Rohm and Haas Ion Exchange

REGENERATION
OF MIXED BED UNITS
(in-situ regeneration)

Regeneration procedure
H2O NaOH Regeneration of mixed bed units is very specific.
Each individual step is critical for the good
performance of the system. The steps are:
1. Separation by backwashing
2. Settling
3. Draining (optional)
4. Regenerant injection, simultaneous or sequential
5. Regenerant displacement
6. Draining water to resin level
7. Mixing with nitrogen or air
8. Filling the unit
9. Final rinse
We will review each of these steps. Special
regeneration equipment and procedures are
available for systems with external regeneration to
H2SO4 or HCl minimise cross-contamination. We are considering
here only internal regeneration.

Water used for regeneration steps

Backwashing can be done with the feed water to the MB unit.
Regenerant dilution and slow rinse should be done:
• Demin water polishers: with the water from the primary demineralisation line.
• Condensate polishers: with clean condensate.
• "Working MBs": with MB treated water, taken from the demineralised water storage
tank or from a twin unit.

Regeneration schematics

1. Backwash
Backwashing a mixed bed results in the separation of the anion resin from the cation resin.
The anion resin, having a lower density, goes up in the stream. Backwash flow rate should be
adjusted so as to obtain enough bed expansion so that even the lowest layers of the mixed
bed are fluidised. Otherwise anion resin may be left "entrapped" in the bottom cation resin
layer. It is often necessary to backwash a mixed bed with stepped velocities, beginning with a
relatively high flow rate (about 15 m/h) to start bed fluidisation, and then reducing the flow
rate to prevent the anion resin from escaping. Backwashing should be done for at least 20 to
25 minutes. In case of high crud (suspended solids) load, the backwash time can be extended
to 40 or 45 minutes. Bed expansion in mixed bed vessels should be:
• At least 60 % for AmberjetTM resins
• At least 75 % for AmberliteTM or AmbersepTM resins without inert
• 100 % for Ambersep resins with inert (TriobedTM)

MB Regeneration 1 2nd edition FD Mar 2007

Rohm and Haas Ion Exchange

2. Settling
It takes a few minutes for the bed to settle after separation. After settling, the separation as
observed through the sight glass must be absolutely sharp, and the visible cross-
contamination (anion resin in the cation layer and vice-versa) must be completely absent or
negligible.

3. Draining (optional)
Draining the water in the unit down to about 300 mm above resin surface will prevent the
caustic regenerant from being diluted through the water in the vessel. This step is of course
not necessary for units equipped with a specific caustic distributor just above bed surface.
When water is drained and the regenerant comes from the top of the column, it will "rain"
unto the water surface in the vessel.

4. Regenerant injection
Caustic soda is injected from the top and the spent caustic is collected at the middle collector.
Sometimes but not always a specific caustic soda distributor is located just above the resin
bed surface.
Acid should be injected from the bottom (not from the middle collector) and extracted at the
middle collector as well.
In general, injection time should be more than 20 minutes, ideally around 30 minutes.
Regenerant quantities and concentrations
As the chemical efficiency of a mixed bed unit is not very good, regenerant dosage is on the
high side. Concentration is typically 4% for NaOH, 5% for acid (when there is no calcium in
the feed, there is no need to dilute H2SO4 to low concentrations).

Regenerant dosage as 100% Concentration

per litre resin
HCl 80 to 150 g/L 5 to 6%
NaOH 80 to 160 g/L 4 to 5
H2SO4 120 to 200 g/L 5 to 6%*
* This is assuming that the feed does not contain calcium; otherwise a low concentration must
be used.
Regeneration can be simultaneous or sequential.
Simultaneous injection
Acid and caustic are injected at the same time. The time for injection + regenerant
displacement is adjusted in such a way that their sum is identical for both regenerants.
Example from an existing plant:
• Acid injection 24 minutes, acid displacement 57 minutes (sum = 81 minutes)
• NaOH injection 33 minutes, caustic displacement 48 minutes (sum = 81 minutes)
Sequential injection
If for any reason it is not possible to inject acid and caustic at the same time, one should start
with caustic soda. During NaOH injection, a small buffer flow of water should be introduced at
the bottom of the unit to prevent the caustic from contaminating the cation resin layer.
Once caustic injection and displacement are finished, the acid is then injected, also using a
small buffer flow of water from the top of the column to prevent the acid from diffusing into
the regenerated anion resin.

MB Regeneration 2 2nd edition FD Mar 2007

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5. Regenerant displacement (slow rinse)

After the prescribed quantity of regenerant has been introduced, the regenerant stream is
stopped and only the dilution water continues to be injected to displace the regenerant.
Displacement is stopped when the pH approaches neutrality (in case of sequential
regeneration). A thumb rule is to use 3 bed volumes of displacement water.

6. Draining
Before air mixing can take place, the water in the vessel must be drained down to the level of
the resin. Otherwise it is impossible to obtain a homogeneous mixture of resin, the
components having the tendency to separate again when settling. The level of water must be
drained down to less than 50 mm (2 inches) above the resin bed surface.
For those who love precision, free water above the surface of the resin bed should be 20 to
30 mm per 1000 mm of bed depth.

7. Mixing
The resin bed is mixed using nitrogen or clean air. General recommendations:
• Air or nitrogen pressure 40 kPa (0.4 bar, 6 psi), more for high bed depth
• Mixing time 10 minutes (more than 5, less than 15)
• Air flow 60 to 80 Nm/h (1.0 to 1.3 Nm3/m2/min, 24 to 32 gpm/ft2)
(≈ 140 m/h at 50 kPa)

8. Filling
The vessel is filled with water (from the top) before the final rinse. This will take a few minutes
again.
To prevent disturbance of the resin bed after mixing, sometimes the first few minutes of filling
are done with the NaOH dilution water, then the column is filled with the feed water at service
flow rate.

9. Final rinse
Fast final rinse is carried out at service flow rate until the required effluent quality is obtained.
With good resins, and when regeneration was successful (absence of cross-contamination) the
final rinse should consume less than 10 bed volumes of water.

External regeneration
The above procedure describes in-situ regeneration, i.e. the resins are regenerated in the MB
unit itself. In external regeneration, the resins are transferred from the MB unit to dedicated
backwash and regeneration columns. There are several different systems, which we will not
describe here. However, the basic regeneration steps are the same, except for additional
transfer steps from the backwash column into anion regeneration column and mixing/holding
tank.

© Rohm and Haas Company

MB Regeneration 3 2nd edition FD Mar 2007