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Open access peer-reviewed chapter

Brusque Review of Salt Recovery from Reverse Osmosis Rejects

Submitted: November 21st, 2018 Reviewed: July 19th, 2019 Published: October 15th, 2019

DOI: 10.5772/intechopen.88716

From the Edited Book

Salt in the Earth

Edited past Mualla Cengiz Çinku and Savas Karabulut

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Abstract

The membrane treatment is a physical separation which also generates considerable amount of waste, chosen as refuse/concentrate. The refuse/concentrate is more than three times concentrated than the feed h2o in terms of feed water salts. Recovery of valuables from reverse osmosis (RO) decline for its reuse of inorganic salts would be most obvious solution to eliminate ecology harm. In this study what are the available methods for the recovery of valuables from waste saline stream past selective crystallization method, chemical precipitation and physico-thermal route discussed in details. Besides, methods to treat organic contamination in the residual solution through avant-garde oxidation treatment methods.

Keywords

  • reverse osmosis
  • salt recovery
  • reactive precipitation
  • crystallization

i. Introduction

The need of beverage h2o led to significant improvements in the membrane separation process in water and waste-water treatment. Specially for developing countries, the demand of water supply is increasing and no less provision to mitigate the challenges. The land and central governments agencies are formulating strategy through ecology policies to mitigate the h2o scarcity. During last three decades significant expansion and upgradation of membrane filtration have been happening around the globe to lower it production costs. In market, there are many custom made membrane technologies that are available for both domestic and industrial applications. Contrary osmosis is 1 of the important technologies among which has free energy and cost constructive membrane organization for producing potable water from brackish and saline water sources [i, 2, 3, four, 5, 6, 7]. RO process tin can generates 50–80% of h2o drink or dischargeable quality as permeate [seven] and the balance 20–thirty% formed as RO refuse or retentate or concentrate. Generally, concentrate is immune to avert membrane fouling, coagulation and flocculation process over membrane surfaces as it cannot be further purified due to high osmotic pressure. The common application of membrane separation processes comprising ultrafiltration and reverse osmosis for the disposal of reverse osmosis (RO) rejects through thermal evaporator or multiple effect evaporator.

1.1 Characteristics of membrane concentrate

Membrane separation is a physical process which involving the separation of particulate, and dissolved organic/inorganic compounds from a feed liquid using a semi-permeable membrane system. The feed stream is fractionated into two streams: (i) a permeate stream that contains the solvent (h2o) that passes through the membrane, and (ii) the reject stream known as concentrate, reject or alkali contains the solute. The characteristics of this reject stream depend primarily on the membrane engineering used, the quality of feed h2o, the per centum recovery of water, the physico-chemic treatment methods followed for cleaning procedures. The volume of refuse stream varies widely from ten to sixty% of the feed h2o volume [7]. However, the reject stream arises from industrial effluents such as textile, pharmaceutical and tanneries are turbid and opaque, may be due to the presence of micro and macro organic molecules and inorganic ions, such as chlorides, sulfates, phosphate, carbonate, bicarbonate, sodium, calcium, magnesium and other heavy metallic ions [8]. The characteristics of RO stream generated in leather industry are presented in Table 1. The TDS of water is increased from five.58 ± i.8 to 20 ± half-dozen.fourteen thou/L in RO reject stream leaving production water with a TDS of 0.25 ± 0.13 chiliad/L during separation process. The TDS concentration of RO rejects four fold higher than the initial TDS concentration. Similarly, concentration of sodium, chloride and sulfates ions were constitute to be increased significantly after RO separation procedure in reject stream.

Table 1.

Characteristics of untreated, treated, RO permeate and RO pass up stream generated in leather industry.

one.two Impacts of membrane concentrate discharge without handling

Belch of RO turn down stream into bounding main/ocean is considered to cause the "sea desert" in vicinity to pipe outlet because of dissolved substance with high specific weight and thus sink in bottom of the ocean/sea, which severely affecting local marine biota. Marine species have been affected by the salinity of the brine discharged into the body of water include grass prairies called such equally Cymodocea nodosa and Caulerpa prolifera or red algae [9]. Direct land disposal of RO reject stream from effluent handling plants acquired soil and groundwater contamination past the diffusion of inorganic impurities from it, and thus soil and footing water are turned unsuitable for human consumption for their harmful or toxic substances. Hence, there has been abiding exploration to manage the RO turn down stream.

one.3 Options for membrane concentrate disposal

Various options have been reported for the disposal of RO reject stream generated in membrane separation. This choice is belch to surface water, deep wells, solar evaporation ponds, and thermal evaporators. The option of technologies for the disposal of RO rejects is based on the prevailing environmental regulations, investment and maintenance costs, and site-specific conditions [10, 11].

The reduction of concentrate book is existence achieved by incorporating zero liquid discharge technologies. The concentrate streams later on conventional RO are beingness evaporated in thermal evaporators to sufficiently dry inorganic salt. The most mutual way is vertical falling film brine concentrator followed forced-apportionment crystallizer, where it is heated above its normal boiling temperature with steam through heat exchanger. It requires 65–80 kWh of power per grand l of crystallizer feed water. Crystallizers and spray dryers accept been implemented at the commercial level to reduce RO pass up stream into a solid product for landfill disposal. One or more evaporation steps could also be considered to recover pocket-sized amounts of water from the near soluble salts in RO decline stream. The primary practical obstruction in implementing thermal evaporators is size and complication of the equipment. In addition, evaporators and crystallizers are relatively complex to operate and loftier energy intensive process compared with other zero liquid discharge (ZLD) methods.

The evaporators and crystallizers are used to reduce the refuse book upward to five% of the feed volume and the residual 95% was reclaimed every bit distillate (water) afterward condensation. Generally, the decline stream generated from leather industry is evaporated in solar evaporation pans to reduce its volume (for small book of discharge and making use of solar free energy to reduce the cost of evaporation) or in a multiple result evaporator (MEE) (for big volume of belch) leaving behind a solid residue known as residue afterwards evaporation (RAE).

1.iv Limitations on disposal of residue subsequently evaporation generated from leather manufacture

The disposal of RAE onto secured landfill sites is banned by the pollution control agencies because the constituent ions are suspected to exist leached into aqueous solution, and the treatability of leachate would exist more difficult for its loftier salinity. Hence, RAE is collected and being stored in the storage yard without further reusable options in many textile and leather industries. The high concentration of mixture of inorganic and organic salts present in RAE restrains it from disposal [thirteen, 14].

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two. Desalting process for RO concentrate

Recovery of salts from RO concentrate is increasing for its environmental safety way to reuse of waste volume of reject. The modify of solution temperature either by evaporation and cooling used to extract salts from concentrate has been widely used worldwide. In which, electro-dialysis, ion-substitution, eutectic freezing, and chemical processing are being practiced to recover salts from concentrate. Further, in accelerate hybrid systems which consisting of combination of two or more separation process techniques, such as the nanofiltration—opposite osmosis—thermal processes, are being deployed actively to increase the corporeality of extracted salt and reduce the final volume of turn down.

Buckley et al. has proposed detailed routs for the management of RO reject [12]:

  1. Apply of technology knowledge: incorporation of engineering science unit operation/procedure to reduce dissolved solids in the turn down stream.

  2. Chemical conversion of reject to products: chemical conversion of rejects to other reusable salts from waste RO turn down.

  3. Directly and indirect discharge of concentrated brine by dilution without affecting receiving environment.

  4. Stabilization of concentrate to inert textile: stabilizing the waste product concentrate into chemically stable cloth.

ii.i Evaporation and cooling

Recovery of valuable salts or minerals can be obtained from RO concentrate or stagnant water by altering solution temperature either by evaporation or cooling effect. There are reports on evaporators are being practiced in brine management, among which multiple effect evaporator (MEE) are most promising and cost effective. The MEE operate based on the principle of reducing the vapor pressure of solution within the system to let humid occurs at depression temperature. The multiple effect evaporator feed water is boiled and pumped into tube side in the evaporator in series. The result of steam has been condensed over the tube wall of the evaporator and collected as water to reuse. The backlog heat is further used for the boiling of inlet water.

In other way, vapor compression distillation (VCD) is used for the desalination procedure. In VCD inlet water is boiled through heater to vaporize and discharged through evaporative compressor. The generated vapor has been compressed and used equally steam supply for boiling concentrate and the condensate product is obtained after pinch procedure.

ii.two Electro-dialysis (ED) and ion commutation

Electro-dialysis system consists of anion-exchange and cation-exchange membranes are being arranged alternately in a large cell of compartment betwixt an anode and a cathode. The influence of applied electric field, the various ions could migrate towards the electrodes based on its ionic charge. The membranes are permeable but to cations or anions, through which the water between the membranes are alternately depleted and enriched with common salt ions. The cation membranes allow only positively charged ions to diffuse through them. Similarly, anion substitution membrane allows merely negatively charge ions. Electro-dialysis is being considered used as a pre-treatment or a pre-concentration method for brine direction [xv, xvi, 17]. This method of application significantly reduces the concentration of calcium or sulfate ions from gypsum crystallization during farther evaporation [xv]. Even so, fouling by colloidal material, organics, and bio-growth should exist taken care for the effective and sustainable use of the equipment.

The functioning of ion exchange processes based on packed bed column resin, which are generally organic resins that contains hydrogen ions and is capable of exchanging positive ions nowadays in the feed water. The ion exchange processes are being studied, investigated, and applied for many desalting process over several decades [xviii, nineteen, 20, 21, 22, 23, 24, 25]. However, this method of handling applies only to low concentrations of salts containing alkali water and its cost of regeneration is also college.

2.3 Eutectic freezing crystallization (EFC)

In this process, the feed concentrate stream is frozen continuously until it reaches a eutectic temperature. The ice being forming.

If the unsaturated concentrate is reaching its freezing bespeak. At the specific eutectic point of crystallization, the alkali salt is crystallized out every bit product. The energy required for the EFC procedure are institute to exist very less than the conventional method of evaporative and cooling crystallization procedure and its theoretically possible way to complete the conversion of concentrate water into h2o and solidified solutes.

Through this route magnesium sulfate heptahydrate (MgSO4·7HtwoO) from a magnesium sulfate industrial stream is existence recovered using EFC procedure [26, 27]. In which MgSO4·12HiiO was formed in the crystallizer and afterwards recrystallization MgSO4·7H2O is formed spontaneously. In addition to EFC, coupling of cooled deejay cavalcade crystallizer (CDCC) helps to recover CuSO4 crystals from copper sulfate solution [28, 29]. The cost towards energy required for EFC can be reduced up to 70% than conventional evaporative crystallization processes, further 100% conversion of concentrate into water and salt separation is achieved by this route.

2.iv Chemical procedure

Recovery of CaCO3 from nanofiltration reject is being achieved past reactive precipitation on addition of NaHCO3/NaiiCO3 aqueous solution [thirty]. Similarly, recovery of MgSO4·7HiiO from the reject from seawater nanofiltration, Catwo+ ions were precipitated as carbonates past reaction with NaHCO3/NaiiCO3 to get calcium sulfate by precipitation, Sodium-bi-carbonate solutions are beingness produced by reactive transfer of carbon dioxide into sodium hydroxide solutions. This technique has been used successfully to recover magnesium sulfate from sulfate rich brine, stone forming minerals, and salty lake water [31, 32, 33]. There are many sequential extraction of salts from rejected brine thus which high concentration of dissolved sulfate, potassium, and magnesium salts are being separated through multiple result evaporator and cooling crystallization method, reactive precipitation methods [15, 28]. The utilise of lime favors selective separation of magnesium hydroxide from concentrate solution and thermal calcination of concentrate having sodium sulfate helps to recover Na2SOfour from wastewater [34]. The reject generated from material dyeing manufacture contains large corporeality of Na2Then4 and thus being recovered through multiple effect evaporation and/or calcinating the full-bodied reject in a muffle furnace at a temperature range of 300 and 800°C [35].

2.5 Extraction of potentially profitable material from RO rejects

2.v.1 Calcium

The recovery of calcium from RO turn down is done to avoid secondary RO scaling [36, 37, 38]. Bond and Veerapaneni [36] accept developed detailed methodology for the recovery of calcium carbonate by chemical precipitation, in detail to carve up calcium during desalination. Several other researchers have evaluated fluidized bed crystallizers for the production of calcium carbonate pellets from RO turn down [36, 39], further studies have been reported on influence of anti-scalants, impurities, metals, and ions on calcium carbonate precipitation [40, 41, 42]. The concentration of calcium ions in seawater and desalination reject is relatively high, through this calcium carbonate pellets has been prepared from brackish h2o in Southern California [39]. However, the extraction of calcium sulfate from RO reject has non received meaning attending, due to low price of commercial form gypsum. Besides, the mechanisms of calcium sulfate atmospheric precipitation have been observed to form scaling minimized equipment failure in separation process [43, 44, 45, 46]. The ion-substitution resin is being used to selectively excerpt calcium sulfate salts from RO reject by controlling the pH of the mixture of anion and cation regeneration solution.

2.5.2 Magnesium

The main unit processes used for the extraction of magnesium is evaporation cum crystallization, precipitation, and ion-commutation. Ohya et al. [47, 48, 49] proposed a series of integrated processes (crystallization, electro-dialysis, ion-commutation) to recover salts of calcium carbonate, sodium chloride and magnesium sulfate from RO refuse. Drioli et al. identified a process of membrane crystallization/distillation to separate out various inorganic salts from reject streams from an integrated NF/RO process [30, 50]. In Russian federation, a large scale extraction institute is besides existence operated for the recovery of magnesium from seawater using ion-exchange, and extraction of magnesium from RO decline from seawater desalination system.

2.5.three Potassium

Worldwide potash consumption is increasing every year approximately at a rate of 3% due to population growth and other increased demand for fertilizers [51]. The main source of potash product is done by conventional shaft mining or deep-well solution mining process techniques. Currently, potassium is being produced from seawater as a byproduct from solar common salt evaporation. Every bit an alternative to solar evaporation/atmospheric precipitation, several researchers take suggested that, potassium could exist produced from RO decline using an evaporation/crystallization procedure [52, 53]. The extraction of potassium is done using natural zeolite (clinoptilolites) ion-substitution materials which has high substitution capacity for potassium through a two-footstep dual-temperature procedure.

ii.5.4 Sodium

The production of sodium compounds from desalination reject is obtained through evaporation technologies, followed by crystallization [54, 55], membrane crystallization [56, 57], electrodialysis followed by multiple issue distillation (ED/MED) [54, 55, 56, 57, 58], and evaporation ponds [59, 60]. Membrane crystallization (MCr) is existence practiced to produce relatively pure salt crystals from a synthetic NF reject solution having calcium and magnesium [66]. Tanaka et al. [17] developed an electro dialysis procedure for the production of table salt from seawater reverse osmosis (SWRO) turn down with less than eighty% energy than conventional process. A similar process developed by Davis [47] on electrodialysis metathesis which has integrated evaporator unit to carve up out sodium sulfate and sodium chloride [61]. The SAL-PROC procedure (Geo-Processors USA Inc) is beingness used to produce sodium chloride, calcium sulfate, calcium chloride, and magnesium hydroxide from concentrated solutions including brackish water reverse osmosis (BWRO) and seawater contrary osmosis (SWRO) concentrate.

two.5.5 Nitrogen

In general, RO turn down stream was found to be more than 40 mg of nitrogen per liter. The available method to recover ammonia-nitrogen by struvite atmospheric precipitation, since extraction of ammonia is economically poor.

two.5.half-dozen Sodium chloride

The SWRO turn down through either electro-dialysis (ED) or electro-dialysis reversal (EDR) step is sufficient to carve up out impurities and that the salt produced is fit for human consumption; however, there is footling data available on terminal product purity using this arroyo Tanaka et al. [17]. Electrolytic method of simultaneous separation of chlorine and sodium chloride has good market place potential for the constructive management of RO reject. Melian-Martel et al. [62] used membrane electrolytic cells to recover chlorine, hydrogen and sodium hydroxide from seawater RO reject. Boopathy et al. reported separation of sodium chloride from the RO reject generated in leather processing industries through reactive precipitation techniques [63].

ii.5.6.1 Precipitation of sodium chloride from evaporated residue of RO rejects

The motion of ions during precipitation is expressed in the class of chemical equations every bit given below:

RAE + H 2 O → Na + , Cl − , Ca ii + , SO iv 2 − , Mg 2 + , Org − / Org + , H 2 O

E1

( Na + ,Cl − ,Ca two + ,SO 4 2 − ,Mg 2 + ,Org − / Org + ,H 2 O ) + HCl ( 1000 ) → NaCl ( Southward ) + [ H 3 O ] + + Na + + Cl − + Ca ii + , Then iv ii − , Mg 2 + , Org − / Org +

E2

The residue of RO rejects has been dissolved in water to gear up saturated RAE solution every bit shown in Eq. (ane). The increase in ionic concentration in the saturated solution shifts the reaction to backward direction by common ion consequence. In this study, hydrogen chloride gas was prepared and purged to increment the concentration of Cl− ions in the RAE solution. The incremental increase in Cl− ion concentration shifted dynamic equilibrium by increasing the ionic product of Na+ and Cl−. The ionic product of Na+ and Cl− exceeded the solubility product of sodium chloride [solubility product of NaCl, (Grandsp) is 36 (mol/50)2] and thus the precipitation of sodium chloride was achieved from the saturated solution of RAE as illustrated in Eq. (2). The schematic flow diagram of separation of sodium chloride from RAE solution generated in leather industry has been illustrated in Figure 1. Outset saturated RAE solution has been prepared past dissolving sixty% (w/v) RAE in water and the insoluble grits are removed afterward gravitational settlement. The articulate supernatant solution was taken in reactive precipitation reactor and HCl gas has been purged continuously for the reactive precipitation of sodium chloride. The required HCl is being prepared and used spontaneously. Since the prepared HCl gas cannot be stored, if we store which may condensate and plough into liquid form. After successful purging of HCl gas the sodium chloride salt is separated out from the solution by reactive precipitation as per the reaction given in Eq. (2).

Figure ane.

Schematic flow diagram for the selective atmospheric precipitation of sodium chloride from RAE generated in leather industry.

2.5.6.2 Outcome of HCl gas injection fourth dimension and RAE concentration on NaCl recovery

The HCl gas purging time for the separation of sodium chloride from RAE solution was carried out by varying time from 0.5 to 3 min at its native pH, eight.0 and temperature, twoscore°C. The optimum status for the recovery of NaCl is accomplished within 3 min of contact time as shown in Effigy 2a. The optimum time of iii min of contact time yield 81% recovery of sodium chloride. This is explained that the equilibrium was established i.e. the rate of atmospheric precipitation of NaCl becomes equal to the charge per unit of dissolution of NaCl in the solution. The mass of precipitated NaCl at the optimum fourth dimension was 26.7 m with 81% recovery with respect to the dissolved salt concentration (solubility of NaCl is 35 one thousand in 100 mL of water).

Figure ii.

Precipitation of sodium chloride (a) outcome of fourth dimension (conditions: pH, eight.0; temperature, 40°C; mass of RAE, threescore% (w/v)), (b) effect of concentration of RAE (conditions: fourth dimension, 3 min; pH, 8.0; temperature, 40°C).

The concentration of RAE [40–65% (west/v)] was varied to place the effect on precipitation of NaCl. The results in Figure 2b, shows that the percent of salt recovery increased with the increase in concentration of RAE. In general, precipitation depends on the concentration of dissolved ions in solution. As the initial concentration of RAE increased, the dissolved ions concentration was also increased in the solution and reached the saturation limit at concentration 60% (west/five). The maximum amount of NaCl precipitation was achieved with 82% recovery for 60% (w/v) RAE solution. Further to bear witness that the recovered common salt is NaCl, SEM and EDAX analyses were carried for the recovered NaCl as shown in Figure 3. The surface morphology of RO turn down looks aggregated mass like structure and thus may be due to mixture of many inorganic and organic salts. This is confirmed by EDAX spectrum shows presence of inorganic salts. Withal the recovered salt has a cubical structure, which is a feature morphology of sodium chloride and thus it claim that the recovered salt is sodium chloride. Further EDAX spectrum peak observed simply for Na and Cl and thus confirmed that the recovered salt is NaCl.

Effigy three.

Scanning electron microscopy images of: (a) RAE, (b) recovered NaCl from RAE and free energy dispersive Ten-ray spectra of (c) RAE, (d) recovered NaCl from RAE.

2.5.half-dozen.3 Mass remainder on grooming of saturated RAE solution

mass of RAE + deionised water → saturated RAE solution + grit 0.6 kg + 1 kg → 1.32 kg + 0.28 kg

E3

The mass of saturated solution of RAE was one.32 kg, obtained past dissolving 0.6 kg of RAE in 1 l of deionized water. The undissolved grit (0.28 kg) mainly consists of sand, lime and clay being non-hazardous in nature, which tin be disposed off onto secure landfill.

2.5.6.four Mass balance on precipitation of sodium chloride

saturated RAE solution + HCl gas → precipitated sodium chloride + residual solution 1.32 kg + 0.105 kg → 0.268 kg + 1.157 kg

E4

The maximum precipitation of sodium chloride of 0.268 kg was resulted from ane l of saturated RAE solution under the optimized conditions.

The proposed process for the management of RAE was relatively lower in cost than the other disposal methods, and also the procedure has the scope to recover sodium chloride. The proposed process recovered 0.203 kg of NaCl from 1 kg of RAE. The resulted acidified supernatant solution (RAS) was considered for separation of sulfate ions every bit calcium sulfate. The sulfate ion in the RAS solution and constructed RAS solutions were separated by the addition of various neutralizing agents. Amidst the selected neutralizing agents, Ca(OH)2 was constructive for the separation of sulfate ions from the RAS solution and synthetic RAS solutions. The total cost for the direction of one kg of RAE by the proposed process was 0.155 USD while the cost on landfill disposal was 0.xi USD. The recovered salts proposed to be reused for the hibernate/skin presentation in slaughter house [63].

ii.six Integrated process

Common salt recovery or recovery of valuables from concentrate are being finer washed through an integrated arroyo by combining one or more separation procedure which serve as a pretreatment or post treatment step [64]. In electro-dialysis for concentrating turn down brine solution, multi-stage wink being employed for desalting water, and crystallization for recovering salts, or with RO may be used instead of the multistage flash evaporator [65]. In another approach, RO reject are being supplied to an ion-exchange membrane electrodialyzer as post handling, and so concentrated brine from the electrodialyzer is sent to a multi-effect vacuum evaporator to crystallize the salts present in water stream [58]. Variety of inorganic salts is also sequential extracted from rejected brine for the loftier concentration levels of dissolved sulfate, potassium, and magnesium salts through multiple issue evaporation and cooling of saline wastewater, chemical reactions, crystallization, washing, and dewatering. The processes developed by researchers to recover various valuables from RO decline are presented in Table two. The combined procedure helps to recover both salts and water from textile rejects [66, 67, 68].

Table ii.

Recovery of valuables from RO refuse through integrated approach.

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iii. Conclusions

The thermal routes of evaporation are the most studied procedure techniques for the recovery of inorganic common salt from RO reject; notwithstanding, membrane separation techniques are cheaper for the recovery of product quality. The membrane separation procedure has generates pass up volume which need further treatment. The ion-commutation, electro dialysis, eutectic freezing, and chemical reaction are also being explored more than in recent times for its cost and efficiency on recovery of valuables from the decline stream. The integrated systems are beingness studied by combining i or more unit of measurement performance or process techniques to increase the recovery percentage of valuables. The selection of process or techniques may be selected based on the salt to be recovered, geological, hydrological, climatic, and economic conditions for its local specific.

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Acknowledgments

The author is thankful to the Council of Scientific and Industrial Enquiry for the laboratory and funding to carryout research activity.

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Conflict of interest

There is no conflict of interest with whatever funding agencies.

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Nomenclature

RO reverse osmosis
kWh kilowatt hour
ZLD zero liquid discharge
MEE multiple consequence evaporator
RAE residuum after evaporation
VC vapor pinch
ED electro-dialysis
EFC eutectic freezing crystallization
CDCC coupling of cooled disk column crystallizer
NF nano filtration
MED multiple upshot distillation
MCr membrane crystallization
EDM electrodialysis metathesis
BWRO brackish water opposite osmosis
SWRO seawater reverse osmosis
EDR electro-dialysis reversal
RAS resulted acidified solution
USD The states dollar

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Boopathy Ramasamy

Submitted: November 21st, 2018 Reviewed: July 19th, 2019 Published: October 15th, 2019

© 2019 The Author(s). Licensee IntechOpen. This affiliate is distributed nether the terms of the Artistic Eatables Attribution 3.0 License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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