PLANT DESIGN FOR THE PRODUCTION OF 30,000 KILOGRAM PER ANUM OF

ZEOLITE FROM KAOLIN

AKPAN, Anthonia Athanasius

AK14/ENG/CPE/006

A Plant Design Project Submitted to the Department of

Chemical/Petrochemical Engineering, Akwa Ibom State University, Mpat Enin

In Partial Fulfilment of the Requirement for the Award of Bachelor of

Engineering (B.ENG) in Chemical/Petrochemical Engineering

January, 2022
EXECUTIVE SUMMARY
 CHAPTER ONE

INTRODUCTION

1.1 Background of Studies

Zeolites are crystalline aluminosilicates earth minerals comprising of a three dimensional

network of SiO4 and AIO4- tetrahedral of open structures with cations positioned within

materials pore with diameters of molecular dimensions (0.3 to 1.4 nm) (Olaremu et al., 2018;

Abdullahi et al., 2017). They are formed under hydrothermal conditions and were first

recognized as a new type of mineral in 1756 (Farag and Zhang, 2018). Currently there are

some 40 different natural zeolites and roughly 150 synthetic zeolites (Abdullahi et al., 2017).

Most commercial zeolites are high purity synthetic products made from inorganic materials.

Zeolites can selectively absorb or reject molecules based on difference in shape and other

properties. These characteristics have resulted in variety of uses of zeolites. Such as, water

softening in detergents (replacing undesirable polyphosphates), absorbents for oil in

industrial spills, gas separation, water filtration and heavy metal removal in water purification

and wastewater treatment. The major application of zeolite is in the petroleum industry where

it is used as a catalyst for Fluid Catalytic Cracking. Industrial estimates of worldwide sales of

zeolitic FCC catalysts are approximately $1 billion per year and constitute a major portion of

the $2.16 billion worldwide refinery catalyst market (Olaremu et al., 2018). Zeolite catalysts

have been the source of major improvements in gasoline yield and octane as well as in the

production of cleaner fuels and lubricants with enhanced performance (Olaremu et al., 2018).

zeolite Y continues to provide the greatest gasoline yield at the highest octane with the

greatest degree of catalytic stability. Various applications of zeolite have led to the need of

increase production at low cost (Ahmed et al., 2018).

Kaolin clay offers a unique, environmental friendly and sustainable route toward the

manufacturing of Zeolite. Kaolin-based zeolites are produced from natural and cheap

resources as against the conventional process that employs pure sodium silicate and sodium

aluminate which are expensive with negative impact to the environment and hence not

sustainable (Abdullahi et al., 2017). Kaolinite is a clay mineral with 1:1 clay layer and with a

structural formula Al4Si4O10(OH)8 and the theoretical chemical composition is SiO 2, 46.54%;

Al2O3, 39.50%; and H2O, 13.96% (Murray, 2007).

Basically, there are two steps in producing zeolite from kaolin: metakaolinization which

involves transforming kaolin to metakoalin by chemically activating kaolin clay and

Zeolinization which involves the hydrothermal treatment of the metakaolin with aqueous

alkali solution to form the required zeolite.

1.2 Problem Statement

The conventional process employs pure sodium silicate and sodium aluminate for the

synthesis of zeolite which are expensive with negative impact to the environment and hence

not sustainable.

1.3 Aim

This research work is aimed at designing a plant for the production of 30,000 kilogram per

anum of zeolite from kaolin.

1.4 Objectives

i. Material and energy balance for the production of 30,000 kilogram per anum of

zeolite from kaolin

 ii. Equipment design for the production of 30,000 kilogram per anum of zeolite from

kaolin

iii. Simulation of plant for the production of 30,000 kilogram per anum of zeolite from

kaolin

iv. Instrumentation of plant

v. Costing and economic evaluation

vi. Plant safety, environment and HAZOP

1.5 Scope of the Design

The focus of this research is to approach the objectives of a more efficient and economically

more viable zeolite production.

Kaolin clay offers a unique, environmental friendly and sustainable route toward the

manufacturing of Zeolite. Kaolin-based zeolites are produced from natural and cheap

resources as against the conventional process that employs pure sodium silicate and sodium

aluminate which are expensive with negative impact to the environment and hence not

sustainable.
 CHAPTER TWO

LITERATURE REVIEW

2.1 Review of Previous Designs

Synthesis of zeolite through the hydrothermal route is a multiphase reaction-crystallization

process, usually encompassing at least one liquid phase and both amorphous and crystalline

solid phases (Abdullahi et al., 2017). An alternative zeolite synthesis route based on fluoride

containing compositions as mineralizing media has been reported by (Flanigen, 2001).

Nevertheless, (Cundy and Cox, 2003) maintained that the major synthesis route for many

zeolite and zeotypes is the hydrothermal process.

Kaolin clay offers a unique, environmental friendly and sustainable route toward the

manufacturing of Zeolite. Kaolin-based zeolites are produced from natural and cheap

resources as against the conventional process that employs pure sodium silicate and sodium

aluminate which are expensive with negative impact to the environment and hence not

sustainable (Abdullahi et al., 2017).

Previous work has shown that the improvement of the properties of kaolinite by chemical

methods is difficult due to its low reactivity. This clay mineral is not significantly affected by

acid or alkaline treatments, even under strong conditions (Reyes et al., 2010). Therefore, it is

usually used after calcination at temperatures between 550-950 °C to obtain a more reactive

phase (metakaolinite) under chemical treatments, with the loss of structural water with

reorganization of the structure (Farag, 2012). Only a small part of AlO 6 octahedral is

maintained, while the rest are transformed into much more reactive tetra- and penta-

coordinated units (Reyes et al., 2010). The optimum conditions for obtaining a very reactive

metakaolinite have been discussed by several authors who reported values between 600-800

°C. Calcination at higher temperatures leads to the formation of mullite and cristobalite
(Abdullahi et al., 2017). Several authors have reported the synthesis of metakaolinite based

zeolitic materials.

2.1.1 Clay conversion process (Kaolin conversion process)

Basically, there are two steps in producing zeolite from kaolin: metakaolinization and

Zeolinization.

A. Metakaolinization

Metakaolinization involves transforming kaolin (Al2Si2O5(OH)4) to metakoalin (Al2Si2O7) by

chemically activating kaolin clay. This is done by air calcinations at 500 – 600 °C, to form

meta-kaolin according to the reaction.

Al2Si2O5(OH)4 → Al2Si2O7 + 2H2O (at 550 °C)

At high temperature (1000 – 1100 °C) the meta-kaolin is broken down to calcined kaolin,

called mullite (Si2Al6O13), and SiO2 called cristobalite.

3Al2Si2O7 → Si2Al6O13 + 4SiO2 (at 1000-1100°C)

B. Zeolinization

Zeolinization involves the hydrothermal treatment of the metakaolin with aqueous alkali

solution to form the required zeolite.

Farag in 2012 simulated a process of zeolite 4A and 5A manufacture from kaolin by the basic

process of metakaolinization and zeolinization. He reacted mullite and cristobalite with

caustic soda and water in a gel make-up tank to produce zeolite 4A gel.

12NaOH + 204H2O + Si2Al6O13 + 4SiO2 (200 F) → 3(2Na2O+Al2O3+2SiO3+70 H2O) Zeolite

4A Gels
To produce zeolite 5A, zeolite 4A gel is fed to an ion exchanger, where it is mixed with

calcium chloride and water. In this process some of Na + ions in zeolite 4A gel are replaced by

calcium ions, Ca2+.

(2Na2O+Al2O3+2SiO2+70H2O) (Zeolite 4A Gel) + 0.7 CaCl2 (200 F) →

0.7CaO+0.3Na2O+Al2O3+2SiO2+70H2O (Zeolite 5A wet) + Na2O + 1.4NaCl

Wet zeolite 5A will pass through dryer to remove part of the water and form the dry zeolite at

1000℉.

0.7CaO+0.3Na2O +Al2O3+2SiO2+70H2O (1000℉) → 65.5H2O + 0.7CaO+0.3Na2O

+Al2O3+2SiO2+4.5H2O (Zeolite 5A dry)

The zeolite 5A dryer product has a particle size distribution which has to be incorporated into

the process simulation model.

2.2 Extent of Past Designs

 CHAPTER THREE

MATERIAL AND ENERGY BALANCE

3.1 Process Description