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THERMAL

KM

THERMAL CRACKING KINETICS-I

CRACKING OF ETHANE, PROPANE

AND THEIR MIXTURES

SUNDARAM and G F FROMENT

Laboratorlum voor Petrochemlsche Technlek, Rllksumversltelt, Gent, Belgium

(Received 1 J uly 1976, accepted 18 August 1976)

Abstract-Molecular reaction schemes for the thermal cracking of ethane, propane and then matures have been

derived from observed product dlstnbutlon, radical mechanisms, and thermodynamic prmciples The rate

parameters were determmed ma systematic way by estimatmn techmques mmimztng a multi-response ObJ ectWe

fun&Ion Dlscrunmatlon between rival models was based upon physical cntena and statM~ca1 tests The reaction

scheme obtamed by the superposlhon of smgle component crackmg also safisfactonly fits the data for the crackmg

of mixtures of ethane and-propane

INTRODUCTION

Hydrocarbon pyrolysis IS the major source of ethylene,

propylene, butadlene and aromatics, the pnmcpal feed-

stocks of the petrochemical Industry For the design of

the crackmg cod an overall kmetlc equation for the feed

disappearance 1s generally not sufficient, since the pre-

dlctlon of the product drstnbutlon 1s a very nnportant

design aspect This then requires a set of kmetic equa-

tions for a set of reactions ylelchng the products of

interest Although the reactions proceed via free radical

mechamsms[l], for slmulatlon or design purposes sun-

phfied so-called molecular schemes are adopted to cm-

cumvent the mathematical dlaculties encountered with

the integration of the system of stti ddferential equa-

tions associated with radical reactions Several molecular

reaction schemes have been published for the crackmg

of ethane and propane[2,4-fj] They lead to sets of

dlfferentlal equations contammg a large number of

kmetlc parameters and these have been obtained so far

by a tnal and error procedure, untd the results of the

mtegrafion match the experimental results Such a trial

and error procedure for the estimation of the parameters

1s not qmte satisfactory In other areas of applied

kmetlcs, e g m heterogeneous catalysis the kmetlc

parameters are obtamed m a much more systematic and

rigorous way, e g by least square estimation Further,

statistical tests are apphed to mvestlgate the validity of

the model and of the associated parameters The present

paper applies such a systematic approach to the kinetic

modeling of the crackmg of hydrocarbons molecular

reaction schemes are postulated, accounting as much as

possible for the true radical mechamsm, the model

parameters are estimated by regression and the relevant

statistical tests are applied A scheme leading to slg-

mficantly negative parameters or to abnormal values for

the activation energy of one or several of the reactlons 1s

rejected If more than one model is left m competition

after these crlterla have been applied, the fit of the

models IS compared to permit selection of the final

model The strategy outlined above IS completely analo-

gous to that used m the kmetlc modelmg of hetero-

geneously catalyzed reactions accordmg to Hougen and

Watson and recently discussed by Froment[7]

EXXANE CRACKING

Expenmental data

The experimental data used m tlus modeling work are

those published by Froment et al [3] These data were

obtamed m a pilot reactor for outlet total pressures of 1 5

and 2 atm abs and dtlution factors of 0 4 and 10 kg

steam/kg hydrocarbon The outlet temperatures ranged

from 780 to 85OC, the reference temperatures used m

the calculation of the equivalent reactor volumes from

775 to 825C The Reynolds number varied from 5000 to

10,000, the pressure drop from 0 3 to 0 5 atm

Reactton schemes

The basis for the development of the reaction schemes

are the product dlstibubons In ethane crackmg the mam

products are ethylene, hydrogen and methane Small

quantities of propane, propylene, acetylene and bu-

tadlene are also found Imtlatlon, propagation by radicals

and termmatlon steps are involved 111 the process The

radical reactions are used here as a guide for buddmg the

molecular model The maJor pathway to ethylene may be

written

C,Hs + H A C,H: + H,

(1)

C,H; *I_ C,H, + H

(2)

Addition of these two radical reactions yields the mole-

cular equivalent

C2H6 - C2H4 + Ht (3)

The correspondmg kmetlc equations may be wntten

9 = k; (C,H&H) (4)

601

602 K M SUNDARAM and G F FROMENT

When pseudo steady state 1s attamed

k;GHdW) = W3-I;) (6)

Ehmmatlon of (CzH3 between (5) and (6) leads to

w = L;(C,HJ(H)

(7)

These equations show that the rate of formation of HZ

and C2H4 obeys first order with respect to C2Hs, which IS

m agreement with the experimental observations

The followmg radical reaction also takes place

&Ha + H - C,H:

(8)

and this leads to adding a reverse step to the molecular

reaction (3) From thermodynamics It follows that such a

reactmn 1s indeed reversible under normal crackmg

condltlons Reaction (3) accounts for more than 90% of

the total reaction rate and 1s therefore common to all the

models developed These dtier by one or more of the

secondary reactions For these secondary reactlons gross

molecular models have been used hke, e g [5,6,8]

CzH4--+ b,H, + b,CH, + b&H,

whereby b,, 6, are chosen to satisfy the mass

balances for carbon and hydrogen This approach 1s

hmlted to a narrow range of operating conditions,

however, and it was preferred to reflect the true nature

of the reactions more closely The following reactions

have been proposed to account for acetylene

production [2, i]

It follows from

C,H, - CzH, + H,

(9)

C,H, - &Hz + CH,

(10)

thermodynamic calculations based on

Rossmls tables for free energies of formation[9] that (9)

1s not feasible under the usual pyrolytic condltlons, so

that only (10) was retained

To account for propylene formation Pacey and

Purnell[lO] proposed the followmg radical reaction at

temperatures above 640C

C,H; + C,H, - C,H, + CH;

(1 >

The molecular equrvalent was wrltten

C,Hs + CzH4 - C,Ha + CH,

(12)

Propylene may result from the decomposition of propane

accordmg to, m molecular terms

C,Hs - CsH6 + Hz

(13)

The formatlon of propane IS accounted for by

2CZH.5 - C,Hs + CH,

(14)

It IS well known from propane crackmg, however, that

the reaction

C,H, - CzH4 + CH.,

1s equally important

(15)

The followmg reactlon was also mcluded m one of the

models to account for methane formation

2C2H,5 - CzH4 + 2CH.,

(16)

Finally, the butadlene formation was ascribed to the

decomposltlon of the C,H; radical The latter ongmates

from

C,H, + C,H: - C,H;

(17)

and therefore the butadlene formation 1s wrrtten as

C,H, + C,H, - CdH6

(18)

Three models were set up on the basis of the above

considerations They are aven m Table 1 Models II and

III dfier from I m that they dont include propane

decomposltlon reactions

Model drscnmmaflon and parameter eshmatron

The kmetlc equations for the reactions are given m

Table 1 All the reactions, except (2) (Table 1) were

considered to be elementary, so that the order cor-

responds to the molecularrty Reaction (2) LS more com-

plex and first order was assumed for it

To determine the model parameters the kinetic equa-

tions of model I, II and III have to be substituted mto the

appropriate contmmty equations for the components,

and these have to be mtegrated and compared with the

Integral reactor data It should be mentioned here that

the experimental data were reduced to lsothermahty by

means of the equivalent reactor volume concept, dls-

cussed and applied by Van Damme et al [2] and by

Froment et al [3] The contmmty equations for the com-

ponents can be written

-f$=-R,=-zs,,r,

e

(19)

where S, represents the stolchlometnc coefficient for the

Ith component m the lth reaction

The parameters were estimated by non linear regres-

sion by means of Marquardts algorithm The multl-

response nature of the problem was accounted for by

mmlmlzmg the weighted sum of squares of residuals on

the molar flow rates F, of the reaction components at the

exit of the reactor

where w, 1s the weighting factor The second summation

Modehng of thermal crackmg kmetlcs-I 603

Table 1 Models for ethane crackmg

(1)

(2)

(3)

(4)

(5)

(6)

(1)

(2)

(5)

(6)

(7)

(8)

(1)

(2)

Model I

CJ-L

& CJ -I , +H,

Z&H, A C,H. + CH,

C,H. * C,H, + H,

C,H. 3 C,H, + CH,

C&J6

&GH,+C&

C,H, + CZH, A C,H,

Model II

CZH,

&C&_,+Hz

ZCZH, * C,H, + CH,

C&L

&C2Hz+CH,

C,H, + C,H, A C&

2&H, a C,H, + 2CJ-L

C,H, + C,H, -% C,Hs + CH.

Model III

C,& *I GIL + I-L

*2

2&H, - C,H, + CJL

775 800 825C

Kc, 8 895 x IO- 1 276 x lo- 1 800 x lo-

Kc< 9 847 x lo- 1 375 x 10-Z 1 890 x lo-

IS carried out over the n experiments The Integration of

the set of dlfferentlal equations was performed by means

of the Runge-Kutta-GB routme

Model I was reJected, since several parameters were

found to be negative Model II was reJected, m spite of

positive values for the parameters, because ks (Table 1)

was found to be mdependent of temperature and because

kl (Table 1) was not slgmficant at the 95% confidence

level With model III all the parameters were positive,

slgndicant at the 95% confidence level and temperature

dependent As shown m Fig 1 no bias could be detected

m the calculated vs experimental fiuxes for ethane,

ethylene, hydrogen and methane Estunated parameters

for Model II and III at 800 and 825C are shown m Table

2 The bmary correlation coefficients between the

parameter estimates were found to be very small The

temperature dependence of the rate coefficients 1s shown

m the Arrhemus plot of Fig 2 The parameters were not

estimated at 85OC, smce only five expenments were

available at that temperature Also, at 775C the yields of

acetylene, butadiene and propane were extremely low

Therefore, the weights of these responses were set zero

at that temperature and only k, and k, were estnnated

The activation energies and frequency factors are gven

m Table 3 A value of 65 20 kcallmole IS obtamed for the

main reactlon (1) m Table 1 From a study of the overall

kmetics Froment et al [3] derived values rangmg from

59 30 to 6194 k&/mole depending upon the experlmen-

tal condltlons It should be added that Model II, Model

III and even Model I lead to an almost identical value of

65 00 kcal/mole, which IS not surpnsmg, smce the mam

reaction accounts for roughly 90% of the total ethane

conversion Finally, it should be added that more ac-

curate rate parameters for some of the minor secondary

reactions could be obtained from processes m which

they are more important This will be the case, e g for

the parameters of reaction (3) (Table l), wbch 1s far

more important m propane crackmg In this way It

becomes possible to develop a coherent and precise set

of kmetrc data which can be used for the crackmg of

mixtures of hydrocarbons This will be illustrated m what

follows

PROPANE CRACKING

Expenmental data

The data used m this work were obtamed by Van

Damme et al [2] m the followmg range of operatmg

varrables Propane flow rate from 2 to 5kg/hr, steam

dilution 0 3-l 0 kg/kg propane, outlet temperature 700-

87OC, outlet pressure 1 2-2 3 atm abs , pressure drop

0 3-O 5 atm

Notation used in Table 1

F, = sum of flow rates of reactants, products and steam

= 2 F. +steam

r-1

K,,, Kc, = equhbrmm constants based on concentration

604 K M SUNDARAM and G F FROMENT

Er per l ment al Imol/Ohr) CHL

2,s 75

Fig 1 Expenmental vs calculated fluxes at the extt of the reactor for ethane crackmg Model III

Table 2 Estimated parameters for ethane crackmg for models II and III

Temp = 800C Temp = 825C

Rate parameter value parameter value

coefficient (set- or tl mole- set-) t value (set? or tl mole-set-) 1 value

Model II

k, 2 4054 77 8 4 9350 48 3

k+ 0 0171 37 3 6044 x 1o-3 021

k, 21 9302 69 43 1333 53

k, 6 4322 x 103t 36 6 5244 x 1Ot 42

k, 9 7872 x 10m3 77 3 7839 x lo- 109

ks 27 9250 115 71 OOOO 91

Model III

2 4160 80 5 4 937s 513

1 9893 x 10-Z 93 3 9919 x 10-2 12 2

29 8083 82 44 2055 62

4 0638 x 103t 36 6 3128 x 10t 43

30 7083t 192 715306t 21 0

Table 3 Arrhemus parameters for ethane crackmg Model III

Rate coefbent A (see- or tl mole- set-) E (kcal/mole)

k, 4 652 x lOI 65 20

kz 3 850 x 10 65 25

% 9 814 X lo* 36 92

% 1 026 x lO*t 41 26

k, 7 083 x 1Ot 60 43

Reactron scheme

Several molecular models have been proposed for

propane crackmg, most recently by Van Damme et al [2]

and Murato and Salto[6] The parameters were deter-

mmed by a trial and error procedure Detaded radical

mechamsms for this reaction have been dlscussed and

reviewed recently by Buekens and Froment [ 1 l] and Al-

lara and Edelson[ 121 The molecular reaction schemes

presented here were constructed on these bases They

consist of 9 reactions, contams 10 species and are shown

m Table 4 Only the malor reactions not encountered yet

m the section on ethane crackmg wdl be discussed here

The followmg radical reactions account for the for-

mation of propylene and hydrogen

C,H, + H - C,H; + H,

(20)

&HI; - C3H6 + H

(21)

By adding up these two radical reactions the de-

hydrogenation already mentioned m the section on

ethane as eqn (13) 1s obtamed

Modehng of thermal crackmg kmetlcs--I 605

kfhr-lor(llt/mol hr l k(Lath

A

- 0 PROPPlNE CRACKlNG

---. ETHANE CR*CK,NG

II hr)

C,H, - CzH, + CH,

(24)

Ethane formatlon 1s accounted for by the followmg

reactlons

106

C,H, + C,H: - C,H; + CzH6

(25)

C,H, + H - C,H;

(26)

Addltlon of (25), (26) and (21) leads to the molecular

reactlon

C,H, + C&H, - CxH6 + CzHs

(27)

Secondary reactlons leadrng to acetylene and hutadlene

were dlscussed under ethane crackmg already

The monotomc mcrease of the ethylene and methane

selectlvlty and the dechne of the propylene selectivity 1s

accounted for by

and

2GHa - 3&H, (28)

2C3H6 - 3cH.# + l/2&

(29)

04

(lIK) In (29) Cs really represents the C, fraction although in

propane crackmg this mamly consists of benzene The

amount of hydrogen m the C,-compound IS neglected In

propane cracking the C5+-weight yield varies between 3

and 6%, depending upon the total pressure and the steam

tiufion The followmg reactions were mtroduced mto

Model II, shown m Table 4 Instead of reactions (3) and

(5) of Model I, also shown m Table 4

Fig 2 Arrheruus plot for ethane cracking (Model III) and pro-

pane cracking (Model I)

Table 4 Reachon schemes for propane crackmg

Model I

(1) C,H, - C,H, + CH,

(2) C,H. = C,H, + Hz

(3) C,H. + CzH. - C&L + WI.

(4) 2C,H, - 3&H.

(5) 2C3H, - 0 Xa + 3CH,

(6) C H 3 6-

- CzH, + CH,

(7) &Ha + C,H,-, GH. + CH,

(8) C,H, z=+ GH. + Hz

(9) C,H, + &Hz - C&.

Model II

(1) C,Hs - CzH, + CH,

(2) C,H. e C,Hs + Hz

(4) 2C,H, - 3GH.,

(6) C,H, = C&I, + CH,

(7) c,& + GIL - C,H, + CH,

(8) C,H, = CzH. + Hz

(9) C,H. + &Hz - Cd%

(10) 2C,H, - CJL. f CJLo

(I I) 2C,Hs - C,H, f (XL. + CH.

Kc, values 77SC, 0 074, 8OOT, 0 102, 825C. 0 138

The following reactions account for the formatlon of

ethylene and methane

C3Hs + CH; - CJH; + CH,

(22)

C,H; - C2H4 + CH;

(23)

Addition of the two reactions ytelds

2C,Hs - CzH6 + C,I&o

2C,H, - C,Hs + &He + CH,

Model drscnmrnatron and parameter estmatrott

Because of the large number of parameters to be

es&mated the computation time increased drastically

Precise estunatlon of the parameters of the secondary

reactlons was difficult Both Models I and II contain

reactions hke (8) and (9) which are more unportant m

ethane crackmg and for which the parameters had al-

ready been determined accurately It 1s then preferable

to take over these parameter values In add&on, k6 and

k, related to minor reactions mvolvmg acetylene and

butene were estunated by tnal and error The parameter

estunates obtamed by Marquardts algorithm at 800C are

shown by way of example m Table 5

Model II led to slgmiicantly negative values for the

rate coefficient of reaction (11) (Table 4), at all tem-

peratures and was rejected for this reason All the

parameters of Model I were posltlve and the activation

energes were plausible It should be mentioned, though,

that k3 1s less accurately determmed than the other

parameters This IS not surprlsmg smce the ethane selec-

tivity does not exceed 3 2% Further, ethane was also

present m the feed as an Impurity, and this decreased

somewhat the accuracy of Its determination Dficulfies

606 K M SUNDARAM and G F FROMENT

Table 5 Estimated parameters for propane crackmg at 800C

Model I Model II

Rate parameter value parameter value

coefficient (set- or tl mole- see-) t value (se& or tl mole-set-) t value

kl 23409 80 3 2 8549 610

k, 2 126.5 79 4 18572 73 7

k, 23 6350t 18 - -

k, 0 7208 160 0 2674 57

k, 0 8164 22 1 - -

k 0 6 7880 x lo-* 28

k I I - - - 8 5283 x lo-* -20

were encountered in estlmatmg kJ at 85OC, so that its

value at that temperature was extrapolated from the

values at 775, 800 and 825C

All the estnnated parameters of Model I were highly

sign&ant at the 95% confidence level

The bias was tested by plottmg the calculated and

experlmental molar flow rates at the exit of the reactor as

shown m Fig 3 for 825C, e g The rate parameters all

obey the Arrhemus relation The frequency factors and

the activation energies for Model I are hsted m Table 6

and shown m Fig 2 Since the first two reactlons of

Table 6 Arrhemus parameters for propane crackmg Model I

Rate wefficlent A (set- or tl mole- see-) E (kcal/mole)

k,

kz

?

k:

k,

k,

k,

kg

4692x 1O1O 50 60

5 888 x 100 51 29

2 536 x lO*V 59 06

1 514 x 10 55 80

1423 x 109 45 50

3 794x 10 59 39

5 553 x lo.? 60 01

4 652 x lOI3 65 20

1 026 x 10t 41 26

Model I account for more than 90% of the total propane

consumption the overall rate of disappearance of pro-

pane was based upon these two reactrons The activation

energy was found to be 50 93 kcal/mole, a value which

has to be compared with 52 4 kcallmole obtamed by

Buekens and Froment [ 1 l] at zero converslon and 49 6 to

51 2 kcal/mole (dependmg upon the total pressure and

steam ddutlon) obtamed by Van Damme et al [2]

E-PROPANE MIXTUWS

Recently, Murata et al [13] set up a radical reaction

scheme to explain the experlmental results of the

pyrolysis of par&n hydrocarbon mixtures The

parameters were determmed by trial and error

In this work a molecular reaction scheme, shown m

Table 7, was constructed, contammg all the major reac-

tlons of ethane and propane crackmg The parameters of

the reactions were sunply taken over from the pure

component crackmg, dependmg upon the Importance of

the reactlon m either ethane or propane crackmg The

source of each parameter value 1s also given m Table 7

Only the frequency factor of a minor reaction, namely

butene formatlon had to be shghtly adapted, since it was

Ex~rerrmcnta, ,molIh:!

30 40

20

3 H6 f-J H6

Fig 3 ExperImental vs calculated fluxes at the exit of the reactor for propane crackmg Model I

Modelmg of thermal crackmg kmetlcs-I

Table 7 Reaction scheme for ethane-propane murture crackmg

607

Reachon A llsecor t& E (kcal/mole) Source

1 C,H. - C,H, + CH,

2 C H -C,Ha+H~

3 8-

3 C3Hs + CJ-L - C,Hs + CSHG

4 CaHd - 3&H,

5 ZC,Hs - 0 5C, + 3CH.

6 C,H, + CzH, + CH.

7 C,H, + C,H, - Cd& + CI-L

8 C,H, = CzH, + Hz

9 C,Hd + C,Hz - C.H,

10 C,H, -I- C,H, - C,H, + CH,

4 692 x 10

5 888 x 10

2 536 x 10t

1 514 x 10

1 423 x lo9

3 794 x 10

1 0 x 10-t

4 652 x lOI

1 026 x 109

7 083 x 10V

50 60 P

51 29 P

5906 P

55 80 P

45 50 P

59 39 P

60 01 P*

65 20 E

41 26 E

60 43 E

P, propane, E, ethane, P *, frequency factor modtied w&h respect to propane

less sigmficantly determmed from the smgle component

crackmg The model was checked agamst experimental

data obtamed with feeds contammg 25, 50 and 75 wt%

ethane at several steam ddutlons and total pressures and

reported m detad by Froment et al [3] The slmulatlons

accounted for the experlmental temperature and pressure

profiles Some results of the slmulatlons are compared

with the experlmental data m Fig 4 The agreement 1s

excellent, mdlcatmg that the model resultmg from the

superposition of the models for ethane and propane

crackmg does account for the interaction reported by

Froment et al [3] This IS probably due to the close

connection of these molecular models with the true

radical schemes of the reactions

CONCLUSIONS

In tlus work a rather rigorous approach has been

adopted for model buddmg m thermal crackmg reactions

Molecular reaction schemes were set up, based as

closely as possible on radical schemes The dlscnmma-

tlon between rival models was based upon physlco-

chemical constramts for the parameters and the good-

ness of fit of the model The parameters were obtained

by estnnabon, usmg a multlresponse approach and

mmlmlzmg a we&ted sum of squares of residuals by

means of Marquardts non linear regression routme

w

This puts model bulldmg m thermal crackmg reactions

on the same ngorous basis as that m reactions catalyzed

by sohds

Acknowledgemenf-The support of the Process Data Group of

K T I , The Hague, The Netherlands, IS gratefully acknowledged

NOTATION

frequency factor, set-, or 1 mole- set-

coefficients m gross molecular reaction

actlvatlon energy, kcal/mole

molar flow rate of Jth component, moles/hr

estimated molar flow rate of Jth component,

moles/hr

total molar flow rate, mole&r

eqmhbrmm constant m concentration units

(moles/l )*,

rate coefficient for ith reaction, set- ,

1 mole- set- or hr-, 1 mole- hr-

change m moles, moles

total pressure, atm

reaction rate for rth reaction

gas constant, kcal/mol K or atm 1 mole- K-

stolchlometrlc coefficient of component 1 m &h

reaction

temperature, K

Fig 4 Product dlstrlbutlon vs propane conversion Cracking of a 50/50 wt% mixture of ethane and propane

Dllutlon factor 0 4 kg steam/kg mixture Lines, expernnental, Pomts, calculated

608

t

v,

x,

W,

K M SUNDAUM and G F FROMENT

t values

equivalent reactor volume, 1

propane conversion

wetghttug factor for Jth component

[5] Petryschuk W F and Johnson A I, Can J Chem Engng

1%2 46 172

[6] Mnrata M and Smto S , J Chem Engng Jopan 1975 8 39

[7] Froment G F , A ZCh E I 1975 21 1041

[8] Huato M and Yosloka S , Int Chem Engng 1973 13 347

[9] Rossrm et al, Selected Values of Thennodynamrc Properties

REFEXFNCES

of Hydrocarbons and Related Compounds Carneme Press

1953

[l] Laldler K J , Chemical Kmetxs, 2nd Edn McGraw-Hdl, [lo] Pacey P D and Purnell J H , Znd Engng Chem Fund1 1972

New York 1%5 11 233

[2] Van Damme P S , Narayanan S and Froment G F ,

AZChEJ 1975 21 1065

[3] Froment G F , Van de Steene B 0, Van Damme P ,

Narayanan S and Goossens A G , Znd Eng Chem Proc

Des Devpt 1976 15 495

[l l] Buekens A G and Froment G F , Znd Engng Chem Proc

Des Devpt 1968 7, 435

[12] Allara D L and Edelson D , Int J Chem Kmefxs 1975 7

479

[4] Shah M I, Znd Engng Chem 1967 59, 71

[13] Murata M , Takada N and Ssuto S , I Chem Engng Jopan

1974 7 286

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