Journal of Petroleum Science and Engineering 166 (2018) 283–289

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Journal of Petroleum Science and Engineering

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Cleaning of ceramic membranes for produced water filtration

T. Zsirai a, H. Qiblawey b, P. Buzatu a, M. Al-Marri a, b, S.J. Judd a, c, *
a
Gas Processing Center, Qatar University, Qatar
b
Department of Chemical Engineering, Qatar University, Qatar
c
Cranfield Water Science Institute, Cranfield University, United Kingdom

A R T I C L E I N F O A B S T R A C T

Keywords: The application of ceramic microfiltration membranes to the tertiary treatment of produced water from an
Produced water Arabian Gulf oilfield has been studied using a dedicated pilot plant. Studies were based on a previously published
Ceramic membranes protocol in which the retentate stream was recycled so as to successively increase the feed concentration
Chemical cleaning throughout the experimental run. Chemical cleaning in place (CIP) was applied between each run and the flux and
Footprint permeability recovery recorded for various cleaning protocols studied, the CIP being based on the combination of
Flux
caustic soda (NaOH) and citric acid. Surface analysis of the membrane, and specifically its hydrophilicity, was also
conducted.
Results indicated the main influencing factor on permeability recovery from the CIP to be the employment of
backflushing during the CIP itself. A final flux of 700 L m
2 h
1 was sustained through the application of 6 wt%
NaOH with 6 wt% citric acid combined with backflushing at approximately twice the rate of the filtration cycle
flux. A consideration of the impact of this flux value on the viability of two commercially-available ceramic
membrane technologies indicated the footprint incurred to be slightly lower than that of the upstream induced gas
flotation technology and corroborated a previously published estimate. The flux was sustained despite surface
analysis indicating a loss of the innate hydrophilicity of the ceramic membrane.

1. Introduction MF membrane was shown to provide a significantly higher flux than the
UF membrane, but was also subject to greater flux (and permeability)
Produced water (PW) generated from oil exploration requires decline. Moreover, it was noted that there was a marked deterioration in
rigorous removal of suspended matter (free oil and particulate solids) as both permeate water quality and permeability with successive experi-
tertiary treatment (downstream of hydrocyclone and gas flotation) if it is mental runs on the chemically-cleaned membrane. The work emphasised
to be desalinated for reuse (Alzahrani et al., 2013) or re-injected into the need to improve the efficacy of the chemical clean-in-place (CIP)
low-permeability reservoirs (Judd et al., 2014; Xu et al., 2016). The applied between runs to recover both the permeability and selectivity of
application of membrane technology for this duty has been recently the membrane.
reviewed (Munirasu et al., 2016; Dickhout et al., 2017), and the option of The current paper reports a series of trials conducted to identify the
ceramic membrane filtration widely explored (Ebrahimi et al., 2010; optimal protocol for applying a CIP so as to sustain a viably high
Guirgis et al., 2015; Weschenfelder et al., 2015, 2016). permeate flux. The impact on the technology footprint was then deter-
The viability of membrane processes generally is largely dependent mined, using a previously published protocol (Judd et al., 2014), based
on sustaining a high membrane flux to minimise the process footprint, a on the specifications of two commercially-available candidate ceramic
particularly important attribute on offshore oil platforms where available membrane filtration systems for tertiary PW treatment.
space is at a premium. The use of silicon carbide (SiC) ceramic mem-
branes for this duty has been demonstrated to provide a reliably high 2. Materials and methods
treated water quality (6.3–7.6 mg/L oil and grease (O&G), 4–8 NTU
turbidity) for microfiltration (MF, pore size 2 μm) and ultrafiltration (UF, The pilot plant operation methodology has been described previously
pore size 0.04 μm) membranes based on recent pilot-scale studies (Zsirai (Zsirai et al., 2016). The pilot plant (Fig. 1) and membrane elements were
et al., 2016) using real PW from an offshore oil platform. The larger-pore supplied by Liqtech International (Ballerup, Denmark), the membranes

* Corresponding author. Gas Processing Center, Qatar University. Qatar.

E-mail address: [email protected] (S.J. Judd).

https://doi.org/10.1016/j.petrol.2018.03.036
Received 28 May 2017; Received in revised form 5 March 2018; Accepted 6 March 2018
Available online 9 March 2018
0920-4105/© 2018 Elsevier B.V. All rights reserved.
T. Zsirai et al. Journal of Petroleum Science and Engineering 166 (2018) 283–289

Fig. 1. Pilot plant.

having been pre-conditioned through their used for 15–17 trials in a were not immediately re-deposited onto the membrane surface by the
previous campaign prior to the commencement of the current study. The flow of cleaning reagent. Reagents employed comprised an organic acid
plant comprised two streams fitted with tubular membrane modules (citric acid), supplemented with sulphuric acid to lower the pH to 2, and
operated in crossflow mode. The plant allowed operation at a fixed caustic soda at pH 13 (Table 1). Whilst both base-acid and acid-base
conversion with automated physical cleaning provided by backflushing sequential cleaning were initially studied, no apparent consistent
and manually-applied chemical cleaning in place (CIP). Experimental change was noted between the two sequences. The feedwater quality and
runs were conducted with recirculation of the retentate (the concentrate CIP protocols employed for the trials conducted based on two different
stream from the membrane), intended to increase the feedwater sus- batches of PW, denoted by trials 1–3 (Batch 1) and a-e (Batch 2), are
pended oil and solids concentration over the course of the run and so summarised in Table 2, the increase feed concentration arising from the
increase the challenge to the membrane. All runs were operated at a recirculation of the retentate.
transmembrane pressure of 0.55–0.6 bar with backflushing for 5 s every Surface analysis of the virgin and used membrane material was by
600 s at a back-pressure of 3 bar and a filtration cycle conversion of 20%, contact angle measurement, conducted according to standard methods
these conditions having been identified as being optimal in previous (APHA, 2001), to assess the surface hydrophobicity. SEM-EDAX mea-
studies (Zsirai et al., 2016). The selection of the cleaning reagents was surements were also made to assess the extent of formation of calcium,
similarly based on this study. barium and iron alkaline scales. The autopsies were intended to provide
Experiments were conducted on single MF and UF SiC membrane an indication of the degree of permanent fouling from oil and inorganic
elements (25 mm diameter, 305 mm long, 37 channels of 3 mm square reagents. Analysis for turbidity and oil and grease (O&G) was according
and with a total membrane area of 0.09 m2) which were chemically to standard methods (SMWW 2130 B and 5520 C).
cleaned between runs. The MF and UF membranes were rated as 2 μm
and 0.04 μm pore size respectively. The elements were challenged with 3. Results
PW shipped in 5-tonne batches from an oil platform operating in the
Arabian Gulf, two different batches being employed throughout the trials The flux and permeability profiles followed the same trends as in
with the PW nitrogen-blanketed to suppress oxidation. The PW was previous studies (Zsirai et al., 2016), with the flux decline over the
sampled downstream of the induced gas flotation (IGF) step of the PW filtration cycle and recovery during the backflush cycle both decreasing
treatment train of the oil platform, the train being based on a classical with time (Fig. 2). As outlined in previous work, the end permeability
two-stage hydrocyclone-IGF process. The work was limited to eight runs refers to the permeability resulting from the same hydraulic load and, if
conducted on the two preconditioned membrane elements. based on the same PW batch, roughly the same pollutant load between
Experiments were conducted on 200 L feed volumes of PW with tests. The start and end permeabilities between tests (respectively the
retentate recycling throughout which served to agitate the feed by jet green and red bars in Fig. 3) are therefore directly comparable.
mixing during the experimental run. Further jet mixing of the storage Results indicate a significant difference in fouling propensity between
tanks was conducted prior to dispensing of the 200 L volumes to ensure the two batches. There are a number of possible explanations for this,
an even dispersion of the oil and solids in the stock solution. Chemical including an approximate doubling of the O&G content and more than
cleaning in place (CIP) studies were then carried out between each order of magnitude increase in turbidity (Table 2). It is also possible that
filtration run according to a multiple-stage protocol (Table 1), applying Batch 2 had a higher concentration of organic matter of higher fouling
supplementary backflushing during the CIP for the final three runs (c – e). propensity. This would include production chemicals based on flocculent
The backflushing was designed to help ensure that any dislodged solids polymers, which are known to foul polymeric membranes though are less
onerous to ceramic materials. However, the very significantly higher
colloidal content, manifested as the turbidity, is the most likely cause of
Table 1 the decreased end permeability from Run 3 to Run a for the MF mem-
Cleaning-in-place procedure. brane (Fig. 3b). This is corroborated by the far less significant corre-
Reagent, ~50 L aliquots Recirculation time and temperature
sponding decrease for the UF membrane (Fig. 3a), which would be
expected to be more resistant to colloidal fouling.
1. Mains water 30 min at ~25  C
Notwithstanding differences in fouling propensity of the two batches
2. 6% NaOH 30 min at pH 13
3. Mains water 30 min at ~25  C the greatest impact on sustaining permeability is from the application of
4. 6% citric acid 30 min at pH 2 backflushing during the CIP (Runs c-e) for both the UF and the MF
5. Mains water 30 min at ~25  C membranes, although for the final UF run the CIP failed to recover the

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Table 2
Feed water quality and CIP conditions.
Run Feed O&G Feed turbidity Cleaning reagents Cleaning BF

Start End Start End NaOH Citric acid sequence

1–3 24–25 32–84 21–34 39–74 2% 2% B-A N

a 52 148 123 202 2% 6% A-B N
b 40 76 99 158 6% 2% A-B N
c 47 52 72 461 2% 2% A-B Y
d 50 95 408 955 2% 6% A-B Y
e 42 93 663 998 6% 2% A-B Y

Runs 1–3 refer to Batch 1, Runs a-e refer to Batch 2; B-A base followed by acid; A-B acid followed by base; BF backflush during CIP.

Fig. 2. Typical filtration transient: flux and pressure transient from the first (a) and the last hours (b) of the concentration test.

permeability (Fig. 3a). In the case of the MF a final permeability of be- in keeping with the outcomes of the previous study employing the same
tween 1190 and 1280 LMH/bar was sustained for the three runs protocol (Zsirai et al., 2016). The use of the backflush during the CIP also
(Fig. 3b), with the CIP recovering the permeability to 1480–1630 LMH/ appeared to stabilise the permeate turbidity to <25 NTU, corresponding
bar for the start of the following run. This compares with final perme- to >98% removal which is assumed to take place at the membrane sur-
abilities of 210–310 LMH/bar for Runs a and b, prior to the introduction face. The rejection provided by the MF membrane following the back-
of backflushing during the CIP. In the case of the UF membranes the flushed CIP was slightly higher than that of the UF for both turbidity and
corresponding final permeability values were 367–384 LMH/bar for the O&G, which is counter-intuitive given the significantly higher selectivity
backflushed CIP tests compared with 202–232 LMH/bar prior to the expected for the UF membrane given the rated pore size.
introduction backflushing during the CIP. The increased efficacy of the The membrane autopsy indicated only negligible quantities of inor-
backflushed CIP was thus almost four times greater for the MF membrane ganic scalants and metal hydroxides (calcium and iron) on the membrane
compared to the UF. surface for both the MF and UF membranes, as might be expected given
A mean treated water quality of <7.1  1.6 mg/L O&G (oil and the strength and rigour of the acid cleaning sequence of the CIP. This was
grease) in for the UF membrane and 8.5  1.6 mg/L for the MF was despite the PW being heavily supersaturated with hardness (between 9
maintained throughout. This arose despite the increase in feed water and 15 g L
1 as CaCO3). However, the surface was evidently affected by
O&G concentration and the impact of recycling of the retentate, and was contact with the oil, with the contact angle measurements

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Fig. 3. Permeability trend with successive experimental runs (a) UF, and (b) MF.

(θ ¼ 106–116 ) indicating significant hydrophobicity for the used run. A final flux of around 700 LMH was correspondingly sustained for
membranes, compared with complete hydrophilicity (θ ¼ 0 ) for the the MF membrane, notwithstanding the loss of membrane surface
virgin membrane material. It can therefore be surmised that the decline hydrophilicity.
in permeability is primarily attributable to the oil content of the PW,
rather than the inorganic scales. Since the membranes had already been 4. Discussion
used for a number of tests prior to the current study (Section 2) it is likely
that they were in a hydrophobic state throughout the campaign. There have a number of studies of the application of ceramic mem-
Examination of the filtration transients for Runs c-d, where back- brane technology to the treatment of real petroleum industry wastewa-
flushing during the CIP was applied, indicated a negligible permeability ters reported since 2010 (Table 3). Few of these have been conducted at
decline between backflush events for the final 5–7 backflushes of each pilot scale, challenged with real oilfield produced water (OFPW), and/or

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Table 3
Studies of MF/UF membrane filtration of PW and other petroleum effluents.
Oil (TSS) concn mg/L, Scale Material Pore size Init flux, Fin flux, TMP, bar Fin perm (range), time, T,  C Reference
water source μm LMH LMH LMH/bar h

200–1000, tank b(m) AlO 0.2 128 28 1 28 2 60 Ebrahimi et al., 2010

dewatering effl
200–1000, tank b(m) TiO 0.05 80 4 1 <5 2.5 60 Ebrahimi et al., 2010
dewatering effl
200–1000, tank b(m) 120 30 1 120–30 2 60 Ebrahimi et al., 2010
dewatering effl
OFPW p TiO, SiC 0.01–0.1 200 - 0.5–3.5 60 120 – Pedenaud et al., 2011
0.25–1.5 135
221–722 (7–17), OFPW p SiC 0.04–0.1 - 135–590 0.35–0.95 450–1020 26 – Prado-Rubio et al., 2012
20 (2.9), OFPW 0.6 520
3–25 (24–74), OFPW p SiC 0.1–0.5 25–120 50 0.3–1.5 150 12–14 45 Cometas, 2011
52–458, gas field PW p Al-Zr 0.05 - 170–255 – 190–240 600 25 Subramani et al., 2011
-, SAGD effl p AlO 0.05 200 – 1.52 132 – 45 Guirgis et al., 2015
~250, refinery effl. b ZrO 0.1 1000 290 1.5 193 – 45 Weschenfelder et al., 2015
9–43, PW p AlO 0.2 - 295–312 2.5 118–125 – 35–60 Reyhani and Mashhadi
Meighani, 2016

KEY: LMH litres per m2 per hr; SAGD Steam-assisted gravity drainage; OFPW oilfield produced water; TMP transmembrane pressure; TSS total suspended solids; b
bench; b(m) bench, based on membrane module; p pilot; AlO aluminium oxide; SiC silicon carbide; TiO titanium oxide; ZrO zirconium oxide.

operated for a significant period of time. An early site-based trial (Lee and otherwise potentially appropriate for reinjection into the reservoir or
Frankiewicz, 2005), apparently employing a spiral-wound hydrophilic overboard discharge. The retentate stream would be expected to have a
polymeric membrane, achieved a flux of 10–20 LMH and maximum similar composition to that of the return stream of the upstream IGF, and
permeabilities of 6–8 LMH/bar after an extended operating period of could thus be managed in a similar manner.
650 h. Since then somewhat higher fluxes and permeabilities from
similar site based trials using ceramic membranes have been reported,
ranging from 60 (Pedenaud et al., 2011), to more than 1000 LMH/bar 4.2. Footprint
(Prado-Rubio et al., 2012) depending on the feedwater quality and the
state of the membrane (Table 3). The footprint of classical and tertiary PW treatment processes has
However, it is evident that the sustainable flux attainable is greatly been determined with reference to flow normalised against the area (FA)
dependent on the CIP efficacy. Permeability recoveries varying by factors and volume (FV) occupied. FA thus takes units of m/h: m3/h per square
of 2–3 have been reported from pilot plant studies based on real PW metre of floor area in m2. FV correspondingly has units of h
1, it being the
(Prado-Rubio et al., 2012), with significant permeability reduction flow in m3/h per m3 volume occupied. A ceramic membrane skid based
ensuing from insufficiently cleaned membranes. A conclusion common to on vertically-aligned 1 m modules has been determined to have an area
all studies based on real petroleum effluents is the low membrane and volume footprint of ~7 m/h and ~2.6 h
1 respectively based on
permeability due to the gradual build-up of hydrophobic matter on or literature information (Judd et al., 2014), consistent with a
within the membrane material. Enhanced permeability recovery has recently-published study (Weschenfelder et al., 2016) in which a value of
been demonstrated both by adjustment of the physical cleaning (i.e. 6.5 m/h was determined for FA. This value is comparable with the
backflushing) conditions during the filtration cycle (Silalahi and Leiknes, nutshell filter (NSF) alternative tertiary technology in terms of floor area
2009) and by sequential base-acid cleaning (Weschenfelder et al., 2015). but more compact with respect to volume.
The current study suggests that further improvement in permeability To provide a more accurate estimation of the footprint demands
recovery can be attained through backflushing during the CIP, yielding a reference to existing commercial ceramic membrane technologies, of
final sustainable flux of around 700 LMH and a corresponding perme- which there are two which have been implemented for PW filtration: the
ability of ~1200 LMH/bar – somewhat higher than previously reported Liqtech International M99 skid and the Veolia Water Technologies
values (Table 3). ROSS™ system based on the company's Ceramem membranes. The Liq-
There are three aspects to the technical viability of the process for the tech technology comprises 99  250 mm diameter 0.328 m2 membrane
duty envisaged: area modules, compared with the Veolia technology which has
52  142 mm dia. 10.5 m2 modules. These data coupled with the skid
a Attainment of required water quality, dimensions for the respective technologies (Table 4) allow the packing
b Limitation to a maximum footprint, and density, the membrane surface area per unit skid footprint or volume, to
c Impact on operation of other PW process technologies. be determined. As can be seen, the two technologies are similar in
specification.
Determination of the footprint demands certain assumptions Determination of the FA and FV values for the two technologies
regarding process technology design/configuration and the flow and (Table 5) demands assumptions regarding both the conversion of feed-
loads on the oil platform respectively. water into permeate (taking account of the use of permeate for back-
flushing) and the redundancy arising from the requirement for taking a
4.1. Water quality stream off line for periodic chemical cleaning. Redundancy can be
assumed to be manifested as three skids each providing 50% of the flow
It is evident from all measured water quality data for the membranes capacity (i.e. duty-duty-standby), adding 50% to the footprint. Based on
tested that a high treated water quality is sustained regardless of the backflushing for 1% of the time at 150% of the operating flux, the
membrane material or pore size, the residual oil assumed to be in the adjusted conversion is calculated as being 92.5% assuming a conversion
dissolved form. Permeate quality values reported from other studies of 96% for the forward filtration cycle. The resultant net FA and FV values
suggest a total suspended solids (TSS) concentration below 5 mg/L, un- are calculated as being 7.2–7.8 m/h and 1.7–2.6 h
1 respectively. These
less the membrane has been made irreversibly hydrophobic (Prado-R- figures roughly corroborate the values of 7.0 m/h and 2.6 h
1 for FA and
ubio et al., 2012) causing breakthrough of free oil. The permeate water is FV originally estimated in the review article by Judd et al. (2014).

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Table 4
Technical specification of two commercial ceramic membrane filtration technologies.
Technology Skid dimensions, m Module Skid Packing densitya
2 2
L H W A, m No Am, m m2/m2 m2/m3

Veolia 18.3 2.7 1.8 33.5 52 10.7 556 17 6.1

Liqtech 1.2 4.5 1.5 1.80 99 0.328 32.5 18 4.0

A: skid floor area; packing density: membrane surface area per unit skid footprint or volume.
Am: membrane surface area.
a
With reference to skid.

Table 5
Footprint determination, based on two commercial ceramic membrane filtration technologies.
Techno-logy Uncorrected Corrected for Backflushing data Corrected for
redundancy backflushing

Flux FA FV FA FV Freq Flow Vol Conv-ersiona FA FV

1
m/h m/h h m/h h h/d 3
m /h m 3
m/h h
1

Veolia 0.7 11.6 4.2 7.8 2.8 0.24 584 140 92.5% 7.2 2.6
Liqtech 0.7 12.6 2.8 8.4 1.9 0.24 34.1 8.2 92.5% 7.8 1.7

Redundancy: three skids each providing 50% of the flow capacity (i.e. duty-duty-standby).
Ancillary equipment excluded: assumed to be comparable for each technology.
a
Assumes filtration cycle conversion of 96%, based on the experimental data for a conversion of 20% for the 300 mm element, feedwater pre-concentrated by a factor
of ~2.5, and two stages of 850 mm-long full-scale modules.

4.3. Impact filtration cycles, and appears to be sustained despite the tendency of the
ceramic membrane to become hydrophobic as the number of filtration
It would be expected that the treated water could either be discharged cycles (and so exposure to the PW free oil) increases.
overboard, provided the regulated discharge limits are based solely on A consideration of two commercially-available SiC-based technolo-
suspended matter and/or total oil (of 15 mg/L or more in the case of the gies, each fitted with vertical membrane modules, indicates that a flow
latter), or used for reinjection (PWRI). Whilst the high permeate water per unit membrane skid area footprint of 12–14 m/h (or 2.8–4.2 h
1 per
quality generated is generally considered to be appropriate to PWRI, the unit volume occupancy) can be attained at the ~700 LMH flux measured
compatibility is dependent on the precise permeability and other char- for the MF membrane. These values decreases to 7.2–7.8 m/h and
acteristics of the reservoir. These include the formation water chemistry, 1.7–2.6 h
1 respectively if 50% redundancy is assumed and filtration
and specifically the likelihood of the precipitation of supersaturated cycle conversion and backflushing are taken into consideration which
scalants. reduce the overall conversion to 92.5%. On this basis the footprint
In addition to the treated water, a further stream (the retentate) is incurred by the ceramic membrane technology is comparable to values
created which comprises 4.5% of the feed flow and >90% of the solids previously estimated, though this excludes ancillary equipment such as
and organic load. This would need to be managed in the same was as the the valve and pump skids, the control panel and the cleaning in place
concentrate streams from the upstream secondary treatment processes holding tanks and related equipment. Whilst the footprint and process
(the HC and IGF steps). The impact of the additional concentrate stream efficacy, with respect to water purification capability, suggest the process
will therefore be dependent on the capacity of the management system, to be viable for offshore applications, benchmarking against the alter-
but the additional hydraulic load from the membrane return stream native media-based tertiary filtration process (the nutshell filter) is
would be unlikely to add more than 10% to the hydraulic load. This is needed to assess the process viability on-shore. Moreover, benchmarking
based on the assumption that the HC and IGF concentrate streams should necessarily take account of the economic implications of tech-
comprise around 5% of the feed flow. Further analysis of the impact of nology selection (i.e. a technoeconomic analysis). Planned future work in
the backflush stream demands flows and loads information of the PW as this area will encompass a sensitivity analysis of individual operation
managed on an individual platform. A further stream which requires determinants related to the cleaning cycles of both technologies so as to
management is the wastewater from the chemical clean, which makes up assess the relative impact of enhanced cleaning and flux (or filtration
no more than 0.5% of the feed flow. velocity) on overall cost with reference to reagent use and residuals
Finally, the rate of chemical consumption is determined both by the generation and management.
total membrane area and the cleaning frequency (assumed to be daily).
Chemical storage requirements depend upon shipping costs and any Acknowledgement
logistical constraints, but given that the reagents would be stored as
concentrates the storage volume and associated footprint would be This work was funded by Maersk Oil Qatar, whose help and support is
relatively low. gratefully acknowledged, and was completed as part of project number
QUEX-CENG-CHE-13-14-03, Qatar University.
5. Conclusions
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