U.S. patent application number 15/524637 was filed with the patent office on 2017-12-07 for method.
The applicant listed for this patent is DUPONT NUTRITION BIOSCIENCES APS. Invention is credited to Jyrki Airaksinen, Kari Laiho.
Application Number | 20170348613 15/524637 |
Document ID | / |
Family ID | 52118155 |
Filed Date | 2017-12-07 |
United States Patent
Application |
20170348613 |
Kind Code |
A1 |
Airaksinen; Jyrki ; et
al. |
December 7, 2017 |
METHOD
Abstract
The present invention relates to a method for fractionating a
feedstock into two or more fractions enriched with different
components, and more particularly to a method for fractionating a
feedstock into two or more fractions by a chromatographic
sequential simulated moving bed (SMB) system, wherein the SMB
system comprises a separation loop comprising at least 2
compartments; and wherein the method comprises a separation cycle
comprising at least one feeding step, at least one circulating step
and at least one eluting step; wherein the dissolved substances in
the feedstock form a separation profile as they progress through
the separation loop; and the separation profile is progressed more
than once or less than once through the separation loop in each
separation cycle; and wherein at least two flow paths are present
in the separation loop during each feeding step of the separation
cycle; and at least one of said flow paths is an active flow path
and at least one of said flow paths is an inactive flow path.
Inventors: |
Airaksinen; Jyrki; (Kantvik,
FI) ; Laiho; Kari; (Kantvik, FI) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
DUPONT NUTRITION BIOSCIENCES APS |
Copenhagen K |
|
DK |
|
|
Family ID: |
52118155 |
Appl. No.: |
15/524637 |
Filed: |
November 6, 2015 |
PCT Filed: |
November 6, 2015 |
PCT NO: |
PCT/US15/59517 |
371 Date: |
May 5, 2017 |
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
C13B 20/148 20130101;
B01D 2215/024 20130101; C13K 13/007 20130101; B01D 15/362 20130101;
C13B 35/06 20130101; B01D 15/185 20130101; B01D 15/1828
20130101 |
International
Class: |
B01D 15/18 20060101
B01D015/18; B01D 15/36 20060101 B01D015/36 |
Foreign Application Data
Date |
Code |
Application Number |
Nov 7, 2014 |
GB |
1419852.7 |
Claims
1. A method for fractionating a feedstock into two or more
fractions by a chromatographic sequential simulated moving bed
(SMB) system, wherein the SMB system comprises a separation loop
comprising at least 2 compartments; and wherein the method
comprises a separation cycle comprising at least one feeding step,
at least one circulating step and at least one eluting step; and
wherein the dissolved substances in the feedstock form a separation
profile as they progress through the separation loop; and the
separation profile is progressed more than once or less than once
through the separation loop in each separation cycle; and wherein
at least two flow paths are present in the separation loop during
each feeding step of the separation cycle; and at least one of said
flow paths is an active flow path and at least one of said flow
paths is an inactive flow path.
2. (canceled)
3. The method according to claim 1 wherein, during at least one
feeding step, a feedstock is fed into one of the compartments in an
active flow path and at least one product fraction is collected
from a subsequent compartment in the same flow path.
4. The method according to claims 1 or 3 wherein, during at least
one feeding step, a feedstock is fed into one of the compartments
in an active flow path and substantially simultaneously an eluent
is fed into a subsequent compartment in the separation loop.
5. The method according to claim 4 wherein a product and/or recycle
fraction is withdrawn from each of the compartments which receive
the feedstock or eluent.
6. The method according to claims 1 or 3, wherein the separation
loop comprises 2n compartments and in at least one feeding step of
separation cycle n+1 flow paths are present and wherein at least
one of the n+1 flow paths is an inactive flow path and at least one
of the n+1 flow paths is an active flow path; wherein n is a number
between 1 and 20.
7. (canceled)
8. The method according to claims 1 or 3 wherein the separation
loop comprises 2n or 2n-1 compartments and in at least one feeding
step of the separation cycle n flow paths are present and wherein
at least one of the n flow paths is an inactive flow path and at
least one of the n flow paths is an active flow path; wherein n is
a number between 2 and 20.
9. (canceled)
10. (canceled)
11. (canceled)
12. The method according to claims 1 or 3 wherein the ratio of
active to inactive flow paths in each feeding step is between about
3:1 and 1:3.
13. (canceled)
14. The method according to claims 1 or 3 wherein in each feeding
step of the separation cycle the last flow path in the separation
loop relative to the flow path which receives the feed is an
inactive flow path.
15. The method according to claims 1 or 3 wherein in each feeding
step the number of compartments constituting the active flow paths
is equal to the number of compartments which constitute the
inactive flow paths.
16. The method according to claims 1 or 3 wherein the separation
loop comprises four compartments and the method comprises a
separation cycle comprising a feeding step, wherein a flow path
between two consecutive compartments and a flow path between
another two consecutive compartments are present, wherein one flow
path is active and the other flow path is inactive.
17. The method according to claims 1 or 3 wherein the separation
loop comprises four compartments and the method comprises a
separation cycle comprising a feeding step, wherein two active flow
paths consisting of one compartment each and an inactive flow path
between the remaining two consecutive compartments are present.
18. The method according to claims 1 or 3 wherein the separation
loop comprises four compartments and the method comprises a
separation cycle wherein in each feeding step there are two
compartments participating in active flow paths and two
compartments participating in inactive flow paths.
19. The method according to any one of the preceding claims 1 or 3,
wherein one or more of the feeding, eluting and circulating steps
are carried out substantially simultaneously.
20. The method according to any one of the preceding claims 1 or 3,
wherein the separation profile is progressed more than once through
the separation loop in each separation cycle.
21. The according to any one of the preceding claims 1 or 3,
wherein the separation profile is progressed less than once through
the separation loop in each separation cycle.
22. (canceled)
23. A The method according to any one of the preceding claims 1 or
3, wherein the compartments comprise a stationary phase selected
from a chromatographic resin, preferably an ion-exchange resin.
24. (canceled)
25. (canceled)
26. (canceled)
27. (canceled)
28. The method according to any one of claims 1 or 3, wherein the
SMB system has a linear flow rate of 0.4 to 20 m/h, preferably from
1 to 12 m/h.
29. The method to any one of claims 1 or 3, wherein the solution to
be fractionated is selected from the group consisting of beet
molasses, low green, vinasse, fructose/glucose syrups, beet-derived
juices, invert sugar mixtures, starch hydrolysates, wood
hydrolysates, milk whey solutions and other lactose containing
solutions, lactulose-containing solutions, maltose-containing
solutions, maltitol-containing solutions, solutions containing
amino acids, fermentation broths containing various organic acids,
and solutions containing rhamnose, arabinose, mannose, raffinose,
inositol, mannitol, sorbitol, xylitol, erythritol, glutamic acid,
glycerol, and/or tagatose, or isomaltulose and trehalulose
solutions.
30. (canceled)
31. The method to any one of claim 3, wherein the product(s) is/are
selected from a group consisting of glucose, fructose, sucrose,
betaine, rhamnose, lactose, lactulose, maltose, maltitol,
arabinose, mannose, raffinose, inositol, mannitol, glycerol,
xylitol, xylose, sorbitol, erythritol, organic acids, especially
amino acids, such as glutamic acid.
32. The method to claim 3 wherein the feedstock is beet molasses
and a product fraction comprises mainly betaine.
33. The method according to claim 3 or 32 wherein a product
fraction comprises at least about 3 g/100 ml of betaine.
34. The method according to claim 3 wherein the feedstock is beet
molasses and a product fraction comprises mainly sucrose.
35. The method according to claim 3 or 34 wherein a product
fraction comprises at least about 30 g/100 ml of sucrose.
36. A chromatographic fraction comprising at least about 75 wt. %
betaine of dry substance and having a betaine concentration of at
least about 3.5 g/100 ml obtainable by the method according to any
of claims 1 or 3.
37. (canceled)
38. A chromatographic fraction comprising at least about 75 wt. %
betaine of dry substance and having a betaine concentration of at
least about 3.5 g/100 ml obtainable by the method according to
claim 23.
Description
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims priority to Great Britain
Application No. 1419852.7, filed Nov. 7, 2014, which is hereby
incorporated by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to a method for fractionating
a feedstock into two or more fractions enriched with different
components, and more particularly to a method for fractionating a
feedstock into two or more fractions by a chromatographic
sequential simulated moving bed (SMB) system, wherein the SMB
system comprises a separation loop comprising at least 2
compartments; and wherein the method comprises a separation cycle
comprising at least one feeding step, at least one circulating step
and at least one eluting step; wherein the dissolved substances in
the feedstock form a separation profile as they progress through
the separation loop; and the separation profile is progressed more
than once or less than once through the separation loop in each
separation cycle; and wherein at least two flow paths are present
in the separation loop during each feeding step of the separation
cycle; and at least one of said flow paths is an active flow path
and at least one of said flow paths is an inactive flow path.
BACKGROUND OF THE INVENTION
[0003] Continuous simulated moving bed chromatograph has been
disclosed in U.S. Pat. No. 2,985,589 (Broughton et al.). In this
process the mixture to be fractionated is introduced into one
chromatographic resin bed and eluent is introduced into another
chromatographic resin bed, and two product fractions are withdrawn
substantially simultaneously. There are at least four
chromatographic resin beds, forming a single chromatographic
separation loop with continuous circulation of a separation
profile, and the feed and product withdrawal points are shifted
continuously and stepwise in the downstream direction, essentially
at the speed of the circulation of the separation profile in the
chromatographic separation loop.
[0004] For simulated moving bed chromatographic separation
processes two or more loop and two or more profile modes have been
developed in order to better utilise the chromatographic separation
resin bed to achieve increased separation capacity, increased
yields and fraction purities and fraction dry substance
concentrations.
[0005] A sequential simulated moving bed process applied to the
recovery of betaine and sucrose from beet molasses is described in
Finnish Patent 86 416. In this method, one complete or essentially
complete separation profile is circulated in a chromatographic
separation system.
[0006] Finnish Patent 86 416 discloses a method for recovering
betaine and sucrose from beet molasses employing a simulated moving
bed process. The chromatographic system comprises at least three
chromatographic resin beds in series. Betaine and sucrose are
separated in the same separation sequence comprising a molasses
feeding phase wherein the molasses feedstock is supplied to one of
said chromatographic resin beds and eluent water is supplied
substantially simultaneously to another of said chromatographic
resin beds, an eluting phase, and a circulating phase. These phases
are repeated either once or several times during the separation
sequence.
[0007] Also, U.S. Pat. No. 6,093,326 and U.S. Pat. No. 5,637,225
relate to simulated moving bed methods. U.S. Pat. No. 6,093,326
relates to the fractionation of molasses and U.S. Pat. No.
5,637,225 to the fractionation of sulphite cooking liquor. As is
described in these publications, the simulated moving bed method
may include multiple chromatographic separation loops, and multiple
separation profiles in each loop.
[0008] In the method disclosed in U.S. Pat. No. 6,093,326, the
liquid flow is effected in a system comprising at least two
chromatographic resin beds, and the product or products are
recovered during a multistep sequence. A separation cycle comprises
feeding, eluting and circulating phases. During the circulating
phase, the liquid present in the chromatographic resin beds is
circulated in two or more separation loops comprising one, two or
more chromatographic resin beds.
[0009] WO 1997045185 discloses a method for fractionating a
solution into two or more fractions by a chromatographic simulated
moving bed process, wherein at least two separation profiles are
circulated in the same loop. The method can be used for
fractionating a sulphite cooking liquor to give a fraction rich in
monosaccharides and/or a fraction rich in lignosulphonates.
Furthermore, molasses or vinasse can be fractionated in that way to
obtain fractions rich in sugar, such as sucrose, and/or betaine.
The minimum bed length required for the method is at least the
length of two separation profiles without excess overlapping.
[0010] WO 2002089946 describes a method for fractionating a
solution into two or more fractions by a sequential moving bed
process wherein the separation profile is circulated through the
columns more than once or less than once. In the methods
exemplified therein, each feeding step employs all of the
compartments in the chromatographic separation loop.
[0011] There is a need in the art for further methods capable of
providing good separation of complex mixtures providing product
fractions of high yield and purity and good product fraction
concentration.
[0012] The present invention provides alternative/improved
separation methods which provide one or more of the following
advantageous effects: high product fraction yields, high product
fraction purities, high product fraction concentrations and high
separation capacities.
SUMMARY OF THE INVENTION
[0013] In one aspect of the present invention there is provided a
method for fractionating a feedstock into two or more fractions by
a chromatographic sequential simulated moving bed (SMB) system,
[0014] wherein the SMB system comprises a separation loop
comprising at least 2 compartments; and [0015] wherein the method
comprises a separation cycle comprising at least one feeding step,
at least one circulating step and at least one eluting step; [0016]
wherein the dissolved substances in the feedstock form a separation
profile as they progress through the separation loop; and the
separation profile is progressed more than once or less than once
through the separation loop in each separation cycle; and [0017]
wherein at least two flow paths are present in the separation loop
during each feeding step of the separation cycle; and at least one
of said flow paths is an active flow path and at least one of said
flow paths is an inactive flow path.
[0018] In other aspects of the invention there are provided
chromatographic fractions comprising betaine or sucrose as defined
herein obtainable by the method according to the above aspect of
the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] FIG. 1 depicts examples of possible flow paths in a four
compartment SMB system.
[0020] FIG. 2 depicts the steps in the separation cycle of Example
1.
[0021] FIG. 3 depicts the steps in the separation cycle of Example
2.
[0022] FIG. 4 depicts the separation profile formed in the
separation cycle of Example 1.
[0023] FIG. 5 depicts the separation profile formed in the
separation cycle of Example 2.
DETAILED DESCRIPTION OF THE INVENTION
Feedstock
[0024] As used herein, `feedstock` refers to the material which is
the subject of chromatographic purification. In one embodiment, the
feedstock may be a raw material. In another embodiment, the
feedstock may be partially purified, recycled material resulting
from chromatographic methods (recycle fraction). In another
embodiment, the feedstock may be a mixture of raw material and
recycle fraction.
[0025] In one embodiment, the feedstock is a solution comprising a
mixture of components.
[0026] In one embodiment, the feedstock may be selected from
sulphite cooking liquors, beet molasses, especially B-molasses and
C-molasses, low green, vinasse, fructose/glucose syrups,
beet-derived juices, invert sugar mixtures, starch hydrolysates,
wood hydrolysates, milk whey solutions and other lactose-containing
solutions, lactulose-containing solutions, maltose-containing
solutions, maltitol-containing solutions, solutions containing
amino acids, fermentation broths containing various organic acids,
such as citric acid, glucosic acid, bagasse hydrolysates, and
solutions containing rhamnose, arabinose, mannose, raffinose,
inositol, mannitol, sorbitol, xylitol, erythritol, glutamic acid,
glycerol and/or tagatose, and isomaltulose and trehalulose
solutions and the like.
[0027] Preferably the feedstock is selected from sulphite cooking
liquor, beet molasses and low green. More preferably, the feedstock
is beet molasses or low green.
[0028] In this context sulphite cooking liquor means a liquor
employed in the cooking of sulphite cellulose or a part thereof, a
liquor ensuing from the cooking or a part thereof, a liquor used in
the sulphite cooking or a part thereof or liquor removed from the
sulphite cooking during the cooking or a part thereof.
Fractions
[0029] Fractions withdrawn may include product fractions, i.e.
fractions sufficiently enriched in one of the products of interest,
and recycle fractions, i.e. fractions which are intended to be
re-purified.
[0030] The fractions produced by the method of the present
invention may be enriched in products selected from the group
consisting of glucose, fructose, sucrose, betaine, rhamnose,
arabinose, mannose, raffinose, lactose, lactulose, maltose,
maltitol, inositol, mannitol, glycerol, xylitol, xylose, sorbitol,
erythritol, organic acids, especially amino acids, such as glutamic
acid. When these fractions are sufficiently enriched (i.e. product
purity is 80 wt. % or more of dry substance, preferably 85 wt. % or
more of dry substance, more preferably 90 wt. % or more of dry
substance), these fractions may be referred to as product
fractions.
[0031] Alternatively, fractions produced by the method of the
invention may be recycled back to the compartments/column(s) or
combined with raw material. There may also be an operation before
returning these fractions to the separation system, for example
they may be concentrated by evaporation. These fractions may be
referred to as recycle fractions.
[0032] In the method of the present invention, there may be more
than one product of interest and therefore more than one type of
product fraction.
[0033] In one embodiment, the method of the invention provides
fractions enriched in sucrose and fractions enriched in
betaine.
[0034] In one embodiment, the method uses beet molasses as a
feedstock and the product fractions are enriched in betaine or
sucrose.
[0035] Preferably the product fraction enriched in sucrose has a
sucrose concentration of at least about 20 g/100 ml, more
preferably at least about 23 g/100 ml, more preferably at least
about 25 g/100 ml, more preferably at least about 28 g/100 ml, more
preferably at least about 30 g/100 ml, more preferably at least
about 31 g/100 ml, more preferably at least about 33 g/100 ml, more
preferably at least about 35 g/100 ml.
[0036] Preferably the product fraction enriched in sucrose has a
sucrose purity of 80 wt. % or more of dry substance, preferably 85
wt. % or more of dry substance, more preferably 90 wt. % or more of
dry substance, more preferably from 90 to 95 wt. % of dry
substance.
[0037] Preferably the product fraction enriched in betaine has a
betaine concentration of at least about 2.5 g/100 ml, more
preferably at least about 2.8 g/100 ml, more preferably at least
about 3 g/100 ml, more preferably at least about 3.2 g/100 ml, more
preferably at least about 3.4 g/100 ml, more preferably at least
about 3.5 g/100 ml, more preferably at least about 3.6 g/100 ml,
more preferably about 3.6 g/100 ml, more preferably at least about
3.8 g/100 ml, more preferably about 3.8 g/100 ml, more preferably
at least about 4.0 g/100 ml, more preferably about 4.0 g/100
ml.
[0038] Preferably the product fraction enriched in betaine has a
betaine purity of 70 wt. % or more of dry substance, preferably 75
wt. % or more of dry substance, more preferably 80 wt. % or more of
dry substance, more preferably from 890 to 85 wt. % of dry
substance.
[0039] In another aspect, the present invention provides a
chromatographic fraction comprising at least about 75 wt. % betaine
of dry substance and having a betaine concentration of at least
about 2.5 g/100 ml, more preferably at least about 2.8 g/100 ml,
more preferably at least about 3 g/100 ml, more preferably at least
about 3.2 g/100 ml, more preferably at least about 3.4 g/100 ml,
more preferably at least about 3.5 g/100 ml, more preferably at
least about 3.6 g/100 ml, more preferably about 3.6 g/100 ml, more
preferably at least about 3.8 g/100 ml, more preferably about 3.8
g/100 ml, more preferably at least about 4.0 g/100 ml, more
preferably about 4.0 g/100 ml, obtainable by the method of the
invention.
[0040] In another aspect, the present invention provides a
chromatographic fraction comprising at least about 80 wt. % betaine
of dry substance and having a betaine concentration of at least
about 2.5 g/100 ml, more preferably at least about 2.8 g/100 ml,
more preferably at least about 3 g/100 ml, more preferably at least
about 3.2 g/100 ml, more preferably at least about 3.4 g/100 ml,
more preferably at least about 3.5 g/100 ml, more preferably at
least about 3.6 g/100 ml, more preferably about 3.6 g/100 ml, more
preferably at least about 3.8 g/100 ml, more preferably about 3.8
g/100 ml, more preferably at least about 4.0 g/100 ml, more
preferably about 4.0 g/100 ml, obtainable by the method of the
invention.
[0041] In another aspect, the present invention provides a
chromatographic fraction comprising at about 80 to about 85 wt. %
betaine of dry substance and having a betaine concentration of at
least about 2.5 g/100 ml, more preferably at least about 2.8 g/100
ml, more preferably at least about 3 g/100 ml, more preferably at
least about 3.2 g/100 ml, more preferably at least about 3.4 g/100
ml, more preferably at least about 3.5 g/100 ml, more preferably at
least about 3.6 g/100 ml, more preferably about 3.6 g/100 ml, more
preferably at least about 3.8 g/100 ml, more preferably about 3.8
g/100 ml, more preferably at least about 4.0 g/100 ml, more
preferably about 4.0 g/100 ml, obtainable by the method of the
invention.
[0042] In another aspect, the present invention provides a
chromatographic fraction comprising at least about 85 wt. % sucrose
of dry substance and having a sucrose concentration of at least
about 20 g/100 ml, more preferably at least about 23 g/100 ml, more
preferably at least about 25 g/100 ml, more preferably at least
about 28 g/100 ml, more preferably at least about 30 g/100 ml, more
preferably at least about 31 g/100 ml, more preferably at least
about 33 g/100 ml, more preferably at least about 35 g/100 ml
obtainable by the method of the invention.
[0043] In another aspect, the present invention provides a
chromatographic fraction comprising at least about 90 wt. % sucrose
of dry substance and having a sucrose concentration of at least
about 20 g/100 ml, more preferably at least about 23 g/100 ml, more
preferably at least about 25 g/100 ml, more preferably at least
about 28 g/100 ml, more preferably at least about 30 g/100 ml, more
preferably at least about 31 g/100 ml, more preferably at least
about 33 g/100 ml, more preferably at least about 35 g/100 ml
obtainable by the method of the invention.
[0044] In another aspect, the present invention provides a
chromatographic fraction comprising at about 90 to about 95 wt. %
sucrose of dry substance and having a sucrose concentration of at
least about 20 g/100 ml, more preferably at least about 23 g/100
ml, more preferably at least about 25 g/100 ml, more preferably at
least about 28 g/100 ml, more preferably at least about 30 g/100
ml, more preferably at least about 31 g/100 ml, more preferably at
least about 33 g/100 ml, more preferably at least about 35 g/100 ml
obtainable by the method of the invention.
SMB System
[0045] As used herein, `SMB system` refers to the equipment which
enables fractionation of the feedstock and which operates according
to the principles of a simulated moving bed (SMB).
[0046] An SMB system typically comprises at least two compartments
connectable in series and the connecting pipelines. An SMB system
may furthermore comprise pumps, eluent containers, feed and eluent
conduits, circulation apparatus, heat exchangers, product fraction
withdrawal conduits, valves, flow and pressure regulators and
devices capable of measuring concentration, density, optical
activity and conductivity. Suitable systems would be well known to
the skilled person.
[0047] As used herein, `compartment` refers to a section of
chromatographic equipment comprising a stationary phase.
[0048] In one embodiment, a compartment may further comprise, in
addition to the stationary phase, a forepart for distributing
incoming liquid flow onto the stationary phase (distribution
device) and a rear part for collecting the outgoing liquid flow
from the stationary phase (collection device).
[0049] Suitable distribution and collection devices have been
disclosed in WO2004060526 which is herein incorporated by
reference.
[0050] One or more compartments may be arranged in a column. When a
column contains only one compartment the two terms may be used
interchangeably.
[0051] The compartments are interconnected such that they form a
separation loop. As used herein a "separation loop" refers to a
circuit of compartments which are interconnected such that the
inlet of any given compartment is connected to the outlet of the
preceding compartment and the outlet of said compartment is
connected to the inlet of the proceeding compartment.
[0052] In one embodiment, the SMB system comprises a separation
loop comprising 2 to 28 compartments, preferably 2 to 15
compartments, more preferably 2 to 12 compartments, more preferably
2 to 10 compartments, more preferably 2 to 8 compartments, more
preferably 2 to 6 compartments, more preferably 2 to 4
compartments.
[0053] In one embodiment, the SMB system comprises a separation
loop comprising at least three compartments.
[0054] In one embodiment, the SMB system comprises a separation
loop comprising 3 to 28 compartments, preferably 3 to 15
compartments, more preferably 3 to 12 compartments, more preferably
3 to 10 compartments, more preferably 3 to 8 compartments, more
preferably 3 to 6 compartments, more preferably 3 or 4
compartments.
[0055] In one embodiment, the SMB system comprises a separation
loop comprising at least four compartments.
[0056] In one embodiment, the SMB system comprises a separation
loop comprising 4 to 28 compartments, preferably 4 to 15
compartments, more preferably 4 to 12 compartments, more preferably
4 to 10 compartments, more preferably 4 to 8 compartments, more
preferably 4 to 6 compartments, more preferably 4 or 5
compartments.
[0057] In one embodiment, the SMB system comprises a separation
loop comprising at least five compartments.
[0058] In one embodiment, the SMB system comprises a separation
loop comprising 5 to 28 compartments, preferably 5 to 15
compartments, more preferably 5 to 12 compartments, more preferably
5 to 10 compartments, more preferably 5 to 8 compartments, more
preferably 5 or 6 compartments.
[0059] In one embodiment, the SMB system comprises a separation
loop comprising at least six compartments.
[0060] In one embodiment, the SMB system comprises a separation
loop comprising 6 to 28 compartments, preferably 6 to 15
compartments, more preferably 6 to 12 compartments, more preferably
6 to 10 compartments, more preferably 6 to 8 compartments.
[0061] In a preferred embodiment, the separation loop
comprises/consists of four compartments.
Flow path
[0062] As used herein, a `flow path` refers to a temporary route
via which liquid may flow. A flow path can be created within the
separation loop due to the manipulation of the valves controlling
the various inlets and outlets of each compartment in the
separation loop.
[0063] A flow path may be comprised of one compartment or more than
one compartment connected in series.
[0064] A flow path may be an active flow path or an inactive flow
path.
[0065] As used herein, an `active flow path` refers to a flow path
wherein liquid is actively flowing (e.g. being pumped) through the
compartment(s) which constitute the flow path. In an active flow
path, liquid arriving at the outlet of a compartment may be
collected as a fraction, or it may be reintroduced via pipelines to
an inlet at a subsequent compartment.
[0066] As used herein, an `inactive flow path` refers to a flow
path wherein liquid is not actively flowing (e.g. not being pumped)
through the compartments which constitute the flow path.
[0067] For example, in FIG. 1A, a four compartment separation loop
is depicted. The interconnections between the compartments are not
shown, only the flow paths. The separation loop consists of two
flow paths. The first flow path between compartments 1 and 2 is
active because feed is being pumped into compartment 1 and
simultaneously product fraction is being withdrawn from compartment
2. The second flow path between compartments 3 and 4 is inactive
because although compartment 3 and 4 are connected there is no
active flow of liquid between the compartments and nothing is fed
to or withdrawn from these compartments.
[0068] In FIG. 1B, a four compartment separation loop is depicted.
The interconnections between the compartments are not shown, only
the flow paths. The separation loop consists of three flow paths.
The first at column 1 is an active flow path as feed is actively
entering column 1 and product fraction is being withdrawn from
column 1. The second at column 2 is an active flow path as water is
actively entering column 2 and product fraction is being withdrawn
from column 2. The third flow path between compartments 3 and 4 is
inactive because although compartment 3 and 4 are connected there
is no active flow of liquid between the compartments and nothing is
fed into or withdrawn from said compartments.
[0069] In FIG. 1C, a four compartment separation loop is depicted.
The interconnections between the compartments are not shown, only
the flow paths. The separation loop consists of one flow path. The
flow path is active as liquid is actively flowing between all
compartments in the separation loop. Neither feedstock or eluent is
entering any of the compartments nor are any fractions being
withdrawn from the compartments, however liquid in the system is
flowing in a cyclical manner.
Stationary Phase
[0070] The stationary phase may be a chromatographic resin. In one
embodiment, the stationary phase is an ion exchange resin. The ion
exchange resin may be a cation exchange resin or an anion exchange
resin, The resin is selected depending on the raw material mixture
to be fractionated and/or the products to be recovered. Suitable
resins and their properties are well known to those skilled in the
art.
[0071] In one embodiment, the resin is polymer based. Preferably
the polymer is comprised of styrene or acrylic monomers. Acrylic
monomers may be selected from methyl acrylate, ethyl acrylate,
butyl acrylate, methyl methacrylate, acrylonitrile and acrylic
acids.
[0072] The styrene and acrylic skeleton may be crosslinked with a
crosslinking agent, e.g. divinyl benzene (DVB). A suitable degree
of crosslinking is from about 1% to about 20%, preferably from
about 3% to about 15%, more preferably about 3% to about 8%.
[0073] The cation exchange resin may be a strongly acidic cation
exchange resin or a weakly acidic cation exchange resin. The cation
exchange resin may be in a monovalent and/or divalent metal form,
such as Na.sup.+ and/or K.sup.+ form, or Ca.sup.2+, Ba.sup.2+,
Mg.sup.2+ and/or Sr.sup.2+ form. Resins in H.sup.+ and
NH.sub.4.sup.+ form may also be useful. However, other ionic forms
may be used.
[0074] The anion exchange resin may be a strong base or a weak base
anion exchange resin, having preferably an acrylic skeleton. The
anion exchange resins may be in OH.sup.-, Cl.sup.- or
SO.sub.4.sup.2- form, However, other ionic forms may also be
used.
[0075] One preferred stationary phase is a strongly acidic cation
exchange resin in a monovalent metal form, which is predominantly
in Na.sup.+ and/or K.sup.+ form. Another preferred stationary phase
is a weakly acidic cation exchange resin in a monovalent metal
form, which is predominantly in Na.sup.+ and/or K.sup.+ form.
[0076] The resins may also be gel-type resins, Manufacturers of
suitable resins are Finex, Dow, Bayer and Rohm & Haas for
example.
[0077] Carbonaceous pyropolymers and activated carbon bound to a
polymer are also useful as stationary phases.
[0078] In one embodiment, the stationary phase has a mean bead size
of about 50 .mu.m to about 500 .mu.m. Preferably, the mean bead
size is about 50 .mu.m to about 400 .mu.m. Preferably, the mean
bead size is about 50 .mu.m to about 300 .mu.m. Preferably, the
mean bead size is about 50 .mu.m to about 250 .mu.m. More
preferably, the mean bead size is about 50 .mu.m to about 200
.mu.m.
[0079] In one embodiment, the stationary phase has a mean bead size
of about 100 .mu.m to about 500 .mu.m. Preferably, the mean bead
size is about 100 .mu.m to about 400 .mu.m. Preferably, the mean
bead size is about 100 .mu.m to about 300 .mu.m. Preferably, the
mean bead size is about 100 .mu.m to about 250 .mu.m. More
preferably, the mean bead size is about 100 .mu.m to about 200
.mu.m.
[0080] In one embodiment, the stationary phase has a mean bead size
of about 200 .mu.m to about 500 .mu.m. Preferably, the mean bead
size is about 200 .mu.m to about 400 .mu.m. Preferably, the mean
bead size is about 200 .mu.m to about 350 .mu.m. More preferably,
the mean bead size is about 200 .mu.m to about 300 .mu.m.
[0081] In one embodiment, the stationary phase has a mean bead size
of about 250 .mu.m to about 500 .mu.m. Preferably, the mean bead
size is about 250 .mu.m to about 400 .mu.m. Preferably, the mean
bead size is about 250 .mu.m to about 350 .mu.m.
[0082] In one embodiment, the height of the stationary phase within
the compartment is preferably about 0.2 to 6 metres. More
preferably the height of the stationary phase within the
compartment is about 0.2 to 5 metres. More preferably the height of
the stationary phase within the compartment is about 0.2 to 4
metres. More preferably the height of the stationary phase within
the compartment is about 0.2 to 3 metres. More preferably the
height of the stationary phase within the compartment is about 0.5
to 2.5 metres. More preferably the height of the stationary phase
within the compartment is about 0.5 to 2.0 metres.
[0083] In one embodiment, the height of the stationary phase within
the compartment is preferably about 0.8 to 2.5 metres. More
preferably the height of the stationary phase within the
compartment is about 1.0 to 2.5 metres. More preferably the height
of the stationary phase within the compartment is about 1.0 to 2.0
metres.
[0084] In one embodiment, the height of the stationary phase within
the compartment is preferably about 1 to 5 metres. More preferably
the height of the stationary phase within the compartment is about
1 to 4 metres. More preferably the height of the stationary phase
within the compartment is about 1 to 3 metres.
[0085] In one embodiment, the height of the stationary phase within
the compartment is preferably about 2 to 5 metres. More preferably
the height of the stationary phase within the compartment is about
2 to 4 metres. More preferably the height of the stationary phase
within the compartment is about 2 to 3 metres.
[0086] The compartments may be partially or fully packed with
stationary phase. Preferably the compartments are fully packed with
stationary phase. As used herein, the term "fully packed" means
that substantially all of the volume of the compartment is packed
with stationary phase apart from the space occupied by the
distribution and collection devices.
Separation Cycle
[0087] As used herein, `separation cycle` refers to a sequence of
steps which may be repeated. A cycle is a predetermined sequence of
steps in a pre-determined order which includes at least one feeding
step, circulating step and eluting step.
[0088] In one embodiment, a separation cycle comprises/consists of
about 1 to about 50 steps.
[0089] In another embodiment, a separation cycle consists of about
2 to about 50 steps. In another embodiment, a separation cycle
consists of about 10 to about 50 steps. In another embodiment, a
separation cycle consists of about 10 to about 40 steps.
[0090] In another embodiment, a separation cycle consists of about
15 to about 40 steps. In another embodiment, a separation cycle
consists of about 15 to about 30 steps. In another embodiment, a
separation cycle consists of about 10 to about 30 steps.
[0091] In another embodiment, a separation cycle consists of about
6 to about 30 steps. In another embodiment, a separation cycle
consists of about 6 to about 25 steps. In another embodiment, a
separation cycle consists of about 6 to about 20 steps.
[0092] In one embodiment of the method of the invention, the
separation cycle is performed between 1 and 5 times, preferably 1,
2 or 3 times, more preferably once.
[0093] As used herein, a `feeding step` refers to a step in the
separation cycle wherein a feedstock is introduced into the
separation loop, and at least one fraction is withdrawn from the
separation loop.
[0094] As used herein, a `circulating step` refers to a step in the
separation cycle wherein essentially no feedstock or eluent is
supplied to the separation loop and essentially no fractions are
withdrawn from the separation loop.
[0095] As used herein, an `eluting step` refers to a step wherein
an eluent is fed into the SMB system, and at least one fraction is
withdrawn from the separation loop.
[0096] A step in the separation cycle may comprise/consist of one
or more of the above feeding, circulating and/or eluting steps,
i.e. these steps may be carried out simultaneously. Furthermore,
said steps may be repeated one or more times during the cycle.
[0097] In each step of the separation cycle, a flow path or flow
paths is/are created in the separation loop due to the arrangement
of valves which control inflow and outflow of liquid from the
compartments in the separation loop.
[0098] The skilled person would understand that typically the
separation cycle is repeated until an equilibrated separation
profile is reached and then the process is continued advantageously
in equilibrium. The equilibrium is defined by the equilibrium of
the separation profile. Equilibrium of the separation profile is
typically reached after about 6 to 12 cycles, more typically about
6 to 10 cycles, more typically about 6 to 8 cycles. Equilibrium of
the separation profile may be reached after about 7 cycles.
[0099] As used herein, `separation profile` refers to the
relationship between the constituents of the feedstock as they
progress through the SMB system, preferably at equilibrium. The
separation profile may be observed by measuring the conductivity
and/or density over time as liquid flows through the equilibrated
system during a separation cycle. The separation profile comprises
constituents having a low migration rate, constituents having an
intermediate migration rate, and constituents having a high
migration rate. Accordingly the separation profile is a complete or
an essentially complete dry solids profile of the feedstock.
Method
[0100] In chromatographic simulated moving bed (SMB) processes, the
components present in a feedstock are separated in a series of
interconnected compartments comprising a stationary phase.
[0101] In sequential simulated moving bed processes, all of the
fluid streams do not flow continuously. The streams are: the supply
of feedstock and/or eluent, the circulation of the separation
profile, and the withdrawal of fractions. The flow rate and the
volumes of the different feeds and product fractions may be
adjusted in accordance with the separation goals (yield, purity,
capacity). The process commonly comprises three basic types of
step: feeding, eluting and circulating.
[0102] In the method of the present invention a separation profile
may be circulated more then once or less than once through the
chromatographic separation loop before all predetermined fractions
are taken out or before the next feed or feeds and eluent or eluent
feeds of the next cycle are fed in.
[0103] Conventionally, and especially in a sequential simulated
moving bed (SMB) chromatographic, a product or a recycle fraction
are withdrawn from either the first compartment and/or the last
compartment in the separation loop relative to compartment which
received the feedstock in order to fully utilise the stationary
phase.
[0104] In contrast, the present invention provides a method for
fractionating a feedstock into two or more fractions by a
chromatographic sequential simulated moving bed (SMB) system,
[0105] wherein the SMB system comprises a separation loop
comprising at least 2 compartments; and [0106] wherein the method
comprises a separation cycle comprising at least one feeding step,
at least one circulating step and at least one eluting step; and
[0107] wherein at least two flow paths are present in the
separation loop during each feeding step of the separation cycle;
and at least one of said flow paths is an active flow path and at
least one of said flow paths is an inactive flow path.
[0108] It has now surprisingly been found that by holding a part of
the separation profile in the compartments which form the inactive
flow paths, before reintroducing it into the separation profile at
a subsequent step in the separation cycle, one or more of the
following advantageous effects: high product fraction yields, high
product fraction purities, high product fraction concentrations and
high separation capacities.
[0109] In the method of the invention the product or products
is/are recovered using a multi-step separation cycle comprising the
following steps: feeding step, eluting step and circulating
step.
[0110] The method of the invention is characterised in that in each
feeding step at least two flow paths are present and at least one
of the flow paths is an inactive flow path.
[0111] In the present invention a separation cycle is formed of
predetermined steps, which are carried out in a predetermined order
one or more times during the separation method.
[0112] The separation cycle comprises a) at least one feeding step,
b) at least one circulating step and c) at least one eluting step.
Each of these steps a) to c) can be carried out simultaneously.
Steps a) and c) are used as many times as necessary until the
separation profile has circulated through the chromatographic
separation loop more than once or less than once during one
cycle.
[0113] In one embodiment the separation cycle comprises 1 to 10
feeding steps, preferably 1 to 6 feeding steps, more preferably 1
to 5 feeding steps, more preferably 1, 2, 3 or 4 feeding steps.
[0114] In one embodiment, at least the first step in the separation
cycle is a feed step. In another embodiment at least the first two
steps in the separation cycle are feed steps. In another embodiment
at least the first three steps in the separation cycle are feed
steps.
[0115] In one embodiment the first 1, 2, 3, 4 or 5 steps in the
separation cycle are feed steps.
[0116] In one embodiment, during at least one feeding step, the
feedstock is fed into one of the compartments in an active flow
path and at least one product fraction or recycle fraction is
collected from the same and/or a subsequent compartment in the same
flow path.
[0117] In one embodiment, during each feeding step, the feedstock
is fed into one of the compartments in an active flow path and at
least one product fraction or recycle fraction is collected from
the same and/or a subsequent compartment in the same flow path.
[0118] In another embodiment, during at least one feeding step, the
feedstock is fed into one of the compartments in an active flow
path and at least one product fraction is collected from a
subsequent compartment in the same flow path.
[0119] In another embodiment, during each feeding step, the
feedstock is fed into one of the compartments in an active flow
path and at least one product fraction is collected from a
subsequent compartment in the same flow path.
[0120] In another embodiment, during at least one feeding step the
feedstock is fed into one of the compartments in an active flow
path and substantially simultaneously an eluent is fed into a
subsequent compartment in the separation loop. Preferably in this
embodiment, a product and/or recycle fraction is withdrawn from
both of the compartments which receive the feedstock or eluent.
[0121] In another embodiment, the separation loop comprises 2n
compartments and in at least one feeding step of the separation
cycle n+1 flow paths are present and wherein at least one of the
n+1 flow paths is an inactive flow path, and at least one of the
n+1 flow paths is an active flow path; wherein n is a number
between 1 and 20.
[0122] In another embodiment, the separation loop comprises 2n
compartments and in each feeding step of the separation cycle n+1
flow paths are present and wherein at least one of the n+1 flow
paths is an inactive flow path, and at least one of the n+1 flow
paths is an active flow path; wherein n is a number between 1 and
20.
[0123] Preferably n is 1 to 14, more preferably n is 1 to 10, more
preferably n is 1 to 8, more preferably 1 to 6, more preferably 1,
2, 3 or 4, more preferably 1, 2 or 3.
[0124] In one embodiment, the separation loop comprises 2n
compartments and in at least one feeding step of the separation
cycle n flow paths are present and wherein at least one of the n
flow paths is an inactive flow path, and at least one of the n flow
paths is an active flow path; wherein n is a number between 2 and
20.
[0125] In another embodiment, the separation loop comprises 2n-1
compartments and in at least one feeding step of the separation
cycle n flow paths are present and wherein at least one of the n
flow paths is an inactive flow path, and at least one of the n flow
paths is an active flow path; wherein n is a number between 2 and
20.
[0126] In one embodiment, the separation loop comprises 2n
compartments and in each feeding step of the separation cycle n
flow paths are present and wherein at least one of the n flow paths
is an inactive flow path, and at least one of the n flow paths is
an active flow path; wherein n is a number between 2 and 20.
[0127] In another embodiment, the separation loop comprises 2n-1
compartments and in each feeding step of the separation cycle n
flow paths are present and wherein at least one of the n flow paths
is an inactive flow path, and at least one of the n flow paths is
an active flow path; wherein n is a number between 2 and 20.
[0128] Preferably n is 2 to 14, more preferably n is 2 to 10, more
preferably n is 2 to 8, more preferably 2 to 6, more preferably 2,
3 or 4, more preferably 2 or 3.
[0129] In one embodiment, at least one feeding step comprises only
one or two inactive flow paths. In one embodiment, at least one
feeding step comprises only one inactive flow path.
[0130] In one embodiment, each feeding step of the separation cycle
comprises only one or two inactive flow paths. In one embodiment,
each feeding step of the separation cycle comprises only one
inactive flow path.
[0131] In one embodiment, in at least one feeding step of the
separation cycle, the ratio of active to inactive flow paths is
between about 3:1 and 1:3. In another embodiment the ratio of
active to inactive flow paths is between about 2:1 and 1:2. In
another embodiment, the ratio of active to inactive flow paths is
about 2:1. In another embodiment, the ratio of active to inactive
flow paths is about 1:1.
[0132] In one embodiment, in each feeding step of the separation
cycle, the ratio of active to inactive flow paths is between about
3:1 and 1:3. In another embodiment the ratio of active to inactive
flow paths is between about 2:1 and 1:2. In another embodiment, the
ratio of active to inactive flow paths is about 2:1. In another
embodiment, the ratio of active to inactive flow paths is about
1:1.
[0133] In one embodiment, in at least one feeding step of the
separation cycle, the last flaw path relative to the flow path
which receives the feedstock is an inactive flow path.
[0134] In one embodiment, in each feeding step of the separation
cycle, the last flow path relative to the flow path which receives
the feedstock is an inactive flow path.
[0135] In one embodiment, in at least one feeding step of the
separation cycle the number of compartments constituting the active
flow paths is equal to the number of compartments which constitute
the inactive flow paths.
[0136] In one embodiment, in each feeding step of the separation
cycle the number of compartments constituting the active flow paths
is equal to the number of compartments which constitute the
inactive flow paths.
[0137] In one embodiment, the separation loop comprises/consists of
four compartments and the method comprises a separation cycle
comprising a feeding step, wherein the compartments constitute one
active flow path and at least one inactive flow path. Preferably,
the compartments constitute one active flow path and one inactive
flow path.
[0138] In one embodiment of the present invention, the separation
loop comprises/consists of four compartments and the method
comprises a separation cycle comprising a feeding step, wherein a
flow path between two consecutive compartments and a flow path
between another two consecutive compartments are present, wherein
one flow path is active and the other flow path is inactive.
[0139] In one embodiment of the present invention, the separation
loop comprises/consists of four compartments and the method
comprises a separation cycle comprising at least two feeding steps,
wherein a flow path between two consecutive compartments and a flow
path between another two consecutive compartments are present
wherein one flow path is active and the other flow path is
inactive.
[0140] In one embodiment of the present invention, the separation
loop comprises/consists of four compartments and the method
comprises a separation cycle comprising a feeding step, wherein two
active flow paths consisting of one compartment each and an
inactive flow path between the remaining two consecutive
compartments are present. Preferably a feedstock is supplied to one
of the active flow paths and an eluent is supplied to the
subsequent active flow path.
[0141] In one embodiment of the present invention, the separation
loop comprises/consists of four compartments and the method
comprises a separation cycle wherein in at least one feeding step
there are two compartments participating in active flow paths and
two compartments participating in inactive flow paths.
[0142] In one embodiment of the present invention, a the separation
loop comprises/consists of four compartments and the method
comprises a separation cycle wherein in at least two feeding steps
there are two compartments participating in active flow paths and
two compartments participating in inactive flow paths.
[0143] In one embodiment of the present invention, the separation
loop comprises/consists of four compartments and the method
comprises a separation cycle wherein in each feeding step there are
two compartments participating in active flow paths and two
compartments participating in inactive flow paths.
[0144] In one embodiment of the present invention, the separation
loop comprises/consists of four compartments wherein the separation
cycle comprises: [0145] a) A feeding step wherein two compartments
together form an active flow path, and preferably feedstock is fed
to one compartment and product fraction withdrawn from the
subsequent compartment in the active flow path, the remaining
compartments forming inactive flowpath(s); and/or [0146] b) A
feeding step comprising two active flow paths consisting of one
compartment each and one inactive flow path, preferably wherein
feedstock is fed to one compartment and recycle fraction is
withdrawn from the same compartment and eluent is fed to the
compartment of the subsequent active flow path and product fraction
is withdrawn from the same compartment; and/or [0147] c) A feeding
step wherein the two compartments together form an active flow
path, and preferably feedstock is fed to one compartment and
product fraction withdrawn from the subsequent compartment, the
remaining compartments forming inactive flowpath(s).
[0148] In each of the above embodiments, the separation cycle may
further comprise a circulating step, wherein essentially nothing is
fed into or collected from the SMB system; an eluting step, wherein
the eluent is fed into one of the compartments and at least one
fraction is collected from the same or from the subsequent
compartments; wherein the method comprises at least one feeding,
circulating and eluting step per cycle.
[0149] In one embodiment, the one or more of the feeding, eluting
and circulating steps may be carried out substantially
simultaneously. In another embodiment, the feeding and eluting
steps may be carried out substantially simultaneously.
[0150] In one embodiment, the separation profile is progressed more
than once through the separation loop in each separation cycle.
[0151] In one embodiment, the separation profile is progressed
about twice through the separation loop in each separation
cycle.
[0152] In another embodiment, the separation profile is progressed
less than once through the separation loop in each separation
cycle.
[0153] In one embodiment, progression of the separation profile can
be determined by measuring the total volume of liquid (feedstock
and eluent) supplied during the separation cycle.
[0154] In one embodiment of the present invention, the separation
profile is narrow and the chromatographic separation resin bed
(stationary phase) required for good separation result is long. In
this embodiment the separation profile is circulated through the
chromatographic separation loop more than once, then the resin bed
is well utilized. Well utilized means in this context that the
separation profile essentially fills all packing material. The
separation profile can be circulated for example 1.5 times, 1.7
times, twice, or 3 times etc. depending on the number of the
columns. If the dry substance profile is circulated 1.5 times, it
means that in a 6-column system the first step of the cycle is
repeated during the next cycle three columns later. Advantageously
the separation profile is circulated twice.
[0155] In another embodiment of the present invention the
separation profile is long, i. e. broad and the bed length needed
for the good separation is short then the separation profile is
circulated less than once through the chromatographic separation
loop before the first step of the next cycle. The separation
profile can also be circulated, for example 0.7 times, through the
chromatographic separation loop. This means that for example in a
10-column system the first step of the next cycle is repeated
already after 7 columns.
[0156] The method of the invention is preferably carried out at a
temperature between 10.degree. C. and 90.degree. C. More preferably
a temperature of about 40.degree. C. and 95.degree. C. More
preferably a temperature of about 60.degree. C. and 95.degree. C.
More preferably a temperature of about 65.degree. C. and 95.degree.
C. More preferably a temperature of about 65.degree. C. and
90.degree. C. In another embodiment, the method of the invention is
preferably carried out at a temperature between 20.degree. C. and
90'C. More preferably a temperature of about 20'C and 60.degree. C.
More preferably a temperature of about 20.degree. C. and 40.degree.
C.
[0157] The method of the invention is preferably performed using a
system pressure of about 1 bar to about 15 bar. More preferably
about 1 bar to about 10 bar.
[0158] In one embodiment, the eluent employed is a solvent, such as
alcohol, especially ethanol or water or a mixture thereof,
especially a mixture of ethanol and water. Preferably the eluent
used is water.
[0159] The method of the invention is preferably performed at a
linear flow rate of about 0.4 to about 20 m/h, preferably the
linear flow rate is from 1 to 12 m/h.
EXAMPLES
Reference Example 1
Chromatographic Separation of Molasses (NSRL)
[0160] The separation loop of the SMB system comprised four
compartments connected in series, feed pump, circulation pumps, an
eluent water pump as well as inlet and outlet valves for the
various process streams. Each compartment contained a single resin
bed of height 2.2 m and diameter 0.111 m. The resin used was strong
acid cation (SAC), DVB 6.2%, mean particle size 283 .mu.m.
[0161] The feed material was C-molasses diluted to B.times.50 with
Recycle fraction. The composition of the feedstock is provided in
the table below.
TABLE-US-00001 HPLC %/DS Sucrose 58.89 Betaine 4.91 Glu + Fru 1.00
Raffinose 1.66 Others 33.54
[0162] The fractionation was performed by way of a 19 step
separation cycle (FIG. 2) as set forth below. The separation cycle
was run 10 times before withdrawing any fractions.
[0163] Step 1: 2.9 l of feedstock was fed to column 1 at flowrate
70 l/h and2.9 l of recycle fraction was collected from Column
4.
[0164] Step 2: 1.8 l of feedstock was fed to column 1 at flowrate
21 l/h and 1.8 l of Raffinate was collected from column 1.
Simultaneously 1.5 l of water was fed to column 2 at flowrate 90
l/h and 1.5 l recycle was collected from column 4.
[0165] Step 3: 1.8 l of feedstock was fed to column 1 at flowrate
21 l/h and 1.8 l of Raffinate was collected from column 1,
Simultaneously 7.7 l of water was fed to column 2 at flowrate of 90
l/h and 7.7 l sucrose was collected from column 4.
[0166] Step 4: 2.9 l of feedstock was fed to column 1 at flowrate
70 l/h and 2.9 l of sucrose fraction was collected from Column
4.
[0167] Step 5: 2.5 l was circulated in a loop at flowrate 70 L/h,
formed by columns 1, 2, 3 and 4.
[0168] Step 6: 5.0 l of water was fed to co rate 70 l/h and 5.0 l
of raffinate was collected from column 2.
[0169] Step 7: 5.2 l of water was fed to column 1 at flowrate 70
l/h and 5.2 l of betaine was collected from column 4.
[0170] Step 8: 4.6 l of water was fed to column 1 at flowrate 65
l/h and 4.6 l raffinate was collected from column 3. Simultaneously
6.7 l water was fed to column 4 at flowrate 90 l/h and 6.7 l of
betaine was collected from column 4
[0171] Step 9: 5.0 l was circulated in a loop at flowrate 70 l/h,
formed by columns 1, 2, 3 and 4.
[0172] Step 10: 4.6 l of water was fed to column 1 at flowrate 70
l/h and 4.6 l raffinate was collected from column 4.
[0173] Step 11: 5.1 l was circulated in a loop at flowrate 70 l/h,
formed by columns 1, 2, 3 and 4.
[0174] Step 12: 4.5 l of water was fed to column 2 at flowrate 70
l/h and 4.5 l raffinate was collected from column 1.
[0175] Step 13: 5.4 l was circulated in a loop at flowrate 70 l/h,
formed by columns 1, 2, 3 and 4.
[0176] Step 14: 4.5 l of water was fed to column 3 at flowrate 70
l/h, and 4.5 raffinate was collected from column 2.
[0177] Step 15: 5.4 l was circulated in a loop at flowrate 70 l/h,
formed by columns 1, 2, 3 and 4.
[0178] Step 16: 4.5 l of water was fed to column 4 at flowrate 70
l/h and 4.5 l raffinate was collected from column 3.
[0179] Step 17: 5.4 l was circulated in a loop at flowrate 48 l/h
formed by columns 1, 2, 3 and 4.
[0180] Step 18: 4.5 1 of water was fed to column 1 at flowrate 75
l/h and 4.5 l raffinate was collected from column 4.
[0181] Step 19: 2.1 l was circulated in a loop at flowrate 80 l/h
formed by columns 1, 2, 3 and 4.
[0182] The sucrose concentration, yield and purity of the fractions
is provided below as well as the mean betaine concentration, yield
and purity of the fractions.
Example 2
Chromatographic Separation of Molasses (iNSRIL)
[0183] The SMB system comprised four compartments connected in
series, feed pump, circulation pumps, an eluent water pump as well
as inlet and outlet valves for the various process streams. Each
compartment contained a single resin bed of height 2.2 m and
diameter 0.111 m. The resin used was strong acid cation (SAC), DVB
6.2%, mean particle size 283 .mu.m.
[0184] The feed material was C-molasses (as used in Example 1)
diluted to Bx50 with Recycle fraction. The composition of the
feedstock is provided in the table below.
TABLE-US-00002 HPLC %/DS Sucrose 59.25 Betaine 5.88 Glu + Fru 0.90
Raffinose 1.82 Others 32.15
[0185] The fractionation was performed by way of a 19 step
separation cycle (FIG. 3) as set forth below, The separation cycle
was run 10 times before withdrawing any fractions.
[0186] Step 1: 2.9 l of feed solution was fed to column 1 at
flowrate 60 l/h and 2.9 l of betaine fraction was collected from
column 2. Simultaneously columns 3 and 4 were inactive.
[0187] Step 2: 4.5 l of feed was fed to column 1 at flowrate 56 l/h
and 4.5 l of Raffinate was collected from column 1. Simultaneously
5.0 l of water was fed to column 2 at flowrate 68 l/h and 5.0 l
betaine was collected from column 2. Simultaneously columns 3 and 4
were inactive,
[0188] Step 3: 1.0 l of feed solution was fed to column 1 at
flowrate 60 l/h and 1.0 l of betaine fraction was collected from
column 2. Simultaneously columns 3 and 4 were inactive.
[0189] Step 4: 4.3 l was circulated in a loop at flowrate 50 l/h,
formed by columns 1, 2, 3 and 4.
[0190] Step 5: 4.5 l of water was fed to column 3 at flowrate 50
l/h and 4.5 l of raffinate was collected from column 2.
[0191] Step 6: 5.2 l was circulated in a loop at flowrate 55 l/h
formed by columns 1, 2, 3 and 4.
[0192] Step 7: 4.5 l of water was fed to column 4 at flowrate 60
l/h and 4.5 l raffinate was collected from column 3.
[0193] Step 8: 5.2 was circulated in a loop at flowrate 60 l/h
formed by columns 1, 2, 3 and 4.
[0194] Step 9: 4.3 l of water was fed to column 1 at flowrate 60
l/h and 4.3 l raffinate was collected from column 4.
[0195] Step 10: 5.0 l was circulated in a loop at flowrate 60 l/h,
formed by columns 1, 2, 3 and 4.
[0196] Step 11: 4.2 l of water was fed to column 2 at flowrate 60
l/h and 4.2 l raffinate was collected from column 1.
[0197] Step 12: 5.4 l was circulated in a loop at flowrate 60 l/h
formed by columns 1, 2, 3 and 4.
[0198] Step 13: 4.1 l of water was fed to column 3 at flowrate 60
l/h and 4.1 l raffinate was collected from column 2.
[0199] Step 14: 5.2 l was circulated in a loop at flowrate 60 l/h
formed by columns 1, 2, 3 and 4.
[0200] Step 15: 4.2 l of water was fed to column 4 at flowrate 65
l/h and 4.2 l raffinate was collected from column 3.
[0201] Step 16: 5.4 l of water was fed to column 3 at flowrate 63
l/h and 5.4 l sucrose was collected from column 2.
[0202] Step 17: 4.0 l of water was fed to column 1 at flowrate 65
l/h and 4.0 l sucrose was collected from column 2. Simultaneously
4.0 l of water was fed to column 3 at flowrate 65 l/h and 4.0 l of
raffinate was collected from column 4.
[0203] Step 18: 1.7 l of water was fed to column 1 at flowrate 65
l/h and 1.7 l recycle fraction was collected from column 2.
Simultaneously 1.1 l of water was fed to column 3 at flowrate 65
l/h and 1.1 l of raffinate was collected from column 4.
[0204] Step 19: 2.1 l of water was fed to column 3 at flowrate 60
l/h and 2.1 l of recycle fraction was collected from column 2.
[0205] The method was run twice and the mean sucrose concentration,
yield and purity of the fractions is provided below as well as the
mean betaine concentration, yield and purity of the fractions.
Results
TABLE-US-00003 [0206] Sucrose conc. Betaine conc. Sucrose conc.
Betaine conc. g/100 g g/100 g g/100 ml g/100 ml Example 1 26.6 2.9
29.56 2.92 (Reference) Example 2 28.3 3.8 31.58 3.80
TABLE-US-00004 Sucrose yield Betaine yield Sucrose purity Betaine
purity Example 1 92.2 88.2 92.7 76.7 (Reference) Example 2 93.0
93.1 92.6 79.5
[0207] The results demonstrate that the method of the invention
provides a significant increase in the concentration of sucrose
fraction and a large increase in the concentration of betaine
fraction. Both sucrose and betaine yield are improved as well as
betaine purity. Sucrose purity is maintained.
[0208] All references, including publications, patent applications,
and patents, cited herein are hereby incorporated by reference in
their entirety and to the same extent as if each reference were
individually and specifically indicated to be incorporated by
reference and were set forth in its entirety herein (to the maximum
extent permitted by law).
[0209] All headings and sub-headings are used herein for
convenience only and should not be construed as limiting the
invention in any way.
[0210] The use of any and all examples, or exemplary language
(e.g., "such as") provided herein, is intended merely to better
illuminate the invention and does not pose a limitation on the
scope of the invention unless otherwise claimed. No language in the
specification should be construed as indicating any non-claimed
element as essential to the practice of the invention.
[0211] The citation and incorporation of patent documents herein is
done for convenience only and does not reflect any view of the
validity, patentability, and/or enforceability of such patent
documents.
[0212] This invention includes all modifications and equivalents of
the subject matter recited in the claims appended hereto as
permitted by applicable law.
* * * * *