United States
                   Environmental Protection
                   Agency
Air and Energy Engineering
Research Laboratory
Research Triangle Park, NC 27711
                   Research and Development
EPA/600/S7-88/017 Dec. 1988
&EPA         Project  Summary
                   Mixture  Effects  in  the Catalytic
                   Oxidation  of  VOCs in Air

                   S. Gangwal, K. Ramanathan,  P. Caffrey, M. Mullins, and J. Spivey
                     Most volatile organic compound
                  (VOC) releases into the environment
                  are  mixtures.  However, most
                  fundamental studies of the catalytic
                  deep oxidation of  such compounds
                  are  usually  confined to single
                  components.  This study examines
                  the  deep oxidation  of  organic
                  mixtures over  a heterogeneous
                  catalyst in  an attempt to  explain
                  earlier observations concerning the
                  apparent  inhibition or enhancement
                  of destruction of  some components
                  to establish a  scientific basis for the
                  design and operation of  catalytic
                  incineration systems for VOC control.
                  To elucidate these  effects,  the
                  oxidation kinetics  of n-hexane,
                  benzene,  ethyl acetate, and methyl
                  ethyl ketone in air were examined
                  over a commercial catalyst (0.1%
                  Pt/3% Ni on  Y-a'umina.) Reaction
                  rates  of  these components
                  individually  were  determined at
                  temperatures  of 150 to 360 °C from
                  differential  reactor studies. When
                  these were  compared to overall
                  destruction efficiencies from integral
                  reactor studies for both  individual
                  compounds  and  mixtures,  the
                  Mars/van Krevelen (MVK) reaction
                  rate model satisfactorily represented
                  the results for some single organic
                  compounds at lower temperatures.
                  By incorporating  pore  diffusion ef-
                  fects, the MVK model adequately
                  explains the single component  data
                  over the entire temperature range for
                  some of  the  compounds. A multi-
                  component MVK model incorporating
                  competitive adsorption effects is
                  moderately successful  in predicting
                  the observed  behavior for a binary
 mixture of  benzene and n-hexane;
 however, it  cannot  predict  the
 apparently  enhanced reaction rate
 observed for ethyl acetate at higher
 temperatures  (>220°C).  Other
 reaction pathways available  for
 compounds  with  carbon-oxygen
 linkages  and/or the  advent  of
 catalytically supported homogeneous
 combustion with  free radical
 precursors  may  explain this
 phenomenon. The enhancement of
 ethyl  acetate  conversions  in
 humidified air streams suggests that
 autocatalysis  by-product water may
 be a possible mechanism.
  This Project  Summary  was
 developed by EPA's Air and  Energy
 Engineering  Research Laboratory,
 Research  Triangle Park, NC,  to
 announce key findings of the research
 project that is fully documented in a
 separate report of the same title (see
 Project Report ordering information at
 back).


 Introduction
  The goal of this study was to establish
 a scientific basis for the selection  and
 evaluation of heterogeneous catalysts
 and operating conditions for the control of
 gas  streams containing mixtures of
 volatile  organic compounds (VOCs).  The
 research  was  devoted  to both
 experimental evaluation of the catalytic
 oxidation of VOC-containing mixtures
 and the kinetic interpretation/modeling of
 the results.

 Experimental
  A schematic diagram  of the experi-
 mental setup is shown in Figure 1. Table

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                            Control Thermocouple
                  Measurement Thermocouples
                                                                                                        GC Carrier Gas
                                                   Valve-Oven with 10-Port valve
                FC:          Differential flow controller
                PR:          Two-stage pressure regulator
                BFM V        Soap bubble flow meter and vent
                                      Process lines
                                      Electrical
                    Integrator
                     Actuator
                    Controller
                    and Timer
   Figure 1.    Microreactor system.
1 details the mixtures studied, and Table
2 describes the experimental conditions.

Results
   Figure 2  shows the inhibition of  n-
hexane conversion in mixtures.  Figure 3
shows the enhancement of ethyl acetate
conversions in  mixtures.  Experiments
were conducted in humidified air streams
to ascertain  if hydrolysis by-product
water may be  responsible for the en-
hancement. Figure 4  shows  the en-
hancement of ethyl  acetate conversions
in humidified air streams.
   Detailed experiments were carried out
to obtain fundamental rate constants for
the catalytic oxidation of the compounds
in Table 1 as single components. These
constants  were  incorporated into a
reactor model based on  the Mars/van
Krevelen kinetic  mechanism to try  and
predict  the  observed  mixture effects.
Figure 5 represents the fit of the model
to the single component benzene data.
The fits for  n-hexane  and ethyl acetate
were not as good.  Mixture effects in a
binary  n-hexane/benzene mixture were
also marginally predicted by the model.
Conclusions
   • Conversions of components  in  a
     mixture of  organics  may be
     significantly higher  or  lower  than
     when present by themselves.

   • Mars/van  Krevelen  (MVK)  kinetic
     mechanism  is  an  adequate
     representation  for  the  deep
   oxidation  of  single  organ
   compounds over the catalyst  use
   in this study.

•  A reactor model incorporating poi
   diffusion effects and MVK kinetic
   adequately  explained  singl
   component benzene data over tt
   entire temperature range of intere
   (150to360°C).

•  A multicomponent reactor  mod
   incorporating pore diffusion  effec
   and a simple proposed extension
   MVK kinetics  was  marginal
   successful  in predicting benzeni
   n-hexane mixture behavior.

•  Conversions of oxygenated speci<
   such as ethyl acetate are higher
   mixtures  than  in  single  con

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                      Table 1. Test Gas Mixtures
                                                      Concentration in Air (ppmv)
                       Single Hydrocarbon
                       Binary Mixtures
 benzene: 9, 69, 163, 375, 525
 ethyl acetate: 53, 109, 238, 450
 n-hexane: 201, 410, 566
 methyl ethyl ketone (MEK): 25,  50, 70, 135, 190, 298

 1 93 ppm benzene + 1 72 ppm ethyl acetate
 1 89 ppm benzene + 1 90 ppm n-hexane
 184 ppm ethyl acetate + 190 ppm n-hexane
                  135 ppm MEK
                  135 ppm MEK
                                           149 ppm n-hexane
                                           160 ppm benzene +
                       Ternary Mixtures       143 ppm benzene
 143 ppm benzene + 174 ppm ethyl acetate
 90 ppm n-hexane; 103 ppm n-hexane + 10'
 benzene + 93 ppm MEK
                                                                           104 ppm
ponents. The MVK  model appears
to explain  the  data in  the  kinetic
regime. MEK oxidation shows lower
apparent enhancement  than ethyl
acetate. Other  reaction pathways,
including thermally  enhanced free
radical  mechanisms and  the
interactions of  oxygen  containing
species with  partially reduced
metal surfaces  may explain the
observed  phenomena.  Further
experimentation  is  necessary
before a specific  model can  be
postulated  for the  oxidation of
oxygenated compounds.
The presence of water vapor in the
gas   stream   increases   the
conversion  of  ethyl  acetate
significantly. This  suggests  that
autocatalysis by-product  water
may  be  responsible  for  the
observed  enhancement described
above.  The  fact  that  MEK
conversions  are  not  significantly
affected by  the presence of water
vapor  lends  credence to  this
theory.
                    Table 2. Experimental Conditions
                     Pressure:
                     Temperature Range:

                     Space Velocity at ReactionTemperature:
                     Catalyst Bed:
                     Hydrocarbon Concentration in Air:
                     Catalyst Particle Size:
                     Ratio of Reactor Diameter to Particle Diameter
                          1 atm

                          140 to 360 °C (isothermal
                          operation)

                          50,000 to 1,000,000 rr1
                          17 to 20 mg
                          10 to 600 ppmv
                          120 to 170 mesh
                          20:1

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   110
   100
    90
    80
    70 -
 I 60
 <3
O  SO
I
u
">-  40 •
   30 -
   20 •
   10-
                410 ppm n-hexane in air
+  190 ppm n-hexane with
    184 ppm ethyl acetate in air


•  730 ppm n-hexane with
    189 ppm benzene in air

•  90 ppm n-hexane with
    174 ppm ethyl acetate in air
    143 ppm benzene in air

 17 mg, 120 x 170 mesh catalyst
 WHS V = 209
                                       l
                                     260
                                      I     I     1     I
                                    300       340      3SO
        140        180

                                  Temperature (°C>

Figure 2.    Effect of multicomponent mixtures on n-hexane conversion.

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  I
  I
  
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             •   Dry
             •  0.01 g Water/g Air
             WHSV- 209
             150 ppm ethyl acetate
   10 I—
      160
             180     200      220     240     260    280    300
                                     Temperature (°C)
                                              320   340
Figure 4.    Comparison of ethyl acetate conversions in dry and humidified air streams.
            100
         
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