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SiC MEMBRANE PILOT ULTRAFILTRATION TEST FOR PRODUCED WATER TREATMENT OCELOTE field – HOCOL (COLOMBIA) August 2012
Prepared by: Oscar Andrés Prado‐Rubio Project Manager, LiqTech David Cardona Technical profesional, Conconcreto Revised by: Tore Svendsen Application Manager, LiqTech Linfeng Yuan Project Manager SiC membranes, LiqTech 1
Table of Contents
1. Introduction ................................................................................................................................ 3 1.1. 1.2. 1.3. 1.4. 1.5. Problem description ............................................................................................................ 3 Test objectives ..................................................................................................................... 5 Test facility .......................................................................................................................... 5 Facilities description ............................................................................................................ 8 Experimental methodology ............................................................................................... 13 Operating window identification ‐ Operability investigation .................................... 13 Continuous operation tests ....................................................................................... 14 Chemical cleaning efficiency evaluation ................................................................... 14
1.5.1. 1.5.2. 1.5.3. 1.6. 2. 3.
Activities schedule ............................................................................................................. 14
Water permeability test ............................................................................................................ 16 Experimental evaluation point: Before the skimming tanks ..................................................... 18 3.1. 3.2. 3.3. 3.4. 2.5 Characteristics of the inlet water – field information ....................................................... 18 Preliminary tests – conventional ultrafiltration ............................................................ 19 Operating window identification ‐ Operability investigation ........................................ 20 Continuous operation ................................................................................................... 25 Conclusions.................................................................................................................... 30
Experimental evaluation point: After the skimming tanks ....................................................... 32 4.1. 4.2. 4.3. 4.4 Characteristics of the inlet water – field information ....................................................... 32 Operating window identification ‐ Operability investigation ........................................ 33 Continuous operation ................................................................................................... 37 Conclusions.................................................................................................................... 41
Cleaning in place evaluation ..................................................................................................... 42 Final remarks ............................................................................................................................. 43 Evaluation point before skimming tanks: ..................................................................................... 43 Evaluation point after the skimming tanks: .................................................................................. 43
Future challenges ...................................................................................................................... 44 Appendix: Critical flux estimation ............................................................................................. 45
HOCOL is a private company, with over half a century of presence in exploration and production of oil and gas in Colombia. HOCOL currently has exploration projects in the Upper Magdalena Valley, Lower Magdalena Valley, the Eastern Plains and the Llanos Foothills. Besides, it has engaged production operations in the states of Huila, Tolima and Meta, pumping the produced crude oil through their own pipelines in the Alto Magdalena. Currently, HOCOL has an average production of 32,307 barrels (gross) per day in fifteen fields and a portfolio of net 2P reserves of 57.7 million barrels and 0.9 giga cubic feet of gas waiting to be developed efficiently and with high operational excellence. In 2011, the company produced 9.9 million barrels of oil. HOCOL showed interest to test new technologies for the separation of oil in water emulsions, as a way to bring innovation into their installations, in that way fulfilling their future expectations in produced water treatment. A process proposed by the consortium Conconceto/LiqTech, based on Silicon Carbide (SiC) membrane technology. LiqTech is a Danish company who manufactures the membrane. For the last 11 years, LiqTech has been at the leading edge in developing and marketing its own proprietary products to the environmental industry. LiqTech’s core is its ability to manipulate SiC, which has allowed it making a high value, high performance products for liquid and gaseous filtration. Conconcreto has joined LiqTech efforts to promote this technology in South America. Conconcreto is a Colombian company with more than 50 years of experience providing services in South America, mainly in the construction area. Recently, Conconcreto has created an innovation department to provide cutting edge technologies for domestic and industrial water treatment. The produced water application is one of the most promising applications of SiC membranes. LiqTech/Conconcreto and HOCOL have agreed to perform a test of the SiC membranes for produced water treatment. This test is relevant for the consortium LiqTech/Conconcreto since it is a great opportunity to improve its understanding of the separation and at the same time validate the technology under Colombian conditions. The intention of this test is to gather sufficient data to allow Conconcreto/LiqTech propose a commercial service solution for the produced water treatment.
1.1. Problem description
The pilot plant testing has been conducted in “Campo OCELOTE”, inside of the crude processing area referred to as “Fluid Processing Central – CPF” (see Figure 1). During the oil recovery process, an interesting challenge is to separate the oil and water mixture. This separation is limited by the stability of the oil in water emulsion. Conventionally, emulsion breakers are added in order to facilitate the oil separation and to allow the filters to remove the suspended solids. The HOCOL’s processing area is divided into two sections, first the oil recovery plant and secondly the produced water treatment plant for reinjection.
The oil and water mixture coming from all drilling points is sent to the processing area through two pipelines. Those enter the CPF in a manifold where temperature is adjusted for the subsequent oil recovery section. The oil treatment process is composed in two (02) Surge tanks, one (01) Gun barrel and finally two (02) Storage tanks. The outlet stream has an average concentration of 500 ppm of oil in water (OiW) and total suspended solids (TSS), respectively. From the oil recovery plant, 55.000 BWPD are sent to water treatment facilities. This section consists of two skimming tanks, one microflotation unit and two walnut shell filters. From the skimming tanks there is an oil recovery which is sent back to the oil processing plant. The treated water goes to the microflotation unit with OiW concentration of around 75 ppm and 500 ppm of TSS. From the microflotation process, the produced water stream has 7.5 ppm of OiW and 50 ppm of TSS approximately. Currently, the Microflotation process has been by‐passed and the outlet from the skimming tanks is sent directly to walnut shell filters. The water at the end of the process should have a maximum of 5 ppm of OiW and TSS. Finally the produced water is sent to the storage tanks, and then re‐injected.
Figure 1. Diagram of the fluid processing central CPF at OCELOTE field. Red square shows the oil recovery plant. Green square shows the produced water treatment plant.
As an alternative solution for the produced water treatment, the SiC membrane technology offers reliable performance. This technology exploits the oil droplets and suspended solids size to achieve the separation. The separation is possible due to the membrane is highly hydrophilic allowing the water to pass through and retaining the oil drops and suspended solids.
The objective of the test is to determine the operability of the pilot plant at the field conditions. Therefore, the necessary information is gathered to evaluate the technical feasibility of this technology for the produced water treatment which will be reflected in a commercial design. It is aimed to deliver water with concentrations below 5 ppm of OiW and TSS. The activities involved during the test are: Evaluate the effect of the operation variables on the separation performance at different sampling points in the OCELOTE field Reveal the most appropriate operation conditions given the input water quality and clean water requirements. Investigate the inlet characteristics variance at the interesting sampling points in the field. Investigate the influence of the inlet water quality on the separation performance Determine the water and oil separation efficiency at field conditions Determine the total suspended solid separation efficiency at field conditions Evaluate the sustainable continuous operation of the pilot plant.
The test rig is a Multibrain pilot unit from LiqTech (CFU8), it can be seen in Figure 2. The PID can be seen in Figure 3.
In addition. In addition. the unit is equipped with a BackPulse Hammer (BPH) The unit consists of three pumps: a feed pump delivering the feed solution into the recirculation loop. The pilot unit is equipped with a feed pump which pressurizes the feed stream. Pilot unit located at OCELOTE-CPF. a recirculation pump which generates the cross-flow and a pump for backflush. The pressure and flow rates inside the system are controlled by adjusting the position of control valves and pump speeds. Figure 2. which delivers high frequency water pulses from the permeate side in order to keep the membrane clean and free of foulants. the pilot unit is equipped with a Back Pulse Hammer (BPH). The BPH system is a pulse generator. a recirculation pump generating the cross‐flow and a pump sitting at the permeate side for Backflush. The filtration membrane element is based on Silica Carbide (SiC). 6 .
PID-diagram of the test unit. Figure 3. The LiqTech Multibrain CFU08 is an industrial pilot unit for water filtration applications 7 .
beside the Microflotation unit. Figure 4. this location allow having the connections for the first and second test points very close to the pilot plant. General Layout of CPF area (The precise location is indicated with the red circle in the layout) 8 . The following figure shows the localization of the pilot unit inside the CPF area.4.Facilities description The pilot unit was located inside CPF area. 1.
Figure 5. outlet surge tanks. The equipments that complement the pilot plant are: Transformer: the voltage in the field is 480V. The connections for the first and second point of operation with the pilot unit were suitable by HOCOL. Therefore was necessary to install an electrical transformer to reduce the voltage to 440V (see Figure 7). First point of connection. 9 . Second point of connection. Figure 6. installing a valve for control the feed flow rate (as can be seen in Figure 5 and Figure 6). outlet skimming tanks.
Figure 8. 32A. a pump and the computers that use 440V and 110V (Figure 8 and Figure 9). Electric panel for connection 220V and 110V. Panels: as protection for the equipment. heater. 10 . Figure 7. 480V to 440V. there are different electrical panels that allow connecting the pilot plant. Electrical transformer.
where particles with size larger than 300 micrometers are retained. Figure 9. In these tanks the chemical cleaning solution with alkaline and acid is prepared for the membrane cleaning (Figure 10). permeate and retentate hose’s. Prefilter: this equipment filters the water through a mesh. with a configuration of pipelines and valves that allow connecting the feed. Cleaning in place unit (CIP). Cleaning in place unit (CIP): Consist of two plastic tanks with 250 liters of capacity. Electric panel for connection 440V. This is a protection device which avoid that these 11 . Figure 10.
Figure 12. used for feed of produced water. Storage tanks: There are two plastic tanks. Figure 11. pump shown in the right side. There is a small pump (8 m3/h) to generate flow if necessary (Figure 11). particles enter the pilot unit. Prefilter is showed in the left side. the first with 1000 L of capacity. and in the right side the clean water tank. is employed for clean water storage to be used for the membrane washing. In the left side of the picture is showed the feed tank. 12 . The emulsion is kept in the tank by strong agitation and temperature regulation. The second tank with a capacity of 2000 L. in that way preventing the obstruction the feed channels.
The influence of flux increments is evaluated through a conservative stepwise strategy. the mixture properties and how the system is operated. a hierarchical structure is employed. The following inputs. The separation performance is assessed in terms of well‐established indexes like: flux. In that way viable and reproducible results can be obtained. 1739‐1747. that define the membrane performance. a stepwise methodology is proposed. solutions). The operating mode selected for the experiments is constant flux. During the filtration of any mixture (e. The transmembrane pressure should reach a relatively stationary average value.5.Experimental methodology In order to evaluate the influence of operating variables on the separation behavior. The most appropriate operating conditions are estimated from an analysis of the independent experiments based on the mentioned indexes. can be controlled by the membrane pilot unit: Flow conditions: cross‐flow velocity Driving force: transmembrane pressure (TMP) Cleaning: combination of the available cleaning strategies (backpulse hammer.5. which analogous to the constant flux operation). 1. For this pilot unit. 1.1. backflush and cleaning in place) The separation efficiency is determined by the membrane characteristics. In order to determine the best way to operate the process. Critical Flux Determination by Fux Stepping.P. The used methodology is called “step up‐down” method for the estimation of the sustainable flux1. S. Operating window identification Operability investigation In order to minimize the number of experiments. G. thus on the separation performance. it is important to identify the influence of the operating conditions on the mentioned phenomena. recovery and sustainability. The first series of experiments on a new type of water application are initiated with the smallest flux possible and maximum cross flow velocity. suspensions.3 bars and the cross‐flow should be kept as high as 2 m/s (50 m3/h). which can be automatically controlled (in a selected experiment the constant TMP mode is tested. the solvent flux through the membrane is always lower than the pure water flux due to two tightly coupled phenomena referred to as concentration polarization and fouling. For that purpose. 13 . An additional advantage of this procedure is that the membrane has an appropriate time to get used to the environment. The experiment starts with an initial flux which is gradually increased. AIChE Journal 56(7). indicating a situation where there is equilibrium between the 1 Beier. emulsions. each increment is followed by a relaxation period. After each increment. permeate quality.g. and Jonsson. This is necessary in order to avoid an initial irreversible fouling and at the same time more carefully follow the separation performance. an experimental design is used. the transmembrane pressure should be kept below 0. the transmembrane pressure will increase as a consequence of the higher desired flux.
resources and troubleshooting that were necessary for the correct development of the project. Using the test results. The analyses are performed following the standard protocols used in the field laboratory (ANTEK)2. the recommended cleaning strategy is refined in order to match an acceptable water permeability recovery at field conditions. recover the initial stable separation potential of the membrane. there is a loss of separation performance which cannot be recovered. 2 ANTEK is a certified laboratory that makes all quantitative measurements in the field. backflush or backpulse). the physical cleaning variables are tested such as frequency and intensity. After considerable irreversible fouling. The separation performance is followed using quantitative measurements of the total suspended solids and oil in water. every one of these has a time line defined.3. During the continuous tests. the sustainable operation is evaluated using continuous operation.5. thus it is an important parameter to identify. 1. since exceeding that point is not possible to achieve a stationary operation. the water quality is determined regularly. This equilibrium is achieved due to the efficiency of the equipment to remove the reversible fouling.6. before and after the skimming tanks. 1. The objective of the chemical cleaning is to remove the accumulated organic matter. 14 . meaning that there is not equilibrium between the fouling formation and removal by the cleaning strategy (cross‐flow. The cleaning efficiency is quantified through the water permeability assessment. As a preliminary experiment.5. increasing the operation window. the first evaluation point includes a test of conventional ultrafiltration. amount of material being deposited on the membrane surface and material being removed by the cross‐flow and employed cleaning strategy. including labor. Above the critical flux it is very difficult to maintain a sustainable production due to the formation of a dominating irreversible fouling. The determination of the critical flux methodology is applied at two different points in the produced water treatment. It is not recommended to operate the equipment above the critical flux. the efficiency of the chemical cleaning is evaluated. 1. Activities schedule The activities are organized in four main areas. Thus. The idea of the experiments is to find the so called critical flux. The initial tests are performed at moderated operating time. Chemical cleaning efficiency evaluation As a parallel activity to the experimental design. The frequency of the cleaning strategies has a big influence on the operating cost of the pilot plant. Continuous operation tests Once the operating conditions are identified. solids and precipitated salts in both surface and internal structure of the membrane.2. During the experiments for each flux conditions.
In the following figure. Closing Operation consisted in un‐mounting of the equipment. 15 . the time line for every area is depicted. Work schedule for the test period at OCELOTE field-HOCOL The Assembly and Installation of the pilot unit and was started 27/06/2012. Therefore. The experimental phase was divided in two tests: the first sample point used feed water from the outlet of surge tanks. HOCOL had promised 440V but at the end there was no way to provide it in the field. The order of the tests was imposed by HOCOL. This activity took a week. Figure 13. and the second used water from the outlet of skimming tanks. a transformer was installed. The installation of the pilot plant was delayed due to the absence of 440V in the field. These activities were started the 04/08/2012 and finished 06/08/2012. cleaning and shut down of the pilot unit. All these activities were started the 10/07/2012 and finished 03/08/2012.
This water is not in optimal conditions neither for cleaning nor for water permeability estimation but there is no other initial water source. The permeability is defined as the ratio between the flux and the applied transmembrane pressure. 3 LiqTech International A/S. (a) Drinking water. However. which is an extreme case seen in the at the beginning of the experiments. The results are shown in the Figure 15. In the field. The water permeability is used to evaluate the state of the membrane. The initial permeability changed from 1550 to 4500 LMH/bar at the lowest TMP evaluated. There is a limitation since there is not a drinking water line available (see Figure 14a). The cleanest source available is the outlet of the walnut shell filter 2. At higher TMP. at HOCOL). It can be seen how the flux increases very fast by raising the pressure at low TMPs. The results are clearer by looking the permeability in Figure 16. the membrane permeability is estimated according to the water quality available. reported by LiqTech3. (b) Example of bad quality water from the walnut shell filter 2 (not all the time was bad). this average information was provided by the Latin‐American treatment personal. It is believed that this effect is due to the quality of the water that was coming from the walnut shell filter (OiW: 1 ppm and TSS: 3. CoMem Conduit – OD146mm diameter Round Channels data sheet.3 ppm. The quality of this water changes a lot as it can be as bad as it is shown in Figure 14b. a high recovery is achieved and the permeability tends to decrease. Water permeability test The ultrafiltration membrane used for the experiments was LiqTech‐103377. The water flux was estimated as a function of the TMP. At moderate TMP. Despite the water quality. the color is due to a severe oxidation of the pipelines. (a) (b) Figure 14. the slope tends to settle. 16 . 2.1 bar. it rapidly stabilizes around 3000 LMH/bar at TMPs higher than 0. the results agree with the expected value of 3000 LMH/bar. Quality of the water available in the field.
3 0.00 Water flux (LMH) 600.00 100.00 300.00 0.00 500.00 200.4 Transmembrane pressure (bar) Figure 15.2 0.00 1000.05 0.00 3000.00 Permeability (LMH/bar) Field Perm 3500.35 0.4 Transmembrane pressure (bar) Figure 16.00 4000.00 0 0.00 4500.15 0.25 0.00 0 0.00 700.2 0. 900.00 1500.1 0.25 0. Water permeability test using water from the walnut shell filter 2 (12/07/12). Water permeability test using water from the walnut shell filter 2 (12/07/12).1 0.00 800.35 0. 17 .00 2500.3 0.00 500.00 2000.00 400.15 0. 5000.00 0.05 0.
00 ST 1 300. The place where the inlet is taken is a point where the 3 shown streams are combined. GB: Gun Barrel (Information provided by Latin-American treatment personal. 700. Experimental evaluation point: Before the skimming tanks The test in this evaluation point took place between the 11/07/2012 to 28/07/2012. 18 . heavy oil load has been received especially in the middle and at the end of the experiment. 3. the heaviest load has been seen during the period with continuous operation of the pilot plant. According to this record. The surge tank 2 manages the lowest variance and the Gun barrel manages lower outlet concentrations. The average values during the testing days are shown in the following plots. 3. Oil in water average concentration at the outlet of the oil recovery section.00 600. the oil in water and total suspended solids are quantified twice per day.00 ST 2 GB Figure 17. however it has a substantial variance. at HOCOL) It can be seen in Figure 17 that the OiW outlet concentration of the surge tank 1 is considerably higher than the other units.00 OIW (ppm) 400.00 200.1. This period included testing time and maintenance of the pilot plant due to some unexpected situations.00 100.00 0.00 500. ST: Surge tank. Characteristics of the inlet water – field information In the field.
This event took place during the continuous evaluation of the operating point. GB: Gun Barrel. 19 . The idea was to determine the sustainable flux during conventional ultrafiltration. At the same time. Preliminary tests – conventional ultrafiltration The purpose of the first experiment was to provide a fast indication of the fouling challenge in this evaluation point.00 20. at HOCOL) 3.00 TSS (ppm) 80.00 40. An inspection of this data would provide relevant information about how fast the flux is limited by irreversible fouling. The ultrafiltration test has shown that the critical flux without any in situ cleaning mechanism occur at relatively low TMP.2. they do not really represent the variance that can be seen in the field. On the other hand. this point is a comparison standard to evaluate the efficiency of the in situ cleaning strategies. However. there is an atypical event at the end of the test where there is a tremendous increase in the TSS concentration (six times higher concentrations).00 ST 2 GB Figure 18.00 0. Therefore.00 100. ST: Surge tank.00 120. Total suspended solids evolution in the lines at the outlet of the oil recovery section.00 ST 1 60. It has to be mentioned that these concentrations are average of two samples per day. (Information provided by Latin-American treatment personal. 140. For this experiment. the total suspended solids concentrations show lower variance and the concentrations are below 20ppm (see Figure 18). the operating and relaxation time per operating point were 60 and 30 minutes. but give an overview of the challenges faced during the experiments. The summary of the results are shown in the Table 1.
3.2 Average inlet concentration TSS (ppm) OiW (ppm) 28. this strategy was advantageous due to the constant monitoring of the inlet concentrations along the experiments. The first 3 tuning experiments were performed in this way. These results have been influenced by the initial fouling generated by the quality of the clean water available in the field (during the permeability test). strong agitation and temperature regulation were provided. Table 1. it was expected to have approximately constant inlet concentration for each experiment (the variation would be due to the accumulated material within the equipment).38 117. On the other hand. Nevertheless. Results from the conventional ultrafiltration operation mode. it introduces the inlet concentrations as variables within the experimental design. while the retentate and permeate where disposed out of the system. it was decided that as long as the water coming from the walnut shell filter 2 showed bad aspect. it was decided to perform the remaining tuning experiments using a continuous feed stream to the feed tank.5 m3/h. 3. The cleaning frequency should be moderate in order to avoid irreversible fouling formation. Crossflow (m3/h) 30 Critical TMP* (bar) 0. it was evidenced that irreversible fouling is formed at relatively low TMPs and LMH. In this scenario. Besides. This water was collected in one of the 2000L tanks available. This was mainly due to the oil tendency to stick to the feed tank surface and to some extend within the equipment. 20 . In that way. it was noticed that there was a considerable oil inlet concentration decrease along the experiments (see Figure 21). This operation mode brought new challenges due to the variance of the inlet oil and suspended solid concentrations along the tuning experiments. From this experiment it can be stated that there is a need of using the in situ cleaning strategies for this application.7 Critical Flux LMH Permeate (m3/h) 150 1. respectively. Operating window identification Operability investigation A sequence of experiments were performed in order to determine the sustainable operation conditions of the plant according to the given water quality. which is relevant for the plant design and operation. but it was decreased along the experiment. The permeate flow rate increase was initially 0. the permeate water would be used for those purposes. providing more information about the system. It has been seen that completely unsustainable operation is achieved already at 170 LMH.53 *This TMP has been already affected by an initial irreversible fouling during the experiment From the preliminary results. The initial strategy was to emulate continuous operation by having around 500 L of produced water in the feed tank and recirculating both retentate and permeate streams. Due to the variable quality of the clean water used for washing and permeability estimation between experiments. Therefore.
00 200. For the last experiment the constant TMP operating mode was tested. It is referred as dynamic due to the operation of the in situ cleaning strategies.00 100.00 13:55:12 15:07:12 16:19:12 17:31:12 18:43:12 Time (h:m:s) Figure 19. the challenge of the separation can be seen due to the low fluxes obtained from the beginning. Only the results certified by ANTEK laboratory are reported. The tuning experiments at constant flux started using a low recovery and it was increased step wise between experiments.00 0. Summary of the operating conditions for the tuning experiments.00 150.00 350. Flux profile during the critical flux determination (DUF3) 21 . The summary of the operating conditions for the experiments are shown in the Table 2. Table 2. 400. Test* DUF 1 DUF 2 DUF 3 DUF 4 Crossflow Feed pump Backpulse (auto) (auto) (s) 30 29‐38 60 30 30‐50 60 30 32‐56 60 30 28‐42 60 Backflush (s) 300 300 300 300 Permeate 04V04(%) 40‐90 60‐100 100 80‐100 Retentate 03V01(%) 03V02(%) 100 100 100 70‐100 60 60 40 50 *DUF – Dynamic Ultrafiltration As an example of the results obtained. It can be seen that the backpulse and backflush operation disturb the system having the noise effect.00 Permeate flux (LMH) 300.00 50. the dynamic behavior of the 3th experiment (DUF 3) is shown in Figure 19 and Figure 20.00 250. The experiments labels stand for Dynamic Ultrafiltration (DUF). This disturbance is rejected by the constant flux controller that manipulates the feed pump. From the flux values in the figure.
35 19 0.8 1. flux conditions LMH 63 125 175 150 TMP REC PERM 0.6 0.55 28 0.50 22.15 17 750 0.55 40 260 Maximum flux conditions LMH 200 280 276 435 TMP REC 0.10 7 720 0. there is a reduction around 50% from DUF2 to DUF3. It can be seen that the operating window was extended for the last experiments. Despite the first experiment was performed using the highest average inlet concentrations.4 TMP (bar) 1. Summary of the tuning experiments before the skimming tanks.60 33 310 0. The minimum flux condition is the starting point. it has shown the best permeabilities. 2 1. Table 3.4 0. This result is expected since the membrane was new.39 4.07 Initial PERM ** 1860 600 1250 1500 * From our measurements ** The variance in the initial permeability is highly correlated to the quality of the cleaning water The results depicted in Table 3 give the range of operating conditions achievable given the inlet concentrations. where higher TMPs were tested. The second and third experiments are interesting since they have similar water quality in oil concentration but different suspended solids concentration (TSSDUF3 is more than 2 times TSSDUF2).2 0 13:55:12 15:07:12 16:19:12 17:31:12 18:43:12 Time (h:m:s) Figure 20.6 1.25 65. This effect is visible in the 22 .50 3.32 7. The impact in the permeability is evident at minimum and maximum flux conditions. Values taken by inspection from the display during operation. The maximum flux conditions correspond to the point where the maximum permeate flow was evaluated.2 1 0.5 74.95 62 PERM 700 310 172 435 Average inlet (ppm)* OiW TSS 106. before the BPH.8 0. TMP profile during the critical flux determination (DUF3) The summary of the tuning experiment results are depicted in Table 3.11 70. Point DUF 1 DUF 2 DUF 3 DUF 4 Min.90 24 1.
where a much higher TMP is required in DUF3 to achieve basically the same flux. The water quality during the tuning experiments is shown Figure 21 and Figure 22. From the reported values. Latinametican chemical treatment also measures the concentrations along the process. as mentioned previously (notice that the concentration increases in DUF4).5 0 2 1. between 30% and 65% of the average values reported by the field laboratory4. The situation that generated the change in the feed strategy. with inlet concentrations comparable to the second experiment. This is an indication that effect of the suspended solids on the process does not depend entirely of the concentration. Oil in water concentration at the inlet and outlet of the pilot plant for the tuning experiments For the DUF 3 experiment. The last experiment showed the highest flux at moderate TMPs. it can be seen how the OiW concentration decreases along the test.5 Oil in water oultet (ppm) 120 100 80 60 1 40 20 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 Sample (1 hour difference) DUF 4 ‐ inlet DUF 3 ‐ oulet 0. 180 160 140 Oil in water inlet (ppm) 3. the measured inlet OiW concentrations were considerably lower. The samples 1‐5 were taken the 20/07/2012 (DUF 3) and the remaining samples the 21/07/2012 (DUF 4). The OiW outlet concentration does not necessarily follow the trend in the inlet concentration in the evaluated flux conditions. The data are certified by ANTEK laboratory. and why average concentrations do not entirely represent the system.5 DUF 3 ‐ inlet DUF 4 ‐ outlet Figure 21.5 3 2. all 4 In the field. It has to be accounted for that during DUF 3 the inlet concentration decreased along the experiment while during DUF 4 it increases. 23 . This confirms the variability of the concentrations measured in the field. maximum flux tested. According to the data reported by the field.
Total suspended solids concentration at the inlet and outlet of the pilot plant for the tuning experiments 24 . The TSS concentrations in the permeate stream are very low.3% is the last point in Figure 22.3% and 100%. The maximum outlet concentration is around 3 ppm.3 Total suspendes solids outlet (ppm) 7 6 5 0. Notice that the 82.25 4 0.2 3 2 1 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 Sample (1 hour difference) DUF 3 ‐ inlet DUF 4 ‐ inlet DUF 3 ‐ oulet DUF 4 ‐ outlet 0.35 0. the reduction in the TSS is seen when the feed is in continuous mode (DUF4). The oil removal from the inlet stream during the tuning experiments was between 83.15 0.4%. permeate water fulfill the required the target (max 5 ppm).4 0. for all the other samples the TSS removal was above 95%. For both experiments. Regarding the total suspended solids concentrations.45 0.6 and 99. Some examples of the water quality during DUF 3 and DUF 4 can be seen in Figure 23. the inlet concentration is between 3 and 10 ppm.05 0 Figure 22. in some cases below the detectability of the instrument.1 0. It means that the equipment is not able to distinguish between distillated water and the permeate samples. Interestingly. 9 8 Total suspended solids inlet (ppm) 0. The TSS removal during the tuning experiments was between 82. and does not entirely represent the overall behavior.5 0. there is no concentration decrease along the experiment DUF 3 (see Figure 22).
4. 3. The biggest challenge for these experiments is to achieve stable operation given the disturbances in the inlet concentrations. Higher TMP´s would require a considerable increase in the feed channels pressure in order to keep the constant permeate flux.7 to 1 bar for the evaluated concentrations. backpulse frequency and recovery values were tested. However. From the analysis. A summary of the pilot plant inputs is shown in the Table 4. The purpose of the experiments is to determine a sustainable operation of the system. The precise value for each inlet concentration can be estimated from a rigorous analysis of the experimental data. 12 and 27 hours). This issue is particularly difficult to handle due to the frequency and amplitude of the disturbances. it was seen that the sustainable operation was in the neighborhood of 0. a qualitative inspection of the data provides sufficient preliminary information in order to plan the continuous experiments. Besides. Continuous operation The continuous operation of the system was evaluated at three different operating times (6. In other situations the recovery was manipulated in order to increase productivity or handle disturbances. Pictures of the inlet water and treated water during the tuning experiments The shown flux ranges correspond to the tested values. 25 . the system was operated at constant TMP. the influence of different crossflow. (b) DUF 4 (a) DUF 3 Figure 23. Taking advantage of the longer operation time.
Since the last continuous experiment is the most interesting.20 7.65 63 280 Maximum flux conditions LMH 495 370 610 TMP REC 0.70 35 190 0. the TMP was slightly raised further increasing the flux and the recovery. the flux had decreased more than 50% and reached a new stationary operation point at 240 LMH.70 51 250 0. 5 hours of stable operation was achieved at 0. Despite of this situation. 26 . Table 4. it will be discussed further. Summary of the continuous experiments before the skimming tanks Point CDUF 2 CDUF 4 CDUF 5 Minimum flux conditions LMH 185 135 200 TMP REC PERM 0.14 Initial PERM* 1200 484 2400 * The variance in the initial permeability is highly correlated to the quality of the cleaning water The operation of the CDUF 5 is shown in Figure 24 and Figure 25. First of all.56 16.95 81 0. This operation window represents the best evaluated case. At this point. This prolonged shut down had a negative effect in the plant performance. Later. The operation was recovered after 2 hours.55 bar with 590 LMH and 80% recovery.35 54 0. there was a problem with a valve in the retentate line that forced a shut down. Summary of the operating conditions for the continuous operation of the treatment before the skimming tanks. During the experiment CDUF 4. The impacts of this event are clear on the flux and permeate quality. it can be noticed that the inlet concentrations are substantially higher than during the tuning experiments. Different exogenous events affected the length of the experiments. Test CDUF 2‐ 6h CDUF 4‐ 12h CDUF 5‐ 27h Crossflow Feed pump (auto) (manual) 30 30‐35 30‐40 35‐40 30‐32 30‐35 Backpulse (s) 60‐90 60‐120 60‐90 Backflush (s) 300 300 300 Permeate Retentate 03V01 03V02 04V04(%) (%) (%) 100 40 45 100 55‐60 55‐60 100 40‐70 45‐70 For the continuous operation.91 13. This material is characterized by high OiW and TSS content.4 bar was used. In order to evaluate the plant performance without chemical cleaning. there was a material recirculation from the sludge treatment plant trough the line used for the feed. Nine hours after the incident.60 87 PERM 540 925 1000 Average inlet (ppm) OiW TSS 221. At 10:00 am. In the last continuous experiment (CDUF 5) there was an atypical situation that generated an unsustainable condition. Initially a conservative TMP of 0.74 367. beyond the limits managed in the produced water treatment plant. the results are shown in table 5. the obtained fluxes are within the expected values. it was decided to continue the experiment. This was possible due to the quality of the inlet water.33 722. Table 5. obtaining stable operation for approx 9 hours at an average of 490 LMH with a recovery of 70%.
5 1 TMP (bar) 0. 1000 900 800 700 600 Flux (LMH) 500 400 300 200 100 0 19:54:46 00:42:46 05:30:46 10:18:46 15:06:46 19:54:46 Time (h:m:s) Figure 24. TMP profile during the continuous experiment CDUF 5 27 . Flux profile during the continuous experiment CDUF 5 1.5 ‐1 Time (h:m:s) Figure 25.5 0 19:54:46 00:42:46 05:30:46 10:18:46 15:06:46 19:54:46 ‐0.
some oil was able to pass through the membrane. 1400 1200 200 1000 800 600 400 50 200 0 0 5 CDUF 2 ‐ inlet CDUF 2 ‐ outlet 10 15 20 CDUF 5 ‐ inlet CDUF 5 ‐ outlet 25 Sample CDUF 4 ‐ inlet CDUF 4 ‐ outlet 0 150 Oil in water outlet (ppm) Oil in water inlet (ppm) 250 100 Figure 26.4% and 99. The non satisfactory OiW concentration in the treated water was also influenced by some non complete recovery of the water permeability between experiments. Oil in water concentration at the inlet and outlet of the pilot plant for the continuous operation 28 . only in the average values. The OiW removal is between 67. the permeate water quality indicates that the membrane was saturated with oil.4 and 53. The OiW concentration behavior during the continuous tests is depicted in Figure 26. Evidently. there are big differences (between 40 and 60%. Comparing the inlet concentrations with the average values reported by the field laboratory. Despite the plant achieved a new stationary operation point.4% after the incident in CDUF 5. Meaning that during some periods the pilot plant was operated at higher TMP´s than recommended. the difference at certain points is even higher with the actual concentration being up to 5 times the average. see Figure 17). where the amount of oil in the permeate stream is far beyond the desired value. Due to time constraints. This effect can be seen along the continuous experiments and it is critical in CDUF 5 after the incident.5% for most of the data. it was decided to continue the experiments being aware of the possible consequences. As a consequence. with atypical values of 23. These concentrations are considerably higher than the values used for the equipment tuning.
These values are similar to the average values reported by the field laboratory (see Figure 18). the difference between the expected feed water and the recirculated sludge can be seen.5 1 0. the suspended solid concentrations during the continuous operation are shown. Some pictures of the continuous experiments are shown in Figure 28. The suspended solid removal during the continuous experiments is between 92. Operation at higher TMP’s does not have a significant effect in the concentration in the permeate TSS concentration. 30 Total suspended solids inlet (ppm) 5 Total suspended solids outlet (ppm) 4. the operation was satisfactory and the quality evident.5 2 1.5 0 CDUF 4 ‐ inlet CDUF 4 ‐ outlet Figure 27. Total suspended solids concentration at the inlet and outlet of the pilot plant for the continuous operation In Figure 27.5 and 100%. Despite the concentration picks. After the incident. Due to the low residence time in the machine the effect in the permeate quality is immediate. In the Figure 28(b).5 3 2. the TSS concentrations in the treated water are kept below 2 ppm.5 25 20 15 10 5 0 0 5 CDUF 2 ‐ inlet CDUF 2 ‐ outlet 10 Sample 15 20 CDUF 5 ‐ inlet CDUF 5 ‐ outlet 25 4 3. In Figure 28(c). 29 . due to the incompressible nature of the suspended solids. the water looks like in Figure 28 (d).
30 . Pictures of the inlet water and treated water during the continuous experiments 2. it can be seen that there is considerable variance from day to day.5 Conclusions From this first testing it can be concluded: From the laboratory analysis of the average inlet water characteristics. (a) CDUF 2 – satisfactory performance (b) CDUF 5 – satisfactory performance (c) CDUF 5 – incident time (left the sludge fed) (d) CDUF 5 – after incident Figure 28. where the concentration can easily increase more than 100% The need of the in situ cleaning strategies is evident. since the sustainable fluxes where increased more than 3 times (depending on the inlet concentration and nature).
the oil content in the water indicated the need of a premature chemical cleaning. The oil and TSS removal were up to 99. implying a significant reduction in the flux. 60 s of backpulse frequency and 300 s of backflush. The accidental recirculation of the sludge is the worst water in the field to treat. it is expected that a longer trial time would provide the necessary information for an improved plant operation. The qualitative analysis of the obtained data indicated that the best sustainable operation can be achieved with TMP´s between 0. These variables have a significant influence in the plant performance. Therefore. This result is also influenced by the slope in the inlet concentration. The recommended operating conditions are 30‐40 m3/h of crossflow.5 % and 100%. 31 .7 and 1 bar. large disturbances were evidenced in the feed concentration. There is a considerable variance in the nature of the treated water since it comes from several oil wells in the area. It is relevant to notice that the OiW and TSS loads during the tuning experiments were considerably lower than during the continuous operation. not higher than 5 ppm. the plant operation can be adapted to handle the concentration peaks. Despite new stationary operating points were achieved. It is expected that using this strategy the plant can operate longer time avoiding a premature chemical cleaning. since duplicating the TSS had a significant effect in the TMP necessary to obtain the same flux. Both of these strategies would require continues measurement of OiW content. These results indicate how important is to monitor the inlet concentrations in order to have an appropriate plant operation. During the continuous operation of the plant. respectively. In an industrial scale. even atypical situations.4 % and 100%. The tuning experiments showed a preliminary indication that the concentration and nature of the suspended solids in this field can be a limiting flux factor. The alternative is to have a flexible stages design that allows modifying the plant configuration to guarantee the permeate quality. and still good oil and TSS removal were achieved (up to 99. The tuning experiments showed that the OiW and TSS target concentrations where achieved. One option is to reduce the plant productivity (lower TMP) during abnormal conditions. respectively).
The place where the inlet is taken is a point where the outlet of the 2 skimming tanks is combined.00 30. SK: Skimming tank (Information provided by Latin-American treatment personal. the oil in water and total suspended solids are quantified twice per day.00 80. The average concentration at the inlet of the skimming tanks in those days was between 200 ppm and 400 ppm. 32 .00 40. The average values during the testing days are shown in the following plots.00 20.1. at HOCOL) In contrast to the previous feed point. The two skimmers behaved similarly.00 70.00 60. the variance in the inlet concentration is not that high. Characteristics of the inlet water – field information In the field. 4. the skimming tanks were able to remove around 85% of the oil.00 SK 1 SK 2 Figure 29. 90. Experimental evaluation point: After the skimming tanks The test in this evaluation point took place between the 30/07/2012 to 03/08/2012. Oil in water concentration at the outlet of the oil recovery section.00 0. There is only one pick the 31st of July during the tuning experiments.00 OIW (ppm) 50.00 10. 4.
00 SK 2 Figure 30. However. The operating conditions for the tuning experiments are shown in Table 6. The purpose of the skimming tanks is to recover the remaining oil in the water.00 TSS (ppm) 4. the water quality from the filter was exceptionally good (below 1 ppm OiW/TSS).00 2. parts of the suspended solids are hydrocarbons of interest (soluble in xylene) and are supposed to be recovered in the skimmers.00 7. SK: Skimming tanks. approximately 60% of the solids were removed with the oil. part of the suspended solids is removed too.00 5. According to the current understanding of the nature of the suspended solids by the people in the field. During this part of the experiment. Operating window identification Operability investigation The experiments were carried out using a constant feed coming from the skimming tanks and at constant permeate operation mode. In these days. The variance is moderated having a pick the 31st of July as well. 4. the tuning experiments started using a low recovery and it was increased step wise between experiments. 8. Once again.00 0. The water for washing and permeability estimation was taken from the walnut shell filter 2.00 6.00 1. Total suspended solids concentration at the outlet of the Skimming tanks.2.00 SK 1 3. 33 . (Information provided by Latin-American treatment personal. at HOCOL) The TSS concentration follows the behavior of the OiW.
Flux and TMP profile during the critical flux determination TMP (bar) 34 It can be seen that for the given inlet concentration of the last tuning experiment. Table 6.5 1 0. Summary of the operating conditions for the tuning experiments Test DUF 1 DUF 2 DUF 3 Crossflow Feed pump Backpulse (auto) (auto) (s) 30 28‐38 90 30 29‐50 90 30 28‐58 90 Backflush (s) 300 300 300 Permeate 04V04(%) 100 55‐90 60‐100 Retentate 03V01(%) 03V02(%) 70‐80 70‐80 50‐60 50‐60 40 40 As an example of the results obtained.5 0 Flux (LMH) 600 500 400 300 200 100 0 17:45:36 18:28:48 19:12:00 19:55:12 20:38:24 21:21:36 22:04:48 Time (h:m:s) Figure 31. .5 2 1.5 3 2. higher fluxes are achievable compared to the previous feed point and the noise is reduced.5 4 3. The summary of the results for the tuning experiments are depicted in Table 7. the dynamic behavior of the 3rd experiment (DUF 3) is shown in Figure 31. 1000 900 800 700 5 LMH TMP 4.
70 60 Oil in water inlet (ppm) 10 9 Oil in water outlet (ppm) 8 50 40 30 20 10 0 0 5 10 Sample DUF 1 ‐ inlet DUF 1 ‐ outlet DUF 2 ‐ inlet DUF 2 ‐ outlet DUF 3 ‐ inlet DUF 3 ‐ outlet 15 20 25 7 6 5 4 3 2 1 0 Figure 32.21 Initial PERM * 1700 1300 2400 * The variance in the initial permeability is highly correlated to the quality of the cleaning water From the table can. respectively). The data 1‐5 were taken the 30/07/2012 (DUF 1). Table 7.95 71 1. the fluxes do not increase in the same ratio.15 74 1600 Maximum flux conditions LMH 501 692 816 TMP REC 0. it be seen that the initial and final fluxes where increased as well as the recovery between experiments. The influence of the OiW and TSS concentrations is not clearly visible from the results.30 3. Oil in water concentration at the inlet and outlet of the pilot plant for the tuning experiments 35 . High permeabilities are evidenced at minimum flux conditions.23 3.65 85 PERM 1200 767 490 Average inlet (ppm) OiW TSS 8. Comparing the fluxes from DUF 2 and DUF 3 at similar TMPs.02 22.35 46 0. Considering the reduced OiW and TSS load in the feed. 6‐13 taken the 31/07/2012 (DUF 2) and 14‐22 taken the 1/08/2012 (DUF 3).2 31 1250 0. The water quality during the tuning experiments is shown in Figure 32 and Figure 33.15 40 1300 0. The last tuning experiment has shown the highest flux and recovery (816 LMH and 85%. a situation that changes for the maximum flux conditions.58 6. the results are comparable despite the differences in the inlet concentrations (results not shown in the table).17 38. Values taken by inspection from the display during operation before de BPH Point DUF 1 DUF 2 DUF 3 Minimum flux conditions LMH 250 250 315 TMP REC PERM 0. Summary of the tuning experiments before the skimming tanks.
15 0.35 Figure 33. where the biggest difference is 21%.5 0. in several cases the removal was 100%. There is not a clear trend in the OiW inlet concentrations.3 0.2 0. The oil removal from the inlet stream during the tuning experiments was between 55.05 0 0 DUF 1 ‐ inlet DUF 1 ‐ outlet 5 10 Sample DUF 2 ‐ inlet DUF 2 ‐ outlet DUF 3 ‐ inlet DUF 3 ‐ outlet 15 20 25 TSS oulet (ppm) 7 6 5 4 3 2 1 0 0.8 and 100%. there is only one value that is slightly above the desired limit. it is expected to have the sustainable operation using TMPs between 0. Pictures of the treated water can be seen in Figure 34. Comparing the average oil concentration measured during the experiments (Table 7) and the values reported by the laboratory in the field (Figure 29).25 0. achieving between 91. 10 9 8 TSS inlet (ppm) 0. our values are between 50% and 100% higher.45 0. The remarkable low concentrations in the treated water has to be highlighted. Regarding the outlet concentration. but the lowest is an atypical data since most of them are above 95%. 36 . From the inspection of the tuning results.1 0. The TSS removal from this inlet stream is considerable superior compared to the previous feed point.2% and 100%. Total suspended solids concentration at the inlet and outlet of the pilot plant for the tuning experiments The suspended solid concentrations are more in accordance with the values reported by the laboratory in the field. Some examples of the water quality during DUF 2 and DUF 3 can be seen in Figure 33.4 0.8 and 1 bar.
The initial flux was around 400 LMH which declined with time and achieved stable operation at around 340 LMH after 5 hours of operation. Only one point is evaluated due to time constraints. a moderate TMP was chosen to start with. the operation in this point was more stable and potentially 37 . Continuous operation The continuous operation of the system was evaluated for 26 hours without a chemical cleaning. Table 8. (a) DUF 2 (b) DUF 3 Figure 34.3. Summary of the operating conditions for the continuous operation of the treatment after the skimming tanks. The system was operated at constant TMP. The system achieved a new stationary operating point at a TMP of 1. The biggest challenge is still to achieve stable operation given the disturbances in the inlet concentrations. When the experiment started. Pictures of the inlet water and treated water during the tuning experiments 4. The sustainable flux was very similar to the fluxes obtained for the previous feed point. After 19 hour of operation. A summary of the pilot plant inputs is shown in the Table 8. Based on the tuning experiments it should provide a flux of approximately 500 LMH. This flux was maintained all night slightly increasing the TMP. it is decided to operate at constant flux conditions with a target of 440 LMH.2 bar. Test CDUF 26 h Crossflow Feed pump (auto) (manual) 30‐40 28‐45 Backpulse (s) 60‐90 Backflush (s) 300 Permeate Retentate 03V01 03V02 04V04(%) (%) (%) 80‐90 40‐50 40‐50 For the continuous operation. the results are shown in Table 9 and data shown in Figure 35 and Figure 36. However.
86 Initial PERM* 1700 * The variance in the initial permeability is highly correlated to the quality of the cleaning water Flux (LMH) 500 400 300 200 100 0 13:55:12 18:43:12 23:31:12 04:19:12 09:07:12 13:55:12 Time (h:m:s) Figure 35. longer operating time between chemical cleanings. Flux profile during the continuous experiment CDUF 26h 38 . Table 9. Summary of the continuous experiments after the skimming tanks Operating Minimum flux conditions point LMH TMP REC PERM CDUF 26h 310 0. specially using the constant permeate operating mode.6 63 490 800 700 600 Maximum flux conditions LMH TMP REC PERM 440 1.36 2.2 68 390 Average inlet (ppm) OiW TSS 20.
Oil in water concentration at the inlet and outlet of the pilot plant for the continuous operation 39 . 45 40 Oil in water inlet (ppm) 0.5 0.0 0.3 0.5 18:43:12 23:31:12 04:19:12 09:07:12 13:55:12 Time (h:m:s) Figure 36.5 0.5 TMP (bar) 1. 2.0 1. TMP profile during the continuous experiment CDUF 26h The water quality during the continuous experiment is shown in Figure 37 and Figure 38.7 0.2 0.0 13:55:12 ‐0.6 0.4 0.1 0 0 2 4 6 Sample 8 10 12 Oil in water outlet (ppm) 35 30 25 20 15 10 5 0 CDUF 1 ‐ inlet CDUF 1 ‐ outlet Figure 37.
40 . Total suspended solids concentration at the inlet and outlet of the pilot plant for the continuous operation The suspended solids inlet concentration was stable at the beginning of the experiment whereas some disturbances appeared towards the end.4 0.25 0. Some pictures of the continuous operation of the plant are depicted in Figure 39.3% and 100%.5 4 3. 5 4.05 0 Total suspended solids (ppm) Total suspended solids(ppm) Figure 38.5 1 0. Only at the end there was a considerable increase in the concentration. The TSS removal was 100% in most of the cases.2 0. It can be seen in Figure 37 that at the beginning of the experiment the OiW concentration was rather constant for 18 hours.5 3 2.5 0.1 0.5 2 1. only one point showed a lower removal (96.3 0.45 0.4 %). Despite this moderate variation.35 0. the OiW content in the treated water was kept below 1 ppm.5 0 0 2 4 6 Sample CDUF 1 ‐ inlet CDUF 1 ‐ outlet 8 10 12 0.15 0. The oil removal was between 96.
it is not that relevant to monitor the inlet concentration. From the tuning experiments it is expected to have better fluxes. Stationary operation was achieved at moderate flux conditions first 340 LMH and later 440 LMH. At this feed point.4 Conclusions (b) Suspended solids Figure 39. During the continuous operation of the plant. not higher than 5 ppm. The tuning experiments of the second sampling point (after skimming tanks) showed improvements in the maximum flux compared to the first feed point evaluated (before skimming tanks). it can be seen that there is considerable variance from day to day. where the concentration can easily amplify several times (eight for OiW and two for TSS). a backflush frequency of 300 s.8 and 1 bar. around 30%. The oil and TSS removal were up to 100%. The qualitative analysis of the obtained data indicated that the best sustainable operation can be achieved with TMP´s between 0. this result is not linearly correlated with the changes in the inlet concentrations for both points. a backpulse frequency of 60 s. the OiW and TSS target were achieved (concentration below 5 ppm). 41 . (a) OiW content 4. Pictures of the inlet water and treated water during the tuning experiments From this first testing it can be concluded: From the laboratory analysis of the average inlet water characteristics. using 30 m3/h cross flow. The tuning experiments shown that the OiW and TSS target concentrations where achieved. However. since the Skimming tanks act storage tanks that buffer the inlet disturbances. moderate disturbances were evidenced in the feed concentration. During the continuous operation.
It is acceptable to have a flux recovery above 70%. 5. Initially the cleaning strategy consisted of one washing cycle: 1. TMP.0 Recovery (%) 70. It can be concluded that the type of fouling evidenced in the field is reversible to the desired point in most of the cases. Flux recovery after chemical cleaning. 4.0 90. it was difficult to recover permeability. 50 m3/h crossflow Flushing with water 100. The results of the experiments are depicted in Figure 40. Flushing with water Alkaline cleaning: 30 min with 1% NaOH.0 10. a loss of cleaning efficiency was evidenced the 14/07/2012 and 21/07/2012.0 60. was decided to use 2 washing cycles in order to recover the water permeability. 2. even after the 2 washing cycles.0 0. After the continuous tests performed on the 24/07/2012.0 50.0 40. Cleaning in place evaluation The cleaning strategy was evaluated through the water permeability evaluation. However. The initial water permeability was 2800 LMH/bar. The initial water permeability of the membrane was 2800 LMH/bar at a TMP= 0.0 30.0 Figure 40. However. The 21/07/2012.2 bar and using a cross flow of 30 m3/h. recovery and operation time. 3. The fouling load in each of the experiments was different mainly due to changes in inlet concentrations.0 80. the desired permeability was restored after the 26/07/2012. Those dates correspond to the second sampling point (after skimming tanks). 42 . 5. One cleaning cycle was enough during the first operation days. cleaning water quality.0 20. 50 m3/h crossflow Flushing with water Acid cleaning: 30 min with 1% Oxalic acid.
2 Operability Monitoring level required: significant Changes in the operating conditions: significant Chemical cleaning frequency: largely depends on the atypical events faced during continuous operation Longer operation might show other operation challenges (i.2 Operability Monitoring level required: low Changes in the operating conditions: low Chemical cleaning frequency: considerable lower than in the first evaluation point.1.e.1.1 Inlet water quality Variance in the inlet water quality: high Variance in the outlet water quality: low 5. Final remarks Evaluation point before skimming tanks: 5. 6. Membranes arrangement: parallel/series configuration with multiple membrane housings could be exploited Evaluation point after the skimming tanks: 126.96.36.199. The appropriate frequency can be estimated from and OPEX analysis 5. scaling and irreversible fouling) 5.3 Other aspects Technical feasibility: it is recommended to include a buffer tank to assist the membrane operation.1 Inlet water quality Variance in the inlet water quality: moderate Variance in the outlet water quality: negligible 5.1.3 Other aspects Technical feasibility: high Membranes arrangement: parallel/series configuration could be exploited 43 .
making the estimation of the sustainable operation more difficult. 7. The methodology used for the determination of the operative window is impaired by fluctuations in the inlet concentrations. This information is not only relevant for the operation but to improve the cleaning strategies. These topics remain for investigation. The variance in the inlet concentration is probably the biggest obstacle to tune the system and to operate in continuous. Besides. Further developments in the tuning strategy are needed. Future challenges It is important to understand further the characteristics of the feed streams. the interactions between the acid and alkaline solutions and the chemicals added. 44 . Further electric protection for the system can avoid damage. In the field there are interactions between the pilot plant and the existing installations at industrial scale. Monitoring of the inlet concentration is relevant for the appropriate operation. not only concentrations. There is a lack of understanding of the interactions between the added chemicals in the actual treatment and the membrane.
the TMP cannot be restored when moving from the next step due to the higher flux in between. Additionally. and Jonsson. Good examples of the obtained plots are shown in Figure 41 and Figure 42. The critical flux is determined for a notable increase in the fouling rate by increasing the flux. Details of the methods can be found in the mentioned paper.1 Evaluation before the skimming tanks For this test point. referred to as average pressure and fouling rate methods. the flux is increased step wise aiming to find where the production becomes unsustainable for the given input water quality. The critical flux is estimated using two different methods. This method evaluates the difference TMP for the same flux level steps. It should be mentioned that not all the experiments behave as in the ideal case. a) Average pressure: this method evaluates the average TMP against the average flux along the experiment. meaning the presence of a maximum flux. so they are referred to as dynamic ultrafiltration (DUF). When fouling starts to get irreversible. It is believed that the concentration changes along the experiments are the main reason.P. the variance in the inlet concentration is the biggest obstacle to determine the critical flux. there are four tuning experiments. AIChE Journal 56(7). Appendix: Critical flux estimation The critical flux was estimated using two different methodologies described in literature5. b) Fouling rate method: this method evaluates the fouling rate (dP/dt) against the average flux along the experiment. 8. G. 5 Beier. 8. As mentioned extensively along the report. c) Irreversible fouling: it should be understood as the onset of the irreversible fouling. According to the employed methodology during the experiments. Small description of the methods is presented bellow. 45 . it is better to aim for identification of the critical flux window for each of the evaluated test points. so it is called conventional ultrafiltration (CUF). Critical Flux Determination by Fux Stepping. The remaining experiments use the backpulse and backflush. The critical flux is determined by the deviation from linearity. 1739‐1747. Therefore. A summary of the results for all experiments are shown in Table 10. the step up‐down test allows identifying when the irreversible fouling starts forming. The first one does not use the in situ cleaning strategies. S.
450 400 350 Average flux (LMH) 300 250 200 150 100 50 0 0.74 0.72 0.84 0.82 0. Fouling rate method results for critical flux estimation.76 0.8 bar) 18 16 14 12 dP/dt (bar/h) 10 8 6 4 2 0 100 110 120 130 140 150 Flux (LMH) 160 170 180 190 200 Figure 42.78 0. Average pressure method for critical flux estimation. Results from CUF experiment (Critical flux 150 LMH) 46 . Results of experiment DUF4 (Critical flux at 0.86 Average TMP (bar) Figure 41.80 0.
05 218.41 0.5 0. From the experiments.63 186. However.97 26.84 341. In Figure 44.09 240. the maximum evaluated flux is shown.65 1.80 0.23 0.5 0.09 240.00 155. both methods gave considerable different results (approx. 25%).80 0. the information gathered was used in the following experiments. that the critical flux was not achieved in DUF1 and DUF2.41 0.72 Critical flux Method (dP/dt) Flux TMP dP/dt (MLH) (bar) (bar/h) 150 0.21 352.24 2.69 2.5 0.30 170. it can be seen that the critical flux lies between 200 and 350 LMH.53 352. Critical flux from the tuning experiments before the skimming tanks Only for the conventional ultrafiltration.61 * Critical flux not achieved.69 2. The results are presented in Figure 43 and Figure 44.69 182.05 205. For this reason. Table 10.96 186.23 0.54 15. Experiment CUF DUF 1* DUF 2* DUF 3 DUF 4 Critical flux Method (Avg P) Flux TMP dP/dt (MLH) (bar) (bar/h) 187.56 0.95 6. Critical flux estimation from the tuning experiments before the skimming tanks. the critical flux is not achieved in all cases. the critical TMP 47 .72 Irreversible fouling flux (LMH) 150. It can be seen in Table 10.24 2.03 0. 400 350 Critical flux (LMH) 300 250 200 150 100 50 0 CUF DUF 1 DUF 2 Experiment dP/dt Avg. This range is broad and totally depends on the concentrations given during the tuning experiments. Therefore. the operating TMP is considered as a better way to delimit the operating window since the operation mode is constant TMP. P DUF 3 DUF 4 Figure 43. then maximum value depicted Due to time constraints performing the experiment.
and referred to as dynamic ultrafiltration (DUF). For that reason. there are three tuning experiments.24 0.2 0 CUF DUF 1* DUF 2* Experiment dP/dt Avg. Table 11.14 573. Critical TMP from the tuning experiments before the skimming tanks 8.4 0.8 0.25 Critical flux Method (dP/dt) Flux TMP dP/dt (MLH) (bar) (bar/h) 405.24 0.32 ‐0. All the experiments use the backpulse and backflush. window can be identified between 0.2 Evaluation after the skimming tanks For the test after the skimming tanks.97 Irreversible fouling flux (LMH) N/A 486.94 600. Good examples of the obtained plots are depicted in Figure 45 and Figure 46. In most of the cases the onset of the irreversible fouling formation is lower than the critical flux (see Table 10).14 573.32 536.24 11.69 1.6 0.03 0. P DUF 3 DUF 4 Figure 44.69 1. the continuous experiments were performed using a conservative TMP and sustainable operation was achieved due to the in situ cleaning strategies.87 * Critical flux not achieved. The summary of the results of all experiments are shown in Table 11.97 0.03 0. Critical flux estimation from the tuning experiments after the skimming tanks Experiment DUF 1* DUF 2* DUF 3 Critical flux Method (Avg P) Flux TMP dP/dt (MLH) (bar) (bar/h) 405. 1 Critical TMP (bar) 0.7 and 1 bar.88 1. This confirms the conclusions obtained in the field for this testing point.28 1.94 703.32 ‐0. then maximum value depicted 48 .
00 0. Notice that the first two experiments. Results from DUF experiment (Critical flux 645.40 0. Results of experiment DUF3 (Critical flux at 1. DUF1 and DUF2. The results from Table 11 are depicted in Figure 47 and Figure 48. 800 700 Average Flux (LMH) 600 500 400 300 200 100 0 0. 49 .20 0. and then the last with relatively low fouling rate is selected (notice that the second plot has only 4 points.40 Average TMP (bar) Figure 45. did not achieve the critical flux.86 LMH) In the average pressure method (Figure 45). In the second method the critical flux lies between the last two evaluated points.60 0. Average pressure method for critical flux estimation.00 1.80 1. Fouling rate method results for critical flux estimation.24 bar) 12 10 dP/dt (bar/h) 8 6 4 2 0 400 450 500 550 600 650 700 750 Average flux (LMH) Figure 46. this is due to a lost in the data for this experiment).20 1. the deviation from linear behavior occurs in the maximum flux evaluated.
it is estimated to have sustainable fluxes between 600 and 700 LMH. For evaluation of this point. P DUF 3 Figure 47. Critical flux from the tuning experiments after the skimming tanks From the experiments. In that case. 1. For this testing point. more conservative sustainable fluxes are expected. Nevertheless.5 Critical TMP (bar) 1 0. P dP/dt dP/dt Avg. the obtained critical fluxes are slightly different (approx. Critical TMP from the tuning experiments after the skimming tanks 50 . it is difficult to determine if both methods are giving the same results since only one experiment achieved the critical flux. This was confirmed during continuous operation where the system operated at maximum 440 LMH.5 0 DUF 1* DUF 2* Experiment Avg. … DUF 3 Figure 48. 800 Critical flux (LMH) 600 400 200 0 DUF 1* DUF 2* Experiment dP/dt Avg. The limited information was collected in this evaluation point due to time constraints. this result depends on the evaluated concentrations. 16%).
2 bar. This confirms as well the proposed operating window investigated during continuous operation. the onset of the irreversible fouling formation occurs again at fluxes lower than the identified critical fluxes (see Table 11). Once again. 51 . It can be seen in Figure 48 that the TMP operating window lies between 0.8 and 1. it is relevant to determine the TMP operating window. Finally.