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Dow

Liquid Separations

DOWEX
Ion Exchange Resins

DOWEX ion exchange resins for


HFCS deashing and polishing

Reference Manual
DOWEX ion exchange resins for HFCS deashing and polishing

Table of Contents Page


Corn Sweetener Processing ________________________________________________________________________1
Operating Guidelines ______________________________________________________________________________2
Typical conditions during syrup service ______________________________________________________________2
Regenerating deashing resins _____________________________________________________________________2
Regenerating DOWEX* 88 and DOWEX MONOSPHERE* 88 strong acid cation resins ________________________5
Regenerating DOWEX 66 and DOWEX MONOSPHERE 77 weak base anion resins __________________________7
Regenerating mixed bed polishers _________________________________________________________________9
Resin Properties _________________________________________________________________________________11
Pressure drop as a function of flow rate ____________________________________________________________12
Backwash expansion characteristics _______________________________________________________________14
Storage and Handling_____________________________________________________________________________17
How to get more information on Dowex products and Dow support services_______________________________18
Tables
Table 1 Suggested operating conditions for DOWEX deashing and mixed-bed polishing resins________________2
Table 2 Recommended regenerants for DOWEX deashing and mixed-bed polishing resins __________________6
Table 3 Recommended quality of regenerants ______________________________________________________6
Table 4 Relative selectivity of DOWEX 88 for cations ________________________________________________7
Table 5 Typical resin properties for DOWEX deashing and mixed-bed polishing resins _____________________11
Figures
Figure 1 Sweetening-off deashing systems _________________________________________________________3
Figure 2 Comparing sweetening-off curves for dextrose deashing _______________________________________4
Figure 3 Backwashing deashing resins ____________________________________________________________4
Figure 4 Countercurrent vs. cocurrent regeneration __________________________________________________5
Figure 5 Cation and anion rinses _________________________________________________________________7
Figure 6 Weak base anion regeneration and rinsing __________________________________________________8
Figure 7 Series and recirculation rinsing ___________________________________________________________8
Figure 8 Sweetening-off and regeneration of mixed beds ______________________________________________9
Figure 9 Rinsing and blowdown of mixed beds _____________________________________________________10
Figure 10 Resin mixing in mixed beds _____________________________________________________________10
Figure 11 Recycle rinsing of mixed beds ___________________________________________________________10
Figure 12 Pressure drop with DOWEX 88 resin______________________________________________________12
Figure 13 Pressure drop with DOWEX 66 resin______________________________________________________12
Figure 14 Pressure drop with DOWEX MONOSPHERE 88 and MONOSPHERE 77 resins____________________12
Figure 15 Pressure drop with DOWEX 88 MB resin __________________________________________________13
Figure 16 Pressure drop with DOWEX 22 resin______________________________________________________13
Figure 17 Backwash expansion of DOWEX 88 resin__________________________________________________14
Figure 18 Backwash expansion of DOWEX MONOSPHERE 88 resin ____________________________________14
Figure 19 Backwash expansion of DOWEX 66 resin__________________________________________________14
Figure 20 Backwash expansion of DOWEX MONOSPHERE 77 resin ____________________________________15
Figure 21 Backwash expansion of DOWEX 88 MB resin ______________________________________________15
Figure 22 Backwash expansion of DOWEX 22 resin__________________________________________________16

*Trademark of The Dow Chemical Company


Corn Sweetener Processing
The use of DOWEX ion exchange resins in corn sweetener processing

Millhouse Starch Slurry Gelatinization Dextrinization Saccharification

Adsorbent Decolorization Vacuum Filtration


DOWEX* OPTIPORE* SD-2 Adsorbent Evaporation or Membrane Separation
(some systems) of Insolubles

Dextrose Side Deashing


DOWEX MONOSPHERE* 88
Cation Resin

DOWEX MONOSPHERE 77 Evaporation Isomerization


Anion Resin (some systems)

Fructose Side Deashing


Adsorbent Decolorization
DOWEX MONOSPHERE 88
DOWEX OPTIPORE SD-2 Adsorbent
Cation Resin

DOWEX MONOSPHERE 77
Evaporation 42% Fructose Product
Anion Resin

Mixed Bed Polishing Separation

DOWEX 22 DOWEX MONOSPHERE


80-90% Fructose Blending
Anion Resin 99 Resin
DOWEX 88MB
Cation Resin Mixed Bed Polishing
80-90% Glucose
DOWEX 22
Anion Resin
DOWEX 88MB
Raffinate Cation Resin
(Recycled in Process)

Evaporation

55% HFCS Product

1
Operating Guidelines they operate must be maintained with-
in certain parameters. In particular,
Typical conditions during syrup DOWEX products vary in their temper-
service ature sensitivity. Table 1 provides data
on suggested operating conditions
To obtain optimum performance and such as maximum syrup temperatures.
long life from DOWEX ion exchange
resins, the conditions under which

Table 1 – Suggested operating conditions for DOWEX deashing and mixed-bed polishing resins

DOWEX 88 DOWEX DOWEX 66 DOWEX DOWEX 88 MB DOWEX 22


strong acid MONOSPHERE weak base MONOSPHERE strong acid strong base
cation 88 anion 77 cation anion
strong acid weak base
cation anion

Maximum syrup 200° F 200° F 140° F 140° F 200° F 115° F


Temperature 93°C 93°C 60°C 60°C 93°C 46°C
(H+ form) (H+ form) (FB form) (FB form) (H+ form) (OH- form)

Bed Depth, 36 inches 36 inches 36 inches 36 inches 36 inches 36 inches


(minimum) 91 cm 91 cm 91 cm 91 cm 91 cm 91 cm

Regenerant 6-7 lbs/cu. ft. 5-6 lbs/cu. ft. 5-6 lbs/cu. ft. 4-5 lbs/cu. ft. 6-7 lbs/cu. ft. 4-5 lbs/cu. ft.
Level 96-112 kg/m3 80-96 kg/m3 80-96 kg/m3 64-80 kg/m3 96-112 kg/m3 64-80 kg/m3
(100% basis)

Regenerant 7% HCl 7% HCl 4% NaOH 4% NaOH 7% HCl 4% NaOH


Concentration

Regenerant 200°F 200°F 140°F 140°F 200°F 115°F


Temperature 93°C 93°C 60°C 60°C 93°C 46°C
(max.)

Substitute 5% Na2CO3 5% Na2CO3 7% Na2CO3


Regenerants @ 7-8 lbs/ft3 @ 6-7 lbs/ft3 @ 5-6 lbs/ft3
(112-128 kg/m3) (96-112 kg/m3) (80-96 kg/m3)

5% NH4OH 5% NH4OH
@ 5-6 lbs/ft3 @ 4-5 lbs/ft3
(80-96 kg/m3) (64-80 kg/m3)

When to regenerate deashing unit. This point, called breakthrough, Regenerating deashing resins
resins is determined by measuring the con-
While specific configurations of deash-
ductivity and/or the pH of the syrup as
In a double pass system, when the pri- ing units vary in the industry, the basic
mary deashing unit becomes exhaust- it leaves the primary deashing anion
principles involved in regeneration are
unit. When the conductivity increases
ed to the point where syrup quality relatively standard. This section offers
to around 20-30 micromhos per cen-
drops below an acceptable level, it is a broad overview of the process.
timeter or the pH drops to around 4.5,
taken off-line and replaced with the Specific procedures may vary, and
it is generally time to regenerate the
secondary unit. An off-line, regenerat- additional steps may be required,
unit.
ed unit then becomes the secondary depending on the design and opera-
tion of your system.

2
Never use oxidizing agents such as Sweetening-off The use of deionized (condensate)
nitric acid, perchlorates, or hydrogen When the on-line deashing unit reach- water is not essential for sweetening-
peroxide with ion exchange resins. es breakthrough, the syrup feed is dis- off; however, hard (raw) water will fur-
The reaction can cause slight to continued and water (generally at the ther exhaust the resins. A rule of
severe degradation of the resin, possi- process flow rate) is used to push the thumb for water usage is to use the
bly producing explosive reaction prod- syrup off the resin bed (Figure 1). The water of highest conductivity for
ucts. Also, the use of H2SO4 to full strength syrup exiting the bed dur- sweetening off and save the best
regenerate cation resins is typically ing the early stage of sweetening-off water for regeneration final rinse.
discouraged because CaSO4 can pre- goes forward in the process. On the Due to better resin kinetics,
cipitate in the ion exchange resin. dextrose side, when sweetwater (dilut- DOWEX MONOSPHERE ion
Since the performance of ion ed syrup) starts to exit the bed, it can exchange resins sweeten-off more
exchange resins is dependent on often be put back into the process. efficiently, resulting in 30-40% less
proper regeneration, it is important to With fructose side deashing, however, sweetwater and 40-60% less waste-
closely monitor your regeneration pro- sweetwater is not generally recycled water generated per cycle on both the
cedures. For example, routinely have because it contaminates the glucose dextrose and fructose sides. Figure 2
your quality assurance lab check stream with fructose. When the dis- shows the shorter, steeper sweeten-
regenerant quality and concentration. solved solids concentration of the ing-off profile of a DOWEX
Also be sure that meters, pumps, and syrup gets down to a fraction of a per- MONOSPHERE 88 and 66 resin pair
valves are working and are maintained cent, the effluent is switched to waste. compared with conventional deashing
properly. resin pair.

Figure 1 – Sweetening-off deashing systems

Water

Cation Anion
Resin Resin

Full Strength
Syrup Process

Sweet Water

Waste

3
Figure 2 – Comparing sweetening-off curves for dextrose deashing
This graph tracks the dextrose side
cation-anion effluent during sweetening-off.
Notice the shorter, steeper profile of DOWEX
3.0 360 MONOSPHERE resins. More efficient rinsing
and longer service cycles each lead to
2.5 300 significant reductions in sweetwater and
wastewater.
2.0 240

grams ds/liter
Lbs ds/gal

1.5 180
DOWEX
1.0 MONOSPHERE Standard resins 120
resins
0.5 60

0 0
0 0.4 0.8 1.2 1.6 2.0
Bed Volumes

Backwashing decreased when using colder water.


The next step is backwashing, fluidiz- Backwash expansion curves for
ing the bed by pumping water upflow. DOWEX resins are provided on pages
By lifting and separating the beads, 21-23 to help you determine the
backwashing aids in thorough clean- expansion of your beds at a given
ing of the bed and also allows the temperature and flow rate.
beads to reclassify in the bed, improv-
ing flow distribution. Backwashing
removes residual syrup, resin fines,
microorganisms, and other matter to
allow good regenerant contact and Figure 3 – Backwashing deashing resins
flow through the bed (Figure 3). A
minimum 50% expansion of the bed Waste Waste
volume during backwashing is recom-
mended; 100% expansion is even
better.
Unscreened backwash outlets are
most effective because they allow the Expanded
contaminants to freely exit the bed;
however, backwash expansion must
be monitored carefully to ensure that Cation Anion
resin beads don’t escape the bed. Settled Resin Resin
This is particularly true with anion
resins, which are less dense than
cation resins.
Problems sometimes occur when
the water temperature is lower than
normal because colder water will Deionized Deionized
expand the resin bed more at a given Water Water
flow rate. Flow rates should be

4
Regenerating DOWEX 88 and Figure 4 – Countercurrent vs. cocurrent regeneration
DOWEX MONOSPHERE 88 strong
acid cation resins Cocurrent Countercurrent
Two methods of regenerating are in
common use: cocurrent (in the same 7% HCI Waste &
direction as syrup flow) and counter- Acid
at 5.7 Recovery
current (opposite syrup flow). We rec- Ibs/cu. ft.
ommend countercurrent cation regen-
eration at normal regenerant loads,
particularly for single pass systems, Na Na Na Na Na
Ca Mg Ca Mg Ca Ca Mg Ca Mg Ca
because it results in lower sodium
leakage when the unit is returned to Na Na Na Na Na
service. Salt "heel"
Since 100% regeneration of the
resin is not economical, a small per-
centage of exchange sites will still be Waste & Acid Recovery 7% HCI at 6 Ibs/cu. ft.
occupied by salts. With cocurrent
regeneration, these residual salts
(called the salt heel) end up at the bot- Cation resin regeneration Acid contact time is also important
tom of the bed and can result in higher efficiency to regeneration efficiency. We recom-
than acceptable sodium leakage when Prudent operation of ion exchange mend a minimum of 45 minutes acid
the bed is returned to syrup service systems is a trade-off between appar- pumping time to allow mass action to
(Figure 4). ent short-term savings and long-term take place.
With countercurrent regeneration, operating costs. The most important Regeneration efficiency is also
the salt heel ends up at the top of the factor in cation resin regeneration effi- dependent on the purity of the acid
bed, and even if the syrup picks up ciency is the acid concentration. and dilution water. Table 3 gives the
some of this salt, it will be removed by Since the resin’s active sites have a minimum purity requirements for
the more fully regenerated resin lower greater affinity for the salts they have regenerants commonly used with
in the bed. Salt leakage due to cocur- picked up than for hydrogen ions, a DOWEX resins.
rent regeneration is more pronounced sufficient acid concentration is Regeneration efficiency is reduced
in single pass systems than in double required to overwhelm and drive the by increased amounts of calcium and
pass systems (at equivalent acid salts off these sites. Technically, this magnesium loaded on the resin
loads). is called mass action. Even though because of the high selectivity of the
With both methods of regeneration 40% over the stoichiometric amount of cation resin for these salts (Table 4).
a build-up of calcium and/or magne- acid will not completely regenerate the Extra acid (120-140% of the recom-
sium may occur on the resin over sev- resin, the use of additional excess mended load) may be required to dis-
eral cycles. This may require extra acid is not justified by the economics. place these salts.
heavy acid dosages on a periodic The standard recommendation for Bead size also affects the regener-
basis in order to maintain normal oper- regenerating DOWEX 88 strong acid ation efficiency. Larger beads require
ating capacities. cation resins is 7% hydrochloric acid longer acid contact time for complete
(2N) at 6-7 pounds of 100% HCl per regeneration than smaller beads.
cubic foot of resin.1 These conditions Because they permit a smaller aver-
have proven to be the most efficient age size bead to be used without
and economic for routine regeneration excessive pressure drop, DOWEX
in most systems. Higher concentra- MONOSPHERE resins regenerate
tions or loads will regenerate the more efficiently than standard
resins more completely, but the mini- DOWEX resins. This can result in
mal capacity gained is generally not higher operating capacity and 15-20%
worth the extra cost in acid. Lower longer service cycles. Longer cycles
concentrations or loads will result in translate into fewer regenerations in a
inefficient regeneration of the ion given time span, significantly reducing
exchange resins’ capacity and regenerant costs and increasing resin
reduced lifetime due to irreversible lifetimes.
accumulation of impurities.
1For DOWEX MONOSPHERE 88 resin, the recommended load drops to 5-6 pounds per cubic foot.

5
Table 2 – Recommended regenerants for DOWEX deashing and mixed-bed polishing resins

DOWEX 88 DOWEX DOWEX 66 DOWEX DOWEX 88 MB DOWEX 22


strong acid MONOSPHERE weak base MONOSPHERE strong acid strong base
cation 88 anion 77 cation anion
strong acid weak base
cation anion
3
Regenerant 6-7 lbs. HCl/cu. 5-6 lbs. HCl/cu. 5-6 lbs. NaOH/cu. ft. 4-5 lbs. (64-80 kg/m ) 6-7 lbs./cu. ft. 4-5 lbs.
1
level ft. ft. 7-8 lbs. NaOH/cu. ft. HCl NaOH/cu. ft.
3
(100% basis) (112-128 kg/m ) 6-7 lbs. 5-6 lbs.
3 3 3
96-112 kg/m 80-96 kg/m Na2CO3/cu. ft. Na2CO3/cu. ft. 96-112 kg/m Na2CO3/cu. ft.
5-6 lbs. 4-5 lbs.
NH4OH/cu. ft. NH4OH/cu. ft.

Regenerant 7% HCl 7% HCl 4% NaOH 4% NaOH 7% HCl 4% NaOH


concentration 5% Na2CO3 5% Na2CO3 7% Na2CO3
(minimum) 5% NH4OH 5% NH4OH

Regenerant 200° F 200° F 140°F 140°F 200° F 115°F


temperature 93°C 93°C 60°C 60°C 93°C 46°C
(max)
1
Assuming a minimum 90% equipment efficiency.

Table 3 – Recommended quality of regenerants


Caustic Soda Hydrochloric Acid Ammonium Hydroxide Soda Ash
(NaOH) (HCl) (NH4OH) (Na2CO3)

100% Basis Grade: Technical Liquid ammonia Grade: Technical,


gassified and white powder
dissolved in water
<1200 ppm NaCl 28% (18° Be”) HCl is generally pure enough Typical analysis:
for regeneration of weak
<3000 ppm Na2CO3 <100 ppm Fe 99% Na2CO3
base anion resins.
<30 ppm NaClO3 <100 ppm organics as O2 2100 ppm NaCl
consumed

<10 ppm Fe <5 ppm oxidants as Cl2 200 ppm Na2SO4

<2000 ppm Na2SO4 <4000 ppm sulfate 22 ppm Fe2O3

<100 ppm SiO2

6
Table 4 – Relative selectivity of Figure 5 –Cation and Anion Rinses
DOWEX 88 for cations
H+ = 1 Slow Rinse Fast Rinse
Na+ = 2
K+ = 3 Water
Mg++ = 3 dome lateral
Ca++ = 6

The fact that Na+, K+, Mg++, and Ca++ all have
Water
a higher affinity for the resins’ active sites than
the hydrogen ion is the basis for the cation feed lateral
resins’ ability to effectively remove unwanted
salts from the syrup stream. Because regener-
ation must overcome these selectivity ratios,
the concentration and contact time of the
regenerant must be sufficient to overwhelm the
sites with hydrogen ions and force these salts
off. Waste Waste
or Water Recovery
Cation resin rinsing
Following regeneration are two rinse Regenerating DOWEX 66 and regenerant at the discharge. The sub-
steps: a slow rinse and a fast rinse DOWEX MONOSPHERE 77 weak sequent fast rinse is continued until
(Figure 5). The slow rinse is per- the discharge conductivity or pH drops
base anion resins
formed in the same direction as the below the syrup cycle breakthrough
regenerant flow. The purpose of the In regenerating DOWEX 66 and
point.
slow rinse step is to extend the con- DOWEX MONOSPHERE 77 resins,
Rinse requirements for weak base
tact time of the acid. This time exten- the objective is to remove the acids
anion resins increase over time as the
sion improves regeneration efficiency picked up during syrup service (i.e.
resin progressively fouls. Ammonium
and allows the displaced salts time to sulfuric, nitric, hydrochloric, and
hydroxide-regenerated resins give the
diffuse out of the interior of the resin organic acids). Regeneration is
lowest rinse requirements. On the
beads and into the rinse stream. Slow almost always done downflow (Figure
other hand, ammonium hydroxide-
rinse is performed at regeneration flow 6). With the proper regenerant con-
regenerated resins tend to foul out
rates using condensate or deionized centration and good flow distribution,
more rapidly.
water. The slow rinse is typically weak base anion resins can be regen-
continued until there is a noticeable erated with nearly 100% efficiency. Series and recirculation rinsing
acid dilution (the pH rises). The minimum regeneration recom-
mendations are 4% sodium hydroxide Series rinsing of cation and anion
Following the slow rinse, a fast beds can be used to conserve rinse
rinse at 2 to 4 times the slow rinse at 5-6 pounds per cubic foot for
DOWEX 66 and 4-5 pounds per cubic water (Figure 7). Series rinsing can
flow rate is performed to wash the also provide deionized water for sub-
residual, dilute acid off the resin. This foot for DOWEX MONOSPHERE 77.
Alternatively, 5% soda ash or 5% sequent rinses and dilutions. Series
rinse is continued until the effluent rinsing involves pumping rinse water
quality reaches the desired level, ammonium hydroxide can be used as
specified in Table 2. As with cation through the cation and the anion beds
typically 3-5 pH. The water used for in series.
this rinse must be of especially high resin regeneration, 45 minutes pump-
ing time is recommended as a mini- Recirculation rinsing is sometimes
quality (condensate or deionized performed when rinse requirements
water). Poor quality rinse water will mum.
become excessive (i.e., older resins)
partially exhaust the regenerated resin and continuous pumping of new rinse
before the resin is even returned to Rinsing weak base anion resins
water isn’t economically justified.
syrup service. If the cation resin has The slow and fast steps of rinsing
Recirculation rinsing involves pumping
been kept reasonably clean, part of anion resins are generally performed
rinse water through the cation and
the rinse water can usually be recov- in the same manner as previously
anion beds in a closed loop. During
ered for subsequent acid dilution described for cation resins. The slow
this process, the residual acid coming
and/or rinse water. rinse is performed at the regeneration
off the cation bed is removed by the
flow rate until noticeable dilution of the
anion resin. At the same time, the

7
residual caustic coming off the anion Figure 6 – Weak base anion regeneration and rinsing
bed is neutralized when returned to
the cation bed. Recirculation rinsing
helps to achieve low conductivity efflu-
ent during the sweetening-on step. It Regeneration Slow
can also help reduce salt leakage dur- 4% Caustic Soda Rinse
ing the syrup cycle. However, recircu- or
lation rinsing consumes a small 5% Soda Ash Water
amount of the cation and anion resin or
capacities. 5% Ammonium
Hydroxide
Sweetening-on deashing systems
The sweetening-on procedure is
essentially the opposite of the sweet-
ening-off procedure. When the on-line
unit pair in the primary position reach-
es breakthrough, the regenerated unit Waste Waste
pair is switched to syrup service. For
a double-pass system, the secondary
unit pair is moved into the primary
position and the fresh unit is brought
Series and recirculation rinsing are techniques to minimize water use
into the secondary position. Thus,
sweetening-on is accomplished in-line,
at the process flow rate. The effluent Figure 7 – Series and recirculation rinsing
from the fresh unit pair is typically han-
dled as treated water and waste. Next Series Rinse
comes sweetwater. Finally, when the
syrup concentration is high enough, D.I.Water
the treated syrup is sent forward in the
process. At the same time the fresh
unit pair is sweetening-on, the Cation Anion
exhausted unit pair is sweetening-off.

Cross-regenerating deashing
resins
Waste & Treated
Weak base anion resins generally Water Recovery
require cross-regeneration with 7%
HCl and 4% NaOH approximately
every 6 weeks, on average. Cross-
regeneration helps clean up organic
fouling and extends the life of the
resin. Cation Anion

Caustic brine cleaning of anion


resins
For highly fouled resin, soaking the
resin in a 2% caustic soda/10% sodi- Recirculation Rinse
um chloride brine solution will help
restore the resin’s capacity. This
treatment may be done every 6 has been done at regular intervals periodically, using caustic soda, rins-
months or so to keep the resin in good starting when the resin was new. ing, then regenerating with hydrochlo-
condition. Caustic brine cleaning is We also recommend cross-regen- ric acid.
recommended only when the cleaning eration of strong acid cation resins

8
Regenerating Mixed Bed Polishers while the anion resin beads rise to the acid cation resin is 6-7 lbs/cu ft of 7%
Regeneration of mixed bed polishers top. After backwashing, the bed is hydrochloric acid. For DOWEX 22
is more complicated than regeneration allowed to settle, resulting in two strong base anion resin, the minimum
of split beds because the anion and distinct layers. recommendation is 4% sodium
cation resins are intimately mixed hydroxide at 4-5 lbs/ cu. ft. or 7% soda
during syrup service. As part of the Chemical addition ash at 5-6 lb/cu. ft.
regeneration the cation and anion The resins are regenerated by pump-
beads must be separated prior to ing caustic soda or sodium carbonate Rinsing and blowdown of mixed
regenerant chemical contact. For through the anion resin from the top of beds
quality guidelines, refer to Table 3, the bed while pumping hydrochloric Following regeneration, a slow rinse
Page 6. acid through the cation resin from the is performed maintaining the same
bottom. Excess regenerants meet at flow directions as the regenerants
Sweetening-off and backwashing the central lateral, neutralize each (Figure 9). Next, a fast rinse is per-
The first step in regeneration of mixed other, and are sent to waste. Since formed from the top and bottom of the
bed polishers (Figure 8) is sweeten- this procedure requires that the inter- bed simultaneously. Both rinses
ing-off in essentially the same manner face of the two resins occurs precisely require demineralized or deionized
previously described for deashing at the same level as the lateral dis- water. A blowdown of the liquid head
units. charge, it is critical that the correct to just above the resin level is typically
Next, the resins are backwashed. cation resin volume is maintained in performed after rinsing to accommo-
Backwashing causes the denser, larg- the bed. date the subsequent mixing step.
er cation resin beads to migrate to the The minimum recommendation for
lower portion of the expanded bed, regeneration of DOWEX 88MB strong

Figure 8 – Sweetening-off and regeneration of mixed beds

Waste

Water

Cation Anion
&
Anion
Mix Cation

Full Strength
Process
Backwash Water
Sweet Water
Waste
Caustic

Anion
Waste
Cation
Acid

9
Remixing mixed beds for syrup Figure 9 – Rinsing and blowdown of mixed beds
service
Complete and intimate mixing of the Fast Rinse
Slow Rinse
cation and anion resins is essential for Deionized Water
proper operation of mixed beds.
Typically, the resin bed is first expand- Deionized
Water Waste
ed using air and water simultaneously Waste & Water
Recovery
to mix the resins (Figure 10). Once
the resins are intimately mixed, water Blowndown
addition is stopped but air continues to Air
Deionized Deionized
be blown into the bed until the bed can Water Water
finish settling without significant sepa-
ration of the anion resin from the mix-
ture. The system is vented, and the
bed starts to settle. As it settles, water
is drained off at a rate which keeps the
water level just above the top of the Water Recovery
resins. This keeps the anion resins
from separating near the top of the
bed. Usually this sequence is part of
the automatic operating program, but
in some systems it is performed Figure 10 – Resin mixing in mixed beds
manually.
Air-Water Mix Air Mix Air Drain
Water Recovery Vent Vent
Recycle rinsing of mixed beds
A recycle rinse is also commonly
used with mixed beds because it helps
achieve a low conductivity effluent
during sweetening-on and syrup ser-
vice (Figure 11). Because the perfor- Water
Recovery
mance requirements of mixed bed pol-
ishers are more stringent than with
deashing beds, effluent rinse water
conductivity should ideally be below Deionized Air Air
Water & Air
10 micromhos/cm near the end of the
rinse. At the completion of the recycle
rinse a blowdown of the liquid head is Figure 11– Recycle rinsing of mixed beds
used to remove the water to just
above the resin level in systems oper-
Fill
ated with air domes.
Deionized Vent
Water Recycle Rinse

Blowndown
Air

Water Recovery

10
Resin Properties
This section provides typical resin
properties as well as pressure drop
and backwash expansion charts for
DOWEX resins.

Table 5 – Typical resin properties for DOWEX deashing and mixed-bed polishing resins

DOWEX 88 DOWEX DOWEX 66 DOWEX DOWEX 88 DOWEX 22


MONOSPHERE MONOSPHERE MB
88 77

Type Strong acid Strong acid Weak base Weak base Strong acid Strong base
cation cation anion anion cation anion,
Type II
Active group Sulfonate Sulfonate Tertiary amine Tertiary amine Sulfonate Quaternary
amine
Ionic form Sodium Sodium Free base Free base Sodium Chloride
(as produced)
Structure Macroporous Macroporous Macroporous Macroporous Macroporous Macroporous
styrene- styrene- styrene- styrene- styrene- styrene-
divinylbenzene divinylbenzene divinylbenzene divinylbenzene divinylbenzene divinylbenzene
Physical form Spheres Uniform spheres Spheres Uniform spheres Spheres Spheres
U.S. standard 16-40 -30 + 40 16-50 -30 + 40 16-35 16-50
mesh (typical) (95%) (95%)
Total capacity 1.8 meq/ml, 1.8 meq/ml, 1.60 meq/ml, 1.7 meq/ml, 1.8 meq/ml, 1.2 meq/ml,
min min min min min min
Weak base 1.35 meq/ml, 1.50 meq/ml,
capacity min min
Water retention 42-48% 42-48% 40-50% 40-50% 42-48% 48-56%
capacity (typical)
Swell, % ~ 5% ~ 5% ~ 20% ~ 22% ~ 5% 12% typical
Na → H form Na → H form Free base → HCl Free base → HCl Na → H form Cl- → OH-

11
Pressure drop as a function of flow rate

The following charts are provided to help you determine pressure drop across beds of DOWEX resins.

Figure 12 – Pressure drop with DOWEX 88 resin Figure 13 – Pressure drop with DOWEX 66 resin
Pressure Drop as a function of flow Pressure Drop with DOWEX 66 Resin
rate with DOWEX 88 Resin
m/h m/h
0 1.2 2.4 3.7 4.9 6.1 7.3 0 1.2 2.4 3.7 4.9 6.1 7.3
3.0 68 3.0 68
2 cp ~ 40% dissolved solids at 120° F

Pressure Drop (psi/ft of bed depth)


2 cp ~ 40% dissolved solids at 120° F
Pressure Drop (psi/ft of bed depth)

10 cp ~ 60% dissolved solids at 120° F 10 cp ~ 60% dissolved solids at 120° F


(10cp)
(12 cp)

Pressure Drop (kPa/m)


Pressure Drop (kPa/m)
2.0 45 2.0 45
(10cp)

(6cp)

(6cp)
1.0 23 1.0 23

(2cp)
(2cp)

0 0 0 0
0 .5 1.0 1.5 2.0 2.5 3.0 0 .5 1.0 1.5 2.0 2.5 3.0
Flow Rate (gpm/ft2) Flow Rate (gpm/ft2)

Figure 14 – Pressure drop with DOWEX MONOSPHERE 88 and MONOSPHERE 77 resins

Pressure Drop with DOWEX MONOSPHERE 88 and MONOSPHERE 77 Resins


m/h
0 1.2 2.4 3.7 4.9 6.1 7.3
3.5 79
Pressure Drop (psi/ft of bed depth)

3 X 68
Pressure Drop (kPa/m)

2.5 56

2 X 45
X
1.5 34
X +
1 X 23
+
0.5 X 11
+

0 0
0 0.5 1 1.5 2 2.5 3
Flow Rate (gpm/ft2)

2 cp + 4 cp X 6 cp 8 cp X 10 cp 12 cp

12
Figure 15 – Pressure drop with DOWEX 88 MB resin

Pressure Drop with DOWEX 88 MB Resin

(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3
3 68
Pressure Drop (psi/ft of bed depth)

2.5 56

Pressure Drop (kPa/m)


X
2 45

1.5 X 34
+
1 23
+
X
0.5 11
+

0 0
0 0.5 1 1.5 2 2.5 3
Flow Rate (gpm/ft2)

2 cp + 6 cp X 10 cp 12 cp

Figure 16 – Pressure drop with DOWEX 22 resin

Pressure Drop with DOWEX 22 Resin

(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3
3 68
X
Pressure Drop (psi/ft of bed depth)

2.5 X 56
Pressure Drop (kPa/m)

2 X 45
+
1.5 X + 34
+
1 X 23
+

+
0.5 X 11
+

0+
X 0
0 0.5 1 1.5 2 2.5 3
Flow Rate (gpm/sq.ft.)

2 cp + 6 cp X 10 cp 14 cp

13
Backwash expansion characteristics

The backwash expansion curves in Figure 18 – Backwash expansion of DOWEX MONOSPHERE 88 resin
this section are provided to help you
determine the expansion of your beds DOWEX* MONOSPHERE* 88 Backwash Expansion Water @ 77 Deg. F 25 Deg. C
at a given temperature and flow rate. (m/h)
Colder water will expand the resins 0 4.9 9.8 14.7 19.6 24.4 29.3 34.2
higher in the bed for a given pump 100
rate.
90
Backwash expansion should be
monitored carefully since insufficient 80

% Bed Expansion
expansion will decrease regeneration 70
efficiency. Excessive expansion may 60
lead to resins escaping the bed - a 50
particular concern with anion resins, 40
To determine flow rate at temperature t
which are lighter than cation resins. 30 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
More information on resin backwash-
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
ing and recommendations for bed
10
expansion are given on Page 4.
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Flow Rate F (gpm/ft2)
Sodium Form

Figure 17 – Backwash expansion of DOWEX 88 resin Figure 19 – Backwash expansion of DOWEX 66 resin

Backwash Expansion Characteristics of DOWEX 88 Resin Backwash Expansion Characteristics of DOWEX 66 Resin
(m/h) (m/h)
0 4.9 9.8 14.7 19.6 24.4 29.3 34.2 0 1.2 2.4 3.7 4.9 6.1 7.3 8.6 9.8 11.0
100 100
Typical Wet Screen Free Base
Mesh % 90 Form 77°F
90 +16 0.0 (25°C)
+20 21.4 80
HCI-H2SO4
+30 64.2 Exhausted
80 70
% Bed Expansion ( Na+ exhausted form)

% Bed Expansion

+35 11.6 77°F Form 77°F


+40 2.3 25°C (25°C)
60
+50 0.5
70
-50 0.0 50
60 40
30
50
20
To determine flow rate at temperature t
40 10 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
0
30 0 .5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
Backwash Flow Rate (gpm/sq.ft.)
20
To determine flow rate at temperature t
Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
10
Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]

0
0 2 4 6 8 10 12 14
Flow Rate F (gpm/ft2)

14
Figure 20 – Backwash expansion of DOWEX MONOSPHERE 77 resin

DOWEX* MONOSPHERE* 77 Backwash Expansion


Water @77 Deg. F 25 Deg. C
(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3 8.6
100 +
90
80
+
% Bed Expansion

70
+
60 +
50
+
40
To determine flow rate at temperature t
30 + Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
+
10
0
0 0.5 1 1.5 2 2.5 3 3.5
Flow Rate F (gpm/ft2)
Free Base Form + Acid Exhausted Form

Figure 21 – Backwash expansion of DOWEX 88 MB resin

DOWEX 88MB Backwash Expansion


Water @77 Deg. F 25 Deg. C
(m/h)
0 4.9 9.8 14.7 19.6 24.4 29.3 34.2
100
90
80
% Bed Expansion

70
60
50
40
To determine flow rate at temperature t
30 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
10
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Flow Rate (gpm/ft2)
Sodium Form

15
Figure 22 – Backwash expansion of DOWEX 22 resin

DOWEX 22 Backwash Expansion

(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3 8.6 9.8
100
90
% Bed Expansion (CI¯ form)

80
70
60
50
40
To determine flow rate at temperature t
30 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]

10
0
0 0.5 1 1.5 2 2.5 3 3.5 4
Flow Rate F (gpm/sq.ft.)
Expansion @ 77 Deg F
25 Deg C

16
Storage and Handling Bringing deashing units back
on-line
Storage 1) Rinse off the NaOH storage solu-
For long shutdowns, cation and anion tion to neutral pH.
deashing resins can be stored in place 2) Cation resins - Regenerate with a
in a manner that provides protection minimum of 1.5 bed volumes of 7%
from microbial growth. The following HCl; rinse to neutral pH. Anion
recommendations will also increase the resins - Cross-clean first with 7%
probability of a trouble free start-up. HCl; rinse to neutral pH; regenerate
with a minimum of 2.2 bed volumes
Cation and anion deashing resin of 4% NaOH; rinse to neutral.
preparation and storage 3) Follow normal procedures from this
1) Backwash the bed to a minimum of point on.
50% expansion for as long as it
takes to produce a clear and color- Handling
less effluent. WARNING: Oxidizing agents such
2) Clean up the resin by passing 2 bed as nitric acid attack organic resins
volumes of 4% (1N) NaOH through under certain conditions and could
the bed; rinse to neutral pH; pass result in a slightly degraded resin up
through 1.5 bed volumes of 7% (2N) to an explosive reaction. Before using
HCl ; rinse to neutral pH.2 strongly oxidizing agents, consult
3) Pass 4% NaOH through the bed until sources knowledgeable in handling
at least a 0.5% (0.1N) concentration such materials.
is detected in the effluent. The
entire vessel should be full of 0.5%
(minimum) NaOH solution for protec-
tion and cleaning of the dome space.
4) During the storage period, check the
NaOH solution periodically by drain-
ing some off the bottom of the ves-
sel. Replace the entire solution vol-
ume with fresh 0.5% NaOH if there
is significant color development.

2Pumping rates of the chemicals should be such that there is a minimum contact time of 45 minutes.

17
How to get more information on DOWEX products
and Dow support services
To learn more about DOWEX prod- Dow technical service representative.
ucts, Dow technical support services, You'll talk with someone who under-
request additional literature, or to get stands your needs and can provide the
help resolving a particular problem, prompt, personal service you deserve.
simply call us toll-free at
1-800-447-4369 or contact your

18
Notes:

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Dow Liquid Separations Offices.
For more information call Dow Liquid Separations:

Dow Europe Dow Pacific Dow North America


Dow Customer Information Group Dow Chemical Australia Ltd. The Dow Chemical Company
Liquid Separations Liquid Separations Liquid Separations
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Tel. +32 3 450 2240 Australia USA

Tel. +800 3 694 6367 Tel. 61-2-9776-3226 Tel. 1-800-447-4369
Fax +32 3 450 2815 Fax 61-2-9776-3299 Fax (989) 832-1465
E-mail: dowcig@dow.com
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Dow Pacific Dow Quimica S.A. http://www.dowex.com
Dow Chemical Japan Ltd. Liquid Separations
Liquid Separations Rua Alexandre Dumas, 1671
Tennoz Central Tower Sao Paulo – SP – Brazil
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Tel. +81 3 5460 2100
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Toll-free telephone number for the following countries: Austria, Belgium,
Denmark, Finland, France, Germany, Hungary, Ireland, Italy, The Netherlands,
Norway, Portugal, Spain, Sweden, Switzerland, and the United Kingdom

Warning: Oxidizing agents such as nitric acid attack organic ion exchange resins under certain conditions. This could lead to anything from
slight resin degradation to a violent exothermic reaction (explosion). Before using strong oxidizing agents, consult sources knowledgeable in
handling such materials.

Notice: No freedom from any patent owned by Seller or others is to be inferred. Because use conditions and applicable laws may differ
from one location to another and may change with time, Customer is responsible for determining whether products and the information in this
document are appropriate for Customer’s use and for ensuring that Customer’s workplace and disposal practices are in compliance
with applicable laws and other governmental enactments. Seller assumes no obligation or liability for the information in this document. NO
WARRANTIES ARE GIVEN; ALL IMPLIED WARRANTIES OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE ARE
EXPRESSLY EXCLUDED.

Published June 2002.

*Trademark of The Dow Chemical Company Form No.177-01711-602QRP