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Desalination 196 (2006) 237247

Inhibition of calcium and magnesium-containing scale by a new


antiscalant polymer in laboratory tests and a field trial
Hai-Yan Li, Wei Ma*, Lu Wang, Ru Liu, Lin-Sen Wei, Qiang Wang
Research Centre of Seawater Desalination and Multipurpose Utilization, School of Chemical Engineering,
Dalian University of Technology, Dalian, 116023, PR China
Tel. +86 (411) 8470-6303; email:mawei@dlut.edu.cn

Received 25 July 2005; accepted 18 November 2005

Abstract
Membrane scaling is caused by the deposition of unsoluble salts as feedwater converted to brine, affectting the
operation of seawater RO plants. Membrane scaling at the Dalian RO desalination plant was analyzed using Dalian
seawater. Based on the characteristics of Dalian seawater, a new environmentally friendly, biodegradable antiscalant
PAP-1 was synthesized in the laboratory. The performance of PAP-1 to inhibit calcium and magnesium-containing
scale was studied both in the laboratory and at the Dalian seawater RO desalination plant. It was found that PAP-1 is
effective in inhibiting scale formation. The experimental results in the laboratory indicate that the proper dose is
35 ppm when the concentration of calcium is 1000 mg/L and of magnesium is 2800 mg/L. The pH of the feed water
was in the range of 39. The efficiency of calcium scale inhibition of PAP-1 is higher than 97.24% and magnesium
scale inhibition is higher than 98.63% with 9 ppm PAP-1. The test performed at the Dalian seawater RO plant
confirmed the scale inhibition ability of PAP-1 compared with the Nalco PermaTreat 191 scale inhibitor. The results
from both antiscalants were similar. The average scale formation rates of calcium and magnesium of 14 samples was
2.822 g/h and 5.562 g/h separately with the addition of PAP-1 in each membrane unit; PAP-1 was more effective than
Nalco PermaTreat 191. At the same time, the algae growth inhibition test showed that the addition of PAP-1 does not
affect the growth of algae, which is an indication that PAP-1 has no toxicity and is a suitable and environmentally
friendly antiscalant.

Keywords: Membrane scaling; Antisclant; RO; Desalination

1. Introduction Desalination of seawater by RO to produce fresh


water has also been widely used in China. Several
The application of reverse osmosis (RO) for
seawater reverse osmosis (SWRO) plants of
desalination of seawater has increased rapidly
30005000 t/d have been constructed in Dalian,
with the construction of large RO plants [1,2].
China.
*Corresponding author.

0011-9164/06/$ See front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2005.11.024

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238 H.-Y. Li et al. / Desalination 196 (2006) 237247

The RO system has become an integral part to of treating the water in tanks to which lime and
the production of potable water and ultrapure soda ash are added. The added lime reacts with
water in industry. It is planned that more than bicarbonate to produce CaCO3 sludge.
200,000 t of fresh water will be produced from One of the most common methods used to
seawater every day before 2010 in Dalian. prevent or control the scaling of different salts in
However, problems that affect the performance of seawater feed is the addition of scale inhibitors.
membranes and the application of RO still exist. Antiscalants have been widely applied for many
High cost is a major one; another critical problem years in RO membranes to prevent scaling and
that affects the operation of SWRO plants is improve RO plant performance and have proven
membrane scaling. The third problem is the effect to be an efficient measure. At present, there are
of brine seawater to the sea environment because various antiscalants on the market, but most of
several chemicals are added to the pretreatment them have problems such as high cost and serious
process. environmental influence, which have been the
Membrane scaling is caused by the precipi- focus of attention. It is calculated that the cost of
tation of unsoluble salts as feedwater is converted chemicals accounts for about 10% in the pro-
to brine [36]. The concentration effect generated duction of fresh water in Dalian. Therefore, it is
by the separation of a pure water stream from important to reduce the cost of antiscalants and
seawater leads to a supersaturation state for reduce their harm to environment. The decrease
sparingly soluble species such as CaCO3, CaSO4, of chemical costs can reduce the cost of product
Ca2(PO4)3, Mg(OH)2, MgCO3, Mg2(PO4)3, BaSO4, water and promote the development of seawater
SrSO4 and so on. This leads to precipitation of desalination.
scale deposits on the membrane surface, which The seawater in China is different from that of
greatly impairs the performance of RO desali- Middle East [1]. The TDS of Dalian seawater is
nation systems [7]. Scale on the membrane sur- lower. Analysis indicates that the concentration of
face results in a progressive decline in perfor- calcium, magnesium, barium, strontium and sili-
mance such as reduction in the permeate flux [8], con in Dalian seawater is all lower than that of
a decrease in salt rejection, increase in energy the Arabian Sea region. The scaling sample
consumption and a high cleaning frequency. If analysis of the Dalian RO desalination plant also
allowed to develop sufficiently, membrane scal- shows that the content of calcium and magnesium
ing can lead to destruction of the membrane scale makes up almost all the inorganic scale;
(membranes represent 2030% of the capital of none of the other sparingly soluble species are
the plant) [9]. found in the scale. Calcium and magnesium scale
Membrane scaling can be prevented by four becomes an important factor that affects the
methods [1012]. The first is acidification. The operation of RO in Dalian, China.
acid consumes part of the bicarbonate in the feed A new antiscalant was developed by using
and converts it to carbon dioxide. The second is laboratory tests and field trials in the Dalian sea-
the scale inhibitor method where scale-inhibiting water RO desalination plant. Test results indicate
chemicals are used to alter the physical or chemi- that the new antiscalant, PAP-1, is environmen-
cal nature or the growth mechanisms of precipi- tally friendly, biodegradable and efficient.
tation and prevent scaling until the brine stream
leaves the RO system. The third method depends
on operating the RO system at low recovery 2. Experimental
where the solubility problems are not encoun- The experimental work was carried out in four
tered. The last method is softening which consists successive stages. In the first stage, membrane
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H.-Y. Li et al. / Desalination 196 (2006) 237247 239

scaling was analyzed by SEMEDS and XRD; but aluminum in the seawater is low, which may
then the feedwater chemistry composition of have been introduced by the flocculation process.
Dalian seawater was examined. In the second In this study, the concentration of calcium and
stage the new PAP-1 antiscalant was synthesized magnesium was selected as indicators to inves-
and tested by IR and viscometry in the laboratory. tigate the effect of scale inhibition on this kind of
In the third stage, a performance test of PAP-1 calcium and magnesium-containing scale.
and its influence on the growth of algae was done
in the laboratory and the biodegradability of
2.2. Feedwater chemistry composition
PAP-1 was evaluated. Lastly, the performance of
PAP-1 compared to Nalco Permatreat 191 was Table 1 shows the typical chemistry compo-
studied at the Dalian SWRO desalination plant. sition of RO feedwater in the Dalian RO plant by
laboratory analysis. Calcium, magnesium, chlo-
ride, sulfate, total hardness, and total alkalinity
2.1. Membrane scale analysis
were measured with titration; iron, silicon dioxide
Fig. 1 shows the membrane scale analysis of and orthophosphate with spectrophotometry; bar-
the Dalian RO desalination plant by SEMEDS. ium, strontium, sodium and potassium with ato-
Cl and Na elements are especially high in the mic absorption spectrometry. Total dissolved
scale, perhaps caused by adsorption of Cl and Na solids were measured by a TDS instrument.
ions on the scale. The content of calcium and
magnesium scale is relatively high among the
2.3. Synthesis of PAP-1
sparingly soluble species. Further examination
using the X-ray diffraction (XRD) spectrum has PAP-1 was synthesized in our laboratory
demonstrated (data not shown) that there were no according to the following approach. First 50.00
peaks to indicate the crystallization structure, doses maleic anhydride was dissolved in 25 doses
suggesting that the scale is amorphous. From the water, then 100 doses 30wt% aqueous ammonia
figure, the main unsolved salts such as CaCO3, hydroxide was added slowly, the reaction last for
CaSO4, Ca2(PO4)3, MgCO3, Mg2(PO4)3 and 6h at 80-85 , then the temperature was increased
Mg(OH)2 probably exist in the membrane scale. to 220 and held at that temperature for about 7 h,
The element aluminum also exists in the scale, a dark, yellow brittle product was obtained.

Fig. 1. SEMEDS analysis for membrane scaling.


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240 H.-Y. Li et al. / Desalination 196 (2006) 237247

Table 1
Typical seawater analysis in Dalian, China

Ion Concentration (mg/L)


Calcium 377.75
Magnesium 1274.50
Barium 0.01
Strontium 0.45
Iron 0.38
Sodium 9854
Potassium 474.30
Silicon dioxide 0.51
Fig. 2. IR spectrum of PAP-1.
Chloride 18072
Sulfate 2270.25
Orthophosphate 0.14 Table 3
Total hardness (CaCO3) 6254.79 Composition of the simulated concentrated seawater
Total alkalinity 122.37
Total dissolved solid 39012.27 Calcium, mg/L as Ca 1000
pH 7.65 Magnesium, mg/L as Mg 2800
Chloride, mg/L as Cl 36950
Sodium, mg/L as Na 20000
Table 2 Bicarbonate, mg/L as CO32- 350
Analysis of characteristic peaks in IR spectrum Sulphate, mg/L as SO42- 5800
Potassium, mg/L as K 950
Wave numbers (cm!1) IR spectrum analysis pH 7.76
3387.96 O-H stretching vibration
1712.11 C=O stretching vibration
1642.43 C=O stretching vibration acids compound was added to the PASP, and the
1551.60 N-H bending vibration mixture reaction continued for 6 h at 50EC. When
1183.54 C-N stretching vibration it was transparent, the synthesis process of PAP-1
1042.22 C-O stretching vibration was completed. Its comparative molecular weight
is between 3000 and 6000 tested by viscometry.
The IR spectrum of the PAP-1 is shown in Fig. 2.
Then the product (about 30 doses) was slurried in An analysis of characteristic peaks in the IR
40 doses of water and the slurry stirred. Sodium spectrum is shown in Table 2.
hydroxide (about 25 doses of 50% wt/wt solu-
tion) was added to the stirred slurry at a rate so
2.4. Performance test in the laboratory
that the slurry temperature did not exceed about
80EC, and the pH value of the slurry did not The scale-inhibiting performance for calcium
exceed about 9.5. After the sodium hydroxide and magnesium-containing scale was evaluated in
solution addition was complete, sufficient water static experiments, also known as beaker experi-
was added to provide a solid concentration of ments. This method used simulated concentrated
about 42 wt%, constituted substantially by the seawater as shown in Table 3. The evaluation was
hydrolyzed product. Polyaspartic acid (PASP) also conducted in parallel tests under carefully
was produced. At last, a kind of polycarboxylic controlled conditions.
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H.-Y. Li et al. / Desalination 196 (2006) 237247 241

2.4.1. Calcium scale inhibition test 2.5. Algal growth inhibition test
This test was designed to measure the anti- This test was used to assess the toxic effects of
scalants ability to inhibit scale formation. The PAP-1 towards aquatic algae. The algal growth
soluble calcium was determined by titration with inhibition test was performed using the Chlorella
EDTA. autotrophica. The algal cells were cultured in test
Tests were made with 1.00, 2.00, 3.00, 4.00, tubes using the culture medium at 25EC under
5.00, 7.00, and 9.00 ppm PAP-1. A blank solu- continuous illumination. This test was carried out
tion was also prepared containing no PAP-1. with 0.00, 1.00, 2.00, 3.00, 4.00, 5.00, 7.00, and
Simulated concentrated seawater (200 mL) was 9.00 ppm PAP-1 in eight culture flasks with
poured into the beaker, the PAP-1 was added and almost the same algae present and the culture
pH was adjusted using NaOH and HCl solutions. medium under the same conditions; the total
Then the beakers were put into a water bath for solution volume was 100 mL in the flasks. Inhi-
8 h at 80EC. When titrating the concentration of bition of the algal growth relative to the blank
calcium in the solution, it was first filtrated and sample was determined by measurements of opti-
then diluted to 200 mL. The calcium scale cal density in a spectrophotometer at a wave-
inhibition test was done at different pHs: 3.00, length of 670 nm and the content of chlorophyll-a
4.00, 5.00, 6.00, 7.00, 8.00, 9.00. This test was (ch-a). Both of the two methods were widely used
repeated three times, and the final result was the to indicate the growth of algae [13]. All details of
average. To calculate the percentage inhibition of the test protocol of ch-a were described in
PAP-1, the following equation was used [6]: GB17378.7-1998, China. The 24 h, 48 h, 72 h
(1) and 168 h values of optical density and ch-a were
Ca 2+ Ca 2+
% inhibition = antiscalant blank
100 measured to calculate the growth of algae.
Ca 2+ Ca 2+
original blank

2+
where [Ca ]antiscalant is the concentration of soluble 2.6. Percentage biodegradability test
Ca2+ in an antiscalant-containing solution (mg/L), Percentage biodegradability of PAP-1 was
[Ca2+]original is the concentration of soluble Ca2+ in evaluated by the shaking-bottle incubating test
the original solution (mg/L), and [Ca2+]blank is the [14]. Test mixtures included activated sludge,
concentration of soluble Ca2+ in a blank solution inorganic salts inoculum and the test compound
(mg/L). The higher the percentage inhibition, the PAP-1. At the same time, blank solutions with
better the scale inhibition ability of the calcium only inoculum were prepared. The test mixture
scale. was mixed by shaking at 120 rev/min and
incubated at a constant temperature of 30EC. The
2.4.2. Magnesium scale inhibition test test lasted for 28 days. Both the potassium
The experiment method was the same for the permanganate index (CODMn) of test mixtures
calcium scale inhibition test. The concentration of and blank solutions at day 1, 4, 8, 12, 16, 20 and
total hardness and calcium were determined by 28 were measured to calculate percentage biode-
titration with EDTA. The soluble magnesium was gradability. The following equation was used:
calculated. To calculate the percentage inhibition
of PAP-1, its equation was:
(%) = 1
(
COD nMn ) 100% (3)
% inhibition =
Mg 2+
antiscalant
Mg 2 +
blank

(2)
100
(
COD1Mn )
Mg 2+ Mg 2+
original blank where n is the number of incubating days; n is
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242 H.-Y. Li et al. / Desalination 196 (2006) 237247

Fig. 3. Process scheme for the RO installation of the field trial.

the percentage biodegradability; (CODMnn) is the Table 4


(CODMnn) of the test mixture minus (CODMnn) Operational parameters of RO installation (units 1 and 2)
of the blank solution; (CODMn1) is the original
Recovery, % 40%
(CODMn1) of test mixture minus (CODMn1) of the
Feedwater conductivity after 45,80047,500
blank solution at the start of the test. filtering, s/cm
Feed flow, m3/h 5657
2.7. Performance test in the RO desalination Product flow, m3/h 2223
Reject flow, m3/h 3435
plant
Pressure of high-pressure pump, bar 51
Based on the satisfactory results in the Salt rejection, % 99.5
laboratory, in the subsequent stage the test was Number of membrane units 96
performed in a seawater RO desalination plant in Feed pressure of RO membrane, bar 51
Dalian for 6 months. The plant consists of two
parallel RO units, both single-stage RO systems.
Each unit was fitted with an antiscalant injection carried out. The random samples of feed, reject
system. Fig. 3 gives the schematic diagram of the and product were analyzed, and simultaneously
RO unit. Operational parameters are listed in scale formation rates of calcium and magnesium
Table 4. were calculated.
The Nalco PermaTreat 191 antiscalant, which
had already been widely applied in scale inhi-
2.8. Calculation of scale formation rates of
bition, was used in Unit 1, while PAP-1 was used
calcium and magnesium
in Unit 2. And the effectiveness of PAP-1 in
controlling scale formation was compared with The method to monitor the performance of
Nalco PermaTreat 191 under the same operating two different antiscalants was the calculation of
conditions. A direct comparison of the perfor- scale formation rates of calcium and magnesium
mance characteristics of the two antiscalants in in the RO system. The lower the scale formation
inhibiting calcium and magnesium scale was rates of calcium and magnesium, the better the
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H.-Y. Li et al. / Desalination 196 (2006) 237247 243

antiscalants performance. To calculate the total To calculate the experimental standard deviation
scale formation rate of the entire RO system, the in the scale formation rates of calcium and
following equation was defined: magnesium, the Bessel formula can be deduced
M C0V0 C1V1 C2V2 as:
= = (4) 1 n
t 1000 t ( 0 i 0 )

2
S2 =
n 1 i =1
When recovery is Y, V1 is equal to (1!Y) times
of V0, and V2 is equal to Y times of V0. Thus, we where S is the experimental standard deviation, n
can deduce the following equation: is the total number of scale formation rate value,
0i is each scale formation rate value separately
V0 C0 (1 Y ) C1 YC2 (g/L), and 0 is the average of all scale formation
= rate values (g/L).
1000 t
Q t C0 (1 Y ) C1 YC2 (5)
3. Results and discussion
t
The SEMEDS analytical results of membrane
= Q C0 (1 Y ) C1 YC2
scaling and composition of Dalian seawater are
where is the total scale forming rate of calcium listed in Fig. 1 and Table 1. It was found that the
or magnesium in the RO system (g/h); C0, C1 and content of barium, strontium and silicon dioxide
C2 are the concentrations of feed, reject and is low in Dalian seawater. From the analysis of
product of calcium or magnesium (mg/L); V0, V1 membrane scaling at the Dalian RO desalination
and V2 are the volume of feed, reject and product plant, it was also found that inorganic scaling is
(L); and Q is the feed flux of the RO system mainly composed of magnesium and calcium-
(m3/h), and t is the running time of the RO containing scale; other soluble species such as
system (h). barium, strontium and silicon were not present. It
Generally, the RO system is composed of can be predicted that magnesium and calcium
many identical membrane units. If the number of scale is the crucial factor affecting the perfor-
membrane units is N, for each membrane unit in mance of RO membranes at the Dalian RO plant.
the RO system, the scale formation rate can be The amount of magnesium scale was larger than
calculated as follows: calcium scale. The proportion between magne-
sium and calcium was nearly 2 to 1.
Q C0 (1 Y ) C1 YC2 Figs. 4 and 5 show calcium and magnesium
0 = = (6) scale inhibition percentages with different doses
N N of PAP-1 at different pHs. The results reveal that
when pH is low, the possibility of forming
2.9. Calculation error in test calcium and magnesium scale is smaller, so the
low dose of PAP-1 displays excellent efficacy.
The experimental standard deviation was
With the increase of pH, the inhibition percentage
calculated to evaluate errors in the real test. It
declines somewhat when the dose of PAP-1 is the
followed the Bessel formula:
same. The proper dose of PAP-1 varies with the
1 n change of pH. When pH is 3, the efficiency to
( xi x )
2
S2 = (7)
n 1 i =1 inhibit scale formation reached 100% with 3 ppm
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244 H.-Y. Li et al. / Desalination 196 (2006) 237247

Fig. 4. Calcium scale inhibition percentage of different Fig. 6. Optical density with different concentrations of
doses of PAP-1 at different pHs. PAP-1.

Fig. 5. Magnesium scale inhibition percentage of dif- Fig. 7. ch-a with different concentrations of PAP-1.
ferent doses of PAP-1 at different pHs.
Fig. 8 shows that percentage biodegradability
PAP-1. When the pH is 9, the calcium scale of PAP-1 reached 38.25% at day 8 and 58.3% at
inhibition percentage of PAP-1 was 97.24% with day 20. PAP-1 was easily biodegraded under the
9 ppm PAP-1 and magnesium scale inhibition test conditions. PAP-1 degraded quickly between
percentage was 98.63%. day 1 and 12; then the degradation rate began to
Using the optical density and the concen- slow, and lastly was turned into a plateau phase
tration of Ch-a as indicators of the growth of on day 20 to the end of the test at day 28.
algae, Figs. 6 and 7 show the effect of PAP-1 on According to the results from this study,
the growth of algae. Eight different concentra- PAP-1 is an environmentally friendly antiscalant.
tions under a concentration of 9 mg/L of PAP-1 Figs. 9 and 10 show the different scale forma-
were applied and the effect was tested after 0, 24, tion rates of calcium and magnesium in each
48, 72 and 168 h. The results indicate that the membrane unit separately compared with two
growth of algae is not limited by PAP-1. kinds of scale inhibitors used in the same RO
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H.-Y. Li et al. / Desalination 196 (2006) 237247 245

Table 5
Experimental standard deviations in the calculation of the
real test

RO system (S2) #1 unit #2 unit

Calcium scale formation rate 0.048 0.142


in each membrane unit
Magnesium scale formation rate 0.488 0.239
in each membrane unit

desalination plant. The results from the plant


performance show that the scale formation rate of
Fig. 8. Percentage biodegradability of PAP-1 vs. days. calcium of Unit 2 in each membrane unit is lower,
which indicates that PAP-1 has a better calcium
scale inhibition capacity. The average scale
formation rate of calcium for 14 samples in
Unit 2 was 2.822 g/h, lower than Unit 1 whose
average scale formation rate was 3.585 g/h.
The results in Fig. 8 demonstrate that magne-
sium scale formation rates in each membrane unit
of both antiscalants are higher owing to the larger
concentration of magnesium in seawater than
calcium. Thus, the content of magnesium scale in
the membrane scaling was more than calcium
scale. The average scale formation rate of mag-
nesium from 14 samples in Unit 2 was 5.562 g/h,
Fig. 9. Comparison of calcium scale formation rate a little lower than Unit 1 whose average scale
between #1 and #2 RO units. formation rate was 5.849 g/h.
The experiment in the RO plant confirmed the
scale inhibition ability of PAP-1. Therefore, it
can be established that PAP-1 is successful in
controlling scale formation at the tested condi-
tions and performance is quite good. The cal-
culation error is given in Table 5.
Fig. 11 shows the variation in product con-
ductivity and feed pressure of RO membranes
monitored in the plant for both RO units. The
results show almost a constant and stable value of
product conductivity for both inhibitors without
a large change from the initial operation con-
ditions. The value of product conductivity varied
Fig. 10. Comparison of magnesium scale formation rate between 187 s/cm and 206 s/cm. The feed-
between #1 and #2 RO units. water conductivity after filtering was 45,800
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246 H.-Y. Li et al. / Desalination 196 (2006) 237247

Fig. 11. Product conductivity and RO membrane mean


pressure vs. day.

47,500 s/cm. Salt rejection is above 99.5%. The The tests performed at the Dalian SWRO
stability of PAP-1 is proven. The test performed desalination plant confirmed the scale inhibition
at the SWRO desalination plant in Dalian was ability of PAP-1 compared to other scale inhi-
conducted continuously for 6 months, during bitors. The average scale formation rates of
which the operation was smooth and steady. Feed calcium and magnesium from 14 samples were
pressure of the RO membranes is also shown in 2.822 g/h and 5.562 g/h separately with the
Fig. 9. The feed pressure of RO membranes was addition of PAP-1 in each membrane unit.
maintained at 51 bar at all times in the two RO The value of product conductivity varied
units. Product flow did not vary greatly, and the between 187 s/cm and 206 s/cm. Feedwater
values varied from 22 to 23 m3/h. This also conductivity after filtering was 45,800
proved the capability of PAP-1. 47,500 s/cm. Salt rejection was above 99.5%.
PAP-1 is a suitable and environmentally friendly
antiscalant.
4. Conclusions
Through the scale inhibition experiments in
Acknowledgement
the laboratory, PAP-1 proved to be effective in
inhibiting scale formation. The proper dose is The authors would like to acknowledge the
35 ppm when the concentration of calcium is support of the seawater RO desalination plant in
1000 mg/L and concentration of magnesium is Dalian and Dr. Hou for the test.
2800 mg/L according to the different pHs. When
pH was 3.00, scale-inhibiting efficiency reached
100% with 3 ppm PAP-1. While pH was 9.00, the References
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