Note: Descriptions are shown in the official language in which they were submitted.
" 1321~ ~
,
IMPROVED PROCESS FOR
DEMINERALIZING A SUGAR-CONTAINING SOLUTION
This invention relates to an improved method of
removing ionic impurities from sugar-containing
solutions, especially high fructose corn syrups, by
contacting the solutions with specific ion exchange
resins.
The preparation of sugar-containing solution
requires the removal of various impurities from the
process streams. The main impurities in sugar are
measured as sulphated ash which contains cations and
anions such as Ca++, Mg+l, Na+, K+, S03--, Cl-, S04--
and the like. For the production of a refined
sugar-containing solution, it is necessary to remove
these impurities. This is achieved by a demineral-
ization process. It is standard practice in the
demineralization process to pass the sugar solution
first through a strongly acidic cation exchange resin
in the hydrogen form, followed by passage through a
strongly basic anion exchanger and/or weakly basic
anion exchanger in the hydroxide or free base form.
Once the ion exchange resins become nearly exhausted,
35,915-F -1-
- .. . .- .
-2- 132i~
it becomes necessary to regenerate their ion exchanging
capacity. Prior to contacting the ion exchange resin
with the regenerating agent, it is necessary to remove
essentially all of the sugar solution from the resin
bed. This is accomplished by passing effective
quantities of water over the resin in order to
"sweeten-off" the sugar solution within the resin bed.
The resulting effluent is known in the industry as
sweet-water.
The "sweetening-off" water or "sweet-water"
after having sweetened-off the sugar from the resin
contains an amount of recoverable sugar. The sweet-
-water is desirably recycled back as a dilution medium
to other process steps (i.e., high fructose corn syrup
saccharification). Typically, there is substantially
more sweet-water generated than can be utilized for
dilution purposes. Also, the sweet-water composition
limits the usefulness of the sweet-water as a dilution
source (e.g., high fructose sweet-water is not added
back to the dextrose solution at the saccharification
step). The excess sweet-water normally requires
concentrating during some step in the refining process.
This is accomplished by removing a substantial portion
of the water without removing any of the sugar which
has been washed off of the resin. This is generally
accomplished by evaporating off an amount of water
which results in a desired dissolved solids content,
3 i.e., sugar content, in the unevaporated sweet-water.
The evaporation of the water is an expensive
unit operation in the process for preparing refined
sugars. Therefore, it is desirable to reduce the
expense incurred during the evaporation operation of
the process without detrimentally affecting the quality
35,915-F -2-
,
...
~, . . ~ . -
: ,.
- . . . . -
.
1321~3
of sugar which is produced by the process. It is also
desirable to increase the operating capacity of the
resins for demineralizing a sugar-containing solution.
The invention is an improved process for
demineralizing a sugar-containing solution. The
improvement comprises using an ion exchange resin in
bead form wherein the volume average diameter of the
beads is from 400 to 700 ~m and which resin exhibits a
bead diameter distribution such that at least 80 volume
percent of the beads have diameters which fall within a
range of +15 percent of the volume average diameter of
the resin used.
The resin of the improved process has a smaller
volume average bead diameter and a narrower bead size
distribution relative to conventional resins used for
demineralizing sugar-containing solutions. The smaller
mean diameter of the beads shortens the average
diffusion distance traveled by exchanging components
within the beads. Therefore, the operating capacity of
the resin for demineralizing a sugar-containing
solution is increased and the volume of water required
to sweeten-off sugar from the resin is decreased.
However, beads with a mean diameter below 400 ~m will
create unacceptably high pressure drops within a resin-
containing column and would therefore limit operating
capacity. Since the resin used in this invention has a
narrow bead size distribution, the volume percent of
beads having a bead diameter less than 400 ~m is
insignificant and would not adversely affect the
operating characteristics of the resin.
35,915-F -3-
-4- 1321~ ~3
In a preferred embodiment, the present
invention relates to an improvement in the
demineralizing of high fructose corn syrup solutions.
Macroporous ion exchange resins which are
capable of removing ionic impurities from sugar-
-containing solutions may be of the anion exchange
variety or of the cation exchange variety or of the
type resin which contains both anion exchange sites and
cation exchange sites.
Macroporous ion exchange resins which are
available commercially may be employed, such as those
which have been offered commercially under the
tradenames DOWEXr~, AMBERLITErU, DUOLITEr~, and others.
The cation exchange resins are those capable of
exchanging cations. This capability is provided by
resins having functional pendant acid groups on the
polymer chain, such as carboxylic and/or sulfonic
groups. The anion exchange resins are those capable of
exchanging anions. This capability is provided by
resins having functional pendant base groups on the
polymer chain, such as ammonium or amine groups.
Resins having both types of exchange groups are also
within the purview of the present invention.
Examples of macroporous strong-acid exchange
resins include the sulfonated styrene-divinylbenzene
3 copolymers such as are offered commercially under the
tradenames DOWEXrU 88, DOWEXrU MSC-1, DUOLITETM C-280,
AMBERLITErY 200, and KASTELr~ C301.
.
35,915-F -4-
- -. ~ - . ,- ~.
-5- 13 2 ~
Acid resins of intermediate strength have also
been reported, such as those containing functional
phosphonic or arsonic groups.
Macroporous weak-acid resins include those
having functional groups of, e.g., phenolic,
phosphonous, or carboxylic types. Some common weak-
-acid resins are those derived by crosslinking of
acrylic, methacrylic or maleic acid groups by use of a
crosslinking agent such as ethylene dimethacrylate or
divinylbenzene. DUOLITErY C-464 is a tradename applied
to a resin having such functional carboxylic groups.
Among the macroporous strong-base resins are
those which, notably, contain quaternary ammonium
groups pendant from a poly(styrene-divinylbenzene)
matrix. DOWEX~ MSA-1 and DUOLITET~ A-191 are
tradenames of strong-base resins reported as having
amine functionality derived from trimethylamine.
DOWEX'Y MSA-2 is a tradename of a macroporous strong-
-base resin reported as having amine functionality
derived from dimethylethanolamine.
Macroporous weak-base anion exchange resins
generally contain functional groups derived from
primary, secondary, or tertiary amines or mixtures of
these. Functional amine groups are derived from
condensation resins of aliphatic polyamines with
formaldehyde or with alkyl dihalides or with
epichlorohydrin, such as those available under the
tradenames DOWEX~U WGR and DOWEXrY WGR-2.
Other macroporous weak-base resins are prepared
by reaction of an amine or polyamine with
chloromethylated styrene-divinylbenzene copolymer
35,915-F -5-
;
-6- 1 3 ~
beads, such as DOWEX~U ~WA-l, DOWEXT~ 66, and DUOLITE
A-392S.
The above-desoribed resins may be used as ion
exchange resins in the demineralization of sugar-
-containing solutions. Sugar solu~ions usually contain
ionic impurities such as Ca++, Mg++, Na+, K+, S03--,
S04--, Cl- and the like. The removal of such
impurities is essential to the preparation of
marketable sugar products.
Examples of sugar-containing solutions include
aqueous solutions of cane and beet sugar, high fructose
corn syrups, high fructose syrups derived from inulin,
tapioca and potato starches, maple sugar, palm sugar,
sorghum derived sugar, and the like, the most preferred
being solutions of high fructose corn syrup. The
disclosed sugar solutions which may be effectively
demineralized exhibit dissolved solids, i.e., sugar
2~ content, ranging from 20 percent to 60 percent.
An effective demineralization may be
accomplished by using a strongly acidic cation exchange
resin in the hydrogen form, followed by an anion
exchange resin preferably in the hydroxide or free base
form. The sugar solution to be demineralized may be
contacted with the resin by any conventional means
which results in intimate contact between the resin and
the sugar solution. Such methods include batch
vessels, packed columns, fluidized beds and the like.
The contacting may be of a batch, semi-continuous or
continuous nature. Preferably the sugar solution and
the resins are contacted continuously in an ion
exchange column.
35,915-F -6-
: ~ : : . : : .
~ :'' ' ' ''' ~:
~7~ ~ 321~ ~3
The resins and the sugar solution are
effectively contacted for a period of time sufficient
to remove a substantial portion of the ionic
impurities. The contact time is largely dependent on
the type of vessel used to contact the resin and the
sugar solution, the amount of resin used, the pH of the
sugar solution, the temperature, the level of
demineralization desired, and the like. The resin may
be used until the ion exchange capacity of the resin
becomes nearly exhausted as evidenced by an increase in
the mineral content of the sugar solution after having
been treated with the resin. At this time it becomes
necessary to regenerate the ion exchange capacity of
the resin in order to prepare it for reuse.
The regeneration of the demineralizing resins
involves the steps of (1) "sweetening-off" the sugar
solution from the resin, (2) backwashing the resin to
remove impurities, (3) contacting the resin with an
appropriate regenerant solution in an amount effective
to regenerate the ion exchange capacity, and then (4)
rinsing the resin to remove any of the excess
regenerant. The resin is then ready to be reused as a
demineralizing resin and may be contacted with the
sugar solution to be demineralized.
The step of "sweetening-off" the sugar solution
from the resin involves the washing of the resin with
water in order to remove essentially all of the sugar
from the ion exchange resins. This is accomplished by
contacting the ion exchange resin which has been
sweetened-on with an amount of water effective to wash
substantially all of the sugar solution from the ion
exchange resin. The resin and water are contacted
until essentially only water is coming off of the resin
35,915-F -7-
~, .
. ., ..;
-8- 1321~
bed. The sweetening-off is considered complete when
there is essentially no sugar in the effluent sweet-
-water stream.
The sweet-water, which results from the
sweetening-off of the sugar from the resin, contains an
amount of sugar which may go to waste if not recovered
within the system. It is desirable to recover this
sugar in as economical a way as possible. Recovery of
this sugar may be accomplished by recycling the sweet-
-water stream back into the sugar-containing solution
o~ the main process stream. Some of the sweet-water
stream may be needed for dilution purposes elsewhere in
the main sugar process stream. However, most of the
sweet-water volume is returned to the main sugar
process stream as an unwanted dilution medium. This
excess dilution water is removed in preparing the sugar
solution for further processing (i.e., increasing the
dissolved solids level in preparation for
crystallization and/or storage of the sugar solution).
The removal of the excess dilution water may be
~ accomplished by evaporating off some of the water from
the sugar-containing solution. This evaporation
results in an effective increase in the level of
dissolved solids present in the process streams.
It has been discovered that by using ion
exchange resins which exhibit bead diameters which fall
within a specific size distr bution, the operating
capacity of the resins for demineralizing sugar-
containing solutions and the amount of water which must
be used to sweeten-off the sugar solution from the
de~-nineralizing resins may be appreciably decreased,
thus also decreasing the amount of recycled dilution
water which must be evaporated from the diluted main
35,915-F -8-
. . . .
:, ~, . ,
:::. ~ :
-9- ~321~ ~
process stream in order to achieve the desired
dissolved solids level. By increasing operating
capacity and reducing the amount of water which must be
evaporated off, the production costs of the sugar
refining process may be reduced.
The size distribution of the beads employed in
this invention is such that at least about 80 volume
percent, more preferably 85 volume percent, and most
preferably at least about 90 volume percent of the
beads exhibit a bead diameter which falls within a
range of about +15 percent preferably within a range of
+10 percent of the mean diameter of the ion exchange
resins used. Mean diameter is determined by the
following sequential steps: 1) measuring the diameter
of each bead in a population of beads, 2) calculating
the volume percent of beads within the preset ranges of
bead diameters to determine a bead diameter
distribution (determined by dividing the volume of
beads within a preset range of bead diameters by the
total volume of beads in the population), and 3)
calculating the mean from the bead diameter
distribution obtained. The mean diameter which may be
used ranges from 400 ~m to 700 ~m, and more preferably
from 500 ~m to 600 ~m, and most preferably from 525 ~m
to 575 ~m.
The following examples are intended to
illustrate the invention. All parts and percentages
are by weight unless otherwise indicated.
Exam~le 1
35700 mls of a macroporous strong acid cation
exchange resin (available as DOWEX~Y 88 from The Dow
35,915-F _g_
: .
132~3
--1 o
Chemical Company) which had been screened to the
following bead size distributi.on1:
Bead Diameter Range Volume ~
5 (}lm) Resin of Invention
Min. Max ! Example 1
150 300 0.1
300 440 1.7
440 495 7.0
495 505 9.2
505 520 11.7
520 540 17.6
540 555 17.2
555 575 17.1
575 590 9.5
590 620 6.4
620 707 2.4
707 2500 0.0
AVERAGE DIAMETER
VOL[~ME MEAN 540
Volume Range 95.7 percent +15 percent of mean.
: 1Each of the bead size distributions in these exmaples
are determined by a particle size analyzer sold
commercial by the HIAC Division of Pacific Scientific
Company as Model PC-320.
was loaded into a 2.54 cm I.D. glass column system
consisting of two 61 cm, water jacketed sections,
coupled together. A third unjacketed 61 cm long
section is attached on top of the two 61 cm columns to
.: .
35,915-F -10-
.
, , ~ ..
. : .
~ : 1 ' ~ , ,
, .- . , ~ . ,
., : , . -:: :.
- ' ~ ;,. ~. . ,
1 3 2 ~
allow backwashing of the resin. The resin is in the
sodium form.
The bed of resin is backwashed with deioni~ed
(D.I.) water at room temperature at a flow rate
sufficient to expand the bed by 50 percent o~ the
settled height. This is done in order to remove any
unwanted matter present in the bed and also to classify
the beads by size. The backwashing is continued for
about 30 minutes.
The resin is then converted to the hydrogen
form by pumping a minimum of 2 bed volumes of 2N
hydrochloric acid through the bed for a minimum of
1 hour contact time. After converting the resin to the
hydrochloric acid form the resin is rinsed with flow of
D.I. water until the effluent water exhibits a pH of at
least 5.
-
After the backwashing is accomplished the top
unjacketed 61 cm portion of the column is removed and
the column is capped with a glass fritted flow
distributor.
One liter of degassed D.I. water is pumped
downflow while the jacketed columns are being heated to
a temperature of about 50C by circulating hot water
through the column jackets.
One liter of refined 42 percent high fructose
corn syrup (HFCS) exhibiting a dissolved solids (D.S.),
i.e., sugar content, of 50 percent is passed downflow
through the bed with a contact time of 60 minutes.
Next, 1 liter of refined 42 percent HFCS, containing
117 g of sodium chloride, is passed downflow throughthe bed over a period of time effective to exhaust the
35,915-F -11-
. .
, .
. .
.
-12- 132~ ~3
resin to the sodium form, generally about 60 minutes.
The HFCS containing the sodium chloride is followed by
1 liter of refined 42 percent HFCS passed downflow
through the resin bed for a period of 30 minutes. The
resin bed is sweetened-off by passing degassed D.I.
water downflow at 2 bed volumes/hr. During the
sweetening-off process, the flow out of the column is
monitored and samples of the effluent are collected at
recorded intervals in a fraction collector. Each
sample is analyzed for refractive index by using an
Abbe Mark II refractometer and the D.S. content is
determined from industry standards based on the
refractive indices. The results are reported in
Table 1 under Example 1.
A plot of the D.S. concentrations versus the
volume of water used to sweeten-off the sugar solution
from the resin bed may be made and the areas under the
curves integrated by known means. The integration
results give a measure of the total amount of dissolved
solids in the collected samples. From this value can
be oalculated the amount of water which must be removed
from the total volume of liquid collected in order to
return the collected sample to the original D.S. level
of the 42 percent HFCS. This value is then used for
comparison purposes to illustrate how much water must
be evaporated from the sweet-water when an ion exchange
resin which does not exhibit a uniform size
distribution is used.
- The results are summarized in Table 3 under
Example 1.
35,915-F -12-
,
.. . .
-13- ~ 32~ 1~3
Comparative Example 1
The method of Example 1 was essentially
repeated except that the strong acid cation exchange
resin (available as DOWEX~U 88 from The Dow Chemical
Company) used to demineralize the HFCS had the
following bead size distribution:
Bead Diameter Range Volume %
10 (~m) Example C-1
Min. Max. DOWEXrM 88
150 250 o.o
250 297 0.0
297 354 0.1
354 420 l . o
420 500 2.5
500 595 6.1
595 707 1 4.0
707 841 28.4
841 1000 3~.2
1000 1190 11.7
l l 9o 2000 0.0
25 2000 2500 0.0
AVERAGE DIAMETER
VOLUME MEAN 820
Volume Range ~8.6 percent +15 percent of mean.
35,915-F -13-
, :, - ' ~,. , , ~ ' ' , ' '
- . . : .: ~ . ~ .
-14- 132~
The results are summarized in Tables 1 and 3
under Example C-1.
TABLE
Cation Resin
Examele 1 CornParative Example C-1*
Volume of Volume of
Sweet-Water Grams Sweet-WaterGrams
(ml) D.S./100 ml (ml) D.S./100 ml
10299 ~2.06 274 63.04
324 58.71 299 60.71
349 54.49 324 57.98
374 50.0~ 349 54.49
5399 45-79 374 49.81
424 41.07 399 47.51
449 36.36 424 43.89
467 33.04 467 36.93
20488 30.04 488 31.95
508 27.28 508 24.62
528 24.50 528 18.65
548 21.62 548 13.99
568 18.61 568 10.49
25587 12.01 587 7.97
607 6.50 607 6.06
627 3.75 627 4.62 ``
`~ 647 2.06 647 3.38
~ 30667 1 - 15 667 2.45
:`
* Not an example of the invention.
35,915-F - 14-
,.
.
...
.: ` . ~ , ,,
1 ~ 2 ~ 3
- 15 -
TABLE I (Cont.)
Cation Resin
Example 1 Cornparative Example C-1*
Volume of Volume of
Sweet-Water Grams Sweet-Water Grams
(ml) D.S./100 ml (ml)D.S./100 ml
686 0.65 686 1.81
706 0.40 706 1.35
726 0.10 726 1.00
746 0.09 746 0.70
766 0.08 766 0.50
785 0.07 785 o .30
- 805 0.07 805 0.15
-- 825 o. lo
__ 845 - 09
__ __ 865 0.08
-- -- 884 0.07
__ __ 904 0.07
* Not an example of the invention.
~`~ 25
Example 2 ~:
700 mls of a macroporous weak base anion
exchange resin (available as DOWEXrY 66, from The Dow
30 Chemical Company) which had been screened to the
following bead size distribution:
: ` '
35,915-F -15-
. " ~ . ~` . , .. ~
-16- 1 3 2 ~
Bead Diameter Range Volume %
(~m) Resin of Invention
Min. Max. Example 2
250 297 o . o
297 325 0.0
325 350 0.0
350 400 2.7
400 420 3.7
420 450 12.5
450 475 13.3
475 500 14. 6
500 540 24.0
540 595 24.1
595 707 5.1
707 2500 0.0
20 AVERAGE DIAMETER
VOLUME MEAN 510
. Volume Range 88.5 percent +15 percent of mean.
25 was loaded into a 2.54 cm I.D. glass column system
consisting of two 61 cm long, water jacketed sections,
coupled together. A third unjacketed 61 cm long
section is attached on top of the two 61 cm columns to
30 allow backwashing of the resin. The resin is used in
the free base form.
; The bed of resin is backwashed with D.I. water
at room temperature at a flow rate sufficient to expand
35 the bed by 50 percent of the settled height. This is
done in order to remove any unwanted matter present in
35,915-F - 16 -
.
, .
;: ,
-17- 1321~
the bed and also to classify the beads by size. The
backwashing is continued for about 30 minutes.
To insure complete conversion of the resin to
the free base form, a minimum of 2 bed volumes of lN
sodium hydroxide is passed downflow through the resin
for a period of about 60 minutes. After complete
conversion, the resin is rinsed with a downward flow of
D.I. water until the effluent water exhibits a pH of at
least 9.
After the backwashing is accomplished the top
unjacketed 61 cm portion of the column is removed and
the column is capped with a glass fritted flow
distributor.
One liter of degassed D.I. water is pumped
downflow while the jacketed columns are being heated to
a temperature of about 50C by circulating hot water
through the column jackets.
One liter of refined 42 percent HFCS exhibiting
a D.S. of 50 percent is passed downflow through the bed
with a contact time of 2.5 hours. The resin bed is
sweetened-off by passing degassed D.I. water downflow
at 2 bed volumes/hr. During the sweetening-off
process, the flow out of the column is monitored and
samples of the effluent are collected at recorded
intervals in a fraction collector. Each sample is
3 analyzed for refractive index using an Abbe Mark II
refractometer and the D.S. content is determined by
industry standards from the refractive indices. The
results are reported in Table 2 under Example 2.
A plot of the D.S. concentrations versus the
volume of water used to sweeten-off the sugar solution
35,915-F -17-
.
13211~ .
from the resin bed may be made and the areas under the
curves integrated by known means. The integration
results give a measure of the total amount of dissolved
solids in the collected samples. From this value can
be calculated the amount of water which must be removed
from the total volume of liquid collected in order to
return the collected sample to the original D.S. level
of the 42 percent HFCS. This value is then used for
comparison purposes to illustrate how much water must
be evaporated from the sweet-water when an ion exchange
resin which does not exhibit a uniform size
distribution is used.
The results are summarized in Table 3 under
Example 2.
Comparative Example 2
The method of Example 2 was essentially
repeated except that the weak-base anion exchange resin
(~vailable as DOWEXTU 66 from The Dow Chemical Company)
used to demineralize the HFCS had the following bead
size distribution:
,,"
35,915-F -18-
, ' - : :
,, ,; ~ ~
-19- 1321 19~
Bead Diameter Range Volume %
Min Max. DOWEX~U 66
150 250 o . o
250 297 0.4
297 354 2.5
0 354 420 5.9
420 500 10.5
500 595 16.9
595 707 24.3
707 841 22.2
` 15 841 1000 17.3
: 1000 ' 1190 0.0
- ` 1190 2000 o . o
2000 2500 0.0
20AVERAGE DIAMETER
VOLUME MEAN 660
Volume Range 63.4 percent +15 percent of mean.
~ 25 The results are summarized in Tables 2 and 3
:~ under Example C-2.
35,915-F -19-
' ` ' ` : ~: -` :
`' : . , ~
-20- 1~21~ ~3
TABLE II
Anion Exchange Resin
Example 2 Comparative Example C-2*
Volume of Volume of
Sweet-Water Grams Sweet-Water Gra~s
(ml)D.S./100 ml (ml) D.S./100 ml
230.359.85 266.6 58.90
260.057.94 286.4 57.05
279.855.05 306.2 54.63
299.653.10 326.0 52.60
319.450.10 345.8 49.60
339.246.77 365.6 46.61
359.043.28 385.4 44.15
378.839.74 405.2 41.25
398.636.20 425.0 38.15
418.433.17 444.8 34.95
438.230.30 464.6 28.85
458.028.28 484.4 22.43
477.825.06 504.2 17.93
497.617.15 524.0 14.45
507.513.69 543.8 11.28
517.411.10 563.3 8.98
537.27.25 583.4 7.05
547.15.99 603.2 5.64
:
~ 30 * Not an example of the invention.
:`~
35,915-F -20-
- , .
.; - , ,.
, ,, , ; .
:,,
.... - - , ,. ~,
-21- 1321~ ~3
TABLE II (Cont.)
Anion Exchange Resin
Example 2 ComParative Exam~le C-2*
Volume of Volume of
Sweet-Water Grams Sweet-Water Grams
(ml) _ D.S./100 ml (ml) _ D.S./100 ml
557.0 4.72 623.0 4,47
576.8 3.10 642.8 3.33
596.6 1.84 662.6 2.34
606.5 1.14 682.4 1.91
626.3 0.95 702.2 1.42
636.2 0.51 722.0 l.og
` 656.0 0.16 741.8 0.80
675.8 0.10 761.6 0.70
696.6 0.16 781.4 0.50
774.8 0.00 801.2 0.50
~ 821.0 0.38
__ -- 860.6 0. 30
-- -- 880. 4 0.38
~ __ __ 930.4 -
Not an example of the invention.
3o
35,915-F -21 -
.
.
132~1~3
Table III
Volume of Water
(ml)
Which Must be
Removed
to Return to
Original
Example D.S. Level Percent Reduction
1 244
_ 28
C-1* 341
2 358
27
C-2* 485
.~
* Not an example of the present invention.
A comparison of the data indicates that when an
ion exchange resin of claimed bead diameter size
distribution is used, the amount of water which must be
evaporated in order to return the sweet-water to a 50
percent dissolved solids level is reduced by a
measurable amount (e.g., 28 percent) compared to the
amount of water which must be evaporated from the
- sweet-water generated from sweetening off the sugar
solution from an ion exchange resin exhibiting a
3 conventional size distribution. Therefore, the amount
of water which needs to be evaporated within the sugar
refining process is reduced.
35,915-F -22-
,, ,. , :
;, , ,;
- - . ~ .: : , . .
3 132~ ~3
Example 3
Operating capacity data was obtained while
demineralizing dextrose syrup in a full scale high
5 fructose refining plant. In this plant the resins
employed in Examples C-1 and C-2 were set up in
sequence (175 cubic feet of each - 4.96 cubic meters)
and a parallel system employing the same volume of the
same resins which had been screened to the following
bead size distribution was set up:
Bead Diameter Range Volume %
(~m) Cation Resin of
Min. Max. Invention
15 150 210
- 210 370 1.6
370 420 3.7
` ~20 470 10.2
: 20 ~70 500 12. 7
500 525 1 7.0
525 550 18.5
550 575 18.6
25 575 600 11.8
60o 625 5.9
625 650 o . o
650 2500 0.0
AVERAGE DIAMETER
VOLUME MEAN 523 ~m
Volume Range 88.8 percent +15 percent of mean.
35,915-F -23-
-24- ~321~ ~3
Bead Diameter Range Volume %
(~m) Anion Resin of
5 Min~ Max. Invention
250 297 0.2
297 354 1. 5
354 380 2.2
` 380 400 3. 2
400 420 4.8
420 460 1 7.2
- 460 480 16.8
480 500 14.7
15 500 525 16.8
525 ~50 13.3
550 595 9.2
::.
:`~ 595 2500 0.0
20AVERAGE DIAMETER
VOLUME MEAN 483 ~m
Volume Range 92.8 percent +15 percent of mean.
~` 25 Operating capacities were measured as volumes
of dextrose syrup demineralized per cycle with cycles
alternating between conventional resins and resins of
the invention. The resins were regenerated back to
usable form each cycle. The results are shown in the
3 following Table IV.
35,915-F -24-
: ` ` ` ~ : . `,, ` " `
-25- 132~ ~93
Table IV
Average Cubic Mleters
Treated Per Cycle
~Increase
Test Period Conventional Resin of in Operating
- ResinInventionCapacity
A 466.1517.8 11
0 B 449.9504.8 12
C 430.9488.6 13
D 415.2470.0 13
The resins employed in the present invention
show from 11 to 13 percent improvement in operating
:~ capacity over the conventional resins when operating as
a two-bed unit process (cation resin followed by anion
resin in a single pass).
35,915-F -25-
. ~ '~, .,: : ' ,
: : . , .
.- . ,
- ,
- : . -: . . .
