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IPTC 17394

Advanced Technologies For Produced Water Treatment And Reuse


A. Hussain, J. Minier-Matar, A. Janson, S. Gharfeh, S. Adham, ConocoPhillips
Copyright 2014, International Petroleum Technology Conference
This paper was prepared for presentation at the International Petroleum Technology Conference held in Doha, Qatar, 2022 January 2014.
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Abstract
Produced Water (PW) is the highest volume liquid waste stream generated by the petroleum industry. Historically, the
treatment of PW has been limited to free oil and suspended solids removal, using physical separation technologies, and
injection in disposal wells.
However, because of new regulations combined with geological restrictions and local water scarcity, the drive to have a
greater fraction of the PW more extensively treated and ultimately reused is increasing. Moreover, the growth in the
application of water intensive processes to extract unconventional oil&gas resources, in particular in shale plays and oil
sands, has increased the need for cost-effective treatment and reuse of PW to reduce fresh water uptakes.
Therefore, the petroleum industry is investigating new PW treatment technologies given that the physical separation
technologies traditionally used in the past are, in most cases, not capable of producing water of suitable quality to replace
fresh water uptakes.
This paper presents the results of a laboratory investigation carried out by the ConocoPhillips Global Water Sustainability
Center (GWSC), where various treatment processes (membrane processes, membrane-bioreactors (MBRs), membrane
distillation (MD) and ozonation) were evaluated as treatment methods for PW from different oil&gas fields.
The key conclusions of this paper are:
Membrane Processes and Thermal Evaporators are currently operating within the petroleum industry in full scale
PW treatment and reuse applications.
The preliminary results of investigations performed by GWSC confirmed the potential of Membrane Filtration,
MBRs and Ozonation to treat PW and produce an effluent suitable for reuse. Membrane Distillation may have
potential in the longer term. Further investigation is ongoing.
If successfully implemented, the above technologies will contribute to provide the petroleum industry with a
broad range of technologies to cost-effectively treat and reuse PW.

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1. Introduction
Produced Water (PW) is the highest volume liquid waste stream generated by the petroleum industry. The American
Petroleum Institute (API) estimated that in 1995, 18 billions of barrels of PW were generated in the US only from onshore
facilities [1]. Figures published in 2011 [2] and 2007 [3] show that globally, between 70 and 100 billion barrels of PW
were generated in 2007. The same report also projected a steady increase in PW generated in the US until 2025.
Currently, the majority of PW generated worldwide at onshore facilities is re-injected into the soil in disposal wells
and therefore, the treatment facilities are mostly designed to remove dispersed oil and grease (O&G) and suspended solids
(SS), to avoid formation plugging. In offshore operations, because the common practice is to discharge the treated PW to
sea, the main treatment objective is to reduce O&G to acceptable levels and mitigate toxicity impacts on aquatic fauna
and flora. As a consequence, the PW treatment methods applied in the petroleum industry are historically limited to
physical separation technologies such as the API separator, coalescers or hydrocyclones. These technologies are, in most
cases, not capable of producing an effluent compatible with water quality standards for beneficial recycling in the
petroleum industry itself or reuse in, for example, irrigation or other industrial processes.
A combination of factors including new regulations, geological restrictions and local water scarcity, is putting
enormous pressure on the petroleum industry operators to find new ways of treating and managing PW that promotes
water conservation and sustainability. As an example, Canadian oil sands operators using > 500,000 m3 of water per year
have to treat and recycle 75-90% of the PW generated. In 2008 for instance, mining operations in Canada withdrew 151
million m3 of fresh water from rivers [2]. Furthermore, for fracturing operations in shale gas fields, large volumes of
water (as high as 15,000 m3/well) are also required to drill the wells and to make up the fracturing liquids [4]. With
proper treatment, there is an opportunity for treated PW and flowback water to replace these significant volumes of water
extracted from lakes, rivers and aquifers in production operations.
Increasing efforts are being developed by the petroleum industry to develop and adopt advanced technologies that are
capable of further treating PW to produce an effluent compatible with water quality standards for beneficial reuse. This
will ultimately lead to significant water conservation benefits in several growing oil and gas key sectors:

Where PW is currently being injected in wells, the injection volumes will be reduced, diminishing environmental
impacts;

If wastewaters generated in water-intense operations (e.g. unconventional and oil sands resources) are treated and
reused, it will dramatically reduce the volumes of fresh water required;

There is growing evidence that enhanced oil recovery may become more efficient and productive if the injected
water is treated with advanced technologies to meet specific salinity levels.
However, treating PW and producing a good quality effluent is challenging. PW characteristics can vary considerably.
For instance, Total Dissolved Solids (TDS) can vary from >100,000 mg/L in Flowback waters from shale gas wells to less
than 3,000 mg/L in PWs from coal bed methane (CBM) wells [5,6]. However, as a broad generalization the constituents
that offer the greatest concerns from a treatment standpoint are organic content (in particular dissolved fraction) and
salinity. Also, PW from gas fields tend to have higher concentrations of low molecular weight aromatic hydrocarbons
than PW from oil fields, making these significantly more toxic [2]. Therefore, to treat PW to a water quality standard that
enables it to be reused, Advanced Water Treatment Technologies (AWTTs) have to be applied, alone or in combinations.
This paper discusses some of the AWTTs that are being applied in full scale oil and gas operations to treat and reuse
PW, or have the potential to do so. The technologies discussed are:

Membrane Processes (Microfiltration (MF), Ultrafiltration (UF), Nanofiltration (NF) and Reverse Osmosis
(RO));

Thermal Evaporator;

Membrane Bioreactor (MBR);

Advanced Oxidation Processes (AOPs).


To investigate the suitability of the AWTTs presented above to treat and reuse PW from Qatari gas fields, the
ConocoPhillips Global Water Sustainability Center (GWSC) carried out a laboratory investigation where various
treatment processes were evaluated. The treatment methods were selected to target main contaminants identified in PW
from a Qatari gas field:

Membrane Processes - Field chemicals

Membrane Distillation (MD) - Salinity

MBRs - Organics

Ozonation - Field chemicals


This paper also reports the results of this investigation.

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2. Research Conducted
2.1 Overview of AWTTs to treat and reuse PW
The first part of the paper reports case studies demonstrating the application of AWTTs in full scale oil and gas operation
facilities to treat and reuse PW. It also discusses some of the AWTTs that, although not yet applied, have to the potential
to treat PW in full scale operations.
2.1.1 Membrane Processes
The potential for membrane processes to treat PW has been successfully demonstrated in various field studies [7,8,9].
Moreover, a number of upstream petroleum full scale facilities (e.g. oil fields [2], CBM wells [10]) have already installed
membrane processes to treat and reuse PW. The treatment trains are either a combination of different membrane processes
(e.g. MF or UF + RO) or in combination with other conventional water treatment technologies such as media filtration or
clarification. UF & MF present several advantages over conventional media filters and clarifiers for SS and O&G removal
in PW.
Case study - San Ardo Oil Field, US[2]
The San Ardo PW treatment facility in California is considered the first large scale application of RO to treat PW.
Historically, the PW was disposed via deep well injection. However, the PW volumes generated in the field exceeded the
capacity of the disposal wells and the decision was made to install a system to treat and reuse the PW. The OPUSTM
process was installed in 2008 with an installed capacity of 50,000 bbd of PW. The PW generated in the field presented
significant challenges such as high levels of organics and silica. The treatment system was able to overcome these
challenges and the treated PW is now reused for aquifer recharge.
Case study - Arroyo Grande Oilfield, US [2]
The Arroyo Grande Oil field utilizes OPUS - II process for desalination of PW. This facility uses ceramic membrane in
the pretreatment stage before ion-exchange and reverse osmosis. The facility produces 45,000 barrels per day of water.
Over half of the treated water is used for once through steam generation, while the remaining 20,000 bpd capacity is
available as surface-water discharge.
2.1.2 Thermal Evaporators
Thermal evaporators entered the PW treatment market by looking at niche opportunities, particularly in remote locations
where other forms of traditional PW management tended to be more expensive, allowing the energy intensive thermal
processes an opportunity to be cost-effective. Moreover, since almost all waste streams are recycled back to the
evaporator, the volumes of fresh water required for makeup are dramatically reduced. With the proliferation of shale gas
wells in the past decade in the US, the demand for treating flowback water with TDS concentrations greater than 100,000
mg/L has expanded the opportunities for thermal systems. Another niche market where the application of evaporators has
been very successful is the SAGD enhancement recovery process. A leading technology company alone has developed 14
projects involving evaporators for SAGD in oil sands [11].
Case study - Connacher Great Divide Pod 1/ Algar Oil Field, Canada[12]
The Pod 1 Great Divide facility (Pod 1) and the Algar facility each produce 10,000 bbd of oil. Both facilities have
installed 2 parallel evaporators followed by a standard drum boiler to treat PW and generate stream for the SAGD
process. Pod 1 has been successfully operated since start-up in September 2007 and the evaporator treats de-oiled PW.
The Algar facility began operation in June 2010 and the evaporator in this facility treats a mixture of PW, source water
and blowdown generated from the Pod 1 evaporator. In both facilities, the evaporator produces a high quality distillate,
meeting the standards required for the boilers. In Algar for instance, the distillate produced has iron and copper
concentrations < 0.005 mg/L, total hardness < 0.013 mg/L, O&G < 1 mg/L and silica <0.02 mg/L. Furthermore, upsets in
the upstream de-oiling system have very little impact on the distillate quality. The main chemical dosed in the evaporators
system is caustic soda, necessary to keep the high levels of silica in the PW soluble, reducing the risk of scaling on the
evaporator heat transfer surfaces.

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2.1.3 Membrane Bioreactors (MBRs)


Very little information is available on full scale MBRs treating PW. The application of MBRs in the petroleum industry
has not been considered as a standard treatment solution mainly for three reasons:
Cautiousness of the industry towards innovative technologies;
Lack of regulatory requirements for a high quality effluent;
Highly variable feed from location to location, requiring expensive testing for process optimization before full
scale application.
This has changed in recently years driven mainly by factors mentioned earlier resulting in the implementation of more
water reclamation projects. MBRs are now frequently used in petroleum industry, although their application is confined to
downstream applications, mainly refineries or petrochemical facilities. MBRs are now considered by the downstream
petroleum industry as an excellent solution to treat various wastewater streams and MBRs treating 50MLD flows are
presently operating [13]. New MBRs treating larger flows are also being planned or under construction.
Although MBRs have not yet been applied to treat PW at upstream oil and gas facilities, a number of bench scale and
pilot studies report that PW is biodegradable, achieving COD and O&G removals greater than 95% [14,15]. Moreover,
full scale MBRs are also successfully operating in other industries treating highly contaminated organic streams (COD >
15,000 mg/L) achieving COD removals >95% [16]. If the MBR technology is proven successful in treating PW at a full
scale, the opportunities for this technology in water reclamation projects in the oil and gas industry are numerous.
2.1.4 Advanced Oxidation Processes (AOPs)
Similar to MBRs, there is very limited information on AOPs being applied to treat PW in full scale facilities. Bench scale
and field studies are also scarce. One of the few studies assessed a combination of O3/UV/TiO2 to treat PW with 38 g/L
salinity and achieved COD and O&G removals of 74% and 95% respectively, after a 30 minute contact time. After a 60
minutes contact time, COD removal increased to 89% [17]. Published research investigating refinery effluents treatment
with AOPs appears to be more common. Some of these assessed a number of different AOPs and concluded that the
Fenton reaction was able to achieve excellent organic removals (DOC=90%, TOC=70% and COD=98% at optimum
conditions) [18,19]. There are also references of companies that have developed AOP-based patented technologies with
successful applications in full scale chemical, petrochemical and pharmaceutical industries; COD removals >90% were
obtained for systems with CODs of 1,000-10,000 mg/L. Despite the evidence that AOPs may be successful in treating
PW, the petroleum industry has yet to benefit from the many opportunities these processes offer.
Even though AOPs have not been applied commercially to treat PW, results of several works published in the literature
and from experience in full scale applications in other industries would indicate that there is potential for AOPs in niche
PW market treatment applications.
2.2 Investigation at GWSC on various methods to treat and reuse PW
All the tests carried out as part of this investigation were performed at the GWSC laboratories (Doha, Qatar) using stateof-the-art bench scale units designed and assembled by the GWSC research team. The investigation was carried on PW
sampled from a Qatari gas field. This PW was typically high in salinity and organic content, and also contained field
chemicals such as Kinetic Hydrate Inhibitor (KHI).
During the winter season, the combination of pressure and cold temperatures provides an environment in which hydrates
can form causing a blockage in the piping carrying the gas from the gas fields. KHI, a complex organic polymer with high
COD, is typically added to retard the formation of hydrates. The biotreatability of KHI was investigated at GWSC. In
addition, the effect of salinity on biotreatability of PW was also investigated.
2.2.1 Membrane Processes
The effectiveness of UF, NF and RO membranes in rejecting KHI was investigated using a SEPA CF II test cell. The
membranes were tested on a solution of 1.5 wt% KHI prepared in a synthetic brine solution with a TDS around 6,000
mg/L. The objective of the experiment was exclusively to analyze KHI rejection for different membranes.

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Figure 1 SEPA CF II test cell at GWSC

2.2.2 Membrane Distillation (MD)


As mentioned above, the PW collected from the Qatari fields was high in salinity. The ability of MD in treating high
salinity feed waters can make it suitable to reduce the salinity of PWs. In order to further investigate this, the research
team at GWSC initiated an extensive testing program where various solutions with salinities comparable to those of PWs
were tested using a MD direct contact configuration test cell.
Various saline streams (synthetic sodium chloride (NaCl) solutions, seawater and brine from a thermal desalination plant)
were tested under different operating conditions and using different membranes. Salt rejection was assessed by measuring
conductivity and TDS in the feed and product water.

Figure 2 MD bench scale testing unit at GWSC

2.2.3 Membrane Bioreactors (MBRs)


PW also contains soluble organics in various forms including hydrocarbons, organic acids and KHI (during the winter
season). To assess the potential of the MBR process to remove organics, tests were conducted both in batch reactors and
in an MBR each of 1 liter working volume. The effect of salinity on biotreatability of PW was assessed over the range of
salinities from 6,000 mg/L to 31,750 mg/L. Biotreatability was calculated based TOC mass balances and is reported as %
TOC removal. To assess the biotreatability of KHI, the batch bioreactor was fed with a 0.25% KHI (initial tests) or 1.5%
KHI (later tests) added to a standardized brine solution mimicking the inorganic content of PW. In this way, the
biotreatability of KHI could be directly measured. Biotreatability was calculated based on both COD and TOC mass
balances and is reported as % removals.
In a third investigation, an MBR was fed with a PW collected from a different location in the plant. This PW was lower in
both salinity and organics than that used for the salinity experiments. After acclimation, for 5 weeks under steady state
conditions, biotreatability was measured through COD mass balances and reported as % COD removal. The MBR
effluent was also treated with a downstream RO process in order to generate an effluent that can be reused for multiple
applications.

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Figure 3 GWSCs Membrane Bioreactor

2.2.4 Ozonation
The removal of KHI in a synthetic brine solution with a TDS around 6,000 mg/L was tested using an ozone generator
which was then bubbled ozone into a 1L column. The ozone concentrations at the inlet and outlet were continuously
monitored using an ozone detector. The KHI solution was ozonated for 0.5, 1.5, 3 and 4 hours to evaluate ozonation as a
function of time.
The removal of KHI was assessed by calculating the % of KHI oxidized and measuring cloud point.

Figure 4 Ozonation setup at GWSC

3. RESULTS
3.1 Membrane Processes
A Toray brackish water RO (BWRO) membrane was used in the tests. Initially, the membrane was compacted with 10
g/L of NaCl at 500 psi, achieving a stable flux of 10LMH after 14 hours. The synthetic brine solution containing 1.5%
KHI was tested for 22 hours, with the operating pressure kept at 590psi. Throughout the test, the flux decreased from 15
LMH to 10.5 LMH. At the end of the test, the same solution of NaCl at 10 g/L was introduced through the system at
500psi and the permeate flux was 9 LMH, which confirmed that the membrane can be restored to its original compaction
condition (10 LMH). The KHI polymer was completely removed by the RO membrane (99.9% rejection).
A NF membrane from GE Osmonic (Desal-DK) was used in this investigation. The pore size of the membrane was 0.5
nm. The synthetic brine solution containing 1.5% KHI was tested at 150 175 psi for 29 hours. The initial permeate flux
was 33.6 LMH, which decreased to 11.3 LMH. The results show that the NF membrane tested rejected 99.7% of KHI
polymer.

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A UF membrane from GE Osmonic (GK series) was also tested. The molecular weight (MW) cut-off of the membrane
was 3,500 Daltons based on polyethylene glycol. The operating pressure was 50 65 psi and the test was carried out for
24 hours. The flux was constant at 12 LMH and the rejection of KHI polymer was about 83.3%.
The rejections for various elements during the above tests are summarized in Table 1 below.
Table 1 Rejections for tests with RO, NF and UF membranes

Parameter

Unit

Synthetic
brine + KHI
1.5%

RO Rejection
(%)

NF Rejection
(%)

UF
Rejection
(%)

KHI

mg/L

20,738

99.9

99.7

83.3

Chloride

mg/L

3,403

99.2

72.8

2.8

Sulphate

mg/L

40

99.0

100

25.0

Phosphate

mg/L

292

99.7

100

16.6

Sodium

mg/L

675

99.2

14.6

0.0

Magnesium

mg/L

245

99.7

98.9

4.2

Calcium

mg/L

1,017

99.7

97.7

1.2

3.2 Membrane Distillation (MD)


The initial tests were performed with NaCl solutions prepared in deionized water, using a single membrane (membrane
E). Figure 5 shows that flux remained relatively constant at approximately 25 LMH when testing NaCl solutions of 0.1-35
g/L. However, when the salt concentration was increased above 70 g/L, a slight drop in flux was observed (20 LMH),
which may be related to vapor pressure variations and difference in water viscosity that could impact the thermal
conditions at the membrane boundary layer. These results are consistent with the literature [20].
Tests on seawater collected from the Arabian Gulf locally in Qatar were conducted with five different MD membranes.
Although the initial flux was similar, all membranes showed a drop in flux with time, with the exception of membrane B
(Figure 6). This flux decline was not observed when the membranes were tested on NaCl solutions. It should be noted that
no antiscalent was added to the seawater and the pH was not adjusted prior to testing. The TDS rejection by all
membranes was greater 99.99%. Table 2 presents a more detailed summary of the results.
Experiments were also carried out using brine collected from a local full-scale thermal desalination plant (Ras Abu
Fontas) operating in Qatar. Figure 7 shows the performance of membranes A, B & E operating on this brine. The fluxes
were stable throughout the test. It should be noted that the brine was already pre-dosed with antiscalant when sampled at
the desalination plant which could minimize the formation of scale on the surface of the MD membranes. The TDS
rejection was greater than 99.99% for the three membranes tested. Table 2 presents a more detailed summary of the
results.

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Figure 5 Results of MD tests on NaCl solutions (Membrane E)

Figure 6 Results of MD tests on Seawater from the Arabian Gulf (Membrane A, B, C, D and E)

Figure 7 Results of MD tests on Brine from a local Thermal Desalination Plant (Membrane A, B and E)

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Table 2 Rejections for Seawater and Thermal Brine tests with Membrane B

Parameter

Unit

Seawater

Distillate

Rejection
(%)

Thermal
brine

Distillate

Rejection
(%)

Conductivity

S/cm

65,000

>99.99

100,000

>99.99

TDS

mg/L

43,247

<1

>99.99

71,981

<1

>99.99

Calcium

mg/L

416

<0.1

>99.97

718

<0.1

>99.99

Magnesium

mg/L

1879

<0.01

>99.99

3,120

<0.01

>99.99

Sodium

mg/L

13,384

<0.03

>99.99

22,604

<0.03

>99.99

Chloride

mg/L

23,715

<0.03

>99.99

39,274

<0.03

>99.99

The above results demonstrate the ability of MD in reducing the salinity of highly saline feed waters. Therefore, based on
the knowhow captured above, the research team at GWSC has started testing different MD membranes on various types
of PW collected from various oil and gas operations worldwide. These tests are still undergoing and therefore the results
cannot be included in this manuscript.
3.3 Membrane Bioreactors (MBRs)
The characteristics of the PW used during the salinity tests are summarized in Table 3 below.
Table 3 Characteristics of the PW during Salinity Tests

Parameter

Unit

Value

COD

mg/L

1,440

TOC

mg/L

403

O&G

mg/L

14

Conductivity

S/cm

46,000

TDS

mg/L

28,980

Salinity
The salinity of the bioreactor was gradually increased from 6,400 to 31,750 mg/L over an 8 week testing period. During
this period, the F:M increased from 0.01 to an estimated 0.04 gCOD/gMLVSS-d. The daily %TOC removals fluctuated
between 4080%, averaging 65%, over the entire range of salinities. There was no significant effect of salinity on %
TOC removal over this range of salinities.
KHI
Since all the organics present in the feed were attributed to KHI, the %COD removal results directly reflect the
biotreatability of KHI. The results indicate that over the 7 week test period, 50 - 60% of the COD associated with KHI is
removed through biotreatment. The % removal was similar for both at both the low and high KHI concentrations.
MBR
The %COD removal over the 5 weeks of steady state testing indicates that 63% of the COD could be removed through
biotreatment. The UF flux remained excellent over the entire testing period and no intermediate maintenance or soak
cleaning was required. In the posttreatment experiments with an RO, as expected, the effluent produced was excellent
with >98% removal of both the COD and inorganics. The effluent would be suitable for recycle or reuse within the gas
processing facility. Although the RO flux on MBR effluent was lower than the pretest benchmark water flux, upon
completion of the RO tests, a simple flush of the system with tap water restored the flux to the pretest level indicating that
there was no irreversible fouling of the RO membrane.

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3.4 Ozonation
The KHI solution was ozonated for 0.5, 1.5, 3 and 4 hours to evaluate ozonation as a function of time.
From Table 4 below we can see that a KHI removal of 11%, 60% and 75% was obtained with ozonation times of 1.5, 3
and 4 hours respectively. An ozonation time of 0.5 hours did not remove any of the KHI in the synthetic brine solution.
The results clearly show that the effectiveness of ozonation in oxidizing KHI is very dependent on the contact time and
significant removals (75%) can be achieved given the necessary contact time.
The cloud point (the temperature at which turbidity due to precipitation of polymer is observed) also varied with contact
time (Table 4). Visual examination of the treated effluent indicated that the treated effluent was turbid after ozonation.
However, after filtration through a 0.45 micron filter, the treated effluent solution was clear.
Table 4 Ozonation Test Results
Ozonation Time
(h)

KHI Oxidized
(%)

Cloud Point
(C)

40

0.5

33

1.5

11

ND

60

48

75

57

ND Not Detected
4. CONCLUSIONS
The key conclusions of this paper are:
Membrane Processes and Thermal Evaporators are currently operating within the petroleum industry in full scale
PW treatment and reuse applications.
The results of investigations performed by GWSC confirmed the potential of biological degradation and
ozonation to treat PW and produce an effluent suitable for recycle or reuse.
Membrane Distillation may have potential in the longer term as a method for producing a treated effluent also
suitable for recycle or reuse. Further investigation is warranted.
Overall, the AWTTs investigated confirm their potential to treat PW and produce an effluent than can potentially
be reused in various applications: crop irrigation, livestock watering, wildlife habitats and industrial applications.
This reuse could potentially leave more fresh water available for domestic use.
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