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SCHRODT

The Pennsylvania State University, University Park, Pa., and Applied Science Laboratories,

Inc., State College, Pa.

Relaxation Method

with any type of nonideality for which The equation is merely a material

This is an entirely new data are available. I t is not subject to balance stating that the quantity of

method for calculating prod- the difficulties in conventional methods the component present in the holdup

uct compositions in multi- when plate compositions change widely on plate n during interval i +

1 is equal

and in a complex manner with slight to that during interval i, increased (or

component continuous dis- changes in end compositions. Some decreased) by the net quantity added

tillation, when feed con- of these difficulties are particularly and removed as the result of the flows

ditions, flow rates, plate serious when automatic computers are of the two vapor and two liquid streams

used, because of the difficulty of pre- to and from the plate. The basic

efficiency, number of plates, paring adequate instructions for auto- equation can be immediately solved

and reflux ratio are estab- matic choice of successive trial values. to give composition x , ( ~ + ~ )in terms

In the relaxation method calculations of the composition and flows for interval

lished are made for the gradual change in all i. This working equation is

the plate and product compositions that

THE relaxation method has been de-

veloped for calculating the product com-

occur in a column from initial startup

until steady state is reached. The

Xfl(i+l) = Xni + 1 (VY(n.-,),i +

positions in multicomponent continu- equations previously used for batch Lx(n+ - Vya,i - Lxn.i) (2)

ous distillation, when feed conditions, distillation ( 5 ) with appreciable holdup An equation of this kind can be written

flow rates of product streams, plate effi- are used. The calculations may be for each plate and each component,

ciency, number of plates, and reflux started with all plate compositions equal and similar but slightly different equa-

ratio are established. By obtaining to the feed composition, but other tions can be written for the top plate,

several solutions for various numbers of starting compositions may be used. the feed plate, and the still pot. The

plates and various reflux ratios, optimum Use of the material balance equations equation takes a more complex form

operating conditions can be chosen with once for each plate gives a new set of when simplifying assumptions are not

certainty for a particular set of product plate compositions slightly different applicable (4).

purities and yields. Although based from those at the start. Repetition If the compositions and flows at any

on material balance and phase equilib- of this kind of calculation gives one set time,i are known, Equations 1 and 2 may

rium relations and plate calculations, after another of plate compositions, be used to calculate compositions at

the method is entirely different from which gradually approach the steady- time i +1, and the process repeated

any other. Each choice of operating

conditions leads directly to an answer

state compositions. When these are

reached, no further composition changes

to obtain values for time i +

2, and so

on. The necessary values of vapor

in terms of product compositions, re- occur upon repetition of the calculating composition, y, are obtained from the

gardless of the complexity of the problem, cycle. The steady-state solution is in- corresponding value of liquid composi-

number of components, extent of non- dependent of starting compositions and tion, x, by use of the applicable vapor-

ideality, irregularity of thermal re- holdup, but if the real starting compo- liquid equilibrium relation.

lations, or number of side streams. sition, holdup, and corresponding flow This same general procedure has

Thus successive solutions lead directly rates and time lags are used, the cal- Keen used in predicting the course of com-

to the desired optimum solution. No culations describe the approach to position changes and effect of operating

simplifying assumptions or approxima- steady state. variables in batch distillation with ap-

tions are needed. Other methods often preciable holdup ( 5 ) ,and more recently

lead to no solution, unless a great deal Basic Equations in studying the effects of column upsets

of experience and judgment are applied in continuous distillation and related

in choosing trial values. The basic equation is that for ex- control problems (6). Use of the pro-

The relaxation method is not uni- pressing the change in the moles of a cedure for continuous distillation design

versally preferable to conventional component present in the holdup on a calculations is simplified by the fact

methods, but is particularly advanta- particular plate, during any brief in- that the desired steady-state composi-

geous for complicated design problems terval during the distillation operation. tions are independent of the starting

involving multiple columns or compo- This equation is, in general terms, when compositions, and of the path toward

nents, nonideal equilibrium and thermal usual simplifying assumptions of dis- steady state. Thus any convenient

behavior, multiple feed or take-off tillation are applicable, set of starting compositions may be

streams, extremes of concentration, and

automatic control applications (6). I t

+

Hxn(i+l) = H ~ n i (VY(~-I).<+ used, without concern as to the path

followed.

requires an automatic computer, but Lxta+~),d- Vyn.6 - LXn.i) (1)

this need not be fast, nor large, unless where n refers to the plate number, and Basic Calculation Procedure for

many components are involved. Digital i refers to a particular interval of time,

computers are indicated because analog and (i + 1) refers to the next succeeding

Continuous Distillation Design

computers are limited to problems interval. Hrefers to the total moles 03 I t is most convenient to start the cal-

involving relatively few plates and few holdup on the plate; and V and L culations using feed composition values

components. The method can deal refer to the vapor and liquid flow rates. for all the plate liquid compositions,

I

_,

These are taken as the compositions flow rates V and L should be one fifth in the case of multiple feeds) and any

for time zero. The first step is the use to one tenth of the plate holdup, H, side product streams.

of the basic equation for the top plate to avoid distortions and instability in All flow rates (vapor and liquid in the

to calculate the composition of the the calculations. Arithmetical errors column, overhead, bottoms, and feed

and side streams). Absolute quantities

liquid from this plate a t the end of the must be eliminated by making an over- are not necessary, but correct relative

first time interval. The second step is all material balance of each component values must be used, and the feed rate

to use the basic plate equation to cal- after each new set of compositions is per interval must be one fifth to one

culate the composition of the sec- obtained. I t is also desirable to check tenth of the holdup per plate.

ond plate from the top, a t the end first and secondary differences in the Holdup on each plate and in reboiler.

of the first time interval. I n the compositions for successive intervals, The final steady-state compositions are

same manner the compositions at the as appreciable changes in these are in- independent of the choice. but arith-

end of the first time interval are cal- dicative of arithmetic errors. metic relations require that the holdup

be at least five times the feed rate per

culated for each of the other plates

interval.

and the still pot or reboiler. Alterna- Simplifying Assumptions Initial composition of liquid on each

tively the calculations can begin at the plate and in the reboiler. The final

still pot and proceed upward. In fact, The procedure as explained involves steady-state compositions are independ-

the calculations for the various plates some of the usual simplifying assumptions ent of the choice of initial compositions.

(at any one interval) may be done in of distillation calculations, but these are I t is convenient to use feed composition

any desired or random order, as the not inherent in the method. One ad- as the initial plate compositions.

calculation for each plate is independent vantage is the ease with which these

of that for all other plates. When all assumptions can be eliminated to make Application to Benzene-

the compositions for time interval one the method more rigorous, when de- Toluene-Xylene Distillation

have been obtained, the procedure is sirable. The application of new method may

reported over and over to obtain com- be illustrated by checking the solution

Constant molal overflow

positions for time intervals two, three, Perfect plate efficiency to the benzene-toluene-xylene distilla-

and so on. Negligible vapor holdup tion described by Robinson and Gilli-

I n general, most of the compositions Composition of liquid on a plate land ( 3 ) .

change rapidly at first and then gradu- identical with that of liquid leaving the This involves a 16-theoretical plate

ally approach steady-state values. When plate fractionating column with a reboiler

the latter are reached, the compositions which also acts as a theoretical plate.

The methods of modifying the cal-

no longer change from one interval to The column is to be used to obtain a

the next, and these compositions rep- culations to take these complexities

into account have been described in purified benzene overhead from a feed

resent the desired steady-state solution containing 60 mole % ' benzene, 30 mole

to the particular continuous distillation detail ( 5 ) .

% toluene, and 10 mole % xylene. The

problem under consideration. feed, which is a liquid at its boiling point,

Requirements for Calculation enters the column on the ninth plate

Arithmetical Precautions To carry out the calculation proce- from the bottom. The reflux ratio is

The calculation procedure is purely dure for a specific case, the following set at 2 to 1, and 60.17, of the feed is

arithmetical, but requires special pre- quantities must be known, specified, or to be taken overhead.

fixed by choice of a trial value: The moles of feed per interval are

cautions. The time interval must be

sufficiently small to avoid distortions arbitrarily fixed as 10. The correspond-

Total number of theoretical plates, ing overhead rate is then 6.01 moles with

that result when the quantities flowing reflux ratio, and relative quantities of

during an interval are large compared 3.99 moles as the bottom rate. Thus,

overhead and bottoms.

with the holdup on a plate. In general, Location of feed plate (or feed plates V , is 18.03 moles, L, is 12.02 moles. V ,

is 18.03 moles, and L, is 22.2 moles.

The holdup on each plate and in the

reboiler is taken as 50 moles. The cal-

culation is started with liquid of feed

composition on each plate and in the

reboiler.

All the above data were entered into

a digital computer, together with a

program for repeated calculation ac-

The curves show how the mole cording to Equation 2. The curves at

per cent benzene on various the left show the variation of typical

plates would change from plate compositions from the initial in-

initial startup until the column terval to steady state. At steady state

compositions teveled off when the top composition is 99.5% benzene,

steady state was reached. 0.5% toluene, and no xylene. and the

The steady-state compositions bottom composition is 0.5% benzene,

are the desired solution to 74.4%> toluene, and 25.1% xylene.

the continuous distillation Robinson and Gilliland (3) obtained the

problem same result, using the familiar Lewis and

,Matheson method.

10o[

I \ Bottoms

General Use of Relaxation Method

If the Robinson and Gilliland solution

to the benzene-toluene-xylene problem

was not available, and it was desired

'

0 20 40 60 80 100 120 140 to solve the general problem by the re-

NUMBER OF INTERVALS laxation method described, the number

MACHINE COMPUTATION IN PETROLEUM RESEARCH

a - ~ - ~ - ~ - ~ - ~ - aBOTTOMS

~ a , ~ ~ oPRODUCT

~o~a

of plates and the feed plate location

would not be known. I t would there- /a-

fore be necessary to choose trial values OoZ4F /

for these items and carry out a series of

trial calculations. The first might be

for ten plates with feed introduced on

plate 5 from the bottom. This would

give inadequate separation. Twenty

plates would give better separation than

that specified. Fifteen plates with feed

on plate 8 would not quite achieve the

desired separation.

The relaxation method does not avoid

repeated trials for a general distillation

design problem. However, each trial

does give the exact answer for distilla-

tion with the chosen conditions. Re-

peated trials give an assembly of correct

solutions for various conditions of op-

eration and a true over-all picture and

understanding of the effect of variation

in conditions on the results. In using

conventional methods, such as the Lewis- 0.0 I I

20

1

40 60

I

80

I I

100

I

120

I

I40

I

160

Matheson, all the trials except the last INTERVAL NUMBER

give no answer at all, but only a dis- The curves show how the mole fraction of component B of the ternary mixture on

crepancy in material balances that aids the various plates changes from its value of 0.01 2 at initial startup, to steady-

in choosing conditions for the next trial. state values that persist during continuous distillation

The successive trials thus provide but TOP PRODUCT

little over-all information about the ,o-o---rcJ-cJ-o-o--o--o-o-n-u~~~o~cr

especially useful in more complicated

problems where the conventional method

encounters serious difficulties in that

selection, of trial starting values is so 4

complex that it is difficult or impossible to c

find an answer even after many trials.

a 0 BO 4-cp-c-p-o-~-~-a-~-~-4-~-~ FEED P L A T E

5

problems whose solution is most worth P L A T E BELOW FEED P L A T E

i

while-Le., for cases of operation near P

minimum reflux, and where very small 0

a

a column are associated with very large

differences at the other end. Such ? 0 60

problems are easily solvable by the re-

laxation method, but difficult or impos-

sible to solve by conventional methods.

This is particularly true of nonhydro- 050- \ -0-

o/o~-o-o-o-o

BOTTOMS PRODUCT

carbon mixtures.

Side Stream Problem

The curves at the right give the solu- INTERVAL+ NUMBERS

tion to a problem in which a ternary The mole fraction of component A of the ternary first decreases and then rises

mixture consisting of two close boiling on the lower plates, as the progression occurs from initial startup to the steady-

less volatile components (B and C) are state compositions that are indicated b y the flat right-hand portions of the curves,

separated from a single more volatile Component C curves are not shown but would appear as approximately the

component (A). Side streams enter and inverse of those for component A

leave an upper plate, and feed is near the

program is given on page 740. This the interval by interval calculations

bottom. is applicable to any constant molal automatically and prints the answers

overflow three-component fractionation as it proceeds after each interval, or

Computer Program problem for any number of theoretical after any specified number of intervals.

The relaxation type of calculation is plates above and below the feed plate, The overhead and bottoms compositions

not easy without any automatic com- and any reflux ratio. The various flow are printed, but any other compositions

puter. rates in the enriching and stripping in the column may also be printed as

The sample benzene-toluene-xylene section, the holdup on the plates and in desired.

problem was programmed for solution the reboiler, th'k feed composition, and

on Pennstac, a medium-speed digital various constants, such as those found l i m e Required for

computer similar to the IBM 650. in the expressions for relative volatility, typical Solutions

The simplified block diagram for the are entered as data. The machine does The rate of approach toward steady-

as zero. This in no way upsets the cal-

E n t e r Initial Data

I n t o C a l c u l a t e Storage

I culations of the relaxation procedure,

but does cause difficulty in Lewis-

Matheson and other types of conventional

I

I_

I

calculations.

The relaxation method can be adapted

I A

Equilibrium Vapor for multiple feed and for side stream

S u b m u t i n e (EVSR) products, and can be used to solve mul-

Calculate r e l a t i v e v o l a t i l -

Reset t r a f f i c c o n t r o l s tiple column problems where the col-

an6 c y c l e e s c a p e s f o r umns are interrelated-for example, if

next i n t e r v a l .

bottoms from column one is the feed to

column two and part of the overhead

EVSR T r a f f i c Control. from column two is refluxed to column

ReguLates t h e EVSR so it Vi one. In every case the method proceeds

Tolerance Check

c e r t a i n p l a t e and s t o r e

positively and directly to the correct

See i f s t e a d y s t a t e has

been reached.

answers i n proper p l a c e . product compositions for the conditions

chosen, and when successive trials are

necessary, there is no uncertainty in

selection of new starting values. With

some modification, the method can be

EVSR Cycle Escape.

P r i n t i n t e r v a l number used to determine the time to reach

and d e s i r e d Determines when a l l t h e

steady state from an empty column

start, and to study control problems.

1 I I

Escape Acknowledgment

The investigations underlying this

MBSR CYCIE Escape Vateerial Balance Subroutine

(MESR)

work would not have been possible

Determines when a l l t h e new without financial support from the

l i q u i d compositions have Calculate the liquid

been c a l c u l a t e d . c o m o s i t i o n on a p l a t e h’ational Science Foundation in the form

a t t h e end o f an i n t e r v a l . of a grant to the Pennsylvania State

* I University.

MESR T r a f f i c Control.

Nomenclature

R e g u l a t e s t h e hBSR so i t w i l l o b t a i n c o r r e c t

H = total holdup per plate, moles

v a l u e s f o r a given p l a t e and s t o r e L = liquid flow rate, moles per time

answers in t h e c o r r e c t p l a c e . interval

V vapor flow rate: moles per time

=

state compositions is rapid a t first, but of successive trial values can many interval

extremely slow toward the end. Thus times become very complex, particularly x = liquid composition, mole fraction

a n approximate solution can be ob- if there is but little experience with the of any component

tained quickly, but a precise answer system. Shelton and McIntire (7) have y = vapor composition, mole fraction

requires an unduly long period of com- developed automatic computer pro- of any component

putation. The latter can be greatly grams for Lewis-Matheson type solution SUBSCRIPTS

reduced by determining the form of the called the feed mesh methods. Bonner i = number of time interval

first portion of the curve, and then extrap- (2) has developed a similar method. m = to identify a vapor or liquid rate

olating this to steady state. This ex- However, difficulties are sometimes en- below feed plate

trapolation can be included i n the over- countered in the choice of successive n = to identify a vapor or liquid rate

all computer program, so that compu- trial values and these become critical above feed plate

tation time is reduced to a nominal when they must be completely systema- 1, 2 . .16 = to identify a plate by num-

value. tized in advance in the form of program ber, counting from bottom up

instructions for the computer. Amund- Literature Cited

Evaluation of Method son’s (7) method avoids these difficulties (1) Amundson, N. R., Pontinen, A. J.,

The method presented here is basically by setting up simultaneous equations IND.ENG.CHEM.50, 730 (1958).

different from the Lewis-Matheson for the steady-state conditions, and (2) Bonner, J. S., Pittsburgh Meeting, Am.

method in that it determines overhead solving these by a matrix inversion tech- Inst. Chem. Engrs., September 1956.

(3) Robinson, C. S., Gilliland, E. R.,

and bottoms compositions, given the nique which requires a very large, fast “Elements of Fractional Distilla-

flow rates, number of plates, feed plate computer. tion,” 4th ed., pp. 219-29, McGraw-

location, feed composition, and relative Another difficulty in using the Lewis- Hill, New York, 1950.

volatility relations. The Lewis-Mathe- Matheson method is that of extremes (4) Rose, Arthur, Johnson, R. C., Chem.

Eng. Prugr. 49, 15-21 (1953).

son method essentially determines the in composition. For example, the final (5) Rose, Arthur, Johnson, R. C.

number of plates necessary to produce solution to a problem might indicate Williams, T. J., Zbid., 48, 549-56

overhead and bottoms compositions that the overhead is almost pure light (1952).

which are specified or desired. component and the bottoms contains (6) Rose, Arthur, Williams, T. J., Harnett,

R. T., IND. ENG.CHEW48,1008-19

If a problem involves an existing only parts per million of the same com- (1956).

column with a known number of theo- ponent. Under these conditions, the (7) Shelton, R. O., McIntire, R. L., Pitts-

retical plates, the relaxation method has top composition will sometimes be burgh Meeting, Am. Inst. Chem.

a definite advantage. Using this method vey sensitive to minute changes in bot- Engrs., September 1956.

is equivalent to having a pilot plant toms composition. I n the relaxation RECEIVED for review November 21, 1957

method the only effect of very small ACCEPTED March 7, 1958

column and actually operating it to

obtain the answers. Such a problem quantities of a component is that this Division of Petroleum Chemistry, Sym-

component might disappear entirely posium on Application of Machine Com-

can be solved using a Lewis--Matheson putation to Petroleum Research, 132nd

type method only by trial and error. For from the computer registers (usually Meeting, ACS, New York, N. Y., September

multicomponent problems the choice seven or more decimal places) and appear 1957.

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