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KWAME NKRUMAH UNIVERSITY OF SCIENCE AND

TECHNOLOGY

CATALYST PREPARATION METHODS: IMPREGNATION.

SUBMITTED TO:

DEPARTMENTT OF CHEMICAL ENGINEERING,

CATALYSIS (PCE451).

BY
CHARITY MENSAH
7218721

AFIA AMANFO KYEI 7211621

BATSA GABRIEL 7214221

RICHARD KRAMPAH 7218221

ANDY OSEI TWUM 7220521

GODWIN AGBEVA 7216521

RANSFORD ANDERSON
7219821

MENSAH ERIC 7218821

27TH JANUARY, 2025
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TABLE OFCONTENT.....................................................................................................................

1.0 INTRODUCTION.............................................................................................................................................

2.0 TYPES OF IMPREGNATIONS.......................................................................................................................

3.0 CATALYSIS PREPARATION METHOD......................................................................................................

FLOW DIAGRAM..................................................................................................................................................

4.0 ADVANTAGES OF IMPREGNATION...........................................................................................................

5.0 DISADVANTAGES OF IMPREGNATION....................................................................................................

6.0 CATALYST CLASS PREPARED BY IMPREGNATION PROCESS:........................................................

7.0 ILLUSTRATIONS OF IMPREGNATION-PREPARED CATALYSTS AND THEIR

INDUSTRIAL USES:..............................................................................................................................................

8.0 NEW ADVANCEMENTS/CHANGES IN THE IMPREGNATION CATALYST

PREPARATION PROCESS:..................................................................................................................................

9.0 CONCLUSION................................................................................................................................................

10.0 REFERENCES..............................................................................................................................................

TABLE OF FIGURES.

Figure 1 Flow Diagram Illustrating Steps for Catalyst Preparation by Impregnation. ........................................... 6

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1.0 INTRODUCTION
Catalysts play a crucial role in modern industrial processes, enhancing reaction rates and selectivity.

Among the various catalyst preparation methods, impregnation is widely used due to its efficiency in

achieving high dispersion of active components on a support material.

Impregnation is a catalyst preparation technique that involves introducing an active catalytic

component into the porous structure of a support material. This method is fundamental in

heterogeneous catalysis, enabling the creation of high-performance catalytic systems across various

industrial applications.

Manufacturers use catalysts within multiple industrial processes since they increase the efficiency of

transforming reactants into wanted products. Researchers widely use impregnation because it

represents a basic, inexpensive technique to develop metal catalysts on high surface area supports.

This technique involves exposing supports to liquid metal-containing solutions comprising platinum

precipitates either as platinum hexachloride [PtCl6]-2 or platinum tetraammine [(NH3)4Pt]+2 (PTA).

Wet suspensions consisting of supports combined with metal precursors undergo drying and heating

under multiple oxidizing or reducing environments so the metal atoms can detach their ligands and

revert to their fundamental state. A metal oxide platform or an oxide precursor platform can work as

support material regardless of its crystalline or amorphous nature. The chemically impregnated

solution exists as either an aqueous solution or as an organic solution. Various processes regulate their

speeds of operation during the impregnation procedure. Some of these processes include:

• Solvent Evaporation Rate – The speed at which the solvent evaporates during drying.

• Precursor Decomposition – The breakdown of metal precursors into active catalytic forms during
calcination.
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• Adsorption Kinetics – The rate at which metal species adhere to the surface of the support.

• Diffusion Rate – The movement of metal precursor ions into the pores of the support material.

Impregnation has various benefits, including precise control over the catalyst composition, uniform

distribution of active sites, and the flexibility to modify the catalyst's characteristics to specific

performance needs. The success of impregnation depends on rigorous monitoring of parameters such

as precursor concentration, impregnation time, and drying conditions, which all have a major effect on

the final structure of the catalyst.

2.0 TYPES OF IMPREGNATIONS

The classification of impregnation methods depends on the ratio between impregnating liquid

volume (Vimp) and support pore volume (Vp). The three common impregnation methods for Vimp

> Vp are 'Equilibrium adsorption' 'Diffusional' or 'Ion exchange. Additional factors determining

catalyst efficiency have been developed to optimize preparation processes. There are several

impregnation methods being used and they include:

Wet impregnation - Impregnation by soaking of Excess solution (V imp > Vp). Excess liquid is cleared

through drainage. The deposition process requires multiple hours for completion or span over multiple

days. Surface area loss can deliver extensive surface remodeling during this process. This method

provides strict control over the distribution of species while achieving high levels of dispersion. The

method gives its most optimal results when there are interactions between ions and solids.

Dry or pore volume Impregnation - A material such as a catalyst can receive liquid solution loading

through a process called dry or pore volume impregnation. The pore volume of the solid receives

precise liquid volume measurements to achieve complete absorption while avoiding overflow. The

technique ensures active components are evenly spread throughout the material. Drying and optionally
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heating processes both stabilize the substances added to materials after the impregnation step. Material

science together with catalyst preparation routinely makes use of this technique.

(Reactive Adsorption) - Deposition via selective reactivity with the surface of the support. A

controlled amount of solution (Vimp > Vp) stays in contact with the carrier for a specific period

through methods like dipping until the excess is removed. The objective is to form a strong connection

with the surface. The method is rarely used, although it has the ability to graft or anchor active parts to

a support. Substances removed through reactive adsorption receive both physical adsorption treatment

and suffer a chemical transformation. The surface of adsorbents captures target compounds before

initiating chemical reactions to generate new stable products. The approach boosts both selectivity and

removal efficiency. Scientists employ this procedure for gas purification systems along with

contaminant elimination mechanisms and catalytic processing applications. Two notable examples of

reactive adsorption applications involve pulling sulphur out of fuels and trapping carbon dioxide

molecules.

Incipient Wetness impregnation - A process comparable to dry impregnation, except the volume of

the solution, is empirically determined to correspond to the point at which the catalyst begins to

seem wet (Vimp ~Vp).

Impregnation through percolation - Impregnation through percolation is a technique where a liquid

solution slowly flows through a porous solid, filling its pores. This method ensures even distribution

of the active substance within the material. It is commonly used in catalyst preparation and material

modification. After percolation, the material is dried and sometimes heated to stabilize the

impregnation. The process enhances materials’ operational capabilities for applications like adsorption

and catalysis. The carrier beds act as a medium for ion exchange during the impregnating fluid's

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movement through them. The method aligns consistently with impregnation through excessive

solution (A) when Vimp surpasses Vp. Equilibrium reaches more rapidly because of this method. The

process development can be tracked by conducting tests on the waste material. The active material

distribution across the carrier bed might exhibit heterogeneous patterns.

Co-impregnation - The technique of co-impregnation combines multiple active components with a

single solution to introduce them simultaneously into porous materials. The process generates

consistent distribution patterns which allow material components to interact uniformly. It is commonly

used in catalyst preparation to enhance performance and synergy between active species. After

impregnation, the material is dried and sometimes calcined to stabilize the components. This method

improves efficiency in applications like catalysis and adsorption

3.0 CATALYSIS PREPARATION METHOD.

The following are the steps in the impregnation catalyst preparation method:

a. Choosing the Supporting Materials: Based on its physical and chemical characteristics,

compatibility with the active phase and stability under reaction conditions, an appropriate solid

support material is selected. Activated carbon, zeolites, metal oxides (such as alumina, silica,

and titania), and other porous materials are frequently used as support materials.

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b. Impregnation Solution Preparation: To create an impregnation solution, the active phase

precursor is suspended or dissolved in an appropriate solvent, which can be organic or

inorganic depending on the type of precursor used. The compatibility of the solvent with the

precursor and support material is crucial.

c. The impregnation process: involves soaking or immersing the support material in the

impregnation solution to enable the precursor to adhere to the support material. There are

various techniques for carrying out the impregnation, including pore filling, and incipient

wetness impregnation.

d. Drying: The impregnated support material is dried to extract the solvent following the

impregnation procedure. One can use a variety of drying methods, such as freeze drying, spray

drying, oven drying, or supercritical fluid drying.

e. Calcination: Calcination is a method of heating a substance to a high temperature but below

the melting or fusing point, resulting in moisture loss, reduction or oxidation, and dissociation

into simpler compounds.

f. Activation: To change the precursor into the active phase, the impregnated catalyst

occasionally needs to go through an activation process. Activation can be accomplished via

reduction, or other appropriate methods, contingent on the catalyst of choice and the

characteristics of the precursor.

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FLOW DIAGRAM

Figure 1 Flow Diagram Illustrating Steps for Catalyst Preparation by Impregnation.

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4.0 ADVANTAGES OF IMPREGNATION

Precise Control of Active Component Loading: Through impregnation processes you gain
precise management of catalytic material injection volumes into supports. The desired level of
metal or active species loading in the support can be obtained through precise adjustments of
solution concentration combined with impregnation conditions to achieve optimal catalytic
performance.

Versatility: The impregnation technique allows for a significant degree of freedom in selecting

the active phases and support materials. It makes it possible to prepare a variety of catalysts

with various compositions and characteristics.

High Loading: The active phase can be highly loaded onto the support material by the

impregnation technique, which increases catalytic activity.

Homogeneity: A more homogeneous catalyst is produced by the impregnation method, which

often results in good dispersion of the active phase on the support.

Scalability: The impregnation process can be readily scaled up for the manufacturing of

catalysts on a large scale.

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5.0 DISADVANTAGES OF IMPREGNATION

Lack of Control: Using the impregnation process, it can be difficult to obtain exact control

over the size and distribution of the active phase particles on the support material.

Agglomeration: During the drying and activation phases, there is a chance that the active

phase particles would agglomerate or sinter, which could have a detrimental effect on the

catalytic performance.

Limited Accessibility: Because it can result in pore blockage or insufficient penetration of the

active phase into the support material, the impregnation process may not be appropriate for

catalysts requiring high accessibility to the active sites.

6.0 CATALYST CLASS PREPARED BY IMPREGNATION PROCESS:

Supported catalysts can be made using the impregnation process.

• Supported Catalysts: Active phases receive deposition on stable support materials

within supported catalyst systems. The support material enhances active phase

dispersion while expanding surface area and providing mechanical stability. Supported

catalyst systems include palladium on carbon alongside nickel on zeolites and platinum

on alumina are few representative examples.

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7.0 ILLUSTRATIONS OF IMPREGNATION-PREPARED

CATALYSTS AND THEIR INDUSTRIAL USES:

Preparation of Platinum on Alumina Catalyst (Pt/Al₂O₃)

Method: Wet Impregnation

1. Solution Preparation – A water-soluble platinum precursor, such as chloroplatinic acid

(H₂PtCl₆), is dissolved in a suitable solvent, usually deionized water.

2. Impregnation – The alumina (Al₂O₃) support is introduced into the platinum solution,

allowing the pores to absorb the solution by capillary action. The solution volume is carefully

controlled to match the pore volume of the alumina (pore volume impregnation).

3. Drying – The impregnated material is dried at moderate temperatures (100–120°C) to remove

excess water while retaining the platinum precursor within the alumina pores.

4. Calcination – The dried catalyst is heated in air at high temperatures (300–500°C) to

decompose the platinum precursor, leaving finely dispersed platinum particles anchored onto

the alumina surface.

5. Reduction (Optional) – To activate the catalyst, it may be subjected to a hydrogen atmosphere

at 200–500°C, reducing Pt species to metallic platinum (Pt⁰), which enhances catalytic activity.

Industrial Use of Platinum on Alumina Catalyst (Pt/Al₂O₃)

Application: Catalytic Reforming in Petroleum Refining

 Purpose: Platinum on alumina is widely used in catalytic reforming, a process that upgrades

low-octane naphtha into high-octane gasoline components.

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 Process: The catalyst facilitates the conversion of paraffins and naphthenes into valuable

aromatic hydrocarbons through dehydrogenation, isomerization, and cyclization reactions.

 Importance: This process enhances fuel quality by increasing octane rating and producing

valuable byproducts like hydrogen gas, which is used in hydro processing and ammonia

synthesis.

This catalyst is essential in the petroleum industry, helping optimize fuel performance while

maximizing hydrogen production for downstream applications.

Nickel on Zeolite Catalyst:

Preparation of Nickel on Zeolite Catalyst (Ni/Zeolite)

Method: Wet Impregnation

1. Solution Preparation – A water-soluble nickel precursor, such as nickel nitrate

(Ni(NO₃)₂·6H₂O), is dissolved in deionized water to create a uniform solution.

2. Impregnation – The zeolite support is added to the nickel solution, allowing the pores to
absorb the precursor. The solution volume is carefully controlled to prevent excess liquid while
ensuring full pore saturation.

3. Drying – The impregnated material is dried at moderate temperatures (100–120°C) to remove

moisture, ensuring that the nickel precursor remains inside the zeolite structure.

4. Calcination – The dried material is heated in air at high temperatures (400–600°C) to

decompose the nickel precursor and form nickel oxide (NiO) nanoparticles on the zeolite
surface.

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5. Reduction (Optional) – To enhance catalytic activity, the catalyst may be treated with
hydrogen gas at 400–700°C, reducing NiO to metallic nickel (Ni⁰), the active catalytic phase.

Industrial Use of Nickel on Zeolite Catalyst (Ni/Zeolite)

Application: Hydrocracking and Hydrogenation in Petrochemical Processing

 Purpose: Ni/Zeolite catalysts are used in hydrocracking to break down heavy hydrocarbons
into lighter, more valuable fractions such as gasoline, diesel, and jet fuel.

 Process: Under high pressure and in the presence of hydrogen, the catalyst facilitates bond
cleavage in large hydrocarbon molecules, promoting selective cracking and hydrogenation
reactions.

 Importance: This process increases fuel yield, reduces sulphur content in fuels
(desulfurization), and enhances product quality by saturating unsaturated hydrocarbons.

Ni/Zeolite catalysts play a critical role in petroleum refining, offering high selectivity, efficiency, and
stability for hydrocracking and hydrogenation applications.

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8.0 NEW ADVANCEMENTS/CHANGES IN THE IMPREGNATION

CATALYST PREPARATION PROCESS:

The impregnation process has been refined multiple times to enhance the efficiency, selectivity,

and stability of catalysts. Key advancements in the preparation of impregnation catalysts

include the following:

Controlled Impregnation Techniques: New impregnation procedures emerged to enable

better control of catalytically active species distribution during loading processes. The catalyst

deposition at atomic or molecular levels can be managed precisely through atomic layer

deposition (ALD) and controlled pore-filling impregnation methodologies. The precise control

over impregnation solution concentration and flow occurs when research utilize microfluidic

devices during the loading phase. Researchers utilize this technique to build catalysts suitable

for multiple processes including selective hydrogenation as well as oxidation reactions.

Co-Impregnation: Catalytic precursors receive simultaneous treatment on support materials

during co-impregnation processes. This technique enables the formation of catalysts with

matching active site configurations for performance enhancement. Co-impregnation serves as

an effective method for multi-component catalytic systems because it improves both activity

and selectivity while stabilizing operations. Combining metals and oxide components through

co-impregnation enables the development of water-gas shift reaction catalysts that transform

carbon monoxide and water into hydrogen and CO2. A combination of metal and oxide

components enables the catalyst to function effectively while the oxide component serves to

maintain catalyst stability and resist sintering.

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Nanoparticle Impregnation: The impregnation process has been expanded to include

nanoparticles as a catalytic species. This entails impregnating the support material with

colloidal nanoparticles or nanoparticle precursors. Because of the unique properties of

nanoparticles, impregnation offers advantages such as greater mass mobility, increased surface

area, and increased catalytic activity. Impregnating noble metal nanoparticles, such as platinum

or palladium, onto a support material, such as carbon or alumina, can produce extremely active

catalysts for a variety of processes, including hydrogenation and oxidation reactions.

Support Modification: Changes to the support material were studied in order to improve

catalytic performance and catalyst-support interaction. Surface functionalization, doping, and

modification with promoters or modifiers can alter the support material's properties, improving

the dispersion and stability of the catalytic species. Modifying a zeolite support's surface area

and pore structure can increase reactant accessibility and catalytic efficiency. This modified

zeolite can serve as a catalyst for a variety of activities, including hydrocracking and

isomerization procedures in the petroleum sector.

Ligand-Assisted Impregnation: The impregnation process incorporates organic molecules or

polymers that control how catalytic species nucleate while determining growth characteristics

and dispersion distribution. Additionally, this method gives operators superior control

throughout each stage of catalyst development thereby resulting in advanced and more

selective catalytic materials. Through ligand-assisted impregnation technology, researchers

produce metal-containing catalysts supported on surfaces for selective hydrogenation reactions.

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The binding of phosphines and amines ligands with metal ions stops their aggregation process

while generating catalysts that maintain precise hydrogenation product selectivity

9.0 CONCLUSION

Impregnation remains a fundamental and widely utilized technique for the fabrication of supported

catalysts, contributing significantly to productivity enhancements across multiple industrial sectors.

This method enables the precise deposition of active metal species onto support materials, ensuring

optimal catalytic performance while maintaining cost efficiency. Its straightforward implementation

allows for the regulation of catalyst composition, making it an economically viable choice for large-

scale applications. Additionally, the ability to manage particle size distribution presents a technical

challenge, yet impregnation techniques continue to evolve, offering scalability while preserving

operational flexibility. The impregnation process follows a systematic approach consisting of three
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primary stages: the careful selection of a suitable support material, the preparation of an optimized

impregnation solution, and the application of controlled pore-filling techniques to ensure uniform

metal dispersion. Platinum-based catalysts supported on alumina exemplify the practical application of

this method, though traditional impregnation techniques have historically offered limited control over

metal distribution. However, recent advancements have significantly improved the precision and

efficiency of impregnation-based catalyst preparation. Innovations in controlled impregnation

methodologies and nanoparticle impregnation techniques have addressed previous limitations,

allowing for enhanced catalytic activity and stability. As industrial catalysis continues to adapt to

evolving market demands, impregnation remains an indispensable technique, reinforcing its role as a

cornerstone of catalyst development and optimization.

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10.0 REFERENCES
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3. A.S. Bodke, D. Henning, L.D. Schmidt, Catal. Today, 61, 65, 2000.

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5. Barrer, R.M. Hydrothermal Chemistry of Zeoliles, Academic Press, London, 1982.

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Cafalysfs 111, Elsevier, Amsterdam, 1983, p. 485.

11. Delmon, B. and de Keyser, N. In: Ponefaix, J.L. and Figueras, F., Eds., Chemical and Physical
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Aspects of Caralylic Oxidolion, CNRS, Paris, 1980, p. 491. 0 1995 IUPAC,

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Amsterdam, p. 127, 1993.

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