covered with perlite for insulation. The outer casing of the cold box is made of

22
mild steel, enclosed inside are the heat exchangers, condenser unit and the distillation column.
The outer casing for the heat exchangers inside the cold box is made of mild steel with fluid
transporting tubes made of copper for improved heat conduction. The type of heat exchanger
used is the shell and tube heat exchanger. The condenser inside the cold box is made of stainless
steel. The distillation column is made of a top column and a bottom column both at different
pressures, the upper column separates air at a pressure of about 0.5 bars and the bottom column
at a pressure between 5.5-6.0 bars.

5.6 EXPANSION ENGINE

This is a vertical dry type, single acting reciprocating type of engine which produces the cold
required for operating the plant. Its drive unit is similar to any reciprocating machine with usual
parts such as the crank case, crank shaft connecting rod, crosshead etc. The expansion engine
has an extended crankshaft to enable cam accommodation for valve fittings and is housed by a
cam box and the moving parts are lubricated through a hole in a crank shaft. Oil scrapper rings
are provided to prevent oil escape to cylinder unit. The cylinder unit handling process air
consists of cylinder, piston, inlet and outlet isolation valves, pressure gauges and the ball valve
assemblies. The ball valves are actuated mechanically by a push rod as per the timing
transmitted by the came. The push rods are housed in a stuffing box to avoid air leakage. The
hydraulic system is the control system for the expansion engine. The inlet and outlet ball valves
should be maintained properly for efficient performance the expansion engine.

23
Fig 5.4: Unit 1 expansion engine

5.7 LIQUID OXYGEN PUMP

The LOX pump is a single stage, single acting piston pump used for filling oxygen into
cylinders up-to a pressure of 175bars. The cylinder diameter is 42mm and each stroke is 125mm
with the pump operating at 125/150 rpm. The LOX pump consists of a stainless steel inside
liner with liquid inlet and evaporated gas outlet port.

24
5.8 COOLING TOWER

Fig 5.5: RTF circular cooling tower

An RTF circular tower shown above is a type of direct contact heat exchanger designed to cool
water whilst dissipating heat to the atmosphere. Warm water continuously drops down the
cooling tower contacting and upward mass of air thus exchanging heat with the air and this
type of cooling is termed evaporative as some water droplets are also evaporated upon
dissipation of heat to the atmosphere. Fiberglass reinforced plastic fins inside the cooling tower
allows for counter current cooling and their power consumption is minimum.

5.9 CYLINDER VESSELS

These are storage vessels used for storing gaseous oxygen, nitrogen or acetylene at pressures
between 150-200 bars and they are internationally color-coded to prevent mixing of products.
The cylinders are made of aluminium of starting stock cast 6061 and have a Teflon ring placed
inside the o-gland forming a seal between the cylinder and the valve.
Acetylene cylinders are a bit different from oxygen and nitrogen cylinders since they store a
very unstable and explosive gas acetylene. 10% of the cylinder’s size contain a porous

25
monolithic mass which prevents presence of internal voids that can possibly cause
decomposition and it acts as a flame arrestor if any were to develop. 42% of the cylinder is
filled with acetone, a solvent in which acetylene dissolves, this provides even distribution of
acetylene and its stabilization. A small gap is left inside the cylinder to allow for expansion.
The table below shows the type of gases stored and their respective color-codes.
Table 5.1: Color-codes for cylinders
Type of gaseous product Cylinder color-codes
Industrial oxygen Black
Medical oxygen Black with white collar
Nitrogen Grey
Acetylene Brown

5.10 PRODUCT STORAGE

In this section, key emphasis is on the filling and storage of GOX, LIN, LOX.
5.10.1 Gox

The cold box produces liquid oxygen which is then pumped and converted to gas and
immediately pumped to the filling station on the manifold. The filling pressure for cylinders
should be at 175bars. Cylinders are transferred from the empty cylinders’ storage area to the
filling manifold. The cylinders’ valves are opened, the cylinders are arranged on the manifold
and the filling hoses connected. All the cylinders are filled simultaneously and when the
pressure of 175bars is achieved the filling valve is closed and the other section of the filling
manifold opened. The filled cylinders are carried out to the designated site for filled cylinders
(as a shed for storing the cylinders is still work in progress) and arranged according to batch
number. Medical and industrial cylinders should be filled separately as they have different
storage sites. Also the cylinders of different sizes are stored at different places.

The table below shows the size of storage cylinders and the amount of product they can store
when filled at 175bars and with purity of not less than 99.5%.

26
Table 5.2: Cylinder size and capacity
Volume of cylinder (L) Mass of product (Kg)
20 4.5
46.7 10.6
50.1 11.7
60.0 13.4

5.10.2 Lox

During LOX production mode, the product is stored in the batch tanks. The plant has 3 units,
each with its own batch tank of 5 cubic metres in size. Then there is a main storage tank of size
120 cubic metres which is connected to all the batch tanks. The batch tank has a capacity of
5,651kg for oxygen whereas the main storage tank has a capacity of 136,000kg. In accordance
to Good Manufacturing Practice, the batch tanks are used to store only oxygen. Ideally when a
batch is full and product is certified to be of required specifications, it is then exported to the
main tank.

5.10.3 Lin and Gan

As of now LIN is not being stored in batch tanks or cylinders. Work is in progress to erect a
storage tank and build a manifold for filling nitrogen. Upon request, LIN is filled into flasks
capable of carrying 30kg of LIN.

27
 CHAPTER 6: INTERNSHIP ACTIVITIES

6.1 INTRODUCTION

This chapter explains in detail the activities and tasks performed from the day the internship
began noting the key areas that were focused on ton aid with the learning process. All the tasks
that were carried out at Verify Engineering are specified in this chapter under supervision of
the company supervisor and other employees who were involved in overseeing the tasks.

6.2 RESEARCH ON MODIFICATION OF COAL TAR USING SINPs

Coal tar, a black or dark brown viscous fluid of hydrocarbons and free carbon is the most
commonly used road binder in Zimbabwe and its produced from the destructive distillation of
coal residues from local industries. Its excellent resistance to corrosive chemicals has made it
a better option for this use however various studies undertaken proved that tar alone has a
number of problems such as high bleeding at high temperatures causing roads to become slick
and slippery. It also has a low tensile strength resulting in fracture and failure of binder. In
order to improve this a number of methods can be used to modify tar so as to prevent the above
mentioned problems and lower its viscosity.

6.2.1 The Destructive Distillation of coal

This is a chemical process whereby unprocessed coal is decomposed by heating it to a high

temperature in the absence of air. Coal is fed into a distillation unit which is subjected to intense
heating, the more volatile products migrate upwards and out into a collection unit filled with
water. These products include ammonia, coal tar and coal gas (hydrogen, carbon monoxide and
methane). Coal tar which is denser than water settles at the bottom of the collector as a black
viscous fluid with a pungent smell and is used to manufacture various industrial products such
as dies, explosives, roofing materials and as a road sealant. Coal gas being the lightest lies on
top of water and is a fuel of high calorific value. Ammonia is absorbed by water forming
ammoniacal liquor for making fertilizer. A black residue that remains at the bottom of the
distillation unit is coke and is the main source of carbon, also used as a reducing agent in the
extraction of metals.

6.2.2 Methods for coal tar modification

28
6.2.2.1 Addition of polyvinyl chloride (PVC)

This method has been successfully used to improve durability of coal tar pitch over the past
years and not only does it improve tar but also helps to reduce the problems of environmental
issues of plastic waste. Incorporation of the additive onto the coal tar pitch occurs in two
pyrolysis stages. In the first stage, pyrolysis of polyvinyl chloride occurs at 200 producing
hydrochloric acid and polyene (De-HCL PVC). The produced hydrochloric acid produced
decomposes to protons and chlorine. Above 350, polyene is used up in an aromatization
reaction resulting in the production of large, highly active aromatic compounds which
chemically interact with aromatic compounds in coal tar pitch. Despite its improvement in
mechanical properties this method has been banned as it was deemed not environmentally
friendly due to emission of toxic vapours which are irritants to the eyes and respiratory system
if inhaled. The formation of rubbery deposits inside the binder distributer also made spraying
difficult and when exposed to ultra-violet radiation and elevated temperatures, this tar formed
a viscous melt resulting in bleeding.

6.2.2.2 Preparation of low temperature coal tar asphalt

Naphthalene components in asphalt easily separate at low temperatures making coal tar asphalt
liable to cracking. In order to eliminate this problem, molten coal tar asphalt is mixed with raw
materials 1, 2 and 3 defined by the following

 Coking solvent oil, anthracene oil, styrene butadiene styrene block copolymer, waste
rubber powder, regenerated rubber, chloroprene, rubber, butadiene styrene rubber,
ethylene propylene rubber, polyvinyl chloride and polystyrene making up raw material
1.
 Sulphur, thiazoles and octadecanamide class compounds making up raw material 2.
 Trimethyl diphenoquinone (TMDQ), isopropyl phenylenediamine (IPPD) and phenyl-
alphanaphthylamine making up raw material 3.
The resulting coal tar asphalt produced displays improved anti-aging performance, elementary
composition, chemical structure and colloid structure of the low temperature coal tar asphalt.
Also the resultant has excellent ductility, plasticity and no pollution and the method of
modification is very cost effective due to its low energy consumption.

6.2.2.3 Addition of silicon nanoparticles (SiNPs)

29
The use of silicon nanoparticles has attracted great attention in the past decades due to its
fascinating physical properties, active surface state, biocompatibility and characteristic
photoluminescence and economic availability.

Firstly silicon dioxide has to be extracted from natural chrysotile mineral through a number of
processes. Natural chrysotile mineral used is obtained from the old Shabani mine in
Zvishavane. The sequence of processes begin with pre-treatment of chrysotile by soaking in
distilled water to dissolve dirty particles stuck on the surface of chrysotile followed by washing
with distilled water. The cleaned mineral is subjected to drying for moisture removal purposes
then loaded into a milling unit where it is crushed into smaller segments and after screening,
the oversize is recycled back to the miller. Ground chrysotile is mixed with distilled water and
subjected to stirring at room temperature, the resultant is filtered and washed with distilled
water to get rid of form. The residue undergoes a leaching process with hydrochloric acid as
the solvent at room temperature and pressure followed by centrifugation at 5000 revolutions
per minute. This product being the silicon nanoparticle containing composite is washed with
distilled water, dried and then added to molten coal tar for blending in a simple batch reactor
to produce modified coal tar. The block flow diagram below represents the whole processes
involved.

Demineralized
water MANUFACTURE OF SiNP

Underflow
Mixer screen <0.25mm
Chrysotile
Overflow>0.2
5mm
Demineralized
Ball mill leaching water
2M HCl

Vacuum
washing dryer
filter

Excess HCl in
Filtrate water SiNP
Fig 6.1: BFD for production of SINPs

30
The above method is advantageous in a number of ways the first one being that it is cost
effective since chrysotile to be used is obtained from a mineral waste dump lying idle in
Zvishavane and operations are carried out at room temperature and pressure. SINPs also play
an important role in increasing the tensile strength of the tar, strength increases with increasing
composition of SiNPs used. The compressive strength of tar is also improved and the chances
of bleeding at high temperatures are minimized.

Table 6.1: Comparison of coal tar modification methods

Method Advantages Disadvantages

Preparation of PVC modified coal tar
Preparation of low temperature coal
tar asphalt
Preparation of SiNPs modified coal
tar.
 Improves mechanical  Rubbery deposits inside the
properties of coal tar pitch binder distributor makes
 Reduces environmental spraying difficult.
waste  Bleeding at high
temperatures releasing toxic
fumes.
 Process is economical  Durability decreases upon
 Improves anti-aging exposure to UV light and
performance of coal tar higher temperatures.
pitch.
 Coal tar asphalt produced
has improved mechanical
properties.
 Improves mechanical
properties of coal tar.
 Most economical
modification method
(considerably cheap).
 Reduces tar toxicity

A comparison of the methods described above leaves coal tar modification using SiNPs as the
best solution.

6.3 STANDARD OPERATING PROCEDURE

These are a set of prescribed methods to be followed routinely or no-routinely when performing
a certain task in a workplace. These are prepared in order to familiarise plant operators with
the safest working procedures, provide a way of achieving maximum production and reduce
risk factors to a minimum.

31
6.3.1 SOP for LOX export from batch tank to main storage tank

The student prepared this SOP with the help of a fellow intern as the task was assigned to them
as a duo. It describes a procedure for exporting LOX from a 5m3 batch tank to a 120m3 main
storage tank through a vacuum line with ID 50mm. The scope of this SOP was to specify the
proper way for exporting LOX from a batch tank to the main storage tank (Refer to appendix
A).

Other SOPs prepared by the student include procedures for exporting LOX from main storage
to 25 ton LOX trailer and exporting LOX from one batch tank to another.

6.4 FACTORY PERFOMANCE REPORT

This is a short but detailed report produced on a daily basis for as long as the plant is running,
it outlines the plant’s production, utility consumption, product storage, product dispatch and
performance indicators. The key performance indicators for each plant include product purity
read off the portable oxygen analyser, plant availability, LOX and GOX production rates and
oil consumption etc. Preparation included daily visits to the plant to read off batch tank
readings, logbook readings. This information is generated by an excel workbook and the final
FPR is reproduced as a PDF (Refer to appendix B). Enlisted below is a list of formulas used in
the calculations.

number of active hours

plant availability = ………………………………………………. (1)
24 hours

amount of LOX produced (kg)

LOX production rate = ………………………………………. (2)
number of active hours

A similar equation can be used for calculating GOX production rate.

L amount of oil (L)

Oil consumption(ton) = amount of LOX (kg)⁄ ……………………………………….. (3)
1000

32
6.5 CYLINDER STORAGE

This task was carried out in order to determine a better layout for temporary storage of cylinders
whilst the shade is being constructed. Special attention was on whether the cylinders were filled
or empty and on the type of product the cylinder stores. Factors such as distance from the
driveway, filling manifold, ASU, proximity to the electric distribution board and cylinder sizes
were considered. The designed layout proposed that filled cylinders were to be separated from
empty cylinders, the same goes for medical oxygen and industrial oxygen cylinders.

6.6 PLANT OPERATION

As a routine task for anyone in the production department, the student took part in operating
the plant during day shifts. Works done include plant start-up and shutdown, oil top up in
compressors crank-case and expansion engine, emergency shutdown of plant equipment in
response to an immediate problem, MSB heating and cooling, monitoring operating
parameters, exporting LOX from batch tank to main storage tank or to another batch tank,
filling nitrogen flasks and filling within-spec GOX into cylinders at the required pressure of
between 150-200 bars. Operating parameters were checked at the top of every hour and
readings were entered in a log-sheet, if any parameter was to fall out of range the log-sheets
made it easier for identification. All these, the student managed to exercise under the
supervision of plant operators and her industrial supervisor.

6.7 OTHER ACTIVITIES

Besides the common routine tasks prepared for the student, non-routine tasks emerged during
the attachment period which required immediate action and these include

 Physical count of cylinders on site to determine the actual amount of product stored on
site versus the recorded figure followed by preparing the report for that exercise.
 Cylinder tagging and sealing in preparation for dispatch of product to clients.
 Daily visits to acetylene plant to keep track of piping and equipment installations prior
commissioning of the plant.
 Pressure and purity testing of filled cylinders using pressure gauges and portable
analysers respectively.

33
 CHAPTER 7: CONCLUSION AND RECOMMENDATIONS

7.1 INTRODUCTION

This chapter gives a conclusion to the whole report, recommendations and suggestions on how
to maintain or redo certain tasks that will optimize the operation of the ASU.

7.2 CONCLUSION

The whole attachment period successively bridged the gap between theoretical knowledge
attained from school and industrial experience. The student was pleased to have had a chance
to make acquaintance with different people with great expertise in their respective industrial
posts. She feels confident and content knowing that the attachment period was not only fun but
also beneficial and it gave her a sense of belonging to the engineering firm. Routine tasks and
non-routine tasks that the student encountered at VE include preparation of factory
performance reports, starting up of ASU and its operation, preparation of standard operating
procedures in relation to production and researching on modification of coal tar using SINPs.
Weekly attending of management coordination meetings improved the student’s presentation
skills as well as good time management.

7.3 RECOMMENDATIONS

 NUST institution and other national institutions should continue to work and support
good relations with Verify Engineering organisation because of its ability to provide
students with a quality learning platform which helps them to identify their strengths in
the industry, to achieve their dream goals in the future and specifically in Engineering
department, projects which are pursued by the company have greater impact for both
country development and opportunity sustainability for our developing country.
 The best way for the students to develop and adapt in the industrial world is when they
have learnt relevant stuff related to the ever-growing industry whilst still at the
university therefore I recommend that NUST should add more current stuff to the
learning curriculum so that students feel more connected to the real world and the
changing technology.
 Verify engineering as an organisation should arrange trips for students so that they can
familiarise with other VE depots.

34
 In-sync with the oil project carried out by the students, a 3-compartment oil interceptor
which uses the working principles of dense medium separation should be used as a
primary storage for oil drained off from the ASU.

35
 REFERENCES

BOC, 2017. Facts about acetylene. In: s.l.:BOC: A member of the Linde group, pp. 1-7.
Boschi.A, L. &., 2007. Oxygen nitrogen plant, Manual UB 500 oxygen plant. India : s.n.
Engineering, V., 2007. Acetylene gas manufacturing plant. Harare: s.n.
L, K., 2014. Analysis of steady state cryogenic air separation unit of rourkela steel plant and
simulation of fixed bed adsorption separation of air., Legos: s.n.
P, Z., 2011. Environmental management ACT. In: Harare: s.n., p. Chapter 27.

36
 APPENDIX

A: SOP for LOX export from batch tank to main storage tank
Purpose
To describe a procedure for exporting LOX from a batch tank to the main storage tank. This
SOP uses Plant number 1 for reference.

Scope
This procedure specifies the proper way for exporting LOX from batch tank to the main storage
tank at VE gases, Feruka, Mutare.

Responsibility
Production shall have the primary responsibility of preparing the batch/product.

Production shall also have the responsibility of preparing a procedure for LOX export from
batch tanks to the main storage tank which shall be properly followed by the process operators
on shift.

Definitions
Export in this case means withdrawal of LOX from the batch tank through a pipeline to the
main storage tank.

Shift refers to a work schedule that requires an employee to be on duty during a time other than
the traditional work day.

PROCESS INPUT
Process Engineers
Process Operators

Description of activities
Close V8 which feeds LOX to the batch tank.
Before export begins, the mainline supplying the main storage tank must be cleared.

Isolate pipelines which export LOX from Plant 1 batch tank to batch tanks on plant 2 and plant
3.

Open HCV-1, HCV-3 for bottom fill or HCV-2 HCV-4 for top fill and fully open HCV-12 to
vent out vapour from the main storage tank. Clearance of mainline successively achieved.
Open the liquid withdrawal valves, V13 and V21.

Open the priming valve to remove air from the pipeline which when left out may create airlocks
during export.

Switch on the pump electric board and prime up to -1200c until a liquid is visible on the priming
valve then close the valve.
Open the valve which feeds LOX to the main storage tank.

37
Start the pump at -1200c and allow for withdrawal of LOX to the required level.
Open the priming valve this time to get rid of excess LOX in the pipeline.
Close the valve feeding LOX to the main storage tank.
Stop the pump and then switch off the pump electric board.
Close V13 AND V21.
Open V8 if you wish to fill the batch tank.
Key performance indicators
Accurate recording of exported quantity and period of exportation.
Double checking system before resuming export.

Records generated
Logbook- records starting and finishing time for exportation and the initial and final liquid
levels read off the batch tank gauges before and after exportation. Liquid level readings
determine the amount of LOX exported.

References
Internally generated

38
B: Factory performance report template

39
 UNLOCKING VALUE FROM SECONDARY RESOURCES - UTILISATION

OF WASTE CORTUSA-100 FROM VE GASES’ AIR SEPARATION UNIT

INDUSTRIAL ATTACHMENT PROJECT BY

BY

DONGONDA ZVIKOMBORERO

N0188161W

FACULTY: ENGINEERING

DEPARTMENT: CHEMICAL ENGINEERING

INDUSTRIAL SUPERVISOR: ENG T. GOTOZA

ACADEMIC YEAR: 2021/22

This laboratory project was submitted in partial fulfilment of the requirements of the
Bachelor of Engineering (Honours) Degree in Chemical Engineering.
DEDICATION

I dedicate this project to Verify Engineering in gratitude for the time I worked for the
organisation and to my family for their unconditional love and never ending support.

i
ACKNOWLEDGMENTS

I would like to thank Verify Engineering’s staff for all the support provided during the course
of the project. Special thanks to Eng T. Gotoza, Mr Moyo and fellow interns for the advice,
fruitful discussions and the guidance they provided me.

ii
ABSTRACT

Waste lubrication oil is one of the hazardous wastes generated in different industrial sectors, it
should not be utilized and/or disposed in ways which are unsafe to the environment hence
calling for its proper management. This study primarily focuses on the recycling of used oil. It
investigates the extent to which sulphuric acid can be used to recover usable oil from waste
lube oil. VE Gases’ air separation unit loses nearly 12000L of waste oil per year of which this
oil can be recovered. Solvent extraction method with sulphuric acid and activated carbon was
used to recover oil from a 100ml sample of waste lube oil. A recoverability of 42% was
obtained when 20% v/v sulphuric acid was used together with 15% v/v carbon-oil ratio and the
density of the recovered sample was lower than that of virgin oil hence blending can be done.
The study proved that the acid treatment is a process that can effectively remove contaminants
from used lubricating oil. The recovered oil has acceptable qualities indicated by the quality
tests performed thus making it a better candidate for reuse in the manufacturing industry and
also as a fuel.

iii
TABLE OF CONTENTS

DEDICATION...........................................................................................................................I
ACKNOWLEDGMENTS ...................................................................................................... II
ABSTRACT ............................................................................................................................ III
LIST OF FIGURES ............................................................................................................... VI
LIST OF TABLES ................................................................................................................ VII

CHAPTER 1: INTRODUCTORY CHAPTER ..................................................................... 1

1.1 INTRODUCTION................................................................................................................ 1
1.2 AIM ...................................................................................................................................... 2
1.3 OBJECTIVES ...................................................................................................................... 2
1.4 PROBLEM STATEMENT .................................................................................................. 2
1.5 JUSTIFICATION ................................................................................................................. 3
1.6 TIMELINE ........................................................................................................................... 4

CHAPTER 2: LITERATURE REVIEW .............................................................................. 5

2.1 INTRODUCTION................................................................................................................ 5
2.2 WASTE LUBE OIL ............................................................................................................. 5
2.3 WASTE LUBE OIL COMPOSITION ................................................................................. 5
2.3.1 WATER CONTENT IN USED LUBE OIL. .................................................................................. 6
2.3.2 CHEMICAL CONTAMINANTS................................................................................................ 6
2.4 WASTE OIL MANAGEMENT OPTIONS ......................................................................... 6
2.5 RECYCLING METHODS ................................................................................................... 7
2.5.1 THE ACID-CLAY PROCESS ................................................................................................... 7
2.5.2 SOLVENT EXTRACTION METHOD ........................................................................................ 7
2.5.3 VACUUM DISTILLATION AND HYDROGENATION ................................................................. 8
2.5.4 GLACIAL ACETIC METHOD .................................................................................................. 8
2.5.5 MEMBRANE TECHNOLOGY ................................................................................................. 8
2.6 PROPERTIES OF LUBE OIL...................................................................................................... 9

CHAPTER 3: METHODOLOGY ....................................................................................... 11

iv
3.1 INTRODUCTION.............................................................................................................. 11
3.2 SAMPLING ....................................................................................................................... 11
3.3 MATERIALS AND REAGENTS ...................................................................................... 11
3.4 LABORATORY PROCEDURE ........................................................................................ 12
3.4.1 DEWATERING ................................................................................................................... 12
3.4.2 EXTRACTION USING SULPHURIC ACID. .............................................................................. 12
3.4.3 ADSORPTION PROCESS...................................................................................................... 13
3.4.5 ADSORPTION WITH ACTIVATED CARBON .......................................................................... 13
3.5 TEST FOR DENSITY ........................................................................................................ 14
3.6 SAFETY PRECAUTIONS ................................................................................................ 14

CHAPTER 4: RESULTS AND DISCUSSION ................................................................... 15

4.1 AMOUNT OF WATER AND LIGHT COMPONENTS IN WASTE OIL SAMPLE........ 15

4.2 EFFECTS OF DESLUDGING ........................................................................................... 15
4.3 EFFECTS OF ADSORBENT RATIO ............................................................................... 16
4.4 PHYSICAL CHARACTERISTICS OF RECOVERED LUBE OIL.................................. 17
4.5 PRELIMINARY COST ANALYSIS ................................................................................. 18

CHAPTER 5: CONCLUSION AND RECOMMENDATIONS ........................................ 21

5.1 CONCLUSION .................................................................................................................. 21

5.2 RECOMMENDATIONS ................................................................................................... 21
REFERENCES ....................................................................................................................... 23

v
LIST OF FIGURES

Fig 1.1: Timeline for the whole project…………………………………………4

Fig 2.1: Block diagram of reprocessing of used lubricating oil…………………7
Fig 3.1: Heating the sample with the help of a magnetic stirrer………………..12
Fig 3.2: Samples obtained after dewatering…………………………………….13
Fig 4.1: Colour changes after the experiment…………………………………..16
Fig 4.2: Comparison of lube oil properties……………………………………...18

vi
LIST OF TABLES

Table 4.1: Mass obtained before dewatering……………………..……………15

Table 4.2: Mass obtained after dewatering…………………………………....15
Table 4.3: Description of the oil sample……………………………………....16
Table 4.4: Results of the quality tests………………………………………....17
Table 4.5: Imported oil price and freight charge……………………………...19
Table 4.6: Material balance based on 1 litre product yield……………………20

vii
 CHAPTER 1: INTRODUCTORY CHAPTER

1.1 INTRODUCTION

Lubricating oil having good properties plays a vital role in terms of reduction in heat transfer,
minimize friction between moving parts (Shrie et al, 2013), improves efficiency of machinery
and helps save energy. Lubricants employed in automobile engines and compressors can be
deteriorated by different factors, such as operating conditions, quality of fuel and ambient
conditions (Kim, 2006). Waste lubricating oil is a resource that cannot be disposed of randomly
as it has the potential to cause detrimental effect on the environment due to the presence of
pollutants. In response to economic problems and environmental protection, there is a growing
trend to regenerate and reuse waste lubricant (V.B Kreng, 2011). The generation and
accumulation of waste oils is closely linked with an increase in population of automobiles and
industries.

During operation of the air separation unit, Cortusa 100 is used as lube oil for compressor
injector pump, expansion engine and other moving parts in the plant. The viscosity and density
of Cortusa 100 are the primary performance factors for lube oil and these decrease over time
due to the breakdown in the chemical structure of lube oil in response to heat stresses. Due to
the hygroscopic nature of oil, it extracts moisture from cooling water and it loses its lubricity
when there no longer is any functionality of the additives and the used oil turns black in colour
due to carbon from wears. A mixture of oil and other impurities which accumulate during plant
operation is periodically removed from the moisture separator and through the drainage pipes.
This is termed waste oil together with oil drained from the compressors after at least 5000
working hours of the air separation unit (Universal Boschi Compressor Manual) followed by
replacement with new oil. Addition of foreign substances and additives to lubricating oil later
on results in degrading, aging and failure leading to mechanical fault and degraded
performance of equipment. In such cases, the oil is replaced to improve equipment performance
and the waste oil should be collected and recycled not only to prevent environmental pollution
but to preserve natural resources (Fox, 2007).

Consequently, there are various methods which have been developed to reduce environmental
hazards associated with waste oil disposal and conserve valuable used oil which can be
recycled into base lube oil. Solvent extraction, an innovative adaptation of existing crude-oil

1
refining technology is being studied for its potential to recover lube oil. This research project
aims to determine the most suitable solvent for extracting lube oil from waste oil and assess
whether the physical properties of the recovered oil conforms with ASTM D112 test quality.

1.2 AIM

The purpose of this laboratory project is to find out the efficiency of recovering waste oil using
a solvent extraction method with sulphuric acid and activated carbon and the economic and
environmental impact of the process involved in the project.

1.3 OBJECTIVES

 To estimate the maximum amount of lube oil that can be recovered from waste oil
 To assess the physical properties of the recovered oil to see if it conforms to ASTM
D112 test quality.
 To analyse and compare the regenerative techniques for lube oil
 To perform an economic analysis on recycling used lubricant oil.

1.4 PROBLEM STATEMENT

Assuming that all 3 units of the air separation unit are operating on a yearly basis, VE Gases
loses about 12000L of oil as waste but if secondary measures are practiced thousands of dollars
can be saved and also the environment (factory performance reports, 2022, Compressor
Manual). The contaminants in waste oil have adverse environmental and health impacts (Lam
et al., 2016). 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 (L.
Andrews, 2008). Since lubricating oils have predefined usage period in which they provide
sufficient lubricity, delayed removal of degraded oil from the compressor increases friction
hence wear and tear of equipment leading to mechanical faults. It also results in overheating of
compressors thus crippling the cooling of process air which is a major drawback for production.
If put into storm water drains or sewers, they can clog waterways, and affect aquatic life. When
dumped in soil or landfills, they can migrate into ground and surface waters through numerous
land treatment processes. In addition, uncontrolled used oils are a threat to plant and animal
life, which can further result in economic losses, for example, recreation and fishing industries
(R.K Hewstone, 1994).

2
1.5 JUSTIFICATION

The justification is split into 3 parts: how it helps the company, how it helps the environment
and how it helps the student carrying out this research project.
 How it helps the company
As it stands VE Gases has around 1500litres of used lubricating oil lying idle on site. A close
study of the plants’ daily Factory Performance Report as shown below indicates that the
amount of waste oil has the capacity to increase at a rate of 1200litres/annum if all the ASU’s
three units are running. During plant operation, oil is added to the injector pump to provide
lubrication to the pistons and is vented periodically from the plant together with water and other
metal wear impurities i.e. Pb, Cu etc. The amount of oil added is about 12litres/day/unit
meaning the ASU has the capacity to lose approximately 9800litres/annum. Solvent extraction
is a cheap, environmentally friendly and economic way to utilize the oil that would otherwise
go to waste.

 How it helps the environment

VE Gases is also aiming to get ISO certification together with meeting GMP standards and
EMA requirements. With the world now more focused on green industrialization/economy this
is a good way to show that the company takes care of the environment. Successive
implementation of this project will also conform to the country’s NDS1 under environmental
protection, climate resilience and natural resource management with emphasis on sustainable
natural resource utilization and environment protection.

 How it helps the student

By carrying out this research project, the student gains adequate experience in research and
problem solving, decision making with regards to material selection, handling materials and
time management.

3
1.6 TIMELINE

Fig 1.1: Timeline for the whole project

4
 CHAPTER 2: LITERATURE REVIEW

2.1 INTRODUCTION

Over the years, the demand and consumption of petroleum based products has increased due
to depletion of easily accessible sources of petroleum and ever-increasing demand from
emerging economies (J. Motshumi et. al., 2013). Lubricating oils are derived from petroleum-
based and non-petroleum-synthesized chemical compounds. (Frankl, 2005). They are made up
from heavier and thicker petroleum hydrocarbon base stock which consists of hydrocarbons
with carbon range between 18 and 34 blended with additives to improve certain properties
(Beuther, 1989). One of the important properties of lubricant oil that defines its ability to
maintain a lubricating film between the moving parts is viscosity (Frankl, 2005). The viscosity
of a liquid is the measure of its resistance to flow; it must be high enough to provide a thick
lubricating film, but low enough to allow the oil to flow easily around the moving parts under
all conditions (Whisman & Reynolds, 1978). The viscosity of oil changes with temperature, a
measure of how much the viscosity of the oil changes as temperature changes is called viscosity
index. A higher viscosity index indicates the viscosity changes less with temperature than a
lower viscosity index (Georgia, 1990). Other important properties of the lubricant oil are
specific density, pour point, refractive index, total acid number carbon residual and flash point.

2.2 WASTE LUBE OIL

Used/ waste lube oil is defined as lubricant oil which remains after a certain period of useful
life (ASTM, 2004). When the lubricating oil is in use it degrades due to contamination with
metals, water, varnish, ash, gums, carbon residue and other contaminating materials (Whisman,
2002). Also waste oil is used up when there is no function of the additives thus leading to acid
neutralisation and the oil assumes it’s black colour due to carbon from wear As it is
contaminated with time, the lubricant oil loses its lubricating ability and therefore as a result
after a certain predefined useful time it is replaced with unused oil. The replaced oil is called
used/ waste lube oil (Georgia, 1990).

2.3 WASTE LUBE OIL COMPOSITION

A lubricating oil becomes unfit for further use for two main reasons; accumulation of
contaminants in the oil and chemical changes in the oil (Shakirullah & Ahmed, 2006). The

5
main contaminants include metals due to breakdown of additives in oil, water which leads to
sludge formation and rust (Rincon & Canizares, 2005). Others are soot and carbon that make
the oil go black, Lead (Tetraethyl lead) from bearing wear and is likely to be in the 2 - 12 ppm
range (Georgia, 1990).

2.3.1 Water content in used lube oil.

The amount of water found in used lubricating oil depends on the type of equipment in which
it is being used. In normal operating conditions traces of water arise from sources such as
leaking oil coolers, engine cooling system leaks, compressor pumps and crankcases and from
atmospheric condensation (Rincon & Canizares, 2005). The presence of excessive water will
affect the viscosity of the oil and give rise to emulsion formation (Henry, 2015).

In dewatering process the oil can be heated to 180°C and under atmospheric pressure for a
period of 1 hour to eliminate the free water and emulsified water. Since the boiling point of
water is 100°C at STP, temperatures above this point are usually practical, but at higher
temperatures above 200°C, light hydrocarbon fractions are lost and the water is contaminated
requiring thorough treatment (Whisman, 2002).

2.3.2 Chemical contaminants.

The common chemical contaminants mainly are oxidation products where by at an elevated
temperatures some of the molecules of the oil tend to oxidize forming complex and corrosive
organic acids (Georgia, 1990); other chemical contaminants are depleted additive remnants
(Kiss, 2011).

2.4 WASTE OIL MANAGEMENT OPTIONS

Although dumping and oil burning are practiced in most countries, these activities pose a great
threat to the environment thus they are not recommended proper ways to dispose oil (Fox,
2007). The recommended disposal options for waste oils may be one of the following;
regeneration of new base oil, thermal cracking and incineration/ use as fuel. A variety of
technologies has been invented for regeneration of used lube oil to produce various yields of
base oil stream, fuel by-products stream and the stream heavier of residue (Whisman &
Reynolds, 1978). Regeneration process creates fuel by-product streams (the lighter
components) that may be used as fuel and the obtained base oil is used as lubricant oil after

6
blending it with additives. The stream of heavier residues containing carbonaceous species, is
used as a blending component in the bitumen processing industry, for incorporation into
construction products such as road surfaces (Fox, 2007).

2.5 RECYCLING METHODS

2.5.1 The acid-clay process

Historically, the most successful technology for treating used oils is the acid-clay process
developed in Washington State (Hamawand, 2013). It is capable of producing good quality
lubrication stocks, but also produces large volumes of petroleum-contaminated acid-clay
sludge (Fox, 2007). The Resource Conservation and Recovery Act (RCRA) and later
legislation classified acid-clay sludge as a hazardous waste and required proper management
and disposal method (Martins, 1997). Consequently, the acid-clay process is classified as
uneconomic technology because of the high cost of managing residues and is no longer used.
(Hamawand, 2013).

Fig 2.1: Block diagram of reprocessing of used lubricating oil

2.5.2 Solvent extraction method

It produces base oil by improving the stability of the lube oil and improves viscosity -
temperature characteristics of base oils. The solvent dissolves undesired aromatic components,
leaving the desirable saturated hydrocarbon components especially alkanes as a distinguished

7
phase (Rincon & Canizares, 2005). Although the oil produced from this process is comparable
to that produced by the acid-clay method, extraction process causes huge losses of solvent, and
need highly skilled operating maintenance.

2.5.3 Vacuum distillation and hydrogenation

Vacuum distillation and hydrogenation is another method used for recycling used oil. The
Kinetics Technology International (KTI) proposed the combination of vacuum distillation and
hydro-finishing (Beuther, 1989). The process begins with atmospheric distillation to remove
light hydrocarbons and water followed by vacuum distillation at a temperature of 250°C and
finally hydrogenation of the distillation products to eliminate the nitrogen, sulphur and
oxygenated compounds. Also this process has been used for many years to improve the odour
and colour of the oil and produces the products of quality standard with a yield of
approximately 82% of the feed and minimized polluting by-products but it needs high
investment cost (Rincon & Canizares, 2005).

2.5.4 Glacial acetic method

Research shows that acetic acid is very useful for recycling used lubricant oils because it is
very powerful in dissolving and attracting polar contaminants, metal particles contaminants
from used oil (Kiss, 2011). The method has less process costs as compared to the conventional
methods because acetic acid is cheap. Lube oil recovered by this method was found to have a
great potential for reuse as an oil blend for engine lubricants (Rincon & Canizares, 2005). The
KIT research shows that, acetic acid extraction process for used/waste engine oil yields about
80 to 90 % (depending on the method used) of base lubricating. This is to say if the recycling
of the used lubricant oil is carefully handled with proper technology, the significant amount of
base oil will be recovered with relatively cheaper process thus producing high yield and good
quality lubricating oil base stock comparable to virgin lube oil base stock (Henry, 2015).

2.5.5 Membrane technology

Another method used for regenerating lubricating oils is membrane technology. It uses three
types of polymer fibre membranes i.e. polyethersulphone (PES), polyvinylidene fluoride
(PVDF), and polyacrylonitrile (PAN) to recycle waste oil. This process is carried out at 0.1
MPa pressure and 40°C (Martins, 1997) and is a continuous operation which removes metal
particles or dust from waste lube oil and also improves the recovered oil’s liquidity as well as

8
flash point. Despite the above mentioned advantages, the expensive membranes may get
damaged and fouled by large particles (Henry, 2015).

2.6 Properties of Lube Oil.

After all these regenerative technologies have been developed, according to American Standard
of Testing Materials (ASTM), a number of properties of the recovered oil should conform to
the standard test quality otherwise it is deemed unfit for reuse. These properties determine how
and where the oil is going to be used and the extent to which it can be used.

 Pour point.
Pour point of lube oil is simply defined as the lowest temperature at which the oil will remain
in a flowing state (Donald, 1897). The pour point of lube oil is highly affected by the oil’s
viscosity; oils with high value of viscosity are normally characterized with high pour points.

 Viscosity.
Viscosity of a fluid is the measure of its resistance to gradual deformation when shear stress is
applied. There are two related measures of fluid viscosity; Dynamic (or absolute) viscosity and
Kinematic viscosity. Viscosity is a state function of temperature, pressure and density in that,
viscosity varies inversely proportional to temperature. Viscosity testing always gives the
contamination information as is used to indicate the presence of contamination in used engine
oil. The oxidized products as well as polymerized products which are dissolved and suspended
will result in the increase of the oil’s viscosity, while the decrease in the viscosity of engine
oils will indicate the presence of fuel contamination (Diaz & Bernardo, 1996).

 Specific gravity
Specific gravity is the ratio of the mass of a fixed volume of substance to the mass of the same
volume of water which depends on the temperatures at which the mass of the sample and the
water are measured. Specific gravity is highly influenced by the chemical composition of the
lubricant. An increase in the amount of aromatic compounds in the lubricant results in an
increase in its specific gravity, while an increase in the saturated compounds results in a
decrease in the specific gravity (Shakirullah & Ahmed, 2006).

 Flash point

9
Flash point is the temperature above which a combustible liquid will give off sufficient vapour
to form a flammable mixture with air; this mixture should burn momentarily when a small
flame is applied under certain specific conditions. Because it indicates the temperature at which
a flammable vapour is produced, flash point is generally the most useful single index of fire
hazard potential.

 Viscosity index
Viscosity Index is strictly an empirical number which indicates the effect of variation in
temperature on viscosity. A high viscosity index indicates a small variation in viscosity of oil
with temperature, which means better protection of an engine that operates under vast
temperature variations. A high value of viscosity index also indicates the absence of aromatic
and volatile compounds hence good stability in its thermal properties and low temperature flow
behaviours (Singh & Gulati, 2008).

 Refractive index.
Refractive index (RI) is the ratio of the velocity of light in vacuum to the velocity of light in
substances at a specific temperature. The refractive index is used to provide the important
information about the composition of lubricant oils. Low values of refractive index indicate the
presence of more paraffin material while high values indicate the presence of more aromatic
compounds. It can also be used to estimate other physical prosperities such as molecular mass
(Riazi & Roomi, 2001).

 Water and sediments

Water is generally classified as a chemical contaminant when suspended in lubricant oils.
Based on different researches, it has been noted that water contamination of lube oil affects the
oil quality, condition and wear of equipment in service (Hamawand, 2013). The water content
in lube oil is dependent on oil composition, physicochemical properties, production technology
and the conditions of use and storage. Water created in engine oil is a result of: condensation
(humid air entering oil compartments), absorbing moisture directly from the air (oil is
hygroscopic), combustion (fuel combustion forms water which may enter the lubricant oil
through worn rings), heat exchanger (corroded or leaky heat exchangers), oxidation (chemical
reaction) and neutralization (when alkalinity improvers neutralize acids formed during
combustion), and free water entry (during oil changes) (Donald, 1897).

10
 CHAPTER 3: METHODOLOGY

3.1 INTRODUCTION

This chapter outlines the laboratory experiments carried out in this research project. The
purpose of this research project was to determine the extent to which sulphuric acid recovers
lube oil. Further quality tests were taken in order to characterise unused oil, waste oil and
recovered lube oil. The procedure used was a solvent extraction method with sulphuric acid
and activated carbon. The study was accomplished through a series of steps such as; sampling,
dewatering, desluging/extraction by using sulphuric acid and finally adsorption to obtain
recovered lube oil.

3.2 SAMPLING

Cortusa 100 oil samples (unused and waste lube oil) were collected from storage tankers
located behind VE Gases’ ASU. The physical and chemical properties of the sample were
measured at the local laboratory on VE Gases premises. After determination of physical and
chemical properties of these sample, the sample were labelled and stored in a sample store. The
selection of the sample for this study were just based on the availability of samples and their
recorded properties. For the sake of this study, two litres of the used oil were taken from the
sample store and sent to the laboratory for further step. The oil samples were characterised
using appearance, colour, specific gravity and density.

3.3 MATERIALS AND REAGENTS

Beaker Magnetic stirrer

Oven thermometer
Litmus paper hotplate
Measuring cylinder water bath
Filter paper carbon
Mass balance distilled water
Glass tube retort stand and clamps
Marker stopwatch
Buchner Filter

11
3.4 LABORATORY PROCEDURE

3.4.1 Dewatering
A sample of waste oil was heated to 180°C as proposed by Whisman under atmospheric
pressure for a period of 1 hour to eliminate the free water and emulsified water. In this case
500ml portions of the sample was heated in an open beaker with the help of a magnetic stirrer
as shown in Figure 3.1 below.

Fig 3.1: Heating the sample with the help of a magnetic stirrer

3.4.2 Extraction using sulphuric acid.

The acid-oil ratio selected in this stage was 20%v/v as proposed by Kiss & Bartels, 2007. The
process began by mixing 100ml of the oil sample with 20% by volume sulphuric acid in a flat-
bottomed flask. The mixture was continuously stirred using a magnetic stirrer for 2 hours at
around 60oC in order to facilitate uniform mixing (Hamawand, 2013). The mixture was allowed
to settle for 6 hours (as proposed by Rincon & Canizares, 2005) in a separating funnel, a heavy
layer containing sludge appeared to settle at the bottom of the flask and oil layer appeared on
top of it. An acid layer (containing sludge) was gradually discharged at the bottom of the
separating funnel and treated with an alkali for neutralisation of the acid. The oil layer was
removed from the separating funnel, its volume was measured, then labelled based on the acid’s
percentage by volume final. The process was repeated for 98% by volume sulphuric acid. The
treated oil in this stage was black in colour.

12
Fig 3.2: Samples obtained after desludging

3.4.3 Adsorption process

The product obtained from extraction was treated with activated carbon to improve its colour
(Hayalu, 2014). The colour improvement was conducted based on the fact that the black colour
of treated oil may lead into confusion with the used one, therefore this procedures was carried
out to distinguish recovered oil from waste oil. This stage was divided into two steps; the first
step was preparation of activated carbon and the second step involved removing the oil colour
using prepared activated carbon.

 Preparation of activated carbon

In this stage, 500g of pulverized carbon was mixed with 1000 ml of 50% sulphuric acid to
make the slurry. The slurry was then heated for about 1 hour at around 80oC as proposed by
(Udonne, 2011). This procedure was carried down to remove impurities from carbon as well
as to ionize the carbon (Kiss, 2011). The mixture was left for 24 hours in order to create enough
internal space of the carbon for better adsorption (Udonne, 2011). The carbon was washed
carefully with distilled water to remove precipitates and until there was no free SO42- ions (until
pH is 6–7). The carbon was filtered, baked for about 6 hours at 200oC to remove water and
stored in a dry place. The obtained dry and clean carbon is the one called activated carbon
because it is active chemically and electrostatically.

3.4.4 Adsorption with activated carbon

The activated carbon prepared in the above section was used in this adsorption step. Activated
carbon improves the colour and oxidation stability of the acid treated oil (Kiss, 2011). Because
the adsorption process using activated carbon is favoured by temperature range 90-120oC, in
this experiment the adsorption process was performed at 110oC.

13
Using constant adsorption time of 2 hours and constant temperature of 110℃, the oil products
from the extraction process were treated with activated carbon with a carbon-oil ratio of 15%
i.e. 3.75g activated carbon per every 25ml of lube oil. The process was carried out while stirring
using a magnetic stirrer. The adsorption step was repeated with a carbon-oil ratio of 20%.

3.5 TEST FOR DENSITY

25ml samples of unused lube oil, waste lube oil and recovered lube oil were placed in beakers
and the density of each oil sample was tested using hygrometers ranging between 0.65g/ml and
1.2g/ml. A hydrometer was dipped in the oil sample and on reaching the density of the medium,
it floats in such a way that the top level of oil can be read off the hydrometer but if it sinks that
implies that the density of the oil is undetermined using that hydrometer therefore the next
hydrometer with higher densities should be used.

3.6 SAFETY PRECAUTIONS

Handling of sulphuric acid and acidic sludge should be done whilst wearing protective clothing
and gloves.
All experiments producing fumes should be carried in a fume-hood.

14
 CHAPTER 4: RESULTS AND DISCUSSION

4.1 AMOUNT OF WATER AND LIGHT COMPONENTS IN WASTE OIL SAMPLE

The amount of water and light hydrocarbons present in used oil was calculated by considering
the amount (mass) of oil sample used at the beginning of the dewatering process and the amount
of oil obtained at the end of the process. The results below were obtained from a weighing
balance.
Table4.1: Mass obtained before dewatering
Mass of empty measuring cylinder 237.9g
mass of measuring cylinder plus oil 665.8g
Mass of oil 427.9g

Table 4.2: Mass obtained after dewatering

Mass of empty measuring cylinder 169.39g
Mass of measuring cylinder plus oil 587.79g
Mass of oil 418.4g

(𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑚𝑎𝑠𝑠−𝑓𝑖𝑛𝑎𝑙 𝑚𝑎𝑠𝑠)

% 𝑙𝑜𝑠𝑠 = 𝑥 100% ……………………………………………(1)
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑚𝑎𝑠𝑠

(427.9−418.4)
% 𝑙𝑜𝑠𝑠 = 𝑥 100% .......................................................................................(2)
427.9

Since the samples were heated in an open container as shown in Fig 4.1 it was impossible to
collect the distillates (water and some low boiling point components) but the amount of
distillate was determined as the mass lost during the heating process. It was observed that, for
500ml (427.9g) of the sample, the amount of oil remaining after the dewatering process was
approximately 489.5ml (418.4g), this implies that roughly 2% was lost to the atmosphere as
light hydrocarbons and moisture for every 500ml heated.

4.2 EFFECTS OF DESLUDGING

The desludging temperature was 60℃ to avoid the adverse effects of sulphuric acid oxidation
at higher temperatures. However at such low temperatures, the process is very slow hence
sufficient time of 2 hours and rigorous agitation was employed to enable the reaction to reach
completion. A higher desludging acid-oil ratio of 20% was maintained to optimize

15
recoverability. In this step, most of the oxidative and degraded products such as gum, wear-
metal impurities i.e. Pb, Cu, were successfully removed. This was accomplished with the use
of sulphuric acid at lower concentrations which proved to be very effective and efficient
because of its poly-functional nature. However strong sulphuric acid did not produce the
expected results.

4.3 EFFECTS OF ADSORBENT RATIO

It was clearly observed that as the quantity of adsorbent used increased with constant acid
concentration, the total amount of recovered oil has considerably decreased with an increase in
colour visualization.
Table 4.3: Description of the oil samples
Figure Description
4.1 (a) Waste lube oil
4.1 (b) Used oil treated with 20% v/v sulphuric acid
4.1 (c) Base oil produced by using 20% v/v sulphuric acid and 15% carbon
treatment
4.1 (d) Base oil produced by using 20% v/v sulphuric acid and 20% carbon
treatment.

(a) (b) (c) (d)

Fig 4.1: Colour changes after the experiment

16
Base oil obtained from treatment with 20 % activated carbon as shown in Fig 4.2 (d) shows
better results in colour improvement than the one treated with 15% activated carbon in Fig 4.2
(c). However percentage recovery was high for 15 % activated carbon. The time taken for
effective adsorption has a significant effect on the results thus in these experiments, the
adsorption time was kept constant for all samples. It has been observed that an increased
carbon-oil ratio i.e. greater adsorbent concentration, resulted in the production of a clearer base
oil almost similar to virgin oil. The results for the sample produced using 98% v/v sulphuric
acid with different carbon-oil ratios of 15% and 20% were excluded as there was no difference
between the waste oil sample shown in Fig 4.2 (a) and the 98% v/v sulphuric acid produced
base lube oil due to the strong acid concentration which led to further degradation of the oil
sample. This implies that the extent of sulphuric acid’s recoverability cannot be determined at
very high acid concentrations. A recovery of 42% was obtained for 20% v/v sulphuric acid
compared to the 60% recorded in literature, the variances can be attributed to different
adsorbents used.

4.4 PHYSICAL CHARACTERISTICS OF RECOVERED LUBE OIL

In this part only a few physical properties of the samples were selected for measurement. The
selected properties were based on availability of the facilities required to easily conduct the
tests. The selected physical properties include density, specific gravity, colour and water
content and these were limited to the fact that only physical separation methods were used to
recycle the oil. The obtained results were compared with that of the used oil sample and
observing similarities with the virgin oil standards.
Table 4.4 Results of the quality tests
Parameter Virgin lube oil Waste lube oil 20%v/v 20%v/v
sulphuric acid, sulphuric acid,
15% carbon-oil 20 % carbon-oil
ratio ratio
Density (g/ml) 0.89 0.87 0.8895 0.86
Specific gravity 0.89 0.87 0.8895 0.86
Water content 0.0 10.35 3.5 1.7
Colour Orange brown Black brown Pale brown

17
The results of the tests carried out on the recycled oil shows that the specific gravity and density
of the recycled oil are all lower than those of the fresh oil and waste oil therefore the recycled
lube oil can be blended with virgin lube oil for better efficiency of equipment and improvement
on environmental pollution. Fig 4.3 below shows that a sample prepared by 15% carbon-oil
ratio has a density almost the same as that of virgin oil sample and its recoverability was found
to be 42% which implies that it can further treated to remove the remaining water content and
can be reused.

Lube oil properties

12
10.35
10

6
3.5
4
1.7
2 0.89 0.87 0.8895 0.86
0
0
Virgin oil waste oil 15% carbon- 20% carbon-
oil ratio oil ratio

density (g/ml) water content (ml)

Fig 4.2: Comparison of lube oil properties

It was observed that the density of the original sample is higher than the density of treated oils.
The average densities of recovered oils were between 0.86–0.88 g/ml depending on the acid–
oil ratio used. Relatively higher densities were observed with lower acid ratio (0%) i.e. 0.8993
g/ml for all the different adsorbent percentages. However the density decreases significantly
with an increase in the carbon-oil ratio until no further changes can be detected, for instance
when 15% carbon-oil ratio was used an average density of 0.8895 g/ml was obtained. As the
carbon-oil ratio increased to 20%, there were density of oil decreased.

4.5 PRELIMINARY COST ANALYSIS

The primary cost analysis is completed to estimate and compare costs suffered by the
recycling process of used lube oil against the price of importing oil. This assessment of
costs is necessary in giving information concerning the economic feasibility of the study.

18
The laboratory experiment proved that 42% usable lube oil can be recovered from a 100ml
sample. This implies that from a drum of 210L lube oil about 88L can be successively
recovered and blended with virgin lube oil for reuse. In simpler terms for every 25L of waste
oil, 10.5L can be recovered whereas 220L of crude oil is required to produce the same 10L of
recovered oil. Costs accompanying this recycling process comprises of chemical costs,
electrical power costs and labour costs where most of them are operating costs. Costs of
various equipment which will be vital for the construction and assembly of the recycling
plant can also be considered for a complete plant design, which is not the range of this
research.

Pulverized coal for adsorption can be obtained from VE’s Mkwasine depot and preparation
of activated carbon can be done on site.
Table 4.5 Imported oil price and freight charge
Description Unit Quantity Unit cost(ZAR) Total
Lube oil L 835 33901.00 33901.00
Freight per trip 1 15136.56 15136.56
Total 49037.56 49037.56

As shown in table 4.5, a conversion of the above figures into United States dollar (USD),
reaches a conclusion that VE Gases is currently importing each litre at a price of $8.39.

 Material balance based on 1 litre product yield

Calculation for used oil required to obtain 1 litre
(W) = (1-x)/ 0.42, x=0 ……………………………………………………………………(3)
=2.38L
Where W= amount of waste lube oil
X= amount of additive

Calculation of amount of acid required to produce 1 litre

A.A. = U × Acid oil ratio ………………………………………………………………..(5)

= 2.38 x20%

=0.48

Volume of 20% Sulphuric acid produced from 98% sulphuric acid

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C1V1 = C2V2 ………………………………………………………………………………(6)

V2 = (C1V1)/ C2 ……………………………………………………………………………(7)
= (25*0.98)/ 0.2
= 122.5
Where C1 is 98% sulphuric acid
V1 is volume of 98% sulphuric acid
C2 is 20% sulphuric acid
V2 is volume of 20% sulphuric acid

Amount of oil produced from a 25L container of 98% sulphuric acid

Volume of oil produced = 122.5/ 0.48 …………………………………………………….(8)
=255 L
Table 4.6 Material balance based on 1 litre product yield
Description Unit Quantity Unit Cost ($) Total
Waste oil L 2.5 Nil Nil
98 % Sulphuric acid L 1 12.00 12.00

While the cost of 98% sulphuric acid is $12.00 per litre it is important to keep in mind that for
recycling, a dilution of down to 20% is used which implies that the a 25L container can be used
to produce 255L of recovered oil hence less than $5.00 can be used to recover a litre of oil
saving nearly $3.50 per litre lost though imports.

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 CHAPTER 5: CONCLUSION AND RECOMMENDATIONS

5.1 CONCLUSION

This research has shown that waste oil can be recycled by using solvent extraction with
sulphuric acid and activated carbon. The study proved that the acid treatment is a process that
can effectively remove contaminants from used lubricating oil. The recovered oil has
acceptable qualities indicated by the quality tests performed thus making it a better candidate
for reuse in the manufacturing industry and also as a fuel.

Waste oil properties were determined with standard chemical and physical tests. Operational
parameters were established in reference with the common solvent extraction processes and its
modification. Effects of acid and adsorbent ratios were studied on the recovery of usable
lubrication oil. The results showed that the efficiency of the recycling operation depends on
these reagent ratios. It was noted that the recovery yield increases with decreased percentage
in these ratios. A maximum recovery of 42% was obtained when both acid and carbon to oil.
However, while many variables have been studied in this research, there are many others that
need investigation such as temperature, pressure, settling time, mixing, centrifugation speed
and type of adsorbent.

5.2 RECOMMENDATIONS

 If VE Gases can adopt this recycling technique, it would have addressed a number of
problems faced by Zimbabwe and the entire world which are: scarcity of crude oil,
environmental pollution and most importantly the company’s finances.
 The by-products can be converted into marketable end products and the returns from
the transactions can be used to purchase the chemicals needed for recycling.
 The act of protecting the environment can be executed by alkaline treatment of the
acidic sludge producing a salt and water for example sulphuric acid from the desludging
stage and activated carbon preparation stage can be reacted with lime collected from
Acetylene plant’s lime pits.
 Further research is required in order to take this process to a commercial stage.
However, while few variables have been studied in this research, there are many others
that need thorough investigation such as pressure, temperature, settling time, mixing

21
 speed & time and type & size of adsorbent which have significant effects on the
recycled oil qualities.
 Lastly, Further character testing may also be executed to evaluate oxidation stability,
thermal stability and foaming character of the recycled oil. If possible application of
the recovered oil in a real machine can be practised to test the efficiency of the machine
lubricated with recovered oil.

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