Lecture 9

Catalyst preparation

A solid catalyst consists of mainly three components :

1. Catalytic agent

2. Support /carrier

3. Promoters and Inhibitors

Catalytic agent: These are the catalytically active component in the

catalyst. Such as, metals ( e.g Fe, Pt, Ag, etc.).

Support or carrier: Support or carrier provides large surface area for

dispersion of small amount of catalytically active agent. This is
particularly important when expensive metals, such as platinum, are used
as the active agent.

Promoters : Promoters are generally defined as substances added during

preparation of catalysts that improve the activity or selectivity or
stabilize the catalytic agents.

Industrial catalysts

Industrial catalysts can be broadly grouped into three categories:

1. Bulk catalysts: When the entire catalyst consists of the catalytically

active substance ,then the solid catalyst is called a bulk catalyst.

2. Supported catalysts: In supported catalysts, the catalytically active

materials are dispersed over the high surface area support material.

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3. Mixed agglomerates : These catalysts are agglomerated mixture of
active substance and support. These type of catalysts are used less
frequently.

Preparation of solid catalyst

The catalyst preparation methods can broadly categorized as follows :

1. Bulk preparation process

2. Impregnation and ion exchange processes (for supported catalyst)

3. Physical mixing (for mixed agglomerates)

For bulk

and supported
catalyst

For
supported
catalyst

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Basic unit operations involved in preparation of solid catalyst is shown in
Figure.

Bulk preparation processes

(a) Precipitation and co-precipitation

In this process, the desired component is precipitated from the solution.

Co -precipitation is used for simultaneous precipitation of more than one
component. The process can be carried out either in batch mode or in
continuous mode.

(b) Sol gel method

In the sol gel process, initially a stable colloidal solution called sol is
formed. The sol is a liquid suspension of solid particles ranging in size
from 1 nm to 1 micron. After a period of time the sol experiences a
transition from liquid solution to a cross-linked gel state.

Supported catalysts

Supported catalysts are prepared by deposition of the active metal on the

support materials. There are various deposition methods. The methods
most frequently used are:

a. Impregnation process

1. Dry or incipient impregnation:

In this method, a previously dried support is contacted with volume of

solution equal to its pore volume. As soon as the support is placed in
contact with the solution, the solution is drawn into the pores by capillary
suction.

2. Wet / diffusional impregnation:

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In this method, the pore space of the support is first filled with the same
solvent as used in the impregnating precursor solution. The wetted
support is then treated with the impregnating precursor solution.

Impregnation is followed by elimination of the solvent(drying). The

impregnated sample is heated in an oven in a flow of gas.

b. Ion exchange

Ion exchange consists of replacing an ionic species by another ionic

species in electrostatic interaction of the precursors with the surface of a
support.

Washing and filtering

Washing can be done by decantation. In this method the precipitate or gel

is added to a large volume of distilled water and the suspension is
thoroughly stirred. Then, the suspension is allowed to settle. The foreign
undesirable ions are desorbed from particles as they settle down slowly at
the bottom. When a clear interface is visible, the water is removed by
decantation and the process is repeated.

Drying

Drying is described as the elimination of water or solvent from the pores

of the precipitate or gel. It can be done in two ways:

• Solvent evaporation

• Super critical drying

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Calcination or sintering

Calcination is heat treatment process and is done in the presence of

flowing air or oxygen to burn any residual organics or to oxidize the
sample. Multiple changes occur during this process including:

1. Active phase generation.

2. Stabilization of mechanical properties.

3. Loss of chemically bound water.

4. Changes in pore size distribution and surface area due to sintering.

Catalyst shaping and formulation

Formulation and shaping of solid catalysts is done to :

(a) avoid high pressure drop in fixed and moving beds.

(b) increase thermal resistance against sintering fracture or phase

transition.

(c) increase mechanical resistance against crushing and attrition.

(d) ensuring high effective heat conductivity in fixed and moving bed for
strongly exothermic and endothermic reactions.

Some of the common catalysts formulation techniques are :

a. pellet formation

b. granulation

c. extrusion

d. spray drying