NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the...

25
NATIONAL ADVISORY COMMITTEE FOR AERONAUTICS TECHNICAL NOTE 2342 EVALUATION OF PACKED DISTILLATION COLUMNS I - ATMOSPHERIC PRESSURE By Thaine W. Reynolds and George H. Sugimura Lewis Flight Propulsion Laboratory Cleveland, Ohio Washington April 1951 https://ntrs.nasa.gov/search.jsp?R=19930082981 2020-04-02T08:52:04+00:00Z

Transcript of NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the...

Page 1: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NATIONAL ADVISORY COMMITTEE

FOR AERONAUTICS

TECHNICAL NOTE 2342

EVALUATION OF PACKED DISTILLATION COLUMNS

I - ATMOSPHERIC PRESSURE

By Thaine W. Reynolds and George H. Sugimura

Lewis Flight Propulsion Laboratory Cleveland, Ohio

Washington April 1951

https://ntrs.nasa.gov/search.jsp?R=19930082981 2020-04-02T08:52:04+00:00Z

Page 2: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NATIONAL ADVISORY CO4ITEE FOR AERONAUTICS

TECHNICAL NOTE 2342

EVALUATION OF PACKEH) DISTILLATION COLUMNS

I .ATMOSPBEBIC PRESSURE

By Thaine W. Reynolds and George H. Sugimu.ra

SUMMARY

The 6- and the 7-foot-packed-height laboratory glass distillation columns and the 30-foot-packed-height stainless-steel distillation columns in use at the NACA Lewis laboratory were evaluated Four column-packing combinations of the glass columns and four column-packing combinations bf the steel columns were investigated at atmos-pheric pressure using a test mixture of methylcyclohexane and 2,2,4-trimethylpentane. Theoretical-plate values and pressure-drop data were obtained for the column-packing combinations investigated..

It was confirmed that preflooding of a'column was necessary to obtain maximum separating efficiency. The glass column with wire-coil packing had theoretical-plate valuesranging from about 80 to 190 over its operating range. These values were from 2 to 4 times the theoretical-plate values obtained for the other glass columns of the same length.

The 30-foot-packed-height steel column with a 2-inch diameter and. stainless-steel helix packing had theoretical-plate values from

l . to 2 times greater than those obtained with the 1/4-inch Ben

saddles end 2 to 3 times greater than those obtained with the 3/8-inch Raschig rings. The 1-inch-diameter column with helix packing had a maximum theoretical-plate value of over 200 at low reflux rates.

The deviation of the test mixture from Ideality is shown to be sufficient to have considerable effect on the calculated theoretical-plate values.

I1'TR0DUCTI0N

The NACA Lewis laboratory has been engaged in the preparation, of pure hydrocarbons for several years in order to obtain correlations of molecular stru.cture rith engine performance and with other physical and

Page 3: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

2

NACA TN 2342

chemical properties of the compounds. In the purification process to obtain these pure hydrocarbons, distillation is extremely important. Distillations to obtain maximum purity of a compound often consume the greater part of the total time required for the complete synthesis of the compound. Purification of commerbial starting materials also often requires considerable time. Consequently, it is important to know the operating characteristics of the distillation equipment being used. in order to obtain the most efficient performance for any particular required separation.

In order to determine efficiency, pressure-drop, and reflux rela-tions of the various types of distillation column and packing in use at the NACA Lewis laboratory, an investigation was conducted under the various operating conditions commonly used. This report describes the 6- and 7-foot-packed-height glass columns and the 30-foot-packed-height stainless-steel columns, which have been in use at this laboratory for over 8 years, and presents the performance data of this equipment at atmospheric pressure.

APPARATUS

Steel column. - A diagram of the typical stainless-steel distilla-tion column used in this investigation is shown in figure 1. All the columns were basically of the same construction but differed in the type of packing used. The height of the packed. sections were 30 feet, the over-all heights of the columns were 37 feet, and the column diameters were 1- or 2-inch standard pipe size. Pots of 10- and.. 20-gallon charge capacity were used.

All of the metal in contact with the distilling mixture was 347 stainless steel with the exception of the flange gaskets, which were of annealed copper • The pot was heated by three resistance ele - mente wound. concentrically beneath the pot and connected so as to give cntinuous control from 0 to 5 kilowatts power input.

The column section was surrounded by a thin sheet-metal jacket, which was wound with three separate lengths of asbestos- and glass-covered resistance heating wire. Each circuit , had. a capacity of 2 kilowatts and was separately. controlled. by a variable transformer.

The entire column was then lagged. with a 1'-inch thickness of magnesia insulation.

The packing was supported. at the pot flange by a sieve cone with perforated. area equal to the cross-sectional area of the column.

Page 4: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NACA TN 2342

Cooling water was metered to the head. condenser through a rotanieter and its temperature increase through the condenser was taken as a measure of the rate of reflux in the column. Thermocouples were located in the pot liquid, on the column and the sheet-metal jacket at the center of each heating section, and. at the top of the packed section just before the head. condenser.

A manometer for measuring pressure drop was connected. to the pot. and was purged by a very slow stream of nitrogen visually metered through a bubbler system.

Glass column. - The type of glass column used. in this investigation is shOwn in figure 2 • The over-all height of all glass columns was froni 9 to 10 feet with packed heights of either 6 or 7 feet.

The glass column was surrounded by a length of 2-inch' steel tubing around which was wound two separate lengths of resistance heating wire, each of 500-watt capacity and. each controlled by a variable transformer. The column was then covered. with pipe insulation. A •ground-glass joint at the bottom of the column permitted use of various sizes of flasks for the distillations. Pot heat was supplied. by a heating mantle con-trolled. by a variable transformer. The condenser unit Is described. in detail in reference 1. -

The columns were set up so that they could be operated at atmos-pheric or reduced pressures. Pressures below atmospheric were maintained by a commercial metal cartesian-diver-type manostat mounted between a 30-cubic-foot-per-minute vacuum pump and a, 4-cubic-foot-capacity surge chamber. In practice, a bank of several columns operating at the same controlled pressure is connected to one surge tank.

Four different sizes of glass columns were tested: (1) 22-millimeter outside diameter, 6 feet long, (2) 22-millimeter outside diameter, 7 feet long, (3) 32-millimeter outside diameter, 6 feet long, and (4) 22-millimeter-inside-diameter, 6 feet long.

The 22_millimeter_inside-diameter column had a silvered vacuum jacket and. was not covered with resistance heating wire and pipe insulation as were the other columns.

• Packing, - The following packing materials were tested in the steel columns: (1) 1/8-inch single-turn stainless-steel helices, (2) 1/4-inch porcelain Ben saddles, and (3) 3/8-inch porcelain Raschig rings, The packing materials tested in the glass columns were (1) 3/16-inch single-turn glass helices, and (2) a wire-coil packing described. in reference 2.

Page 5: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

-4

NACA TN 2342

TEST vT2(TTJFE

The mixture used for these experiments consisted of methylcyclo-hexane and 2,2,4-trimethylpentane, which was chosen because it had a relative volatility of approximately 1.049 and. was reported. to be ideal (reference 3). In attempting to run check curves on the columns with mixtures covering different composition ranges, however, the mixture deviated considerably from ideality at the low 2,2;4-trimethylpentane end. of the concentration range, This deviation is confirmed. in figure 3, which is plqtted from data of reference 4, and shows this trend. of relative volatility with concentration.

- The theoretical-plate values reported herein were calculated using the following Fenske equation (reference 5) and a relative volatility of 1.049: -

N =(xd'\ /1_Xr1

'loge e ( l-xd) X )J where

N number of theoretical plates including the still

a relative volatility of mixture

Xd mole fraction of more volatile component in distillate

Xr mole fraction of more volatile component in residue

Both components of the test mixture were purified. br fractional distillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

The following refractive index - composition relation was estab-lished at 200 C using known mixtures by measuring the refractive index on a five-place precision refractometer:

40 = 1.39147 + 0.02543x + 0.00612x2 where

0 . 0 n D refractive index of mixture at 20 C

x mole fraction of 2,2,4-trimethylpentane in mixture

I

Page 6: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NACA TM 2342 - 5

1hen a constant value of relative volatility is used., a single plot (shown in fig. 4 and suggested. in reference 6), can 'be made by combining the refractive index - composition curve and. the. theoretical-plate equa tion, This curve is useful in making rapid checks on the theoretical-plate values for given residue and distillate compositions and. shows the limitations of the range of theoretical-plate values that can be measured without large experimental errors. For example, if distillate and. residue compositions are approximately equidistant from a mixture of equal parts and the accuracy of reading refractive index is within 0.00Ol, theoretical-plate values of 60 would then have an ind.eteiminanóy

of thl plate and at 160 plates the indeterminancy would be about ±7 plates. The indeterminancy rapidly increases above theoretical-plate values of l6O

Actual-plate values will be lower than those calculated from the value of relative volatility of 1.049, especially when concentrations very low in 2,2,4-trimethylpentane . are involved.

PROCEDURE

The test mixture was charged. to the column and the pot and. column heats were applied until the material, was refluxing at the top of the column.- The column heats were then adjusted. until the jacket tempera-ture and. the corresponding column temperature were approximately the same. For the glass columns, the, inside temperatures were estimated. from the vapor temperatures at the top and the bottom of the column. The not heat was then' increased. until flooding occurred at the top of the column, after which it was decreased to give a reflux rate just below the flooding point. The column was refluxed under these condi-tions until equilibrium was attained., which required from 24 to72 hours. Test samples from the pot and. head were periodically taken until no• change in composition occurred.. Samples for analysis were then taken and. the reflux rate was decreased The procedure was repeated until the reflux rate had. been decreased to a miniurtim value.

After the flooding point had. been determined, the runs without pre-flooding were mad.e using the procedure previously described except that the initial setting of reflux rate was below the flooding point. The data for the unflooded column with saddle packing were taken at increas-ing rates rather than decreasing reflux rates.

Page 7: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

6 NACA 2342

DISCUSSION OF RESULTS

Glass columns. - In comparing the experimental results of the various columns, it should be noted that the absolute theoretical-plate values are somewhat lower than the values reported herein because of the increase in relative volatility of the mixture at low concentration of 2,2,4-trimethylpentane.

The performance of the four glass columns with and. without pre - flooding is shown in figure 5. The advantage in efficiency to be derived. from preflooding the column (references 7 and 2) is evident from this figure; increases in number of theoretical plates from 17 to 55 percent were ohtined after preflooding.

In figure 6, a comparison of the theoretical-plate values of the four glass coluiis after preflooding is shown. The wire-coil-packed column, with theoretical-plate values anging from about 80 to 190, was from 2 to 4 times more efficient in separating the test mixture than any of the other glass columns. The 7-foot glass column with an outside diameter of 22 millimeters showed. an increase in plate efficiency that would be expected for a corresponding increase in length over the 6-foot column of the same diameter. The column with a 32-millimeter outside diameter showed a slight increase in efficiency over the column with a 22-millimeter outside diameter of the same packed. height. This result is contrary to the usually expected trend. of efficiency with diameter and is undoubtedly a result of the relative size of the packing to column diameter. For any nominal-diameter helix packing there is an optimum column diameter for highest efficiency. At ratios of packing diameter to column diameter less than or greater than the optimum, channeling of the liquid and vapor flows occurs and decreased efficiency results. For the 3/16-inch helix packing used, the optimim column diam-eter is apparently greater than 22 millimeters. The efficiency of all columns increased with decreasing reflux rates.

The pressure drop throuh the four glass columns is shown in figure 7. The pressure drop through the wire-coil-packed coli.mai was 2 to 3 times greater than that through the other columns at the same vapor velocities.

Steel columns. - The theoretical-plate values plotted against reflux rates :or the steel columns are shown in figures 8 to 10. The increase in relative volatility of mixtures low in 2,2,4-trimethylpentane conbentration, hhm in figure 3, is confiined in figure a. As the concentration range of the mixture approaches the low 2,2,4-trimethyl-pentane contents, the theoretical-plate values calculated from the assumed constant value of relative volatility will increase • As shown.

Page 8: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NACA T 2342 7

in figure 8, when smaller concentrations of 2,2 ,4-trimethylpentane were used. in the charged. mixture, the theoretical-plate values were higher for a given reflux rate • In comparing columns, it was therefore necessary to use as nearly the same concentration range of test mixture as was pos-sible for each test in order to make the comparison valid..

The 2 -inch-diameter column with no packing had. theoretical-plate values of from 6 to 12 over the reflux-rate range, as shown in figure 10. The empty column could. not be flood.ed. with the power available. The 2 -inch-diameter column packed. with 1/4-inch Ben saddles had. theoretical-plate valuea of about 84 to 94 after preflooding over the reflux-rate range shown, with a minimum value at a reflux rate of about 8 liters per hour (fig. 9(a)). The 2-inoh-.diamneter column packed. with 3/8-inch Baschig rings (fig. 9(b)) bad. theoretical-plate values after preflood.ing of abou.t 58 to 62 over the reflux-rate range shown with a minimum value at a reflux rate of about 8 liters per hour. This minlimim in the curves has been previously observed. for saddle and. ring packinga (reference 8). The efficiency of all packings in the steel columns was increased. by preflooding.

The high ratio of packing to column diameter in the case of the ring-packed. column caused. poor efficiency in comparison with the saddle-packed column. The size rings tested. was not considered. as optimum but merely representative of the packing that had. been in use in the column for some tithe.

The theoretical-plate values after preflooding for all packings in the 2-inch-diameter column and for the empty 2-inch-diameter column are shown for comparison in figure 10 • The efficiency of the helix packing rapidly drops off with increasing reflux rates, whereas the saddle and. ring packings are nearly independent of reflux rate although they- do exhibit a minimum theoretical-plate value at a reflux rate of about' 8 liters per hour. The efficiency of the empty column is also essen-tially independent of reflux rate, except at very low rates.

The helix packing with theoretical-plate values ranging from about

115 to 179 bad. efficiencies that were about 1- to 2 tImes higher than

those of the 1/4-inch Ben saddles and. about 2 to 3 times higher than those of the 3/8-inch Raschig ring packing.

The 1-inch-diameter column packed. with 1/8-inch stainless-steel helices gave separations at total reflux that were too close to 100 per-

cent to obtain accurate theoretical-plate values from the concentrations. Maximum efficiency exceeded. at least 200 theoretical plates at low reflux

Page 9: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NACA TN 2342

rates. The possible separation that can be obtained is shown in figre 11 by the variation in distillate and residue compositions of the test mix-ture throughout a distillation using this column. The reflux ratio varied considerably during this distillation but averaged about 160 to 1.

The pressure drop through the steel columns is shown in figure 12. The pressure drop through the empty column was too low to be measured with any de'ee of accuracy on the mercury manometer and therefore was not plotted. Pressure drop through the 1-inch-diameter helix-packed column and the 2-inch-diameter saddle-packed column were about the seine below a vapor velocity of . about 0.8 feet per second. The pressure drop through the 2-inch-diameter helix-packed column was the highest of the páckings tested at vapor velocities below the flooding point.

SUM4ARY 0]? RESULTS

An evaluation was made of combinations of four glass and of four steel distillation columns with various types of packing. The following results were obtained°at atmospheric pressure using a test mixture of methylcyclohexane and 2,2,4-trimethylpentane:

1. Pre±'looding increased the theoretical-plate values for all pack-ings tested. The increase over unflooded operation was as high as 55 percent with the glass column with wire-coil Dacking.

2. The 6-foot-packed-height-glass column with wire-coil packing iad theoretical-plate values of about 80 to 190, which were 2 to 4 times the theoretical-plate values of columns of the same height packed with 3/16-inch glass helices.

• 3. The 1-inch-diameter steel column with l/8-inch stainless-steel helix packing gave separations indicating a maximum theoretical-plate value of over 200 at low reflux rates.

4. The 2-inch-diameter steel column with 1/8-inch stainless-steel helix packing had theoretical-plate values of 115 to 179. These values

were l t 2 times higher than those obtained with the 1/4-inch Berl

saddle packing and 2 to 3 times higher than those obtained with the 3/8-inch Raschlg ring packing In the same diameter columns,

Page 10: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NACA TN 2342

9

5. The deviation of the test mixture from .ideallty is sufficient to have considerable effect on the calculated theoretical-plate values.

Lewis Flight Propulsion Laboratory, National Advisory Conmiittee for Aeronautics,

Cleveland, Ohio, August 31, 1950.

PEFEPENCES

1. Diehi, John M., and Hart, Isaac: Vacuum Column Head. Anal. Chem., vol. 21, no. 4, April 1949, pp. 530-531.

2. Podbielniak, Walter J.: Apparatus and Methods for Precise Fractional-Distillation Analysis. mci. and En.g. Chem. (Anal. ed.), vol. 13, no. 9 Sept. 1941, Pp. 639-645..

3. Wlllinghain, Charles B., and Rossini, Frederick D.: Assembly, Testing, and Operation of Laboratory Distilling Columns of High Efficiency. PP 1724, Nat, Bur. Standards Jour, Res., vol. 37, no. 1, July 1946, pp. 15-29.

4. Gelus, Ethrd, Marple, Stanley, Jr., and Miller, M. E.: Vapor-Liquid - Equilibria of Hydrocarbon Systems above Atmospheric Pressure. md. and Eng. Chem., vol. 41, no. 8, Aug. 1949, pp. 1757-1761.

5. Fenske, M. B.: Fractionation of Straight-Run Pennsylvania Gasoline. md. and Rug. Chem. (md. ed.), vol. 24, no. 5, May 1932, pp. 82 485.

6. Lecky, Herbert S., and Ewell, Raymond H.: Spiral Screen Packing for Efficient Laboratory Fractionating C olun3ns. md • and Eng. C hem. (Anal. ed.), vol. 12, no. 9, Sept. 1940, pp. 544-547.

7.Tongberg, C. 0., Laoski, S., and Fenske, M. R.: Packing Material for Fractional Distillation Columns. md. and Eng. Chem. (md. ed.), vol. 29, no0 8, Aug. 1937, pp. 957-958.

8. Kirschbaum, Emil: Distillation and Rectification. Chem. Pub. Co., Inc., 1948, Pp. 313-314.

Page 11: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

.c.

en

10

NACA TN 2342

Vent

Fire 1. - Stainlees-eteel dist111ation column.

Page 12: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

Vacuum pump

'[1 Product receiver

óhamber -Packing Glass column Steel-tubing jacket

Resistance heating wire

-lnsulation

Bubbler

NACA TN 2342

11

Pressure regulator

Condenser Nitrogen

Packing support Cone

F— Mantle and. 110 volt a.c.(? ' I I pot support

Variable transThrnier

I Figiue 2. - Glass distillation column.

Page 13: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

12

NACA TN 2342

V

0 H

4-, a,

"1

4 0

4-, C-) cj

CH

a)

('J

H

0

+'

a,

a'

0 -1 0 C.' H

4.) a, E

d. :1 C

a, a,O a'a)

a,4-i 4a)

a,4 q1

+. a,.

a3 -4.)

c'J -a,

c-I 0 4.)

4.) 9.4.

a)

0o

4-' .,-I HO 1 I

0P4

•d a5 4-) H a,

çr

0 aD H 0 0 0 r H H H

4cqç-oA ATTH

Page 14: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

13 NACA TN 2342

120

100 H 6o

'-4

"-4 '1.0 0

0

20 U

43 "3

'-I '-I '-I 4., U •.-i 0

"'-4 0

4.,

-100

1.390 1.3911. 1.398 1.11.02 1.11.06 1.11.10 1.11.111. i.1a8 1.1122 1.11.26

Refractive index of mixture at 20° C

Figure 11.. - Curve for determining number of theoretical plates from refractive index of distiflate and residue samples for mixture of methylcyclohexane and 2,2, l1.-trimethyl-pentane, N - nd-nr, where N is total number of theoretical plates.

Page 15: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

0 c-4r1

00

* _ _ __

__- __ __

/3/

..1 LI\ 0

zt H

•0 Ii-' (\j

H

0 H

.1-I

a) 4.,

H a, z

14

NACA TN 2342

a)C) Or-I a l p

a) a) a)

H r-I-1 4.'

c',C)

.1-I

a) 4.' 43

0 a) •1-4 El a) I

U) LI)

0•1-4

'- cz4

s3 td t Jo .IOq1mlI

Page 16: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

-

C) _j - ______________ 4- ida) o od 00

- 0 diiH - •t-1 t1H +3

____ ____ ____ ____ ____ ____ ____

- 0 - ___ ___ ___ ___ ___ ___ ___ C-)

/°o •/ •

___________ 4 -)-__ __ __ __ __ __ __ __ __ V

\0 H

a) C.) '-I '-4 a)

HH H

0 0 • C)

0 ..-4 4.,

CD H H - H H .-4

- w .1-I

.1-I

C)to

i-I

0 H ' a) CI_4 a)

'I

-

H H C.)

4.)

a) .-a-).

4.)

I H a-

-4.0

-p a)

a) (\J

4)

to 4.)

0

NACA TN 2342 15

0 0 IC\ 0 - - cY_ (Y C')

s2Id Tr.xoQtfl JO .I3Ufll

Page 17: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

H

(1 H

0 H

r H

a cC a)

4)

H

a)

42 a) a)

C4

N

4.3

.-4 a). a) 'do

OQ) p4

a) S.. a)

H'-f H'

.5

Q5PI .T-1

a)

a)

0 C.)

0 4.) H H 4., a)

•1-4

a) C')

H

0 a, a)

H

a) 4., H. P4a) H OH a) 0

a

•r4 4, 0 0

U-'

a)

f.z4

16

NACA TN 2342

:1 iii 7 0

__

___ ___ - U

____

OLi

0 0

.20 Lf\ L) Lt

LI-' _* (Y

txot. jo .Iaqunl

-('I 0 rr

Page 18: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NACA TN 2342

17

(l '-I

O .1.

H 0

H H 4., a,

4' o H a, a,

-.4-4 'SO' •I-

4'0 bO

a, cO I

a, 0

a) rZ '

\OG) ;a, 'j 4-' OH O • r-1 u-40 4.)O .-

fl.-4

.-i ..

L.r -4O 0 .,-15: Q) - c'J 0 --.

a) a, 4.'

H 0 0

C-)

I

U

q 1 d& o Od

00 HO

O q-,r-1 .,-I cDq-i 4.'

0 0

o - 0 0 0 0 0 c'j co .zr

S3 Td a.xotq. jo .zqumj

Page 19: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

18 NACA TN 2342

- 2 6 8 10 12 i1 16, Reflux rate at boiling point, mi/mm

Figure 6, - Comparative theoretical-plate values after preflooding of glass distillation columns,

20C

18c

i6c

hg

&

2C0

vHHHW Distillation column

v I.D., 22 xrun; packed height, 6 ft 0.D., 22 nun; packed height, 7 ft -0.D., 32 nun; packed height, 6 ft

o O.D., 22 nun; packed height, 6 ft V

iiiiiiIiiiiiiii _\ -

-----------------------

V

= -

ill

H p4

' 12( U

"-I

0 41)

+' 10( 4-4 0

8

Page 20: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

4-'4.,-p4., c-44-I'44-4 '0 L- 'O '0-

4-) .4.) 4.) .4)

•-1 .,-i .,-4 .H ,-i a)a)aQ) N0• 0

•rf C)OC)C.) I___ -p ___ V i-I •, •, sa .n

-p \ • V V •s-4 CJCJC,JCJ

\ - \ - -C\3e4(C'J

. S S S

S - \V \V • S S

4-4000 iiiiiiii N

H 0 C-)

0

4-) a5 H H

4-) CI) C-, .r-4

a) Cl)

In 4-)

Cl) c-i

H to

4.)to 0

0 0 H a)4-) 24 0 0

a a)

Ia)

N-

NACA TN 2342

19

0 0 0 0 0 0 '0 Lc\ - '-. (\j H

(ti 'TA oTjToads) ot ez-y imu 'doip mssIa

Page 21: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

20 NACA TN 2342

iii ii:i

E Pd O\cO . . ON-

0)10 0_ . - l •'

-

1H-0'.° 0 J.

/ II2IIIIII

co H H 1) 0)0

0) H H

Wa)

Or-I 0) H

H in aiu)

H 0J H

Pu -i r.

. 0 - 0

in (_4 4-)' a) +) a)cO i-I-----

•rl OH H 0) -

0)O4

aD '$ 00) H ) 4-I •rI•i-1 0) ind

0 0 •rl 0)0)

r4 E

c-I 0 i-I 4-'O 00

4-40 0) 4.)

H or-I 4.)

o0 • 0 0 0 0 o co '-o - 0 0) H H H H

s td i t1O9t jo

Page 22: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

NACA 'fl'T 2342

21

90

Conditjo of packing

-:--- - 0 Preflooded -

0 Unflood.ed.

0

I

8C

0

Q) SI 0

70 4.)

eM

(a) Packing, 1/4-inch Ben saddles. 0

70

60

I 8

Reflux rate, liters/hr

(b) Packing, 3/8-inch Raachig rings.

Figure 9. - Theoretical-plate values for stainless-steel distillation col1mma with 2-inch diameters with two packings.

0

0

Page 23: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

I IPacking -

1/8-in, stainless-steel helices —G 1/Ii._in. Ben saddles -

0 3/8-in0 Raschig rings _D None -

- - - - -

-

-

- - - -

-

- -_–z—___

0 ____ - 2 - - = == = -

180

i6c

li.0

120 U) II)

4) H P1

lOC C)

43 'V

[r1

6c

2(

22

NACA TN 2342

0 2 11. 6 5 10 12 1 lb Reflux rate, liters/hr

Figure 10. - Comparative performance after prefloodin.g of stainless-steel dis-

tillation columns with 2-inch diameters and various packing materials0

Page 24: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

a) 4., a) Cd H H P H

•1-4 Cd (I)

0

L) 0 0 0 0 C\J

jo .u.rad

NACA 2342

23

0 0) -Ia) 'd a) Cd bD4d Cd

a) Cd

o \0OH. G) -I 0 0 #'.c rI

w) a) a E

0• E'dr1 Lr\ 04C) 0Cda)G) 'd OJQ)a)w a) +'E

Q) r4+'rICO Ha) 00 -4U) H .0 +'Pi ) 0)rl •I --Cd +' +'CI) da)H a) O.Z1 0 Cdd00

0 j Q)4. crp i0 't -* d cO

'3) .rl 'P-. WCjCdH ; 0) i-1 H i(\Jr-1 - 0 •,-ltO . 0 00C.-1H

a)d (30 04 Cd+'

0 r4HP ++'a) 0 Cd 1 1) "'\0

cd '0) - C) -roc-40-H 00) .-4

I G)04 SI H Cd

• OSI .4

-

Cd 4-' Pr- C0tH S-ir-4 •v-4.4

0Fi

Page 25: NATIONAL ADVISORY COMMITTEE FOR AERONAUTICSdistillation and. the samples used. for the column-testing program had purities of 99.5 mole percent as indicated. by freezing-point analysis.

24

NACA TN 2342

7C

6c

5C

j3

Co1n Packing diameter

(in.)

2 .1/8-in, stainless-steel heilces

c) 2 1/11._in. Ben saddles 0 2 3/8-in. •Raschig rings ci 1 . 1/8-in, stainless-steel

helices

-

. . )- '--t---------

1111117 11II ---------7--e-7.

0 .2 .11. .6 .8 . 1.0 1.2 1,11. Vapor velocity, ft/sec

Figure 12, - Pressure drop through various packing materials in 30-foot-

packed-height stainless-steel distillation columns.

NACA-Langley - 4-19-51 - 875