Title of Invention	"A DISTILLATION COLUMN"
Abstract	Improved help is obtained in the operation of a distillation column containing prays with a packin of a pofous container containing a percolate material imimatey asspcined with a resilient component having at least 50 volume 9 open spared. Preferably at least 70 volume g positioned on the trays compared to the trays without the packing. The packing may contain a catalytic particulate material and the distillation may involve reaction and distillation of the reaction products. The particulate material may also he infect and the distillation of the conventional type to separate commoners in the distillation moisture without reaction.

Title of Invention

"A DISTILLATION COLUMN"

Abstract

Improved help is obtained in the operation of a distillation column containing prays with a packin of a pofous container containing a percolate material imimatey asspcined with a resilient component having at least 50 volume 9 open spared. Preferably at least 70 volume g positioned on the trays compared to the trays without the packing. The packing may contain a catalytic particulate material and the distillation may involve reaction and distillation of the reaction products. The particulate material may also he infect and the distillation of the conventional type to separate commoners in the distillation moisture without reaction.

Full Text	DISTILLATION SYSTEM BACKGROUND OF THE INVENTION Field of the Invention The present invention relates to a system for concurrently carrying out distillation or chemical reactions and separating the reactants and products by fractional distillation. Related Art A method of carrying out catalytic reactions has been developed and widely commercialized, wherein the components of the reaction mixture are concurrently separable by fractional distillation. Several systems have been proposed and one commercially successful system uses the catalyst as the catalytic distillation structure. Such a system is variously described in U.S. Pat. Nos. 4,215,011; 4,232,177; 4,242,530; 4,250,052; 4,302,356; 4,307,254; 4,336,407; 4,439,350; 4,443,559; and 4,482,775 commonly assigned herewith., Briefly, the commercial catalytic structure described therein comprises a cloth belt with a plurality of pockets spaced along the belt and containing particulate catalyst material. The cloth belt with catalyst filled pockets is wound into a helix about a spacing material such as knitted stainless steel wire mesh, and these "bales" loaded into a distillation column. Additionally U.S. Pat. Nos. 4,302,356, 4,443,559 and 4,250,052 disclose a variety of catalyst structures for this use. Placing the particulate catalyst loose on standard distillation trays has also been proposed. See, for example, U.S. Pat. No. 4,215,011 and U.K. patents GB 2,096,603 and 2,096,604, U.S.Pat. No. 4,439,350 discloses a clip which holds and supports closed porous containers of catalyst spaced apart from each other on a distillation tray within the liquid on the tray. The placement of the catalyst in the downcomers of standard distillation columns has been proposed as in U.S. Pat. No. 3,634,534. Fluidization of the catalyst on the trays has also been suggested as in U.S. Pat. No. 4,471,154. Some deficiencies of such fluidized beds were recognized in ChemikerZeitung/Chemische Apparatur, vol. 90, no. 13, July 1966 and U.S. Pat. No. 4,215,011. Quang, etal, in U.S. Pat. No. 4.847,430 and Nocca, et al in U.S. Pat. No. 4,847,431 disclose loading the particufate catalyst on alternating trays of a distillation column and with a gas bypass about the catalyst loaded trays. The us The main problems sought to be overcome by the improvements have been the reduction of pressure drop through the column and provision of sufficient contact of the reactants with the catalyst while providing for good vapor liquid contact for the fractional distillation. Many useful catalysts are in the form of fine particulato powders which preclude their use directly as distillation components. Even larger' extruded pellets do not lend themselves well as distillation structures. Hence the use of cloth belts, cages and support trays is the predominant developmental thrust. While larger catalysts structures have been proposed, the porosity requirements of many catalytic materials limit their structural integrity. Many catalysts which rely on outer surface activity only and which might have the strength for larger structures are useful only for gas phase reactions, such && maleic anhydride production. U.S. Pat. Nos. 4,443,559 and 5,266,546 both disclose catalytic distillation structures that may be placed on trays similar to sieve trays for support in a distillation column reactor. . The present invention is related to these structures and catalytic distillation, but it is also related to distillation in general. It is an advantage of the present' . invention that greater tower efficiency may be obtained for conventional distillation ' trays by use of the present system. No art is known to suggest the present invention and In fact conventional knowledge would suggest the present invention would be counterproductive. The unexpected benefit of the present invention will be obvious from the disclosures herein. SUMMARY OF THE INVENTION Surprisingly it has been found that in the operation of a distillation column containing a plurality of trays wherein a packing comprising a porous container containing a particulate material intimately associated with a resilient component, said resilient component being comprised of at least 50 volume % open space, preferably at least 70 volume % and positioned on trays provides height equivalent to theoretical plates (HETP) of less than said trays without said packing. The packing may contain a catalytic participate material and the distillation may involve reaction and distillation of the reaction products. The particulate material may also be inert and the distillation of the conventional type to separate components in the distillation mixture without reaction. The tray may be any of the conventional trays (or modifications thereof), such as sieve trays and bubble trays. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a graph showing improved HETP in inches for the present packed tray column compared to the same tray column without the packing. FIG, 2 is a schematic representation of a partial section of a distillation with the packing in place. DESCRIPTION OF THE PREFERRED EMBODIMENT The present packing may fill the entire space between the trays or only so much of the area so as to obtain the benefit of the lower HETP. The packed trays may have lower capacity than the non packed trays. The limitation on the non packed trays (as used in conventional distillation) is the liquid entrainment, whereas it appears that downcomer capacity is a limitation on the capacity for the present packed trays. Hydraulic calculation indicates the throughput limitation that the downcomer backup is likely to impose on the packed trays. The equivalent clear liquid level in the downcomer must balance the vapor flow pressure drop as follows: ndcfnda ~ hd+2hL where hdc = head of froth in the downcomer, equivalent clear liquid. hds = pressure loss for liquid flow under the downcomer baffle, hd = pressure loss for flow through one tray. hL - pressure loss for the two-phase flow through packing. In this relationship, head can be expressed as clear liquid or as equivalent water, the value of h.L Is obtained from overall tray pressure drop measurements. It has been observed that in a catalyst bed a free space of about 50 volume percent is adequate to obtain operable fractionation. The participate material may be employed by enclosing it in a proof. container such as cloth, screen wire or polymeric mesh, The material used to make . the container must be inert to the reactants and conditions in the distillation or reaction/distillation system. The cloth may be any material which meets this requirement such as cotton, fiber glass, polyester, nylon and the like. The screen' wire may be aluminum, steel, stainless steel and the like. The polymer mesh may be nylon, teflon or the like. The mesh or threads per inch of the material used to'. make the container is such that the particulate material is retained therein and will not pass through the openings. Particles of about 0.15 mm size or powders may bo used and particles up to about 1/4 inch diameter may be employed In the containers. The container employed to hold the catalyst particles may have any, configuration, such as the pockets disclosed in the commonly assigned patents above or the container may be a single cylinder, sphere, doughnut, cube, tube or the like. Each container containing a solid particulate material (inert or catalytic) comprises a particulate component. Each particulate component is intimately associated with a spacing component which is comprised of at least 70 volume % open space up to about 95 volume % open space. This component may be rigid or. resilient or a combination thereof. The combination of catalyst component and spacing component form the catalytic distillation structure. One suitable such material is open mesh knitted stainless wire, known generally as demister wire or an expanded aluminum. Other resilient components may be similar open mesh knitted polymeric filaments of nylon, teflon and the like. It is only necessary that the spacing component intimately associated with the catalyst component will act to space the various catalyst components away from one another as described above. Thus, the spacing component provides in effect a matrix of substantially open space in which the catalyst components are randomly but substantially evenly distributed. Rigid or nan resilient spacing components are disclosed in U.S. Pat No: ' •. 5,730,843 (which is incorporated herein in its entirety) where a rigid frame comprised of at least two substantially vertical duplicate grids, a plurality of substantially horizontal rigid members spacing and holding the grids apart and a plurality of substantially horizontal fluid permeable, preferably wire mesh,- tubes mounted to said grids to form a plurality of fluid pathways among said tubes and preferably at least a portion of said wire mesh tubes contain a particulate material. The container may cloth or other porous material which is inert in the environment of use. Cotton or linen is useful: but fiber glass cloth or "Teflon" cloth is preferred as is wire mesh. The particulate material may be powder, but is generally larger, e.g. from 0.25 to 1mm with larger particles up to 1/4" also being used. The packing surface efficiency IB high. Importantly, the liquid appears to flow through the cloth wall (it is forced to do so) which may provide better penetration of catalyst particles than would be obtained in conventional counterflow. Referring to Fig, 2 a partial column 10 is shown with sieve trays 12 and downcomers 14. Between each tray the packing 16, comprising the particle containers 20 and demister wire 18. The packing 16 is arranoed under th8 downcomer to the tray but leaving the downcomer from the tray on which it sits to remain open. In this embodimentthe last few inches of space ia filled with demister wire. EXAMPLE The data for Fig. 1 was obtained using a column having 6 sieve trays spaced at 18 inches at 24 psla of the separation of a cyclohexane/n-heptane mixture under total reflux. The packing is formed by placing multiple link or continuous tube shaped structures on top of a wire mesh screen, such as demister wire. The tube comprises flexible, semi-rigid wire mesh tubular element filled with a particulate catalytic material the tube shaped structure having a fastener every 1-12 inches (n length to form a multiple link looking like a chain of screen wire saueagea. The packing is that described in U.S. 5,432,890 unrolled and packed in between each tray with demister wire between each layer of the tubing, providing alternating layers of demister wire and close placed tubes of catalyst. The entire space between the trays was packed in this manner, with at least the demister wire going to the tray above. The space over the downcomers was left open to allow liquid to disengage from the packing. The fractionating factor for the packed trays is substantially the same as the sieve trays alone. The invention claimed is: 1. In the operation of a distillation column containing a plurality of trays wherein the improvement comprises positioning on said trays a packing comprising a porous container containing a particulate material intimately associated with a spacing component, said resilient component being comprised of at least 50 volume % open space in an amount to provide height equivalent to theoretical plates (HETP) of less than said trays without said packing. 2. The process according to claim 1 wherein said open space Is at least 7G. volume %. 3. The process according to claim 1 wherein said particulate material comprises a catalytic particulate material and the distillation involves reaction and 4 distillation of the reaction products. 4. The process according to claim 1 wherein said particulate material comprises inert material and the distillation is for separation components in the distillation mixture without reaction, 5. The process according to claim 1 wherein said particulate material comprises catalytic particulate material and the distillation is for the separation of components in the distillation mixture without reaction. 6. The process according to claim 1 wherein trie spacing component is resilient. 7. The process according to claim 1 wherein the spacing component is rigid. 8. The process according to claim 1, 2, 3, 4, 5, 6 or 7 wherein said trays comprise sieve trays, ' 9. The process according to claim 1, 2, 3, 4, 5, 6 or 7 wherein said trays comprise bubble (rays. 10. The process according to claim 8 wherein said column is operated to separate cydohexane from n-heptane. 11. The process according to claim 10 wherein said HETP is less than 28 inches.

Full Text

DISTILLATION SYSTEM BACKGROUND OF THE INVENTION Field of the Invention
The present invention relates to a system for concurrently carrying out distillation or chemical reactions and separating the reactants and products by fractional distillation. Related Art
A method of carrying out catalytic reactions has been developed and widely commercialized, wherein the components of the reaction mixture are concurrently separable by fractional distillation. Several systems have been proposed and one commercially successful system uses the catalyst as the catalytic distillation structure. Such a system is variously described in U.S. Pat. Nos. 4,215,011; 4,232,177; 4,242,530; 4,250,052; 4,302,356; 4,307,254; 4,336,407; 4,439,350; 4,443,559; and 4,482,775 commonly assigned herewith.,
Briefly, the commercial catalytic structure described therein comprises a cloth belt with a plurality of pockets spaced along the belt and containing particulate catalyst material. The cloth belt with catalyst filled pockets is wound into a helix about a spacing material such as knitted stainless steel wire mesh, and these "bales" loaded into a distillation column. Additionally U.S. Pat. Nos. 4,302,356, 4,443,559 and 4,250,052 disclose a variety of catalyst structures for this use.
Placing the particulate catalyst loose on standard distillation trays has also been proposed. See, for example, U.S. Pat. No. 4,215,011 and U.K. patents GB 2,096,603 and 2,096,604, U.S.Pat. No. 4,439,350 discloses a clip which holds and supports closed porous containers of catalyst spaced apart from each other on a distillation tray within the liquid on the tray. The placement of the catalyst in the downcomers of standard distillation columns has been proposed as in U.S. Pat. No. 3,634,534. Fluidization of the catalyst on the trays has also been suggested as in U.S. Pat. No. 4,471,154. Some deficiencies of such fluidized beds were recognized in ChemikerZeitung/Chemische Apparatur, vol. 90, no. 13, July 1966 and U.S. Pat. No. 4,215,011. Quang, etal, in U.S. Pat. No. 4.847,430 and Nocca, et al in U.S. Pat. No. 4,847,431 disclose loading the particufate catalyst on alternating trays of

a distillation column and with a gas bypass about the catalyst loaded trays. The us The main problems sought to be overcome by the improvements have been the reduction of pressure drop through the column and provision of sufficient contact of the reactants with the catalyst while providing for good vapor liquid contact for the fractional distillation. Many useful catalysts are in the form of fine particulato powders which preclude their use directly as distillation components. Even larger' extruded pellets do not lend themselves well as distillation structures. Hence the use of cloth belts, cages and support trays is the predominant developmental thrust. While larger catalysts structures have been proposed, the porosity requirements of many catalytic materials limit their structural integrity. Many catalysts which rely on outer surface activity only and which might have the strength for larger structures are useful only for gas phase reactions, such && maleic anhydride production. U.S. Pat. Nos. 4,443,559 and 5,266,546 both disclose catalytic distillation structures that may be placed on trays similar to sieve trays for support in a distillation column reactor. .
The present invention is related to these structures and catalytic distillation, but it is also related to distillation in general. It is an advantage of the present' . invention that greater tower efficiency may be obtained for conventional distillation ' trays by use of the present system. No art is known to suggest the present invention and In fact conventional knowledge would suggest the present invention would be counterproductive. The unexpected benefit of the present invention will be obvious from the disclosures herein.
SUMMARY OF THE INVENTION
Surprisingly it has been found that in the operation of a distillation column containing a plurality of trays wherein a packing comprising a porous container containing a particulate material intimately associated with a resilient component,

said resilient component being comprised of at least 50 volume % open space, preferably at least 70 volume % and positioned on trays provides height equivalent to theoretical plates (HETP) of less than said trays without said packing. The packing may contain a catalytic participate material and the distillation may involve reaction and distillation of the reaction products. The particulate material may also be inert and the distillation of the conventional type to separate components in the distillation mixture without reaction.
The tray may be any of the conventional trays (or modifications thereof), such as sieve trays and bubble trays.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing improved HETP in inches for the present packed tray column compared to the same tray column without the packing.
FIG, 2 is a schematic representation of a partial section of a distillation with the packing in place.
DESCRIPTION OF THE PREFERRED EMBODIMENT The present packing may fill the entire space between the trays or only so much of the area so as to obtain the benefit of the lower HETP. The packed trays may have lower capacity than the non packed trays. The limitation on the non packed trays (as used in conventional distillation) is the liquid entrainment, whereas it appears that downcomer capacity is a limitation on the capacity for the present packed trays. Hydraulic calculation indicates the throughput limitation that the downcomer backup is likely to impose on the packed trays. The equivalent clear liquid level in the downcomer must balance the vapor flow pressure drop as follows:
ndcfnda ~ hd+2hL
where hdc = head of froth in the downcomer, equivalent clear liquid.
hds = pressure loss for liquid flow under the downcomer baffle,
hd = pressure loss for flow through one tray.
hL - pressure loss for the two-phase flow through packing. In this relationship, head can be expressed as clear liquid or as equivalent water, the value of h.L Is obtained from overall tray pressure drop measurements.
It has been observed that in a catalyst bed a free space of about 50 volume percent is adequate to obtain operable fractionation.

The participate material may be employed by enclosing it in a proof. container such as cloth, screen wire or polymeric mesh, The material used to make . the container must be inert to the reactants and conditions in the distillation or reaction/distillation system. The cloth may be any material which meets this requirement such as cotton, fiber glass, polyester, nylon and the like. The screen' wire may be aluminum, steel, stainless steel and the like. The polymer mesh may be nylon, teflon or the like. The mesh or threads per inch of the material used to'. make the container is such that the particulate material is retained therein and will not pass through the openings. Particles of about 0.15 mm size or powders may bo used and particles up to about 1/4 inch diameter may be employed In the containers. The container employed to hold the catalyst particles may have any, configuration, such as the pockets disclosed in the commonly assigned patents above or the container may be a single cylinder, sphere, doughnut, cube, tube or the like.
Each container containing a solid particulate material (inert or catalytic) comprises a particulate component. Each particulate component is intimately associated with a spacing component which is comprised of at least 70 volume % open space up to about 95 volume % open space. This component may be rigid or. resilient or a combination thereof. The combination of catalyst component and spacing component form the catalytic distillation structure. One suitable such material is open mesh knitted stainless wire, known generally as demister wire or an expanded aluminum. Other resilient components may be similar open mesh knitted polymeric filaments of nylon, teflon and the like. It is only necessary that the spacing component intimately associated with the catalyst component will act to space the various catalyst components away from one another as described above. Thus, the spacing component provides in effect a matrix of substantially open space in which the catalyst components are randomly but substantially evenly distributed.
Rigid or nan resilient spacing components are disclosed in U.S. Pat No: ' •. 5,730,843 (which is incorporated herein in its entirety) where a rigid frame comprised of at least two substantially vertical duplicate grids, a plurality of substantially horizontal rigid members spacing and holding the grids apart and a plurality of substantially horizontal fluid permeable, preferably wire mesh,- tubes

mounted to said grids to form a plurality of fluid pathways among said tubes and preferably at least a portion of said wire mesh tubes contain a particulate material. The container may cloth or other porous material which is inert in the environment of use. Cotton or linen is useful: but fiber glass cloth or "Teflon" cloth is preferred as is wire mesh. The particulate material may be powder, but is generally larger, e.g. from 0.25 to 1mm with larger particles up to 1/4" also being used.
The packing surface efficiency IB high. Importantly, the liquid appears to flow through the cloth wall (it is forced to do so) which may provide better penetration of catalyst particles than would be obtained in conventional counterflow.
Referring to Fig, 2 a partial column 10 is shown with sieve trays 12 and downcomers 14. Between each tray the packing 16, comprising the particle containers 20 and demister wire 18. The packing 16 is arranoed under th8 downcomer to the tray but leaving the downcomer from the tray on which it sits to remain open. In this embodimentthe last few inches of space ia filled with demister wire.
EXAMPLE
The data for Fig. 1 was obtained using a column having 6 sieve trays spaced at 18 inches at 24 psla of the separation of a cyclohexane/n-heptane mixture under total reflux. The packing is formed by placing multiple link or continuous tube shaped structures on top of a wire mesh screen, such as demister wire. The tube comprises flexible, semi-rigid wire mesh tubular element filled with a particulate catalytic material the tube shaped structure having a fastener every 1-12 inches (n length to form a multiple link looking like a chain of screen wire saueagea. The packing is that described in U.S. 5,432,890 unrolled and packed in between each tray with demister wire between each layer of the tubing, providing alternating layers of demister wire and close placed tubes of catalyst. The entire space between the trays was packed in this manner, with at least the demister wire going to the tray above. The space over the downcomers was left open to allow liquid to disengage from the packing. The fractionating factor for the packed trays is substantially the same as the sieve trays alone.

The invention claimed is:
1. In the operation of a distillation column containing a plurality of trays wherein the improvement comprises positioning on said trays a packing comprising a porous container containing a particulate material intimately associated with a spacing component, said resilient component being comprised of at least 50 volume % open space in an amount to provide height equivalent to theoretical plates (HETP) of less than said trays without said packing.
2. The process according to claim 1 wherein said open space Is at least 7G.
volume %.
3. The process according to claim 1 wherein said particulate material
comprises a catalytic particulate material and the distillation involves reaction and
4
distillation of the reaction products.
4. The process according to claim 1 wherein said particulate material
comprises inert material and the distillation is for separation components in the
distillation mixture without reaction,
5. The process according to claim 1 wherein said particulate material
comprises catalytic particulate material and the distillation is for the separation of
components in the distillation mixture without reaction.
6. The process according to claim 1 wherein trie spacing component is
resilient.
7. The process according to claim 1 wherein the spacing component is rigid.
8. The process according to claim 1, 2, 3, 4, 5, 6 or 7 wherein said trays
comprise sieve trays, '
9. The process according to claim 1, 2, 3, 4, 5, 6 or 7 wherein said trays
comprise bubble (rays.

10. The process according to claim 8 wherein said column is operated to
separate cydohexane from n-heptane.
11. The process according to claim 10 wherein said HETP is less than 28
inches.

Documents:

1525-DELNP-2005-Abstract (30-10-2007).pdf

1525-DELNP-2005-Abstract-09-05-2008.pdf

1525-delnp-2005-abstract.pdf

1525-DELNP-2005-Claims (30-10-2007).pdf

1525-DELNP-2005-Claims-09-05-2008.pdf

1525-delnp-2005-claims.pdf

1525-DELNP-2005-Correspondence-Others (30-10-2007).pdf

1525-DELNP-2005-Correspondence-Others-08-04-2008.pdf

1525-DELNP-2005-Correspondence-Others-09-05-2008.pdf

1525-delnp-2005-correspondence-others.pdf

1525-DELNP-2005-Description (Complete) (30-10-2007).pdf

1525-DELNP-2005-Description (Complete) -09-05-2008.pdf

1525-delnp-2005-description (complete).pdf

1525-DELNP-2005-Description (Complete)08-04-2008.pdf

1525-DELNP-2005-Drawings (30-10-2007).pdf

1525-delnp-2005-drawings.pdf

1525-DELNP-2005-Form-1 (30-10-2007).pdf

1525-DELNP-2005-Form-1-08-04-2008.pdf

1525-DELNP-2005-Form-1-09-05-2008.pdf

1525-delnp-2005-form-1.pdf

1525-delnp-2005-form-18.pdf

1525-DELNP-2005-Form-2 (30-10-2007).pdf

1525-DELNP-2005-Form-2-08-04-2008.pdf

1525-DELNP-2005-Form-2-09-05-2008.pdf

1525-delnp-2005-form-2.pdf

1525-DELNP-2005-Form-3 (30-10-2007).pdf

1525-delnp-2005-form-3.pdf

1525-DELNP-2005-Form-5 (30-10-2007).pdf

1525-DELNP-2005-Form-5-08-04-2008.pdf

1525-delnp-2005-form-5.pdf

1525-DELNP-2005-GPA (30-10-2007).pdf

1525-delnp-2005-gpa.pdf

1525-DELNP-2005-Other-Document (30-10-2007).pdf

1525-delnp-2005-pct-210.pdf

1525-delnp-2005-pct-220.pdf

1525-delnp-2005-pct-304.pdf

1525-DELNP-2005-Petition -137 (30-10-2007).pdf

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Patent Number

219642

Indian Patent Application Number

1525/DELNP/2005

PG Journal Number

28/2008

Publication Date

11-Jul-2008

Grant Date

12-May-2008

Date of Filing

15-Apr-2005

Name of Patentee

CATALYTIC DISTILLATION TECHNOLOGIES

Applicant Address

Inventors:

#	Inventor's Name	Inventor's Address
1	FRANK A. SEIBERT
2	LAWRENCE A. SMITH , JR
3	JAMES R, FAIR
4	GARY R, GILDERT

PCT International Classification Number

B01D

PCT International Application Number

PCT/US2003/029108

PCT International Filing date

2003-09-16

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1	10/300, 505	2002-11-20	U.S.A.