Contacting arrangement
10058797 ยท 2018-08-28
Assignee
Inventors
Cpc classification
B01D11/043
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
Contacting arrangements adapted to be installed within a liquid-liquid extraction column, and including pairs of disk and doughnut plates.
Claims
1. A liquid-liquid contacting arrangement, adapted to be installed within a liquid-liquid extraction column, the contacting arrangement comprising: (a) a plurality of pairs of disk and doughnut plates, said pairs stacked in a generally longitudinal stack, said stack being generally perpendicular to broad faces of said disk and doughnut plates, each pair of said disk and doughnut pairs including: (i) a disk plate; and (ii) a doughnut plate, disposed beneath said disk plate; said disk plate having a first liquid-liquid contacting surface along an external perimeter of said disk plate; said doughnut plate having a second liquid-liquid contacting surface along an internal perimeter of said doughnut plate; and (b) a securing arrangement adapted to (i) affix said disk plate and said doughnut plate of said each pair in a first spaced-apart relationship; and (ii) affix, in a second spaced-apart relationship, said disk and doughnut pairs with respect to one another; at least a portion of at least one of said first and second contacting surfaces having teeth disposed in a proximate position to said first and second contacting surfaces, said proximate position defined by:
L.sub.cs-doughnut=K.Math.(D.sub.extD.sub.int), for said doughnut plates; and
L.sub.cs-disk=K.Math.(D.sub.disk), for said disk plates, wherein: L.sub.cs-doughnut is a maximum distance of said teeth on each particular doughnut plate, from said contacting surface of said particular doughnut plate; L.sub.cs-disk is a maximum distance of said teeth on each particular disk plate, from said contacting surface of said particular disk plate; D.sub.ext is an outer diameter of said doughnut plate, excluding any protrusions of said teeth; D.sub.int is an inner diameter of said doughnut plate, excluding any protrusions of said teeth; D.sub.disk is a diameter of said disk plate, excluding any protrusions of said teeth; said teeth having an average length of at least 2 mm; K is a coefficient, K being at most 0.05; and wherein a length ratio of said external perimeter, including said teeth, to a base perimeter of said disk, excluding said teeth, or of said internal perimeter, including said teeth, to a base perimeter of said doughnut, excluding said teeth, is at least 2.0.
2. The contacting arrangement of claim 1, said length ratio being at least 2.6.
3. The contacting arrangement of claim 1, said teeth being disposed on at least one of said disk plates.
4. The contacting arrangement of claim 1, said teeth including teeth disposed on both said contacting surface of said doughnut plate and said contacting surface of said disk plate.
5. The contacting arrangement of claim 1, said teeth including teeth disposed on at least one of a top surface of said doughnut plate and a top surface of said disk plate, and pointing upwards.
6. The contacting arrangement of claim 1, said teeth including teeth disposed on at least one of a bottom surface of said doughnut plate and a bottom surface of said disk plate, and pointing downwards.
7. The contacting arrangement of claim 1, a first disk plate and a first doughnut plate of a particular pair of said being longitudinally separated by a distance L.sub.pair, at least a portion of said teeth having a length of at least 0.03.Math.L.sub.pair.
8. The contacting arrangement of claim 7, said average length of said teeth being at least 0.03.Math.L.sub.pair.
9. The contacting arrangement of claim 1, said average length being at least 3 mm.
10. The contacting arrangement of claim 1, said average length being at least 0.025.Math.D.sub.ext.
11. The contacting arrangement of claim 10, said average length being at most 0.08.Math.D.sub.ext.
12. The contacting arrangement of claim 1, a spacing between said teeth being at least 3 mm.
13. The contacting arrangement of claim 1, further comprising said column.
14. The contacting arrangement of claim 13, further comprising a pulsation mechanism, said pulsation mechanism fluidly communicating with an internal volume of said column.
15. The contacting arrangement of claim 13, at least a particular doughnut plate of said doughnut plates further comprising teeth disposed radially outward with respect to D.sub.ext, between said particular doughnut plate and an internal surface of said column.
16. The contacting arrangement of claim 13, an outer spacing between a particular doughnut plate of said doughnut plates and an inner surface of said column having an area A.sub.spacing, an inner contacting area of said particular doughnut plate being defined by .Math.(D.sub.ext).sup.2/4, and an area ratio of said A.sub.spacing to said inner contacting area being within a range of 1-5%.
17. The contacting arrangement of claim 1, said disk and doughnut pair having at least one of: at least one disk aperture passing through said disk plate, and at least one doughnut aperture passing through said doughnut plate, an aperture area of said disk aperture being of a non-uniform radial distribution along said disk plate, such that an innermost area of said disk plate contains at least 60 area % of said at least one disk aperture, said innermost area being at most 50 area % of said disk plate.
18. A liquid-liquid contacting arrangement comprising: (a) a plurality of pairs of disk and doughnut plates, said pairs stacked in a generally longitudinal stack, said stack being generally perpendicular to broad faces of said disk and doughnut plates, each pair of said disk and doughnut pairs including: (i) a disk plate; and (ii) a doughnut plate, disposed beneath said disk plate; said doughnut plate having a second liquid-liquid contacting surface along an internal perimeter of said doughnut plate; and (b) a securing arrangement adapted to (i) affix said disk plate and said doughnut plate of said each pair in a first spaced-apart relationship; and (ii) affix, in a second spaced-apart relationship, said disk and doughnut pairs with respect to one another; at least a portion of said second contacting surface having teeth disposed in a proximate position to said second contacting surface, said proximate position defined by:
L.sub.cs-doughnut=K.Math.(D.sub.extD.sub.int), for said doughnut plates; and wherein: L.sub.cs-doughnut is a maximum distance of said teeth on each particular doughnut plate, from said contacting surface of said particular doughnut plate; D.sub.ext is an outer diameter of said doughnut plate, excluding any protrusions of said teeth; D.sub.int is an inner diameter of said doughnut plate, excluding any protrusions of said teeth; said teeth having an average length of at least 2 mm; K is a coefficient, K being at most 0.05; and wherein a length ratio of said internal perimeter including said teeth to a base perimeter of said doughnut, excluding said teeth, is at least 2.0.
19. The contacting arrangement of claim 18, further comprising said column and a pulsation mechanism, said pulsation mechanism fluidly communicating with an internal volume of said column.
20. A liquid-liquid contacting arrangement comprising: (a) a plurality of pairs of disk and doughnut plates, said pairs stacked in a generally longitudinal stack, said stack being generally perpendicular to top and bottom broad faces of said disk and doughnut plates, each pair of said disk and doughnut pairs including: (i) a disk plate; and (ii) a doughnut plate, disposed beneath said disk plate; said disk plate having a first liquid-liquid contacting surface along an external perimeter of said disk plate; said doughnut plate having a second liquid-liquid contacting surface along an internal perimeter of said doughnut plate; (b) a securing arrangement adapted to (i) affix said disk plate and said doughnut plate of said each pair in a first spaced-apart relationship; and (ii) affix, in a second spaced-apart relationship, said disk and doughnut pairs with respect to one another; (c) a column housing said longitudinal stack and said securing arrangement; and (d) a pulsation mechanism, fluidly communicating with an internal volume of said column; wherein at least a portion of at least one of said first and second contacting surfaces have teeth disposed in a proximate position to said first and second contacting surfaces, said proximate position defined by:
L.sub.cs-doughnut=K.Math.(D.sub.extD.sub.int), for said doughnut plates; and
L.sub.cs-disk=K.Math.(D.sub.disk), for said disk plates, wherein: L.sub.cs-doughnut is a maximum distance of said teeth on each particular doughnut plate, from said contacting surface of said particular doughnut plate; L.sub.cs-disk is a maximum distance of said teeth on each particular disk plate, from said contacting surface of said particular disk plate; D.sub.ext is an outer diameter of said doughnut plate, excluding any protrusions of said teeth; D.sub.int is an inner diameter of said doughnut plate, excluding any protrusions of said teeth; D.sub.disk is a diameter of said disk plate, excluding any protrusions of said teeth; said teeth having an average length of at least 2 mm; K is a coefficient, K being at most 0.05; wherein a length ratio of said external perimeter including said teeth to a base perimeter of said disk, excluding said teeth, or of said internal perimeter including said teeth to a base perimeter of said doughnut, excluding said teeth, is at least 2.0; said teeth including teeth disposed on at least one of: said top broad face of said doughnut plate and said top broad face of said disk plate, and pointing upwards; and said bottom broad face of said doughnut plate and said bottom broad face of said disk plate, and pointing downwards.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) The invention is herein described, by way of example only, with reference to the accompanying drawings. With specific reference now to the drawings in detail, it is stressed that the particulars shown are by way of example and for purposes of illustrative discussion of the preferred embodiments of the present invention only, and are presented in the cause of providing what is believed to be the most useful and readily understood description of the principles and conceptual aspects of the invention. In this regard, no attempt is made to show structural details of the invention in more detail than is necessary for a fundamental understanding of the invention, the description taken with the drawings making apparent to those skilled in the art how the several forms of the invention may be embodied in practice. Throughout the drawings, like-referenced characters are used to designate like elements.
(2) In the drawings:
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DESCRIPTION OF THE PREFERRED EMBODIMENTS
(30) The principles and operation of the disk and doughnut extraction column according to some embodiments of the present invention may be better understood with reference to the drawings and the accompanying description.
(31) Before explaining at least one embodiment of the invention in detail, it is to be understood that the invention is not limited in its application to the details of construction and the arrangement of the components set forth in the following description or illustrated in the drawings. The invention is capable of other embodiments or of being practiced or carried out in various ways. Also, it is to be understood that the phraseology and terminology employed herein is for the purpose of description and should not be regarded as limiting.
(32) Referring now to the drawings,
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(34) In pulsed disk and doughnut columns, especially in large-diameter columns, non-agitated areas exist in various parts of the contacting volume.
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(36) According to teachings of the present invention, there are provided improved contacting elements on the contours of the disk and doughnut plates. The enhanced mass transfer is achieved by various mechanisms, including: (a) teeth are introduced to the contacting areas of the disk and/or doughnuts to increase the length of the contacting area. The most effective area for mass transfer is the area near the liquid-liquid contacting areas; (b) teeth disposed on the contours of the plates enhance the breakage of droplets; and (c) additional resistance from the modified contours increases the fraction of the dispersed phase (also known as holdup).
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(38) Teeth 330, 331 may be disposed in a proximate position to contacting surfaces 340, 341, with this proximate position defined by:
L.sub.cs-doughnut=(D.sub.extD.sub.int).Math.K, for doughnut plates; and
L.sub.cs-disk=(D.sub.disk).Math.K, for disk plates,
wherein: L.sub.cs-doughnut is a maximum distance of teeth (length) on each particular doughnut plate, from contacting surface 340 of a particular doughnut plate; L.sub.cs-disk is a maximum distance of teeth (length) on each particular disk plate, from contacting 341 surface of a particular disk plate; D.sub.ext is an outer diameter of the doughnut plate, excluding any protrusions of the teeth; D.sub.int is an inner diameter of the doughnut plate, excluding any protrusions of the teeth; D.sub.disk is a diameter of the disk plate, excluding any protrusions of the teeth, the teeth having an average length of at least 2 mm; and K is a coefficient; K being at most about 0.05.
(39) In various embodiments, it may be advantageous for K to be at most 0.04, 0.035, 0.03, 0.025, or 0.02.
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(48) The inventors have found, inter alia on the basis of visual observations, that hold-up may be improved and non-agitated areas may be appreciably decreased at length ratios of at least 2.0, at least 2.2, at least 2.4, at least 2.6, at least 2.8, at least 3.0, at least 3.5, at least 4.0, at least 4.5, or at least 5.0. Typically, the length ratios are within a range of 2.0-6.0, 2.4-5.0, 2.4-4.0, or 2.6-3.5.
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(50) One design principle in the classical design of disk and doughnut stacks is to minimize shortcutting or bypassing phenomena. To this end, the clearance between the doughnut plates and the shell (wall) approaches zero, on average, and disk plates are fabricated without holes or apertures. The inventors have discovered, however, that gaps and/or aperture(s) of 1% to 5% of the total disk plate area may appreciably reduce the non-agitated volume, while the negative ramifications of the bypassing of disks or doughnuts is relatively insignificant.
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(56) As shown in exemplary fashion in
(57) As shown in exemplary fashion in
(58) In some embodiments, at least 20 area %, at least 40 area %, at least 60 area %, at least 80 area %, or at least 95 area % of the doughnut apertures is disposed radially outside of the disk apertures. According to still further features in the described preferred embodiments, at least 10 area %, at least 20 area %, at least 40 area %, at least 60 area %, at least 80 area %, or at least 95 area % of the doughnut apertures is disposed radially outside of the disk plate. In the exemplary embodiment provided in
(59) In some embodiments, at least 40 area %, at least 60 area %, at least 70 area %, at least 80 area %, at least 90 area %, or at least 95 area % of the doughnut aperture or apertures is radially disaligned with respect to the aperture area of the disk plate. In the exemplary embodiment provided in
(60) In some embodiments, at least 10 area %, at least 20 area %, at least 40 area %, at least 60 area %, at least 80 area %, or at least 95 area % of doughnut apertures 733 is disposed in a radially outward fashion with respect to disk plate 721. In the exemplary embodiment provided in
EXAMPLES
(61) Reference is now made to the following examples, which together with the above description, illustrate the invention in a non-limiting fashion.
(62)
Example 1
Apparatus Description
(63) In a pilot facility, the pulsed column had an active section height of 3 m and an internal diameter of 100 mm containing PVDF disk and doughnut pairs having a spacing of 23.7 mm. The upper decanter had an inner diameter of 150, and the lower decanter had an inner diameter of 100 mm. The column was pulsed periodically by a mechanical pulsation mechanism including a positive displacement arrangement of a Teflon piston within a cylinder having a diameter of 120 mm. The length of the stroke was manually controlled by a wheel, providing a displacement length within a range of 0-30 mm. The frequency of the stroke was held constant at 60 strokes per minute.
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(65) Two types of packing were tested in order to examine the influence of the teeth internals:
(66) (1) Standard Internals
(67) The disks had a diameter of 87 mm and the doughnut apertures were 49 mm, yielding open (free) areas of 24% for both disk plates and doughnut plates.
(68) (2) Modified Internals
(69) The open (free) areas and the spacing between the internals were maintained as in the standard internals.
(70) The general configuration of the disk and doughnut plates was according to
(71) Liquid-Liquid System
(72) Organic phase: Kerosene (ShellSolg D70) as the continuous phase.
(73) Aqueous phase: 10 g/L H.sub.2SO.sub.4 as the dispersed phase.
(74) Hydraulic test: no mass transfer.
(75) Phase ratio O: A [v/v]=1:1.
(76) Results
(77) The maximum flux was determined to be about 50 m3/m2/h, for both types of internals.
(78) The holdup was increased by 10-70%. Holdup results at flux 30 and 40 m3/m2/h, respectively, are shown in Table 1.
(79) TABLE-US-00001 TABLE 1 Pulsator amplitude mm 0 4 8 12 16 20 Holdup at [v/v] % Standard 30 23 11 12 10 10 Flux 30 internals m3/m2/h Modified 28 25 16 14 17 24 internals Holdup at [v/v] % Standard flooding 23 17 20 21 20 Flux 40 internals m3/m2/h Modified flooding 30 20 23 26 flooding internals
(80) The quality of dispersion (based on visual observation and characterization) was improved significantly using the inventive internals: the droplet size decreased, and the size of the dead zones below the disk and doughnut plates was appreciably reduced.
Example 2
Apparatus Description
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(82) The barren organic mixture was pumped into the bottom of the column. The loaded organic (upper) effluent overflowed from the upper decanter. The aqueous phase was pumped to the top of the active section.
(83) (1) Standard Internals
(84) As described in Example 1.
(85) (2) Modified Internals
(86) The open (free) areas and the spacing between the internals were maintained as in the standard internals.
(87) The general configuration of the disk and doughnut plates was according to
(88) Liquid-Liquid System
(89) Organic phase: 10% [v/v] DEHPA in Kerosene (ShellSol D70) as the dispersed phase.
(90) Aqueous phase: 55 g/L Zn solution (based on ZnSO.sub.4).
(91) Mass transfer test: Zn transferring from the aqueous phase to DEHPA.
(92) Phase ratio O: A [v/v]=10:1.
(93) The tests were performed at a constant flux of 20 m3/m2/h, and at a constant amplitude of 8 mm.
(94) Significant improvement was achieved using the inventive internals arrangement, as shown in Table 2 (concentrations expressed in g Zn/L):
(95) TABLE-US-00002 TABLE 2 Barren Loaded Aqueous Aqueous Organic Organic NTU.sup.1 HTU.sup.2 in [g/L] out [g/L] [g/L] [g/L] [#] [m] Standard 52.5 36.3 0.1 1.8 1.7 1.8 internals Modified 52.5 32.0 0.1 2.2 2.8 1.1 internals .sup.1NTU = number of theoretical units .sup.2HTU = height of theoretical unit
Example 3
Apparatus Description
(96) The pulsed column system and general apparatus and method used in Example 3 are described in Example 1 (see also
(97) (1) Standard Internals
(98) As described in Example 1.
(99) (2) Modified Internals
(100) The open (free) areas and the spacing between the internals were maintained as in the standard internals.
(101) The contour of the modified internals was substantially as shown in
(102) Liquid-Liquid System
(103) Organic phase: Kerosene (ShellSol D70) as the dispersed phase.
(104) Aqueous phase: 10 g/L H.sub.2SO.sub.4 as the continuous phase.
(105) Hydraulic test: no mass transfer.
(106) Phase ratio O: A [v/v]=1:1.
(107) Results
(108) The maximum flux was found to be approximately 55 m3/m2/h. The results using the standard internals and the inventive internals are provided in Table 3. Using the inventive internals, the quality of dispersion was improved, as shown schematically in
(109) TABLE-US-00003 TABLE 3 Pulsator amplitude mm 0 4 8 12 16 20 Holdup at [v/v] % Standard 8 4 4 4 9 17 Flux 30 internals m3/m2/h Modified 10 5 4 7 11 18 internals Holdup at [v/v] % Standard flooding 14 9 9 13 23 Flux 40 internals m3/m2/h Modified flooding 15 10 11 18 29 internals
Example 4
Apparatus Description
(110) The pulsed column system and general apparatus and method used in Example 4 are described in Example 1.
(111) (1) Standard Internals
(112) As described in Example 1.
(113) (2) Modified Internals (see
(114) The open (free) areas and the spacing between the internals were maintained as in the standard internals. The outer spacing between the doughnut and the column shell had an area equivalent to (a) 0.5%; (b) 1.5%; and (c) 4% of the total cross-sectional area of the column shell.
(115) Liquid-Liquid System
(116) Organic phase: Methyl Isobutyl Ketone (MIBK) as the continuous phase.
(117) Aqueous phase: deionized water as the dispersed phase.
(118) Hydraulic test: no mass transfer.
(119) Phase ratio O: A [v/v]=4:1.
(120) Visual Observations
(121) With respect to the standard internals, the turbulence below the disk and doughnuts plates was not improved for (a). In (b), some improvement and reductions of the dead volumes were observed. In (c), reductions of the dead volumes were observed. However, for much larger outer spacings, significant short-circuiting via the outer spacing was observed.
Example 5
Apparatus Description
(122) The pulsed disk and doughnut column system used was identical to the system used in the experiment of Example 2. The column was identical to that described with respect to Example 1.
(123) This example refers to the purification step in the solvent extraction section in purified phosphoric acid production. The loaded organic mixture was pumped into the bottom of the column. The purified organic (upper) effluent overflowed from the upper decanter. The aqueous phase was pumped to the top of the active section.
(124) (1) Standard Internals
(125) As described in Example 1.
(126) (2) Modified Internals
(127) The open (free) areas and the spacing between the internals were maintained as in the standard internals.
(128) The general configuration of the disk and doughnut plates was according to
(129) Liquid-Liquid System
(130) Organic phase: MIBK (methyl isobutyl ketone) containing 125 mg/kg Fe as the continuous phase.
(131) Aqueous phase: purified phosphoric acid containing 10 mg/kg Fe.
(132) Mass transfer test: Fe transferring from MIBK to aqueous phase.
(133) Phase ratio O: A [v/v]=10:112:1.
(134) The tests were performed at a constant flux of about 20 m3/m2/h.
(135) Significant improvement was achieved using the inventive internals arrangement, as shown in Table 4 (concentrations expressed in mg Fe/kg solution):
(136) TABLE-US-00004 TABLE 4 Aqueous Aqueous Loaded Purified NTU.sup.1 HTU.sup.2 in out Organic Organic [#] [m] Standard 13 1600 125 4 3 0.42 internals Modified 6 2100 125 <1 4.5 0.65 internals .sup.1NTU = number of theoretical units .sup.2HTU = height of theoretical unit
(137) It will be appreciated that certain features of the invention, which are, for clarity, described in the context of separate embodiments, may also be provided in combination in a single embodiment. Conversely, various features of the invention, which are, for brevity, described in the context of a single embodiment, may also be provided separately or in any suitable sub-combination.
(138) Although the invention has been described in conjunction with specific embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art. Accordingly, it is intended to embrace all such alternatives, modifications and variations that fall within the spirit and broad scope of the appended claims. All publications, patents and patent applications mentioned in this specification, including U.S. Pat. No. 2,601,674 to Reman et al., U.S. Pat. No. 4,200,522 to Karr, and U.S. Pat. No. 2,011,186 to Van Dijk are herein incorporated in their entirety by reference into the specification, to the same extent as if each individual publication, patent or patent application was specifically and individually indicated to be incorporated herein by reference. In addition, citation or identification of any reference in this application shall not be construed as an admission that such reference is available as prior art to the present invention.