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Spent caustic recycle at Farleigh mill

Article  in  International Sugar Journal · March 2015

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Lavarack B et al. Proc Aust Soc Sugar Cane Technol Vol 36 2014
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SPENT CAUSTIC RECYCLE

AT FARLEIGH MILL

By

BRYAN LAVARACK, BRUCE STEVENSON,

SHERYL SCHNEIDER, BRETT BAMPTON

Mackay Sugar Limited, Mackay

[email protected]

KEYWORDS: Spent Caustic Soda, Evaporation,

Lime Use, Clarification.

Abstract
CAUSTIC SODA is routinely used in most Australian raw sugar factories to clean
evaporator vessels and other process equipment. After repeated use, the caustic soda
becomes fouled with both soluble and insoluble contaminants. The end result is the
efficacy of the caustic soda is diminished and requires complete replacement. A low
cost method for the disposal of spent caustic is required. Spent caustic soda is
commonly disposed of, if possible, by trickling into the mill’s effluent to control pH
levels in the effluent treatment plant. The other practical option available at present is
removal and disposal by specialist waste treatment companies. Other options for caustic
soda regeneration and re-use are not regarded as viable. This paper examines the recycle
of spent caustic soda to process in the 2012 and 2013 seasons and considers some
impacts on process operations for Farleigh mill. Recycling of spent caustic soda at about
100 ppm sodium hydroxide on cane to primary mixed juice has the potential benefits of
reducing scaling in the multiple effect evaporators and decreasing lime consumption.
Lime consumption reduced by about 33 and 81 ppm on cane during periods of recycle
in 2012 and 2013 respectively. The heat transfer coefficients for the multiple-effect
evaporator at Farleigh mill during periods of spent caustic soda recycling compare
favourably with previously published data. The costs for cleaning chemicals have
reduced from about A$0.152/tonne cane for seasons when recycling was not undertaken
to about A$0.083/tonne cane for the two seasons when recycling was undertaken. The
reduction in cleaning chemical costs could be influenced by good quality cane, fine
weather and good management of the evaporators at the time of the study.
Introduction
Caustic soda is a chemical cleaning agent for the removal of scale from evaporator vessels
and other process equipment in raw sugar factories. After repeated use, the caustic soda becomes
spent and requires disposal.
This paper investigates methods to treat spent caustic soda and reports on factory trials
undertaken on recycling spent caustic soda in the 2012 and 2013 seasons at Farleigh mill. One of
the advantages in dosing sodium hydroxide or caustic soda to mixed juice is the apparent benefits to
clarification. This and other operational factors arising from recycling of spent caustic soda are
examined in the paper.
Background
The use of caustic soda for removal of scale from evaporator vessels and other process
equipment by clean-in-place strategies is well documented in the classic sugar industry texts such as
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Honig (1963b), Hugot (1986), Chen and Chou (1993) and Rein (2007). Caustic soda is highly
effective because it removes many types of scale at relatively low cost. Although not effective for
the removal of all types of scale, caustic soda is routinely used at Mackay Sugar Limited (MSL) and
other Australian raw sugar factories.
At MSL factories, caustic soda is stored in working tanks and supplied to evaporator vessels
and other process equipment to be cleaned in-place. Chemical cleaning with caustic soda is
undertaken at scheduled maintenance stops and on-the-run as required (provided that the factory has
sufficient redundant capacity). The caustic soda solution is returned to the working tank after each
cleaning cycle so that the solution can be re-used later. There is no hard rule regarding the number
of cleaning cycles that should be undertaken for a batch of caustic before the caustic solution is
disposed. The efficacy of the caustic soda solution reduces progressively each time a chemical clean
is undertaken. The caustic soda solution accumulates both dissolved and undissolved impurities
which reduce cleaning performance. Some of the undissolved impurities settle and can be removed
if the caustic is stored in a tank with a conical bottom. The working tank is topped up with fresh
caustic soda as required, but a point is reached when both the hydroxide concentration is low and
contaminant levels in the caustic soda solution are high.
The process equipment does not achieve the required level of performance for satisfactory
operations after a chemical clean. The caustic soda solution is deemed spent at this point and is
transferred to a storage tank or a specially designed holding dam for disposal. Although spent
caustic soda solutions are not used for further in-place cleaning at the factory, the solutions have
high residual concentrations of sodium hydroxide (and high pHs). The spent caustic solution has
value for this reason. Traditionally the spent caustic soda solution is trickled into the feed to the
effluent plant in order to control the pH levels in the plant.
Farleigh mill operates an activated sludge effluent treatment plant. The production personnel
that manage the effluent treatment plant have observed over many years of operation that the
activated sludge plant tends to prefer calcium to sodium ions. High levels of spent caustic soda
addition are considered to have an adverse effect on the activated sludge plant at Farleigh mill.
Also, high sodic levels are not preferred since the treated effluent is often used for the irrigation of
cane. Consequently, the potential for the disposal of spent caustic soda at Farleigh mill is restricted.
This situation has led to progressive increases in the quantity of spent caustic soda being
stored at the factory. Matters came to a head after a series of wet seasons which resulted in the
quantity of stored spent caustic soda reaching unacceptable high levels. A low cost method for the
disposal of spent caustic soda was sought for Farleigh mill; one which had potential benefits for
both the effluent treatment plant and factory process, if possible.
What are some of the alternatives for spent caustic disposal?
Several options were considered for the disposal of spent caustic soda at Farleigh mill; these
include the following:
(1) Regeneration of spent caustic soda for re-use as a chemical cleaning agent
(2) Rudimentary treatment of spent caustic to produce a product for other applications
(3) Removal and disposal by specialist waste treatment companies
(4) Recycle of spent caustic soda as an aid in the clarification process.
Option (1) requires a dedicated plant to regenerate spent caustic similar in concept to that
designed for regenerating brine solutions in sugar refining (Meadows et al., 1992). The regeneration
plant would likely include (i) a coarse filtration step to remove scale particulates and (ii) one or two
membrane filtration steps to remove macro-molecules from the solution. Membrane filtration would
produce a filtered stream (permeate) which could be returned to the caustic working tank.
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The unfiltered material (retentate) from the membrane filtration is purged and requires
disposal. Supplementary caustic soda is required to replace the chemical consumed in evaporator
and other process equipment cleaning as well as the chemical lost in the retentate purge stream. A
rough estimate is that about 10–20% of the spent caustic soda would require replacement with fresh
caustic soda for each regeneration. The simplified diagram of the process is given in Figure 1.

Fig. 1—Option (1) for disposal of spent caustic.

High pressure pumping is required for the membrane filtration step. The safety aspects for
maintaining and operating a plant treating hot pressurised caustic soda are challenging, but not
insurmountable. The safety aspects plus the capital and operational costs for this process meant that
this option was not given serious consideration.
Option (2) requires simple treatment of the spent caustic soda which would likely entail
concentration to achieve a minimum concentration level of caustic soda and coarse filtration to
remove sediment (scale particulates) from the solution. A market for the product is required for this
product. This option requires a capital investment, a detailed examination of the market
opportunities and ongoing marketing of the product. Like option (1), this option was not given
serious attention for development.
Option (3) is the removal and disposal by specialist waste treatment contractors. This option
is adopted if there is no other practical option available. The removal of spent caustic soda has been
undertaken previously by specialist waste contractors for MSL. It is a relatively costly exercise that
can be readily undertaken. It provides a practical answer to the issue, but is not preferred because of
cost.
Option (4) is the recycle of spent caustic soda to the factory to aid clarification. This is the
process investigated and trialed at Farleigh mill in the 2012 and 2013 seasons. This option is
discussed in greater detail below.
How is juice clarification affected by supplementation with caustic soda?
SRI has recently investigated the addition of caustic soda in juice clarification. Doherty
(2011) reports that the addition of lime saccharate to a set juice pH followed by the addition of
sodium hydroxide to a final juice pH or a similar two-stage process where the order of addition of
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the alkalis is reversed prior to clarification reduces the impurity loading of the clarified juice
compared to that of the clarified juice obtained by the conventional defecation process. The
treatment process showed reductions in CaO (27% to 50%) and MgO (up to 20%) in clarified juices
with no apparent loss in juice clarity or increase in residence time of the mud particles compared to
those in the conventional process. This work has suggested that a trial with spent caustic soda
would appear to be worth undertaking at MSL.
Although Doherty notes particular benefits, there are significant issues that require resolving
to be accepted for full-scale implementation at MSL factories.
The first consideration at MSL is for occupational health and safety. Caustic soda is
routinely handled in MSL factories so the management practices developed for handling caustic
soda are extended to cover the recycle of spent caustic soda. The other considerations are condensed
to four key questions.
• Will spent caustic soda recycle reduce or promote scaling in the evaporator stage?
• Does caustic soda recycle reduce lime usage for the factory?
• Are there major changes to the composition of evaporator supply juice (ESJ) with
potential to affect downstream processes?
• Will increased ash levels from spent caustic soda recycle have a noticeable effect on
molasses formation?
Method
A dosing pump and pipeline were installed to transfer spent caustic soda from the small
clay-lined holding pond to the primary juice transfer tank at Farleigh mill. Since spent caustic soda
was added before the lime addition point, no additional pH control equipment is required for the
factory. The flows and concentration of sodium hydroxide in the spent caustic were regularly
monitored. All significant changes to processing conditions in the clarification stage were logged
during the trial.
Samples of ESJ were collected and routinely analysed during shift for pH, turbidity,
phosphate and apparent purity. The ESJ samples were composited over a period of a week or
corresponding period of recycle/non-recycle and analysed for pH, turbidity, phosphate, sucrose, dry
substance, purity and ash. ESJ was composited directly into a sample stored in a deep freezer. The
methods of analysis were the BSES standard analytical methods (BSES, 1984). The composited
samples of ESJ were analysed by SGS Laboratories for calcium, sodium and potassium levels as
well as for platinum cobalt units (PCU) colour. The colour analysis has no pH adjustment and is
measured in PCU on a Lovibond type comparator. SGS analyses are on volume basis, whereas the
Farleigh laboratory analyses are on mass basis.
The test periods for recycle of caustic were (i) crush weeks 14–24 of the 28 week season
starting 8 June 2012 and ending 11 December 2012; and (ii) crush weeks 2–13, weeks 16–18 and
weeks 21–23 of the 23 week season starting 19 June 2013 and ending 23 November 2013.
Results and discussion
An initial trial was undertaken in September 2012, which was followed by a controlled test
program during the rest of the season.
Tests continued in 2013 season. The planned program requiring regular periods of recycle
and non-recycle was not followed in the 2013 season. The holding pond filled with water at the start
of the crush season and a continuous recycle program was instituted to reduce the high levels. The
dose pump was shut off for periods later in the season to obtain data for non-recycle operation. The
concentration of sodium hydroxide in the holding pond was about 1.0% at start of the 2013 season
compared with 3.1% at start of the 2012 season trial.
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Scaling in the evaporators

For the duration of the trials, heat transfer ratios (HTRs) were calculated for the evaporator
stage. These were typically calculated once or twice per week to determine how scaling was
affecting the performance of the evaporator stage. HTRs for Farleigh mill evaporators for the 2012
and 2013 seasons are given in Table 1. [The ratio of the heat transfer coefficient for a particular
evaporator to the heat transfer coefficient for an evaporator at standard Australian conditions is
known as the heat transfer ratio (HTR). For above average performance of the evaporator, the HTR
is greater than 1, but HTRs less than 1 indicate below average performance.]

Table 1—HTRs for Farleigh mill evaporators for 2012 and 2013 seasons.

#1 #2 #3 #4 #5 Average

2012 season – Maximum HTR 1.31 1.47 1.25 1.15 1.03 1.24
2012 season – Minimum HTR 0.64 0.61 0.80 0.74 0.67 0.69
2012 season – Average HTR 0.92 0.98 1.00 0.89 0.86 0.93
2013 season – Maximum HTR 1.15 1.04 0.96 1.23 1.02 1.08
2013 season – Minimum HTR 0.49 0.46 0.69 0.77 0.70 0.62
2013 season – Average HTR 0.67 0.75 0.83 0.98 0.89 0.82

Detailed examination of the heat transfer data on a week by week basis showed that it was
difficult to determine increased or decreased rates of scaling that are meaningful. The evaporator
vessels (effets) at Farleigh mill are known to perform well at the start of the season when clean, but
performance diminishes as the season progresses since the effets foul and do not fully respond to
chemical cleaning.
The HTR data were compared to previously reported data to determine the level of
performance of the evaporator stage on an annual basis. The HTRs calculated for seasons with spent
caustic soda recycling compared favourably with HTRs determined for seasons with no caustic soda
recycling. This is explained in the following paragraphs.
The no.4 and no.5 effets at Farleigh mill are known to be prone to scaling, but performed
well throughout the 2012 and 2013 seasons. The HTRs for no.5 effet averaged 0.86 and ranged
from 1.03 to 0.67 for the 2012 season; and averaged 0.89 and ranged from 1.02 to 0.70 for the 2013
season. Lavarack et al. (2009) noted that the HTRs for no.5 effet at Farleigh ranged from 0.81 to
0.69 for tests during the 2007 and 2008 seasons. Attard (1991) stated the HTRs for no.5 effet ranged
from 0.90 to 0.71 for a test period in the 1990 season.
The scaling in the no.1 effet at Farleigh mill was pronounced during the 2013 season. The
HTRs for no.1 effet averaged 0.67 and ranged from 1.15 to 0.49 in 2013 compared to an average of
0.92 and range from 1.31 to 0.64 in 2012. Lavarack et al. (2009) noted that the HTRs for no.1 effet
range from 0.80 to 0.72 for tests in 2007 and 2008. Attard (1991) noted a range from 0.99 to 0.81 in
1990.
A novel measure for evaluating scaling is the estimation of the costs of cleaning chemicals
consumed in the evaporator stage per tonne of cane processed. The costs of chemicals are
determined on a yearly basis since it is particularly difficult to attribute chemical use to individual
weeks of recycle or non-recycle. The average costs for cleaning chemicals consumed in the 2009,
2010 and 2011 seasons (period of non-recycling) were determined to be about A$0.152/tonne cane
processed. A similar calculation is undertaken for the recycle years (2012 and 2013 seasons) and the
chemical costs are calculated to be about A$0.083/tonne cane.
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All costs for chemical cleaning agents are based on pricing at the start of the 2013 season to
ensure even comparison. There is a significant cost reduction during the recycle years; however the
full quantum of the cost reduction cannot be solely attributed to spent caustic soda recycling. Good
quality cane, fine weather and good management of the evaporator stage are all major factors in
reducing scaling and decreasing cleaning costs (Crees et al., 1992, Rackemann et al., 2012).
Lime usage
The lime consumption rates per tonne cane processed were compared for periods of
recycling and non-recycling in the 2012 and 2013 seasons. The results from the two seasons, as well
as data for the three preceding seasons, are given in Table 2.

Table 2 – Lime usage at Farleigh mill for 2009– 2013 seasons

Lime usage, ppm on cane for periods:
Season Lime saving (a) – (b)
Whole season (a) Non-recycle (b) Recycle
2009 828 828 – –
2010 729 729 – –
2011 917 917 – –
2012 786 796 763 33
2013 764 772 691 81

Lime consumption in the 2011 season is markedly higher than the other seasons because of
the requirement to process stand-over cane remaining from the previous wet season.
It is apparent that the lime consumption decreases when caustic recycling is undertaken. The
additions of spent caustic soda averaged about 98 and 69 ppm sodium hydroxide on cane during the
recycle periods in 2012 and 2013 (calculated from the tonnes cane processed and the concentrations
of sodium hydroxide and flows of spent caustic soda to the primary juice tank). The additions of
spent caustic soda resulted in savings of 33 ppm lime on cane and 81 ppm lime on cane
respectively. If the savings are extrapolated to the whole season and assuming the savings remain
consistent for the whole season, about 58 and 119 tonnes less lime are consumed for 2012 and 2013
seasons respectively. The reasons for the reduced lime saving despite higher caustic addition in the
2012 season compared with the 2013 season are not known. Variations in cane/juice quality and
weather are likely contributing factors.
There is a potential to slightly increase both the flow and concentration of spent caustic soda
recycled to primary juice, by sending caustic soda to the holding pond before it is completely spent.
In which case, the caustic soda consumption will increase and the lime consumption should
decrease by a commensurate amount. Since the cost of caustic soda (solid) is about three to four
times the price of lime, on a mass basis, the benefit of reducing lime consumption by substitution
with sodium hydroxide is limited from a perspective of chemical cost.
Changes in ESJ and downstream processing
The analyses of ESJ for the recycle and non-recycle periods in the 2012 and 2013 seasons
are given in Table 3.
Table 3—Analyses of ESJ collected at Farleigh mill

Phosphate Dry Colour Calcium Sodium Potassium

Season pH Turbidity Purity Ash
ppm substance PCU mg/L mg/L mg/L

2012 Recycle 7.0 14.3 43.8 16.6 91.3 0.435 850 340 91 928
No recycle 7.0 9.0 30.8 16.6 90.3 0.433 1133 353 50 900
2013 Recycle 7.2 14.7 54.0 15.3 91.5 0.465 3630 302 58 978
No recycle 7.6 14.5 42.8 16.2 91.1 0.470 5167 333 39 957
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Lavarack B et al. Proc Aust Soc Sugar Cane Technol Vol 36 2014
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The amount of sodium hydroxide in the recycle is higher in 2012 than in 2013 and this is
reflected in the relative increase in the sodium concentrations in ESJ for 2012. The levels of
calcium in ESJ decrease during the recycle periods. The reductions in calcium concentrations are
relatively small and are less than that reported by Doherty (2011). A very small increase in
potassium concentration is noted during recycling.
The ash levels in ESJ do not change appreciably during spent caustic soda recycling, so the
ash should not have a marked influence on pan stage operations. It is of interest to note that during
recycling the sucrose purity of ESJ increases and the PCU colour decreases. The reasons for this are
not known. The turbidities of ESJ do not show a strong trend with recycling.
No perceptible changes in downstream processing were noted by factory personnel during
the recycle mode of operations.
Molasses formation
Increased soluble ash content in juice is considered to be melassigenic or molasses forming
(Honig, 1963a). During periods of recycling there is an increase in sodium and potassium levels (or
soluble ash) which has the potential to increase final molasses production and reduce exhaustion.
Production data and ash levels in molasses were collected for the 2009, 2010 and 2011 seasons as
for the recycle and non-recycle periods in 2012 and 2013. The data are recorded in Table 4.

Table 4—Final molasses production data for Farleigh mill.

2009 2010 2011 2012 2013

Mol% Ash% Mol% Ash% Mol% Ash% Mol% Ash% Mol% Ash%
cane mol cane mol cane mol cane mol cane mol
Non-
recycle 2.95 13.83 2.79 13.08 2.84 13.40 2.71 13.29 2.89 14.13
Recycle – – – – – – 2.73 13.96 2.77 14.22

The data show that there is no major increase in the final molasses production levels for the
periods of spent caustic recycling either during the season or relative to previous seasons. The ash
levels in the molasses tend to increase slightly during the recycling periods of 2012 and 2013.
Conclusions
The recycling of spent caustic soda to primary mixed juice is considered to have many
benefits provided the rate of addition is maintained at low rates of about 100 ppm sodium hydroxide
on cane. The heat transfer coefficients for the multiple-effect evaporator at Farleigh mill during
periods of spent caustic soda recycling compare favourably with previously published data.
The cost of cleaning chemicals required for the evaporators decreased significantly during
the periods of spent caustic soda recycling, but this could be influenced by good quality cane, fine
weather and good management of the evaporator operations at the time of the study.
Acknowledgement
The management of Mackay Sugar Limited is thanked for allowing the authors to publish
this paper.
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