ABSORPTION AND EXTRACTION

SYMPOSIUM

COMMITTEE

Downloaded by UNIV OF GEORGIA on October 13, 2009 | http://pubs.acs.org
Publication Date: June 1, 1950 | doi: 10.1021/ie50486a013

Ernest W. Thlele, Chairman
James N. Addoms
Walter E. Lobo
Manson Benedict
Elliott J. Roberts
Allan P. Colburn
J. Henry Rurhton
Presented before the Division of Industrial and Engineering Chemistry of the American Chemical Society
a t The Ohio State Universlty, Columbus 10, Ohlo, December 29 and 30, 1949

Commercial Extraction
V. S. MORELLO AND NOLAND POFFENBERGER
THE DOW CHEMICAL COMPANY. MIDLAND, MICH.

T

HE literature on liquidliquid extraction
mainly with phase relationships, stage calculations,
anddiecussion of the mechanism of mass transfer be-

supply a more or less steady
demand. In
I are
listed the major processesin
which the use of commercial
extraction equipment has
been reported+ Most of
tnreen two liquid phases.
designs of such equipment have been reproduced herein.
these processes are well
The published information
established in American inon commercial extraction
dustry, and the processes
could not be operated a t a comparable scale or as efficiently withequipment, particularly the types used and performance data, is
out satisfactory extraction equipment.
rather limited.
Hunter and Nash ( S 4 ) have written several papers containing
GENERAL CONSIDERATIONS FOR DESIGN OF EXTRACTION
brief notes on extraction equipment. Two reviews by Waeser
PROCESSES
(46, 46) written in Germany during the war have become available in this country. Green (19) in England reported on solvent
As disrussed in detail, and particularly as to theory, by Beneextraction with special reference to fine chemical manufacture.
dict ( I ), all physical separation processes essentially are ones in
However, the best discussions to date have been those of Elgin
which power is expended to make a separation. An extraction
in Perry’s Handbook (38)and his several annual reviews (10, 11)
process is only one of the several available means by which the
published since that time.
power may be expended with reasonable efficiency for the desired
This paper is an attempt to summarize all of the information
purpose. Here the power expended is largely the heat required to
available to date on commercial extraction equipment. The
recover the solvent. The primary limitations on the choice of a
sources have been the general literature, patent literature, and
solvent are that its density be different from that of the diluent,
data from manufacturers and operators of extraction equipment.
that i t be at least partially immiscible with the diluent, and that
The review of the patent literature is presented because i t is a
the solvent be recoverable. These basic limitations usually are
tedious process for an individual engineer and not very informaless severe than those for an azeotropic agent, or those for a soltive unless the reviewer goes back to the original patents. The
vent for extractive distillation. Economic considerations add
patent literature contains little performance data on extractors,
restrictions as to dissolving power of the solvent for the solute,
but does furnish many ideas on how extractors may be built and
selectivity, boiling point, chemical stability, and ease of separawhere they are operated. Only a few of the extractors described
tion from both the solvent and the diluent.
in the patent literature can be discussed in the paper. However, a
The cost of operating the extractor itself, which includes capital
complete listing of the patents reviewed and classified is given in
charges, labor, repairs, and power to extractor unit only, are but
the patent bibliography.
a small part of total cost of operating an extraction process.
Major cost items in their approximate brder of magnitude are:
USE OF COMMERCIAL EXTRACTORS
T h i s paper presents an attempt by the authors to Summarize all the available contemporary data on commercial
extraction equipment. Their sources Were the general
literature, patent literature, and data from manufacturers
and operators of extraction equipment. Several patented

The term “commercial extractor” in these discussions means a
continuous countercurrent liquid-liquid contact device which is an
essential part of a process operating to produce a chemical to

1. The power (heat) required to separate the solvent from
the extract and raffinate streams and to fortify it to a specified
purity.
1021

selectivity wetted by the discontinuous phase. except those where special precautions are taken to prevent drop formation. or to redisperse the dispersed phase. INDUSTRIAL AND ENGINEERING CHEMISTRY Major Commercial Applications of LiquidLiquid Extraction Processes I. Gas works liquids. Vol. It merely suggests that the cost of operation of the various possible types of extractors will be close. In many designs of baffle tower. Evans. Wood distillation B. Thus in columns in which both films and droplets are present. Sherwood. particularly as to wetting effect. deasphalting. Perforated Rettler 2. and considerations not directly concerned with the extractor frequently dictate their final selection. Rasohig process.1021/ie50486a013 Table I. Most commercial extractors are of the gravity type. large surfaces are provided upon which the dispersed phase spreads as a film. 2009 | http://pubs. 6 The major classification is determined by whether or not gravity or centrifugal force is used to separate the phases. and decarbonieing operations 11. Contact made with one phase one phase as a film dispersed as droplet8 1. k%ble cap tower 5. contacting is done with one phase continuous and the other spread out to give the necessary large interfacial area. unless the solid accumulation could be easily washed or dissolved from the packing. 42. The writers and the operators believe the major consideration is the selection of a design which gives the greatest freedom from operating and maintenance troubles. Recovery of acetic acid from dilute solutions from cellulose ac0tate. recovery and by-product phenols C. (This varies considerably. and the extraction step serves to remove interfering impurities to a concentration sufficiently low to permit the final purification by distillation. In addition to saving power necessary for redispersion. The above discussion should not be construed to mean that there is nothing to be gained by proper design and selection of extraction equipment. Phenol Recovery A.acs. when the dispersed phase passes the edge of the baffle. Treatment of .1022 Downloaded by UNIV OF GEORGIA on October 13. all play an important part in determining the type of contact. Capital and labor charges of the distillation equipment. Since the processes usually are designed for minimum total over-all cost. Droplet extractors may be divided into two types. This is particularly true where the purpose of the whole process is to obtain one or more materials of high purity. Spray tower 1. When additional . Lubricating oils treated with selected solvents Edeleanu (Jiquid Sod Chlorex [bis(Z-chloroethyl)ether] Duo-Sol Furfural Nitrobenzene Phenol C. seem to favor film-type transfer. This type of extractor has several advantages over other types. Psokedtower with movable members 11. and their flow rates. Baffle tower and 3. For this reason baffled towers. TYPES OF EXTRACTION EQUIPMENT The scheme of Table II is suggested for classifying liquidliquid extraction equipment. perhaps a t an accelerated rate. Dewaxing. have been considered droplet extractors. Petroleum Refining A. when reliable performance data become more widely distributed and accepted. Classification of Extraction Equipment (Liquid-liquid mass transfer equipment) Two Phases Separated by Gravity A. As an example. there is no maintenance of stuffing boxes. Separating one or more groups of compounds from cuts of wide boiling range 1. Chemical Processes with Liquid-Liquid Contacting A. long shafts. primary phenol production B. and Longcor ( 4 8 ) have shown in tne case of spray towers that an appreciable percentage of the total extraction occurs in the actual formation of droplets. large packing. Vitamins and Antibiotics VI. This is done either by forming a film on a solid of suitable design. E x t r a 2. All known types of extractors can be readily classified by this scheme with but few examples where cross or double listing would be desirable. Baffle 4. Separating high purity products Toluene Butadiene Olefins B. and provision is made to direct the flow over the baffles so that there is appreciable contact through films. However. i t is broken into droplets. it is difficult or impossible to evaluate how much mass transfer is provided by the film and how much by the droplet. Packed towers may operate with the discontinuous phase either spread out as a film over the packing or largely dispersed into droplets. The subclassification of the gravity-type extractor (group 1) as to form of interface is not so clear. together with high viscosity of the discontinuous phase andlow flow rates. Packed towers power used to power used Large packing grids maintain disper. Edeleanu ( 0 8 ) 2. Because of the wide choice of solvents possible for a given separation. Sulfonation {questioned because of the danger of over-reaotion V. Separation of water-soluble8y-products B. and those which use additional outside power to maintain the dispersion.org Publication Date: June 1. Here the character of the packing surface. Nitration Here the value of countercurrent operations may be B. Vegetable Oil Refining VII.to redisperse sjon or redisper. Separation of oil-soluble oxygenated by-products 2. Contact made through B. the extraction can be accomplished with a small number of theoretical contacts. 111. Fischer-Tropsch Synthesis of Li uid Fuels A. if there is a tendency for solids to form in the extractor. Here confusion may arise because in many cases contacting is done both through extended films and droplets. 4. Table I I. It is based on the methods used for bringing together and separating the phases and is subclassified according t o type of contact. Few commercial extractors have more than loequivalent contacts. etc. 1950 | doi: 10. Extended surfaces Bi. The apparent trend has been toward this type. labor. Mixer 2. Capital. Reoovery of phenol from a wide variety of solutions IV. Solvent loss. The largest number of designs and patents for extractors are for those which do not use outside power. Gravity separated extractors may be subclassified as to whether the contact between phases is through extended films or droplets. Extraction of Acetic Acid A. and power for extraction equipment. Noadditional Bs. therefore. However.or maintain sion dispersion 1. surface tension. Commercial-sized packed columns almost always employ nozzles or drilled distributors for the initial distribution of each phase and droplets are present. In general. Almost all of the existing successful commercial extractors operate year after year with total on-stream time of 95 to 99% of the elapsed time. the process design frequently is based on considerations which are not necessarily concerned with the extractor. etc. For this reason packed towers are considered as droplet extractors. and viscosity of the two liquids. a simple mixer and settler extractor probably would be more desirable than a packed tower.) 3. No. those which require no power except that available in the streams of liquid going to the extractor. one usually can find a solvent to give good selectivity.kerosene. In general. Two Phases Separated by Centrifugal Force I. in glass laboratory extractors the operation of a packed column usually is accompanied by bubbles. or by dispersing the discontinuous phase into droplets. and i t is safe to predict the trend will continue.

acs. is given in Table 111. The data for nine of these come from Dow operations or from data collected by Dow engineers. Simplifled Drawing of Spray Column power is supplied to redisperee or maintain dispersion. Spray Tower Extraator Extractor of Table I II In Table I11 an attempt has been made to give the importmt details of design: the system on which the column operates.org Publication Date: June 1.1021/ie50486a013 June lgg0 Figure 1. 2009 | http://pubs. classified according to the scheme of Table 11. net flow down Fluid in reverBe flow Figure 3.INDUSTRIAL A N D ENGINEERING CHEMISTRY Downloaded by UNIV OF GEORGIA on October 13. Average phase densities a t the operating temperatures are given. throughput expressed as cubic feet of liquid of each phase per hour per square foot of horizontal empty cross section (which is equivalent to the average linear velocity in feet per hour). 1950 | doi: 10. the extractor is essentially a mixer and settler extractor. Since these densities will . and the efficiency. Figure 4. DESIGN AND PERFORMANCE OF COMMERCIAL EXTRACTORS The performance of 47 extractors. Spray Tower with Tapered End (50) lntrrfacr Av. Film-Type Extraator (49) 1023 Figure 2. expressed as number of defined unit sections of oolumn per theoretical stage contact.

for solids Vol. although sometimes operating a t different conditions from design. which can be determined by some relatively simple test. averages of the densities at the top and bottom of the unit have been taken. 1950 | doi: 10. the operator considers the extractor to be operating satisfactorily. Most extractors reported have delivered the specified product. Coahran (53) Modification of Donut and DiskType Baffle Tower Film-Type Extractors.1021/ie50486a013 Figure 5. The inventors ( 1 7 ) report that it n~ never built on a commercial scale Figure 7. The vertical flow velocities also vary considerably within the unit due to partial miscibility of the Figure 6. If the product meets specifications. and the performance in tefms of theoretical contacts has never been determined. Many of the extractors were originally designed to give a definite number of theoretical contacts for a specified product. 42. not necessarily translatable into numbers of analytical significance. The efficiencies so reportcd should be regarded &s approximations. One gravity extractor wm found that could be classed as a true extruded surface film-type of extractor This has been patented by Gordon and Zeigler (49). The flows reported are the maximum flows for each phase to be found in the extractors. 2009 | http://pubs.I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY 1024 Slowly rotating shoft for scrapor H e w r liquid i n 1 7 Light IAuid out Scraper for ring movinq with shaft -Stationary scraper for shell Light in )Cleanout Downloaded by UNIV OF GEORGIA on October 13. Dons et el. Baffle l o w e r with Scrapers DISCUSSION OF SPECIFIC TYPES OF EXTRACTORS vary within the column owing to variations in temperature and solute removed and distribution of solvent and diluent between the two phases. primarily because they did not ronsider them accurate enough for publication. the flows in the settling chamber have been calculated as though they occurred in the vertical direction. No. In the case of mixcr-settler extractors. In asking for performance data the authors found many people reluctant tf furnish analyses for concentration changes or equilibrium data. (54) Modification of Donut and Disk-Type Baffle Tower . 6 two phases.acs.org Publication Date: June 1.

Extractor 34. as shown in Figure 4. Baffle Plate Extractor Ilowever. However. Baftle Towers.4) for extracting sodium chloride and sodium chlorate to make “rayon grade” caustic soda from electrolytic soda. From the authors’ experience. 1950 | doi: 10. density differences. Although it has been extensivelystudied on a laboratory scale. A common type is the “donut and disk”-type where one baffle. a8 far as the writers can learn it has not been widely used commercially. and the backward flow caused by any of the above-mentioned causes. is built up from elongated cella or ducts which are very broad and long relative to their thickness. Extractor 3.acs. or simply by the friction of the moving bubbles carrying some of the continuous phase along with them. data of the experimental unit IS listed as extractor 1 in Table I11 because of the high efficiency reported. This is extractor 2 in Table 111. Liquid ammonia is the solvent. of Table 111. However. B d e tower extractora are simply vertical towers provided with baffles to direct the liquid flows over baffle surfaces and then over the baffle edge to the next set of baffles.1021/ie50486a013 Figure 9 1. is the difference between a forward velocity greater than average. One solution to the problem is to build the extractor &B a number of small diameter columns in parallel. These are shown schematically in Figure 3. 50LVLNl WFlNAT6 Figure 8.of Table 111. The duck are inclined at an angle to induce layer formation within each individual duct. 2009 | http://pubs. The main advantage claimed for this design is that it will handle the two phases with a minimum of emulsification. Recirculation in the continuous phase may be caused by thermal currents.os ai 02 SPECIFIC GRAVITY DIFFERENCE A4 - 04 Downloaded by UNIV OF GEORGIA on October 13. set by its rate of feed. 2. Many of the spray-type columns used commercially employ redispersion and are really a type of mixer and settler column. Spray Towers. is such a unit. the inventor ( l a ) haa stated that his d e sign has not been used to date for any large or commercial extractor. These are: Elgin (60) has patented a design with a tapered end (Figure 2) for the incoming dispersed phase which reduces *e effect of coalescence. Tlie tendency of the droplets of the dispersed phase to coaleace. the throughput rates are lower than those obtainable in a comparable vertical column.INDUSTRIAL AND ENGINEERING CHEMISTRY lune 1950 1025 as sir -EXTRACT a4 03 02 PHASE Ad de 01 os os 07 - ( FT I SEC I SPECIFIC QRAVITY DIFFERENCE SPECIFIC GRAVITY OF THE CONTINUOUS PHASE BASED UPON VISMSITV OF ICR I I I I 1 01 08 . One of the few commercial applications is that used in the Columbia alkali process (4. based primarily on observations in glass columns 4 inches in diameter and short glass sections of decanters 12 inches in diameter. Figure 10. One would expect this effect to increase with column diameter. and there is some by-passing.was built to operate as a spray tower but did not give satisfactory performance without the packing. This means some of the liquid moves in the direction of flow a t a rate greater than the average. The spray tower is perhaps the cheapest and simplest extractor. Perforated Plate Column Porforationr i n horlrontal plater . Recirculation in the continuous phase. there are two problems presented in the operation of spray columns. shown in Figure 1.org Publication Date: June 1. In this case the average flow of the continuous phase. This apparatus.

. ...1021/ie50486a013 GRAVITY SEPARATED 6 7 0 9 10 11 Donut and disk..13 176 147 11 Phenol Neutral distillate Naphthenes 1.12 12 Hydrocarbon oil 13 Hydrocarbon oil 14A Phenol-lube oil 19-tray perforated plate Phenol tower Neutral distillate Naphthenes oil .00 0. 30-hay perforated piate tower Water a. .. baffletower Propane Acetic acid Reduced &de oil Reduced crude oil Reduced crude .00 0..16 170 180 I2 Dewaxed distil. I .88 0. 1 Aceticacidrecovery from woad diatillation 2 NaOH puriflcatlon Spray column 3 Phenol recovery Spray wlumn.01 0.. . 0... in it.00 0.19 156 116 8 .88 0. (Contact in Commercial Centrifugal Ex .30 157 121 11 Oil GRAVITY SEPARATED i (Perforated plates with Furfural multiple redispersion on each plate) Furfural Hydrocarbon oil Asphaltenes 0. .l&tray perforated plate Propane ing towe East Texas resid. Ethyl acetate i. ..*~ . 160 110 8 230 155 8 0. 6. . No. . 42. Oil 20-tray perforated plate 97% phenol tower withdowncomers and uptakes 20 Phenol-lube oil 21 Phenol-lube oil 22 Phenol-lube oil Phenol Distillate oil Asphaltenes and naphthenes 1.I Nonasphaltenes 1..5 .88 0. . .89 0..12 Hydrocarbon oil Asphaltenes 0 97 0.. F. Centertosidebaffletower :.6 ft.70 030 .70 0. .. .6 0. ..06 0. .20 0 21 X 1 inch cross section. 19 Phenol-lube oil .90 0...... length.00 0.. .org Publication Date: June 1. .07-0. .. .07-0. 16 Phenol-lube oil 20-tray perforated plate Phenol tower Deasphalted d i Asphaltenes and naphthenes 1.85-0 90 0..05 0.*.89 0. ..7 Downloaded by UNIV OF GEORGIA on October 13. 8-inch Benzene pipes in parallel 4 5 15 ft. baffletower Propane Parallel grld.INDUSTRIAL AND ENGINEERING CHEMISTRY 1026 Vol.13 100-130 100-130 3. Liquid NHa aqueous N a C l and NaOH NaClOa 50% Water Phenol 1.Nonasphaltenea uum oil 0 95 0 70 0.. Top Bottom Sacnon.6 2..90 0.. 3.acs.30 160 110 3. diam. .01 0. Center to side baffletower Side to side baffle tower . 2009 | http://pubs. 14B Phenol-lube oil 19-tray perforated plate Phenol tower 150 viscosltyresid.91 0.10 .01 0.. liquor Acetic acid from wood distilmoving scrapers for acetate latlon solids 1.I GRAVITY SEPARATED. slow Ethylandmethyl Wood dist.2 10 0.propylalcoho1 Acetic acid . .. ..16 IS5 173 la 0..90 16 Phenol-lube oil 20-tray perforated plate Phenol tower Deasphalted resid. .52 1.... hole Water .83 0.85-0. ..88 0.16 176 165 la Phenol Neutral distillate Naphthenes oil 1.5 Aceticacidrecovery in cellulose acetate plant Hydrocarbon oil Hydrocarbon 011 Hydrocarbon oil Propane deasphaltin8 Propane deasphalting Propane deasphalting 1... .53 3 0...03 0. I Parallel grid. . 5 . ..03 17A Phenol-lube oil 14-tray perforated plate Phenol tower Neu:ral distillate Naphthenes oil 17B Phenol-lube oil 14-hay perforated plate Phenol tower 18 Phenol-lube oil . .. . 1.89 1. Parallel grld.. . GRAVITY SEPARATED.....91 0..6 ft.16 190 161 11 Neutral distillate Naphthenes oil 1..17 255 210 12 24 Propane deasphalt...Asphaltenes and uum oil naphthenes 1. .15 240 200 9 1..01 0.Ashpaltenes and uum oil naphthenea .05 0... A and B numbers refer to same extractor under different operating conditlons. 1..Naphthenes and late oil aromatics 1.. I . .06 0. Commercial Item" Service Description of Extractor Solvent Diiuent or Feed Solute Heavy layer Average Densities Light layer Difference size of Extractor Temp.25 160 120 10 26 Butane washing Aqueous acetone Acetone Butane 100 0..01 180 160 1.12 125 126 Aceticacldrecovery Donut and disk.18 I80 180 11 23 Phenol-lube oil Phenol Distillate oil Asphaltenes and naphthenes 1. 6 Table I I I. Nonasphaltenes I . 0.00 0. 1950 | doi: 10. .. ..d. (This section continued on page fO-98) .. I .12 170 145 10 Phenol Distillate oil Asphaltenes and naphthenes 1.13 110-120 110-120 3.30 155 117 10 Nonasphaltenes 1..70 .04 0.70 0.. .. baffle tower Propane .84 0..83 0. . 46' angle { n-propyl acetate Wood liquor n.

4s) type extractor reported..... . raffinate Lower. . 1 donut 1 disk + + 53 1 tray I tray 1 tray 1-ft.022 2- 0. .7 None None None None Rop& 83 3 2. I ..9 61. .06 None . .. 8.... (1.6-2.08 . (4 r) (8) DROPLLT CONTACI W ~ O U POWER. 1 tray .ft.) Volume Reflux Ratio ratio. 6.a. I . ..0 None ..9 0.... 20 1-ft.47 39 1 tray 10 ... .6 0.. .. Ea 1 tray ..6-3 0 None ZZ%AcOH -. extract .. IiquldNHt Lower. Ft. BO 1 tray ao .3 16....07 ... 1...... . ..INDUSTRIAL AND ENGINEERING CHEMISTRY June 1950 Extraction Equipment Size of Extractor Unit beight. extract Upper. rallinate LoWW... (m ..2 1.1 0.068% by VOIme of light phase (18....2% NaCIO....9. .4 88..1 26.... 16 . . Propane 4 0 04 3..1 9. I 1 trsY 20 ...8 8. Aqueous ...1 0. raffinate Lower..org Publication Date: June 1. ..... . Upper.. DROPIET CONTACT WITHOVT POWER.(17. Performance f o r (8... 7 2 16.. I-it.s-2.. 61 1 tray 19 ... . raffinate ...6 36..0-2 6 None 8.79 0.2 61 I tray 19 .6 37. rnffinate Lower.. tower 20 -7 -3 32.3 None 80 1my 30 .. 67) . . $7) . 6 4 . .. extract Upper raffikate Lower.. ..43 upper...8 238 .. .0.acs. ..76 60-76 30 2.. . raffinate Lower.1 26... . 6 .13 47 1 tray 14 4-0 10. extract upper... never built in commercial slze COLVMN 40 1-ft. grid ht...8 30. 1 .. . extract upper..2% 0..02 y 0. . . 1 tray 6 6.* .3 0.. 18..6 11.26 .88) 0. extract Upper. ...3 47 1 14 4-6 9. .1021/ie50486a013 46 1 donut 1 disk .. . Only gravity film..9 0../(Hr. .. :os acetone-) 0.7 1. 2009 | http://pubs.0002% None 8% phenol4 0.. 108.2 B.. .2-2...9 0. ... 41 1-ft... SPRAY ... 47 1 tray . raffinate Lower. 13.6 0. .. 88) C a r r y o v e r w a s ($9. 48 48 36 8 10..69 None . . raffinate Lower. NaOH Aqueous . . 11. .4% ... . 68) 4th plate . 18) two t o w m in serien ...66 6a 1 trnY .. ($9) Perforated shower (16) deck baffles Feed Introduced on (%ASS) 4th plate Feedbtroduced on (80.. 8. 11. Total flow both phases 78.*.. -12 Probably a-3 Probpbly ] . .) 0 11 AdlH 103 104 90 -12 -12 -8 .. .. raffinate Lower...6 0....+ 0.32 . (W Speclal s t e g t y p e (5'6) travs Specisl s t e p t y p e (36) travr Perforated shower ( f b ) deck bnfficl over entire area 2 . ... 0.. I.01% *.0.....5 -8 -8 2-3 ..0 0406 Aqueous 21.8 0.7 60 1 tray 20 ...66 None Z...... 37 1 tray .o%NaCl 4 0. 0.3 0. extract Upper.. -20 17. ... of units Total No. (M) Downcomers in oil (So) phpK packed to calm entrained extract . .21 3.4 .. extract Upper...4 0......mdht. ratlinate Lower. .gridht.88 ... .. tower 40 ...2 .3 14.. ....... . T BAFFLETOWER Downloaded by UNIV OF GEORGIA on October 13. extract upper. 1950 | doi: 10. 1.. .)(%. Propane 84.6 17..9 81... length 16 DRCRLET CONTACTWITROUT POWER..76 Unit/ Vertiml Flew Cu. raffinate Lower.755BAcOH-i 0 06% 65 -8 -8 6&7b 26 2..0-2. .3 79.......... plate spa+ (88) (This secfion continued on p40b 1098) . 0 5 0.. 16 .. extract Upper.6 None . 43/tower ..01 - I. .7 23.79 .. ...63 0.. extract Upper.. . dehed Total No.*.. ... . . ..1 44.17 66 1 tray .1 19...... .Ft... Lower.. 41 1-ft.0 0876 2 = 0 0004 'I 0 0048 I .2 92 1 4.. 4 0 . z.....1 18.. extract Upper.of Thee retial Contam Theoretical Stage Contact -20 -0. (W 5-inch tray spacing (47) efficient 16-inch tray spacing ($8.. . . PERFORATED PLATE TOWER .. light/ Reflux/ Concentration Eguillbrium Light Heavy layer heavy layer Feed Changes Data 1027 Continuous Phase ReferRemarks ences CONTACT TRROUCH FILMS tracton Is Mainly through F b ) .. 38. ......6 66 6 0.. .

Diethanohmine Propane steel Raschig ring8 Propane 1 X I l / r inch. 130 r. In a design by Coahran (63)the “donut” sections are stationary. The variations in thickness of the different layers change the ratio of the extended film surface to volume of the two phases and is claimed to result in greater .Brine liquor rings tone HZS 33 Ethylene cyhydrln i.10 0. A.W.18 0 96 0 21 80 BO 1 8 Refined linseed UnsPturatedglyo oil eridr oils 1.34 80-76 60-76 1. 8.15 88-77 68-77 and Mixer. Extractor 4 in Table 111is of this design. Although the original installations of this type of extractor were made before 1930. 2009 | http://pubs.30 60 46 6 b7 ButadiGllt butylenes Mixer. there is a flat disk.6 hp.90 0. 1 -_I_ 1. mixer.I-inch R m h i g ring8 tane 27 Vegetable oil refin. 2 x 10 11 Settler.10 0.. No. Commereial Daoription of Extractor Solvent Mlueat or Feed Solute Henvy layer Average Densfties Light layer Differena slrs of htractw -secllon.Ol 0 89 0 11 125 126 3 3 90 Phenol recovery Phenol 101 0. 42.5 ft.p.3 -6 4. 4.80 0 26 130 I20 5% NaOH s o b Creosote oil ex.96 0.. dlarn. 6 X 1 It. agitators Chlorobenzene Water Phenol 100 1.” These scr.Monohydrlcphr non tract nols Settler.I.90 0.diam Settler..76 46 Nitrobenzenelube Oil Mixer.Unaaturateddyo benn ou etide oils 1. .1021/ie50486a013 ring8 31A Furfural-lubc 011 1-inch Raschig rings Furiural Dewaxed neutral Naphthenes oil 1. agitators 4. or on each side of the ring.Furfural dles ing 28 Vegetable oil r e i hg I/l-inch ceramic R w h i g Furfural rings 29 Furfural-lube oil 30 Furfural-lube oil .” is a ring with a large diameter hole in the center which makes tight contact with the shell. Mauro. horizontal settler Nltrobenzene HaSOi Dewaxed oil Naphthenes 1. -. mixer. 130 r.org Publication Date: June 1. total agitator power. mixer.the baffle and eventually to the bottom of the tower where provisions are made to remove them. Settler.. propane stoek oil aromawx 1 05 0 80 0 26 la0 100 1 05 0.26 X 8 ft.87 o a3 230 160 31B Furfural-lube oil 1-inch Raschig rings Furfural Dewaxed bright Naphthenea stock oil I 10 0 90 0 20 290 226 31 H B from propane 1.10 0 10 110 110 Chlorobenzene Water Phenol 1.14 0 18 80 80 6 6 Butylene hmmonla 400 v i a c o s i t y Asphdtena Texan dbffllate Oil Distillate 011 Asphdtcnw 0 96 1. In it. In the design shown in Figure 5.10 0 86 0 24 260 170 5 6 Downloaded by UNIV OF GEORGIA on October 13.G. mixer.61 0 49-0 59 26 26 Oil -.22 66 60 7. Top Bottom d i m . 2.20 ?her.47 0.07 68-77 68-77 1.00 1. 39 Phenol recovery 40 Phenol recovery 41 Phenol recovery 42 Phenol recovery Light creosote oil Gas liquor Monohydric phenola 1 02 0. 6. d i m . horizontal settler Nitrobenzene Lube distillate oil Naphthenea 1.10 0. Eft.82 0 30 120 80 1 Degummed soy.86 0. the “donut.-.61 116 117 3 t 34 Cyanohydrin 1 X I ‘ / r inch. horizontal Settler Phenol-cresoiand Mixed reduced Par& propane crude OUS n?nmatlC3 ..47 0.3 hp. Temp. total agitator power. and Mapes (64)the distance between the “donut” and “disk” plates is progressively decreased toward the upper portion of the column to decrewe in turn the thickness of the layers as they pass from relatively naphthenic phases (in the specific case of solvent extraction of a petroleum oil stock with Chlorex) in the lower part of the column to more paratlinic phases in the upper portion of the column.61 116 110 HSSfrom propane HlS 1 . the “disks” are rotated a t low speed against fixed scrapers.INDUSTRIAL AND ENGINEERING CHEMISTRY 1028 Vol. 9 ft.7 36 Phenol remvcry ‘/a-inch ceramic Raschig Benzene rhus. while the “disk” sections may be rotated to provide some agitation (Figure 6). dhm. and the shaft that carries the disk also carries scrapers to scrape the stationary “donut.10-1.20 0. Water Furfural 1l/r-Inch ceramic Ralrhlg Furfural Om 0.acs. horlzontal settler Ammoniacal w p Butyleneswith 3 horimntal bafper acetate butane flea 0.apersmove any solids that form in the extractor to the edge of . 13 DuoSol-lube 011 44 DuoSol-lube oil 45 Nitrobenzenelube Mixer. 1. 2 brick-lined towers Water 31 15% HCI Phenol 1 01 0 89 0 18 140 140 1.ao 0. 2 towers In series Water Phenol 1 .6ft. (No K n o w Cam GRAVIIT SEPbRATWA 28 Ammonia from bu.md B nurnbeia refer to name extractor under different operating conditions..06 0.10 0 89 0 21 229 196 13 1. bright! Pslnffins and . horizontal settler Phenol-cremland 96 V. Butadiene *. 6 Table I I I. O F .__ Mixer.Ill-inch ceramic Berl sad. .84 0 12 126 12s 8 7 Phenol recovery ‘/a-lnch ceramic Raschig Benzene rings I-inch ceramic Raschig Benzene rings. some recent patents have been obtained 011 modifications.10 0. GRAVITY SEPARATED.W. In another design (Figure 7 )by Dons. This type has been used for many years in extracting acetic acid from the aqueous demethanolieed liquors from wood distillation. 1950 | doi: 10.8 l h c h Raschig rings Liquid SOI Kerosene Aromatics 1 38 0 89 0 49 10 2 X 2 ft. Above and below.m. 20 B..on 0.p.95 0.G. usually somewhat larger than the hole in the ring.10 110 110 GRAVITY SEPARATLD..m. Diethanolamine steel Raschig r i n g ‘/r-inch carbon Raschig Methyl ethyl ke.26 X 8 ft.20 B. 8 X 8 in.

(8) Each tower # u p (8) plied with trash banzol . .. the baffles can be closely spaced 4 to 6 inches apart and reasonable contact efficiency for the whole tower is obtained.2% 12. ... length MIxGr-aettler 6 .1% 18It.0 0..p&ing ae 30 I-frpacking 23/tower 68 45 4..33 6.93 . 75 ft..) Unit/ Theomtical Stage Contact Llght layer HMVY layer Volume Reflux ratio Ratio. The capacity of this design of bafae tower thus is seen to increase with greater difference in density between the two phases and with decreasing density of the continuous phase.6% phenol z = 0 01 y 0. 2009 | http://pubs.. (14.. oil ..2 I .. furfural Oil ..fL No.0% hesol0... 6 .9 6 redistribution MC.. ./(Hr. I .. length Mlxerdettler .8 in 7 lnencb 0 06-0 24 -ohm* of 4 non mnon.. 1950 | doi: 10.. 13.6 10. .....4 . packing 926 426 2 2 18 8 I4 T I 13 Nan6 16 In dch tower. Aqueoua Aqueous Aqumur 0 09% 17. .01 -- a0 8 0 66 None 11.0 0. .10 theoretical contact per baffle. . Ft. . packing . parked sec.. (W) nons 4-10 it.. .)(Sg. 96: (80) Ca. .35 26. diambutlon sec- 60 16 8 69 0 0 27 0 60 01I 10-6ft.. ~ ~ h e n o l .4 0..p........0 to8...1 1.18 . (8) rnohydrh from brine win. 30 It. 7. .packing 76 .0.. .. .I .. Thia is shown in Figure 8. #/%I 4-b 0.08 .0% 2 mole % Ropnns ...0% Methyl ethyl ketone 0% .1021/ie50486a013 tions tions 60 46 1-ft. packing 65 7 36 1. Similar charta for liquids of other viscosities may be readily prepared from data obtained in laboratory equipment. with the density of the continuous phase as a parameter (Figure 9). .86 10. . Although the contact efficiency is low. Ft.20 0. length Mker-aettler 7-6 6-8 1 4-1 0 046-0. I .1 In 69 I-ft.v/c 9 8 8 3.6% phenol- v- . .. 9%. packing 1... length Mher-Mttler 4 .rt.. ..6 0. Lower. Kerosene ..?e) for heat of r e m tlon of N H r HIO + NH4OH (14. This chart applies specifically to liquids with viscosities of the order of 1centipoise and with interfacial tension of the magnitude of that of benzene-water. .40vol. or center-toside flow in large columns.ft... An empirical design chart given by Wenb worth (47)plota a maximum allowable velocity through the ..ft.I Appltutiolu to Dab) D i o r m ContAff WlTmOo? 20 POWEB... . lWl + 0 3% uppar.. .. 7) tiotu with 10 rediatributlon sec- 34 502 287 21 3-6 mole % Propane H B . . MIXERSP~~WR 4 Mlxer-aettler 8 8 1.0% 3..packcd~c. Extractors 6.0 . A simple design ( 4 7 ) of baffle column which is commercially available employs side-bside flow.05 to 0... lW> 0.2 61 4 0.... of the order of 0... 1. 17. .....64-1. Ugt/ Reflux/ Conmntratlon heavy Feed Equilibrium Data Chrnga Continuous Phase Referencei Remarks QROPUT CONIACXwm?orpT Porn. ..43 0 35 Oil 10-6ft.. oil .O6voI.. . . 1.4 10.12 2 .6 . expressed as the sum of the velocities of the two phases. The capacity of a given baffle column is l i i t e d by the flooding which occurs a t the opening in the baffles through which the two p h a w must pass.f t preking 60 1-It.. of the liquid phases. 19.4 12.(4 7) tions wlth 10 re.. .. 1. NODe 8. .% oxo- Feed I# 16 vol.ft.9% p h a o l + .. (90) C1.07 . . . Downloaded by UNIV OF GEORGIA on October 13. .pacldag ... There are no small holes or .I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY lune 1950 1029 Extraction Equipment (Continued) Skod&mctor TOW hagt.14 0. . 9.acs.14 13.8 ao o m None 7.. matin- ?.org Publication Date: June 1. Oil 47 83 i-ft. (6) tlOM with 4 16 distribution wc...pacldng 3O/tower 2+1 3 22 l4t. .1 13...8 I-ft.. and 8 in Table I11 are of this design.2 5 0 1..61 .. ... . Lower..% Ci 90% removal of cg.3 0.d tunb Unit daanod TOW N0. .0% phenol- 3 Mhu-mettlu 8 6 1.paCUng Shall Is water cooled (8. In many respects the baffle column i s one of the most setisfactory typer.8 13 06 None O .ppclang 40 .. 66 0 0. length Mlmaattler 8 . comparable to that of the liquid in a conventional bubble cap distillation column. 33 It. .. .33 7.% CI . of commercial extractors. .eLing -7 16 6 19 0 4 0 Aqueous None 10%NHi- 4 7 ET 1.-.012 Om 2-0..0 None 6. .1 14 6 Brine 11 8 lean tower 7 6 Bz?z:g- tions Feed la 80 vol... Mlxer-aetthr 7 ... .... . . . against the difference in density of the phases. BWBBIS Cm TOWEB msrei.a% DROPLPT CONSAC? WITH POWER REOWRED TOR REDISPERIION.... 23 In rich tower 2. I .. .( 8 .. 9...1 In dcb tower.3-1.6 0. 6. 111 1 66 None 17.... 10 to We% and 10 to 1 horizontal passage between baffles...8 ao. selectivity of treat.pidaag 30 34 i-ft.6 6. . 67 1. 4... PACKS0 TOWER 1-ft. 2.43 16 ft..d The mUd Contacts Vertical Flow Cu.packedMc.... furfural U p p r .8 vel. 1. 10 Mtxer-mettler 4 .

This emulsion drawoff is shown in Figure 12. =? Figure 13. The perforated plate column frequently is operated with the interface level near the middle of the column. 1950 | doi: 10. but has been found suitable for liquid-liquid extraction. until sufficient hydrostatic head is generated to force the liquid through the perforations. The perforated plate in this design is in the vertical plane. However. If the liquids used are clean and form no precipitates. Perforated Plate Column Downloaded by UNIV OF GEORGIA on October 13. ” I. 42. so that each phase in its particular part of the column is the dispersed phase. distillation contact plate. which break the stream into droplets.acs. Perforated Plate Columns. the holes are to some extent protected from solids. It is claimed that recycling is reduced in this design. The dispersed phase accumulates. 6 of a muck or emulsion layer. 2009 | http://pubs. with by-pass pipes for each phase. The mucklayer is removed from the extractor and the solids removed by breaking the emulsion in any of a number of ways. The dispersed phase travels horizontally phase terfoce control mulsion or muck layer lsion bypass pipes vy phase-canlinuouc Solid lines - heavy Iayar flow E Figure 12. and with suitable side draw connebtions. which can move along with the continuous phase. Modifled Perforated Extraction Tray . the cost of dismantling for cleaning makes them impractical. Figure 13 shows a trough-type design patented by the Standard Oil Development Company (68). and filtering out the solids. The droplets pass through the continuous phase until they are caught by the next plate and the process repeated.light Modification of Perforated Plate Design Trough-type design (68) Light phase-cantiruoul Dolled line 3s There are many modifications of perforated plate designs. One of the most recent innovations in perforated plate-type extractors is the design shown in Figure 14 (66). Columns 14 to 20 of Table I11 are of this design. if there is any accumulation of solids that cannot be removed by solvent. -Downpipd for heavy layu. Here the continuous phase is carried into a chamber in which the interface is maintained. so that there is some sacrifice of height per tray. either above or below the perforated plate. . with holes in the vertical plates. they usually accumulate a t the interface to form almost a third phase t Figure 14. When solids are carried into or form in an extractor. This scheme cuts into the operation of the two adjacent trays (because there is some by-passing).1030 INDUSTRIAL A N D ENGINEERING CHEMISTRY Vol. It wa8 originally developed as a. provision can frequently be made to remove this continuously or periodically while the extractor is in operation. Figure 11. Emulsion By-Pass The type of perforated plate shown in Figure 11 is one of the most widely used columns of this type. However. These extractors also are quite simple. No. In this type the dispersed phase is redistributed into droplets many times by passage through plates perforated with small holes. When this occurs.org Publication Date: June 1. this type of extractor operates with very low maintenance. I. . and unless special provisions for clean-out openings are made.1021/ie50486a013 Perforetlonr In vertical plates passages to plug or to be enlarged by corrosion. This is extractor 25 in the table. Figure 10 shows a column design with the perforations in the horizontal plane (65).

Perforated plate columns. A number of reports of such installations were traced.Downloaded by UNIV OF GEORGIA on October 13. As shown in Table 111.76 theoretical contact per tray is claimed with high throughput. Extractors 26 to 38 in the table are packed tower installations. The favorite packings are Raschig rings and simple grids. is probably the cheapest and most satiafactory extractor to use on very acid solutions. The packed tower. gives redispersion of droplets. and forms extended films. Extractors in this class consist of a mixing ohamber of suitable design followed by a settling chamber . or carbon packing. Packed towers rank next to spray towers in simplicity of construction. In spite of this. Flows in Mixer-Settler Extractors Figure 16. Bubble cap columns probably can be built at a cost equivalent to that of baffle or perforated plate columns. and the plates can be spaced at close intervals. if one recognizesthe fact that 5 to 10 plates may be required to obtain a theoretical contact. Mensing (108) Design for Mixer-Settler Extractor Figure 16. The droplets are swept up against and through a perforated vertical baffle and are redispersed in a second stream of the continuous phase. particularly in the Raschig phenol process. It is not difficult to determine their capacity as far as flow of the two liquids is concerned. but it is difficult to predict their efficieqcy.1021/ie50486a013 lune 1950 1031 INDUSTRIAL AND ENGINEERING CHEMISTRY into a high velocity stream of the continuous phase. They also have been used successfully for phenol extraction. have been quite satisfactory where they have been installed. 1950 | doi: 10. although the height per contact seems high.org Publication Date: June 1. or feet of packing required per theoretical contact. except on the baais of the performance of a rather large pilot unit. In packed towers. stoneware. Extractors 12 and 13 in Table III are of this type. In the cases where their performance has been demonstrated. Mixer-Settler Extractors. particularly those with the perforations in vertical plates. In the petroleum industry they are the favored type for extraction with sulfur dioxide and furfural. I Heavy I Light liquid I n liquid in Wertacs control Mirer Settkr Light liquid out ' IMiaerHewy Settler liquid out figure 17. The caps or liquid distributors disclosed in these patents often are of very unique design. and many duplicate or even larger unite have been built. this figure ranges for 5 to 20 feet. built with a brick-lined tower and using porcelain.acs. Up to 0. They are very popular in the oil industry. The writers have found no commercial applications of bubble cap columns for extractors. Box-Type Mixer-Settler Extr8otor Packed Tower Extractors. The process is repeated several times across the plate. they have been rather satisfactory. They are simply vertical tanks provided with a grid to support the packing and distributors for the two liquids. but invariably they have been found to be perforated plate towers. Bubble Cap Columns. Rogers and Thiele (40) report that bubble cap columns are not very efficient contact devices for liquid-liquid extraction. Two-Stage Mixer-Settler Extractor a4 N /2 Figure 18. 2009 | http://pubs. The packing cuts down recirculation of the continuous phase. the equilibrium conditions are frequently very favorable and good extraction is obtained. a number of patents have been granted on this type of contactor ( 6 W 8 ) . Edeleanu plants have gone from mixer and settlers to packed towers.

It is the safest type to use in designing extractors from laboratory data.. Almost the only design problem is to provide ample settling chambers. woven wire mesh. The units are mounted side by side. A rectangular mixing chamber with propeller agitators on either H vertical or inclined shaft is provided at the end of a settling chsmber of the same width. or baffles in settlers to reduce by-passing and promote coalescence is quite common. below which clear streams can be obtained.org Publication Date: June 1. From the other side. etc. The settling chamber is aimply a tank. packing.75 to 0. However.1021/ie50486a013 1’032 I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY Vol. although it is sometimes provided with elaborate baffles.of The Dow Chemical Company. In almost all cases where data is obtainable. This opening is baffled to reduce turbulence in the settling chamber. coalescence occurs and the excess second phase drops out. Thus the mixer-settler extractor may be considered in extraction to be analogous to the bubble cap column or distillation.Downloaded by UNIV OF GEORGIA on October 13. The flow of liquid liquid fkom stage to stage is maintained by locating the light liquid level overflow weirs on each mixer lower . so that it can be used for almost any pair of liquids. the heavy liquid enters the mixing chamber at the bottom. For this reason a conservative assumption of stage efficiency can be made. witb the mixers a t alternate ends. The larger extractors are built with horizontal tanks. each stream will carry the other phase in amounts in excess of the solubility. 2009 | http://pubs. but so slowly that the design based on this rate would be economical. Extractors 39 to 47 in the table are mixer-settler units in commercial use. but usually is a chamber provided with a propeller or turbine agitator and baffles. Clgure 19. The use of fibers.acs. The mixer sometimes is only a centrifugal pump. contact efficiencies of the order of 0. or from brick. or filled with packing. 42. Bottaro (89) Design for Mixer-Settier Extractor for each stage of the extractor.9 contact per theoretical stage are reported. The earliat record that can be found is its use in 1904 by E. 6 unit. if such a hazy solution passes through a bed where it contacts fine filaments such as glass woo1. 1950 | doi: 10. Usually mixer settlers operate with the hazy phases. to extract benzoic acid from an aqueous solution with toluene. Bmat~w. The first unit was made of wood. Kiersted (101) Design for Mixer-Settler Extractor One design for a mixer-settler extractor is that showit in Figuree 16 and 17 as a two-stage unit. However. The light liquid on one side flows over a weir and is carried to the mixer. screens. The origin of the design is lost. For many pairs of liquids there is an easily discernible settling velocity. although the authors have tried to trace it. Burtis and Kirkbride ( 4 ) gave a good example of the use of fiber glass to coalesce dispersions of petroleum and water. No. Figure 15 shows a typical stage EXTRACTION HEAT RCHAffiXBR Figure 20. in which the settling chamber can be a vertical or horizontal cylindrical tank. It is carried as small droplets or “haze” which will separate in time. This extractor is readily adapted for construction from wood. 0. The mixed liquids flow througb an opening in the partition between the mixer and the settler. The stages may be mounted side by side or one above the other. a t the bottom of the settling chamber. regardless of the size of extractor or the liquids upon which they operate. metals.

patented by Packie and Glazier (30. 37). Figure 18. The Duo-Sol process (117). and any number of unib can be pounted a t the same level. The only design precaution is to have sufficient depth of liquid in the first settler to allow a depth of light layer of about 1foot in that stage. Othmer's (I 09) design is similar. The Bottaro (8e)extractor (Figure 19) is a mixereettler of unusual design. Its performance data is given as extractor 47. 1950 | doi: 10.Downloaded by UNIV OF GEORGIA on October 13. is simiiar except that the lift of liquid by the impeller transfers tho mixture from stage to stage. and the power supplied to the agitators by a shaft running through the length of the tower. and roturn them. mix them. Perhaps the most important development in very large mixer-settler extractors is the use of interface level controllers to maintain the interface level. 2009 | http://pubs. This is shown in the Kiersted design (101) ht Phaco Outlet -y -* I Figure 23. The design of Mensing ( l o g ) . This permits positive movement and control of the flow of both phases. utilizes an extractor of the type shown in Figure 21. which is i n c h e d from the vertical a t an angle to obtain better layer separation.1021/ie50486a013 June 19% INDUSTRIAL A N D ENGINEERING CHEMISTRY 1033 in Figure 20. This interface gradient establishes itself and varies with the flow rates. which distributes the different components of a hydrocarbon feed between a phenolic solvent and propane. Extractors 43 and 44 of Table I11 are of this type. With a total depth of 42 inches of liquid. regardless of Figure 22.org Publication Date: June 1. Many of the largest extraction units in operation are mixer-settler units. in which butadiene is extracted from the other Cc hydrocarbons by a solution of ammoniacal copper acetate. The very efficient Scheibel extractor (41) is essentially this type with the added feature of using packing in the settling section. In this design the return flow may be passed through heat exchangers to maintain desired temperature gradients. Van DlJck (110) Design for Extractor Column Movable Members than on the preceding one. Maycock (107) Derign for Extractor Column with Cylindrical Rotating Contact Surfaces . Several large units of this hype have been built and have given very satisfactory performance. and d e scribed by Asbury (@). as in the case of one patented by McConnell (103). these extractors have been built in units up to 8 stages.acs. uses mixer and settler extractors (6). This is one way of providing reflux within the extractor. Another scheme used is to make the tower simply B aeries of settlers one above the other and to remove the liquids from the tower a t each level. When the stages are mounted one above the other. The flow of the heavy layer is maintained by a difference in level of interface from settler to settler as shown in Figure 17. A large fraction of the butadiene produced in this country is produced in the plants designed by the Standard Oil Development Company. In this process the extraction system. The settling section ie heavily baffled. the mixer chambers can be built inside the extractor.

.. 1949. It is here that these machines are used to best advantage. Gloyer. (48) Willingham. A..6 seconds.. 1949. Chem..5. J. C. IND. C. 12. J. Trans..420. E”. 41. A. Trans. R. E. (47) Wentworth. 2. L. 39. E. and Longcor. and Georgian. 110 (1942). Ebner. Packie. Westhaver. and Mertens.. C. Meier. private communication. (23) Hufnagel. Sedlak. 41 (1947). and Brown. J. S. and equipment industries who have furnished data and information used in this paper. When the product goes below established standards.No...451(Jan. Rossini.. 597 (1939). E. “Chemical Engineers’ Handbook. G.” New York. T. 26 (1946). Murdoch. 1949.. F. Petroleum Technol... ~ I 31. S. 51.Chem. Packie. 33. BIBLIOGRAPHY (1) Benedict. 35.. Standard Oil Co. C. 6 Bryant. This feature is quite important in handling materials which are easilydecomposed.24.47). The Atlantic Refining Co.. 33.. 20.. R.. 21.1050 (1948).. Oil Gas J. and concentration changes follow changes in operating conditions with such a great time lag that i t would be very difficult to attempt to make changes to effect control. E. Petroleum Processing. and‘McCluer. Elgin. W. M. They have limited capacity and require careful maintenance.. Goos. I n plants which operate with regularly scheduled shut downs for repairs... Am.. Tennessee Eastman Corp. Packie.. Inst.. 52 (1944). C. (25) Kalichevsky. M. Engrs. W.. J.. E..ENG. private communication. Petroleum Processing. Nutting. Perry. failure of products of extractors to meet established standards is a rare event. SOC. Burtis. 1947)... Extraction Columns with Movable Members. E. Ind.” 2nd ed.Chem... Reinhold Publishing Corp. 42. ment Co.. W..and Nash. and the solvent and reflux flows set a t values adequate for the most adverse feed concentration conditions. N. D. H. & Met.. J. Centrifugal Extractors.. private communication. L. 1949. and Thiele. D... It is quite fortunate that they are so stable.. Chem. V.. private communication.CHEM..CHEM.1021/ie50486a013 1034 INDUSTRIAL A N D ENGINEERING CHEMISTRY fluctuations in density of the phases. 42. 681 (1948).55.. 1949. and Ehlers.ENG. This is a perforated plate column in which the plates are raised and lowered by a reciprocating mechanism through the main body of liquid. C.80 (1935).. (19) Green. J. C. A.. Fahik. Inst. Standard Oil Development Co. Morrell. 17. private communication. 42. W. M. B. New York. and Kirkhride. (26) Kalichevsky.. H. IND.). Tech. 1 (1941). W. H. Another unusual extractor recently patented by Maycock (10’7) utilizes the principle applied a few years ago by Rossini (@) in distillation. private communication. Cooperative Refinery Assoc. 39. 1950 | doi: 10. 40. W. V. Dow Chemical Co..M. It is only in the last few years that extractors of the centrifugal or second group have been used. 1949. C. 1949. G... W. Poffenherger. No.. R. private communication. L.. R.706 (1947). 1144 (1939). (45)Waeser. private communication. (20) Gunness. G. Horsley. and Britton... IND. (24)Hunter. 19. (21) Hasche. and Cuckney. E. B. The writers have been informed that today there are about 400 of these machines in operation. McGraw-Hill Book Co. U. and Given. Am.. Chem. Eng. Engrs. Packie. and Tears. J. private communiration. W. J. ” Prouress.. E.459. S. END. 23 (1947).78.. Engrs.K. 1949. unpublished plant or laboratory data.38. private communication. V. J . J. T. (43) Thornton. Vol. Trans. it would be well worth extra expenditure for more contacts if this selection of the continuous phase gave lower efficiency. $5. T. 285T (1932). Scheibel. Manley. 18. 473 (1946). W. Engrs.ENG. 2. B. CHEM... A. Magnolia Petroleum Co. A.. 63. private communication. . solvent. 326 (1946). 44. No. 15.acs.. C. Y. H. T. Am. No.660 (1949).132(1946). Chem.. 17. (46) Waeser. (Indiana). Gloyer. OiE Gas J . W. 50.50.40..000-gallon-per-hour throughput for both streams can be built with an inventory of 10 gallons. No. A. 4.. Inst.413 (1946). some installations consisting of banks of 10 machines..4. 2009 | http://pubs. 1938.. Elgin. 7 . Petroleum News. Stanford Research Institute. 1949. Inds.. C. Chemical Age (London). F. A. G. and Glazier. N. (2) Brown. I t can be built with a high throughput to inventory ratio.53 (1948). Inst...CHEM. Petroleum Engr. 1949... Sinclair Refining Co.. C. Natl.Downloaded by UNIV OF GEORGIA on October 13. C. J. C. R. H. C. Princeton University. J. ACKNOWLEDGMENT The authors wish to acknowledge the assistance of many engineers in the chemical... 1949. R.230 (1948). (22) Herthel. O.CHEM.906(May 20. s. 173 (1944).. private communication. Am.CHEM. This type of extractor has one outstanding advantage over the gravity type. Koch Engineering Co.. 3. private communication. $931.... C47 (1949). Chem. C. (18)Gray. J. J.. A.. 1949. W.ENG. Engrs. A very unusual method of supplying power for redispersion is given in a patent by van Dijck (180). with the flow of the feed. Trans. 36 (1941). Cobb. OPERATION AND CONTROL OF EXTRACTORS Whenever possible extractors are operated with the continuous phase either as the cheapest phase or the safest phase. E. V. E. IND. C. in which the annular space between a fixed wall and a rotating cylinder is uaed for contact. Extracting Columns with Cylindrical Rotating Contact Surfaces. Asbury. and this means usually that the feed is definitely off or that the extractor needs cleaning or repairs. Engrs. M. Trans. Refner Natural Gasoline Mfr. L. which allows smooth and even operation of the distillation equipment used with the extraction system. R. private communication. E.. 42. oil.. Patent 2. Extractors are quite stable in operation.. 18.. Chem. Kirberg. B. J. C. Chem. These have been listed in the bibliography (6. W. IND. T. Paltz.. “Modern Methods of Refining Lubricating Oils. C.29. J. Such conditions are found in the new antibiotic3 and vitamins. if the inventory of a ffammable solvent can be reduced to 20% of what it would otherwise be. Fuqua. Inst. B. 519 (1944). A. P. Ver. No attempt has been made by the present authors to cover or list the literature pertaining to centrifugal extractors. J. The design is shown in Figure 22..53. Inst. (to Standard Oil Develop. Badger and Sons Co.. and MoCarty. Chem. and the cleanup and repairs are done carefully. which is equivalent in residence time in the extractor to 3. D.S. A unit with a 10. 1949. Inst. Gordon. (Berlin).. Enu. Minevitch. (42j Sherwood.. M. W..38. Am.No. or which undergo spontaneous degradation in the process liquors... W. Petroleum Processing.40. Obergfell.. 1949. 529 (1937).. L.35 (1949). IND. (to Standard Oil Development Co. E. Appa. because the ratio of inventory to flow is usually high.). Patent 2..1949). 221. even though this may require extra capital for the extractor-for example. D. 1949.39.. Chem. 1949. 49.90 (1946). Chem. private communication.No.Kendall Refining Co. and Reiter.CHEM. private communication. A.. J ..957 (1933). (London). IND. 1941. B. L. A..The Vulcan Copper & Supply Co...228(1948). Kenny. it does so slowly.R-26 (1941). 20-28. Elgin. . Trans. They must be carefully designed and constructed to withstand severe mechanical stresses and therefore are expensive... 43. Continental Oil Co. J. 492 (1947). Goldsmith. G. and reflux set by flow controllers.ENG.. Gulf Oil Corp. J. Rogers.org Publication Date: June 1.Chem. Humble Oil & Refining Co.ENG.. W. C. J. U.815(1946)... 1162 (1948)... Oil Gas J. F. It also provides a constant inventory of each phase in the extractor. E. L. R. 42.49. (44) Twiehaus.. Kenyon. Evans. Figure 23 shows such a design.

L. U. GRAVITY SEPARATED. Ger. Ibid. Martini & Hiineke m. 24. 29.200 (July 3. Ibid. (58) Mangelsdorf. (67) N. C. (to American Cyanamid Co.. 1939). 1941). (Indiana)]. 8.H. 13. 414. (to Standard Oil Development Co. B. R. Jr. M. 2. (to SOC. Ibid. C.. B.). R. 27. 13.s. Ibid. DROPLET CONTACT WITH ADDED POWER. Ger. Patent 598. [to Standard Oil Co.052. M. 1939). G. 24. W.361. 1936). Brit. E.511 279.011.. (73) Standard Oil Development Co. 1943). M.151 (Oct.091. 1936). 1913).774 (same as U.986 (June 25.). R.128 (Feb.651.511 (June 8.186) (Aug. R. Patent 2. and McCluer.696 (March 6. W. (89) Bottaro. Ibid.064.H.838.. and Charles. L. Ibid. and Bronzewerke A...011. (54) Dons. W.734 (same as U.. GRAVITY SEPARATED. E. 2. (April 29. (87) Bamag-Meguin A. H. Petroleum Re(96) Gordon. 1935). 2.892 (Dec. Patent 2. Patent 2. U.864. (to Eastman Kodak Co. 1931). A. Anne. 1937). Ger.281 (June 24. [to Standard Oil Co. 28. and Mott. F. Patent Ger.. and Smith.766. 2... A.. S.945 (Dec.).).651 CAPTOWERS (Jan. Martini & Hiineke m. (to Koppers Co..083. J. Ibid. S. 1942). Patent (92) Dons. Mauro. E. Ger. Brit. 1934). U. S. J. (99) Jones.147. Ibid. 2. (57) Fenske.083.).. F.037. TOWERS (91) Debuch.. R. M. D. HolIey. Patent 373.und Apparatebau-Gee. (Dee.150 (Oct.420. 381. (82) Maschinen. (109) Othmer. 1944).. 2. 2.. S.). (to The Lummus Co.044 (April 26..) U. Patent 584. (to Standard Oil Development Co. Jr. (to Shell Development Co.422 (Dec.. 2. Patent 2.. 14. (to The Lummus Co. 1937). 2. H. (June 27. 1928).. (to Combustion Ut ea Corp.. (52) Albin. E.).876 (Jan. 1947). (to Celanese Corp. [to Standard Oil Co. (to Research Corp. 1937). ftlr chemisohe (118) Whitham.anon.457 (July 5. 1931). (to Penna.291 (Aug..b.b. Ger. Ltd..072.b. G. and Mott. 21. H.897 (Oct. 2. U. 1990. 1938). Olier. Patent 2. 1938). S. U. Brit... 20. 13. (64) Harrington. W. 16. 1938). Patent 1. Ibid.011. Corp. (114) Schoneborn. Patent 1.400. P.077. Patent Industrie m. P. (to The Texas Co. 1928). DROPLETCONTACT WITHOUT POWER. S. (to Standard Oil Development Co. 1939).). E. S.. H. Brit. H.). A. 2. and Jodeck.558 (May 8. S. 1949). 1931). (to Anglo-Persian Oil Co. Martini & Hdneke m. 24. J. 1939). (105) Maschinen. de Bataafsche Petroleum Maat(104) McKittrick. 1946).. U. Petroleum Research Corp. 1..382 (March 2. C.H.). 2. van (to N. 24. (65) Harrington. Research Corp.594.. U.234.871 (Dec. GRAVITY SEPARATED.. U.). Ibid.911(June 28. T. de Bataafsche Petroleum Maatschappij. (85) Tuttle. L. and Zeigler. 1937). T.158 (68) Standard Oil Development Co. de Bataafsche Petroleum Maat1939). 6.186) (Aug. 4.205. R.186 (Aug. (to Forest Products Chemical Co. Miller & Co.151 (Oct. Ibid.. Jr. 1934). Patent 569. de Bataafsche Petroleum Maatschappij.030 (Feb. M. C.766.043. (69) Eckart. (In(77) Fenske.. Brit.).. U. R. Ibid. and McCluer. Patent 521. U.892 (Jan. 2. I. 1927). U. (121) N. U. [to Standard Oil Co. P.429 (Oct. GRAVITY SEPARATED.. J.193 schappij). (to Edeleanu Ges.945 (122) Webb..).474.. 1. chimiques de Clamecy. V. and McManigal. 1933).H.). (103) McConnell.790 (Jan. Patent 27. and White. K.. 2. J. Patent 321. and Guinot. 2. BALPFLE (90) Davis. M. 2.H. DROPLETCONTACT WITHOUT POWER. M . E. 1934). J. W. R.328 (Nov.. (to Standard Oil Development Co. W. Patent (71) Ibid. 0. (93) Edeleanu. (to Penna. (81) Kiersted. R. PERFO. and Zeigler.154. D.132..569 (June 4. O.014 (Nov. (55) Etablissemente A.468.. 1949). (115) Soci6t6 des produits. GRAVITY SEPARATED.. 1937).382 (March 2.962 (May (100) Kester. H. 2.595 (June 15. (Aug. Ibid. BUBBLE (110) Payne. H.132. 2. 1934). and Mapes. Patent 584. P.645 (Aug. D. Gress. 22. U. Ibid. Patent TOWERS 1. Ibid. C. S.. DROPLETCONTACT WXTHOUT POWER. (addition to Ger.. 2. search Corp. Ibid.364. 2.540 (Oct.281 (June 11. Jr.011.. R. 4. 2. Ibid.). Patent 644. E. S. Brit. K. Ger. (to Allgemeine Ges. Ibid. 1940). 17. 2. B..429 (Oct.057 (April 13. 1932). F. 15. GRAVITY SEPARATED. P. Patent Patent 2. Patent 494. B..). TRACTOR WITH MOVABLE MEMBERS (80)Ibid. Patent 2. D. 31. 31. Patent 521. H. 1939).544 (May 13. 1930). S. 566. H. S. (83) Maschinen. (53) Coahran. G. E. schappij). D.). (61) Thompson.). 2. 9.318-19 (April 14. FILM-TYPE TOWERS (49) Gordon. U.. Patent (117) Tuttle. (to Ramage. 2.468. (106) Ibid. (84) Robinson. (113) Robinson. 1934). K. U.). W.164. R. M. 24.-G. Ibid. H. Petroleum diana)]. MIXERAND SETTLER (86) Anglo-Persian Oil Co. (108) Mensing.acs. (Indiana)]. 1941).144. Patent 640. Patent 265.. Ibid. R. G. 1.822 (Jan. A.541 (April 23. (74) Allgemeine Ges. B. (to Eastman Kodak Co.). PACKED (116) Soule. (101) Kiersted.. B. 1936). far chemische Industrie m. 2. Patent 2. Miller and Co. (75) Cattaneo.971 (Sept. T. Ibid. 2009 | http://pubs.. (59) Mann.422 (Dec. B. 16.. 1930). D.Patent 2. (to The Texas Co. (June 18. 1946). 2. (to Eastman Kodak Co. [to Standard Oil Co..943. W.606 (May 7. (56) Fenske.953. 1947). 1938). J. (to Penna. 1949).. M.June 1950 INDUSTRIAL AND ENGINEERING CHEMISTRY Extraction Equipment Patents GRAVITY SEPARATED.. J. 5.. 17.541 (March 23. DROPLET CONTACT WITHOUT POWER. 2. S. Texas Co. 24. 1940). S..b. (to Penna. C. 414. (June 8. Ibid. 1944). 1926). and Jodeck. 9. ) . (to Max B. W. 28. J.). 1932). (88) Bottaro.218. 2. search Corp.). 1938). 15. 9.... DROPLETCONTACT WITH POWER REQUIRED FOR REDISPERSION.044 (April 26. 1. van (to N. 4. F.057 (April 13..982 (Oct.(102) Lewis. Patent 736. (60) Poole. Bowden.org Publication Date: June 1.077. J.. 1. (to Standard Oil Development Co. J.176. Ibid. 1935). SPRAY TOWERS (50) Elgin.)..064. 1936). Patent 2. C.024 (July 27.405. 2.). V. (95) Goldman..845. Patent 521. and Mapes. 1935).. J.281). 0.949. (Ohio)]. 1937). (78) Ibid. D. 16. (62) Atkins. (to Shell Development Co. W. 1932). (119) Wilson.. 13. 1939)... and Wilson. S. 2. G. M. Patent.176. 2. E. (72) Ibid.651 (April 3. P.). (94) Eisen.132. J. 1938).und Apparatebau-Ges. S. 1932).780 RATED PLATETOWERS (Oct. 1. Ibid.507 (April 4. B. DROPLETCONTACT WITHOUT POWER.122.b. 2. J.942 (Feb. GRAVITY SEPARATED. M. (to The (97) Holley. Braun & Co. S. E.401. E.). 1938). 1937). (107) Maycock.007 (66) Koch.080 (Oct. E.. (76) Davis.139. 1913). 2..029 (Dec. 1937). (98) Jodeck. M. D. Ger.). U. P.072. (Indiana)].541). Brit. 1931).144 (April 11.). and Gieske. (to Max B. M. and McCluer. Brit.151 (Oct.. 1950 | doi: 10. S. Patent RECEIVED February 6. (to Shell Development Co. 1936). CONTACT TEROUOH FILMS. Pfeiffer. Patent 2. 1940).. (to Mid-Continent Petroleum 2. C. (112) Ricard. Brit.786 (Feb. (120) Dijck. U. F. T.000. 16.258. Ibid. R... Brit. 1946). 4. 0. (70) Fenske.). Ex(79) Ibid..274. W.). 7.103 (June2. S.284 (111) Poole. S.-G. Patent (June 21. V. U. 1947). 1937). 1939). F.921 (March 11. R. 2. 1934). 15.. Downloaded by UNIV OF GEORGIA on October 13.026. Ibid. (to Mid-Continent Petroleum Corp. 28.1021/ie50486a013 1035 1 .).734 (same as U. G.. Ibid.080). Patent 566. J. T. V. Petroleum ReGer.).. Patent 2.. Patent 1.153. (to Koppera Co. A. 1.132..176.797 (Jan. J. (63) Dijck. W.und Apparatebau-Ges.).074 (Oct. (same as U. usines de Melle).218. 24. J. Patent 2. (to C.. 1936). D. Patent 2.205. Ibid.. (51) Isles. Ibid. W.. H.899 (Oct. Ibid..186 (Aug. 12.).