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CONTENTS SECTION
0 INTRODUCTION/PURPOSE 3
1 SCOPE 3
2 FIELD OF APPLICATION 3
3 DEFINITIONS 3
4 PRELIMINARY CONSIDERATIONS 3
5 REACTOR DESIGN 8
6 ESSENTIAL THEORY 8
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9 OVERALL EFFECTS 20
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TABLES
FIGURES
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Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass
Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance
Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts /
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1 SCOPE
2 FIELD OF APPLICATION
3 DEFINITIONS
With the exception of terms used as proper nouns or titles, those terms with initial
capital letters which appear in this document and are not defined above are
defined in the Glossary of Engineering Terms.
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Reactions between gases and liquids are common in the chemical industry.
Typical examples are:
In all these cases the reactant gas is first absorbed into the liquid and the
reaction then occurs in the liquid phase.
(a) A liquid phase reactor (a vessel) into which the gas is introduced, or
These devices are not always successful or optimal. See Clause 10 for the
appropriate design methods. Newer devices, e.g. gas-liquid static mixers, are
expanding the range of operating regimes.
(1) Viscosity
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From a knowledge of the rate of reaction and the mass transfer rate, it is
possible to determine which family of devices will be appropriate.
The overall flow pattern requirements (i.e. plug flow or back mixed) narrow
down the choice within a family.
The presence of solid particles, the need for heat transfer and the
materials of construction will impose constraints on the selection process.
For low liquid viscosities (say less than about 200 cP [0.2 Ns/m2]),
turbulence can be used to obtain good mixing, high interfacial area and
high heat and mass transfer coefficients.
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Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
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Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
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For high viscosity liquids, turbulence cannot be achieved practically and hence a
laminar mechanism (cutting and folding) has to be used to incorporate the gas.
Highly viscous systems are reluctant to degas under gravity, so degassing is best
done in a thin-film device. Suitable devices include:
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5 REACTOR DESIGN
Ideally the reactor design involves a quantitative idea of both the chemical
kinetics and the mixing and mass transfer. Analysis of the chemistry can be
difficult or impossible and mass transfer prediction is uncertain because of the
effects of bubble coalescence and flow pattern. Design from first principles is
therefore not normally possible.
Small scale experiments should be carried out to determine the relevant rates
and other necessary reaction characteristics such as the heat of reaction, the
degree of foaming and bubble coalescence, which are then scaled-up to the final
plant design. If time and techniques permit, this experimentation also guides the
choice of reactor type and indicates whether mathematical modeling should be
carried out and if so, to what complexity.
Generally, the combination of the difficulties associated with the analysis of the
chemistry and the uncertainties in the gas-liquid fluid dynamics renders the
scale-up of gas-liquid reactors a thorny procedure. Experiments should be
carried out at the final plant conditions (pressure, temperature, catalyst
concentration). Because of the difficulty and cost of experiments,
allowances for the uncertainly be should made in scaling-up.
Methods of calculation for both traditional and newer devices are presented in
Clauses 6 to 9. They also give further guidance on the selection, experimentation
and scale-up for gas-liquid reactions.
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Most industrial reactions are multi-step reactions and therefore their description
is generally simplified by focusing on the rate determining step. For parallel
reactions, the yield is the outcome of competition between two or more
simultaneous rates.
C is the desired product; reaction steps (1), (2) and (3) are first order in dissolved
gas (oxygen), steps (4) and (5) are second order. The overall Rate is determined
by step (1).
Rate (2)
Rate (4) i.e. the dissolved oxygen ratio, and
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For simple reactions the theory is well covered in several works (e.g. see Ref. [2],
Ref. [14] and Ref.[15]) and is summarized below using the film theory.
Note:
Other theories can be used, but they result in almost identical predictions.
The diffusion of a reactant through the gas to the interface and thence through
the liquid film into the bulk liquid with simultaneous reaction is covered. Additional
complications such as:
The treatment centers around the relative rates of gas-liquid mass transfer and
reaction. The reaction rate controls the overall rate if it is very slow; often,
however, it is fast, so that the overall rate is mass transfer controlled. Very fast
reactions can influence the diffusion process, causing enhancement of mass
transfer above the purely physical rate. This enhancement is a function of the
reaction rate. In extreme cases (so-called "instantaneous" reactions) mass
transfer again controls the overall rate of the process.
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Let q = m/n
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If a fast reaction occurs near the interface (within the "diffusion film") it will
enhance the mass transfer rate and equation (2) becomes:
Where:
Note:
k*L depends on the reaction rate, not the hydrodynamics which affects k L, and
CA 0 for these fast reactions since the gas reacts as soon as it is transferred.
The ratio of the diffusion to reaction times in the neighborhood of the gas liquid
interface is conveniently expressed as (tD/tR) which is also known as the Hatta
Number (Ha). Its value determines the extent to which diffusion controls the liquid
phase reaction. Several regimes are identified by the range of (tD/tR) values and
each regime has different requirements for reactor design (see Table 1).
Resistance to diffusion in the gas phase has to be accounted for in many cases.
The rate of transfer through the gas phase alone is given by:
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The regimes can be seen, for example for n = 1 and m = 1, on a graph of the
enhancement factor k*L/kL against the Hatta Number, given in Figure 2.
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Note:
Table 1 lists the Regimes (marked I to V in Figure 2), together with the
conditions, important variables, diagrams of the concentration profiles and
the local rate equations.
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These can occur if the liquid diffusivity of the product is less than that of
the reactant. See Ref. [11] and Ref. [36].
See Ref. [13], Ref. [11], Ref. [16] and Ref. [10].
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Table 1 shows how the various factors dominate reactor behavior according to
the regime. A preliminary choice of the reactor type can therefore be made to
give designs (e.g. film or bulk liquid, high or low kL, etc.) appropriate to the
regime expected, having regard for practically achievable kG, kL, a and eL values.
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There are two basic methods to determine the mass transfer/reaction regime and
thence select and design or scale-up the reactor. One method consists of
measuring the true liquid phase reaction kinetics (without mass transfer
interference) directly and then using this information with typical values of the
mass transfer coefficient (e.g. from Table 3) for the candidate reactors
selected from Table 1. When this is not possible, the other method is to run the
reaction in a laboratory-scale gas-liquid reactor and follow its responses to
certain changes of conditions.
The direct measurement of the reaction kinetics is difficult for fast reactions since
it is necessary to remove all mass transfer influences, i.e. to work in Regime I.
With slow reactions a bubble column or stirred vessel will operate in Regime I.
With somewhat faster reactions a more intense contactor (i.e. high kL) might be
used. Examples are the turbulent static mixer (see 11.11) and the spinning film
reactor (see 11.7).
In either case, experiments should preferably be carried out under steady state
conditions and as nearly at the intended plant operating temperature, pressure
and concentrations as possible with the rate measured by mass balance
between the inlet and outlet streams. The residence time of the liquid phase
should be measured either by tracer tests or by measuring the liquid
throughput and the liquid holdup volume in the reactor. Prior to carrying out the
kinetic measurements the absence of any effect due to changing gas rate or
stirrer speed on the measured rate of reaction per unit liquid volume should be
confirmed.
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The reactants are mixed at a low temperature (such that the reaction rate
is negligible) and the temperature is instantly raised to the desired reaction
condition and progress of the batch is monitored (see Ref. [3]).
This technique is similar to the temperature jump but is intended for gas-
liquid reactions (i.e. without predissolving).
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Laboratory stirred reactors are more commonly available than the specialized
devices and tend to serve as both "kinetic machines" and "semi-tech reactors". If
designed according to the standard configuration given in GBHE-PEG-MIX-705,
the values of kLa and gas hold-up determined in the laboratory can be scaled up.
Laboratory stirred reactors can therefore give useful design information for all
regimes so long as the same regime operates throughout the vessel (beware
that many laboratory autoclaves have a non-standard configuration and use
surface entrainment of the gas, which affects the mechanism, and hence model,
since the gas feed rate depends on the agitator speed).
The partial backmixing of the gas phase may however lead to uncertainties in
relating gas concentration profiles. A thorough study of the film reactions is best
carried out in one of the film reactors described in 7.2.1 and Table 3. The stirred
reactor should be set up to operate at conditions as near as possible to those
intended for the full-scale plant when producing the desired products and yields.
No materials should be omitted if they are to be present in the final process. The
rig should be so designed that agitator speed, temperature, pressure and
gas concentration can be varied. Continuous steady-state experiments are
recommended.
Note:
Processes during which solvent or product boils off may not respond in the ways
inferred by Figure 5 because changes in reaction rate alter the gas hold-up (and
hence the volume of liquid in the reactor if it is level-controlled) and the gas
phase reactant concentration.
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The use of laboratory stirred reactor experiments and the scale-up methods
described in Clause! 9 eliminate the need for data on gas-liquid equilibria
(Henry's Law coefficient, He) and diffusivity (DLA) in the design. These will,
however, be required if the design uses the basic reaction rate constants and the
previously determined mass transfer coefficients.
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9 OVERALL EFFECTS
So far only the "local" effects on the reactions have been described. It is
important to consider how local conditions change throughout the reactor
and what effects the reaction has on the design of the reactor as a whole.
A reaction in Regime I 'sees' the flow patterns in the liquid phase, and may
be influenced by the resulting liquid phase concentration changes through
the reactor, as outlined below. Each reactor type gives a different flow
pattern: see Clause 10.
Three types of ”axial mixing” (mixing in the general flow direction or ”residence
time distribution”) are distinguishable for ”ideal” reactors:
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These types should not be confused with ”radial” or ”cross” mixing, which is
uniformly across the general flow direction and is required for all reactors.
For reactions of the order n 1, the required reactor volume will evidently be
greater for a Backmixed reactor than for plug flow of liquid (e.g. by a factor of
3.91 for 90% conversion, 21.5 for 99% conversion, etc. for first order reaction).
This is also true for gas-liquid mass transfer controlled systems, where it is the
gas phase axial mixing which affects the driving force and hence reactor size for
a given throughput.
For certain more complicated reactions, the yield of the reaction is also
influenced by the mode of mixing. Full discussion of this is outside the scope of
this Guide (see Ref. [14] for an introduction), but, briefly, for consecutive
reactions:
ABC
high yield of B (compared with C) is favored by plug flow, but if C is the desired
product, a backmixed reactor should be chosen. For parallel reactions:
A C (of order q in A)
if p > q, high yield of B requires high CA, hence plug flow is required, conversely if
p < q, high CA has to be avoided, so a backmixed reactor is preferred. If p = q,
the yield is unaffected by the mixing mode.
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To see the above effects, obviously the timescale of mixing has to compare with
the reaction time. The backmixing found in stirred vessels etc. may be described
by a seconds minutes timescale (often called ”macromixing”). If, however, the
reaction is mixing sensitive and is substantially complete within milliseconds, any
yield effects will arise from mixing on the microsecond millisecond timescale
(”micromixing”).
In such cases local effects round the reactant feedpoint (or round the bubbles if a
gas reactant is involved) are controlling, and overall residence time distribution is
irrelevant to the reaction selectivity. High intensity mixers (e.g. turbulent static
mixers) should be considered here. Bourne (Ref. [6]) discussed modelling of
micromixing.
9.3 Gas Flow Pattern: Mean Driving Force for Mass Transfer
In regimes other than I, the overall axial mixing (residence time distribution) of
the gas is important, as it affects the mean concentration difference which drives
the gas-liquid mass transfer. Gas flow patterns depend upon the type of reactor
(see Clause 4) and sometimes its geometry and gas velocity. In using equation
(2) over the whole reactor,
Since CA y 0, for batch gas (rare) or ideal plug flow of gas, this mean value
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Hence backmixing gives lower mean driving force (implying larger reactor
volume), but lower peak gas concentration (which may influence the reaction
selectivity) than plug flow or batch gas.
In real reactors the ideal flow patterns are not achieved, but may be approached.
More detailed flow modeling is required if deviations from the ideals are
substantial, in other words where selectivity is governed by reactions of timescale
similar or faster than the mixing timescale.
More complicated approaches are required when the reaction yield is sensitive to
the mode of mixing, and is carried out in a reactor which is neither in ideal plug
flow, nor perfectly mixed, but somewhere between. The mixing is then described
by a model of the flow pattern, whose equations have to be solved together with
those describing the reaction kinetics. Since backmixing implies some degree of
recirculation, the solution of the equations has to be iterative and generally
requires a substantial computer program.
There are three types of mixing model for continuous reactors, based on:
Much effort has been put into developing type (a) models, (see Ref. [31]) but they
remain unsuitable for scale-up use because they require fitted parameters which
are not available. In other words they can describe mixing but not predict it. They
have not been applied to gas-liquid systems.
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and circulation time distribution, which can be converted to the number of zones,
x, in a loop.
The ultimate model is type (c) which involves a complete solution of the 'Navier
Stokes' equations (with a turbulence model), together with the reaction
equations, using 'Computational Fluid Dynamics' (CFD). Middleton (Ref. [28])
gives an example of this for competing reactions in turbulent stirred reactors. A
wide variety of configurations and conditions can be modelled in detail. GBHE-
PEG-RXT-800 should be consulted for guidance to experts.
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Design correlations for liquids are widely available, but less so for gas-liquid
systems. Correlations are available (see GBHE-PEG-MIX-705) for stirred vessels
and bubble columns, which are frequently used where heat transfer is a problem.
For low gas volume fractions (at least in stirred vessels), say 15%, Edney and
Edwards (Ref. [17]) show that the gas does not significantly affect the heat
transfer to the liquid. With typical boiling systems the extra bubbles
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Selection of materials of construction for plant reactors is often not easy and
should be made at an early stage of experimentation to ensure that research
work is done under conditions, and in devices, that are practical at full scale
considering the materials to be used. Conditions in reactors are often corrosive to
common materials; in gas-liquid reactors erosion/cavitation phenomena add to
these problems, especially for spargers, agitator blades, baffles, and other
high-velocity zones. Specialist engineers should be consulted if problems are
anticipated. High intensity devices (tubular jet mixers, turbulent static mixers),
where applicable, provide small materials weight per unit performance and so
may allow more exotic materials to be used than with vessels (although erosion
problems may be worse).
9.7 Foaming
Tables 4 and 5 summarize the typical properties of gas-liquid reactors from which
the selection may be made. The values given in Table 4 are comparative and
should not be used for design calculations. The design values will depend on the
physical properties of the fluids in the reactor.
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Note:
They are based on air and water physical properties at 20 °C. Approximate
adjustment for other systems may be made by:
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This Clause gives some sources of reference to correlations which can be used
in the design of gas-liquid reactors or in the scale-up from laboratory rigs or other
plants.
Depending on the regime, the design will require quantitative information on:
Bubble columns are simple to build and maintain, have no rotating seal problems
and can be made in large sizes. However, they have a low mass transfer
intensity (especially for coalescing systems), an uncontrolled degree of liquid
backmixing and mediocre heat transfer performance. Low concentrations of
easily-suspended solids can be handled.
These liquid film devices have the advantage of counter-current flow (where
applicable, i.e. for incomplete absorption from a multicomponent gas stream), low
pressure drop and a wide range of available materials of construction. They can
be designed for high or low gas/liquid ratios. The flowrates are limited by
hydraulics.
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These are co-current downflow, low intensity variants of the packed column and
are often used where the packing is or supports a solid catalyst and where co-
current flow has no disadvantage (e.g. irreversible simple reactions with
complete consumptions of adsorbed components or when the gas phase is a
single component). Pressure drop is less and hydraulic limits are wider than
those for countercurrent columns. Heat transfer is difficult and poor.
Plate or tray columns are similar to packed columns, but have a larger liquid
hold-up. The hydraulic operating range is wider and heat transfer is easier.
However blockages due to the presence of solids and problems due to foaming
may be more severe.
The mass transfer and hydraulic design is usually based on the methods
developed by Fractionation Research Inc. (e.g. their program FRISIEVE for
sieve-plate columns). GBHE-PEG-MAS-611and Ref. [32] should also be
consulted.
Spray columns are rarely used because coalescence of droplets often results in
a mediocre interfacial area, and the entrainment of fine droplets into the gas
outflow can be a problem. They are, however, simple and easily cleanable
(therefore suitable for "dirty" gases) and have a low pressure drop on the gas
side.
Design information is sparse; see Froment (1979), page 725 (Ref. [19]).
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Wiped film devices are commonly sold as evaporators for heat sensitive or high
viscosity liquids. Mass transfer intensity is high, but such devices require a heavy
maintenance effort.
These devices are still at the research stage as reactors, although centrifugal
thin-film evaporators are available commercially (e.g. from Alfa-Laval and Luwa).
With a 45° cone, gas-liquid mass transfer is enhanced by surface waves on the
film giving rise to very high values of KL for low viscosity liquids.
Stirred vessels are widely used (in the higher KL regimes) as they provide
flexibility, good intensity of mass and heat transfer and some control of bubble
size and backmixing. The additional cost of the agitator system and possible
shaft sealing difficulties should, however, be considered compared with the
simplicity of a bubble column. Stirred vessels should be used where there are
solids suspension problems. Because of shaft mechanical limitations they are
not usually very tall.
The plunging jet is a low-cost low-intensity contactor which has recently come
into use for aerating effluent ponds and reservoirs. The energy efficiency is good.
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The surface aerator is the older, mechanical equivalent of the plunging jet. It is
less energy efficient and requires more maintenance. The degree of mixing is
difficult to quantify.
When used with low viscosity liquids in the turbulent regime, static mixers give
very high intensities of gas-liquid mass transfer and approach plug flow
conditions. They offer good heat transfer as they can be used within shell-and-
tube heat exchangers. They can be operated at low gas/liquid ratios in bubble
flow for Regime II or at high gas/liquid ratios and gas velocities in
film flow (liquid film on all internal surfaces) for Regimes IV and V or under gas-
film controlled situations. Static mixers are new in the gas-liquid reaction area but
there are some plant applications. "Honeycomb" type static mixers can also be
useful for reactions between a gas and a high viscosity liquid.
Ejectors, venturis and orifice plates can provide high intensity mass transfer if
correctly designed. Ejectors are used in the Buss loop reactor which has several
commercial applications (e.g. H-Acid plant, FCMO).
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The upward flow of gas and liquid supports a bed of particles which can enhance
break-up or coalescence of bubbles depending on the properties of the particles.
They are not widely used or understood.
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[1] Allan J C & Mann R (1979), Chem. Engineering Science, 34, 413.
[5] Bin A K (1982) & Smith J M, Chem. Engineering Commun. 15, 367.
[8] Brian P L T (1965) & Beaverstock M C, Chem. Engineering Science, 20, 47.
[10] Carmichael G R (1980) & Chang S C, Chem. Engineering Science, 35, 2459
and 2463.
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[21] Horak J (1978) & Pasek J, "Design of Industrial Chemical Reactors from
Laboratory Data", Heyden.
[22] Laurent A (1983) & Charpentier J C, Int. Chem. Engineering, 23, 265.
[24] Mann R (1977a), Middleton J C & Parker I B, Proc. 2nd Eur. Conf. Mixing,
BHRA, Cambridge, paper F3.
[27] Middleton J C (1979), Proc. 3rd Eur. Conf. Mixing, BHRA, York, paper A2.
[31] Rao D P (1973) & Edwards L L, Chem. Engineering Science, 28, 1179.
[32] Rase H F (1977), "Chemical Reactor Design for Process Plants", Wiley.
[37] Sim M T (1975) & Mann R, Chem. Engineering Science, 30, 1215.
[38] Stephen H (1963) & Stephen T (eds), "Solubilities of Inorganic and Organic
Compounds", Pergamon.
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GBHE Mixing and Agitation Manual (referred to in 9.7, 11.11 and 11.13).
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