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1 Lenntech Tel Fax

2 Table of contents 1. INTRODUCTION Metals, water and ion exchangers Metal processing industry What are ion exchangers? Ideal products and processes RAW WATER TREATMENT TREATMENT OF PROCESS BATHS Regeneration of acidic process solutions Recycling of chrome baths Recycling of sulfuric acid RECYCLING OF RINSE WATER TREATMENT OF WASTEWATER OUTLOOK CONTACTS

3 1. INTRODUCTION 1.1. METALS, WATER AND ION EXCHANGERS Ion exchangers are versatile filter materials used for adjusting the quality of water and of aqueous solutions. This brochure is all about three things: metals, water and ion exchangers. What do these three have in common? Figure 1.1.: Metals are fascinating materials because of their versatile properties. Metals are sought-after construction materials with special properties that are used in more than half of all industrially manufactured products. Good quality water is of paramount importance when it comes to producing, processing and working metals. Figure 1.3.: Ion exchangers are materials used for purifying water and aqueous solutions and for keeping them clean. This makes ion exchangers valuable tools to the metal processing industry that fulfills the following functions: Ensure the quality of semi-finished and finished products Save resources, such as water, energy and raw materials Reduce wear and tear to technical installations and tools Eliminate toxic substances and ensure onthe-job safety and protection of the environment Figure 1.2.: When it comes to producing, processing and working metals, good quality water is of paramount importance. 3

4 Lewatit ion exchangers are available in more than 150 different product qualities and with various properties that are tailored to the type of application. Numerous plants in the metal processing industry have been relying on Lewatit ion exchangers for decades and are using them to: 1. turn untreated water into quality water that can be used for production 2. maintain and recycle water-based process solutions 3. recycle rinse water and possibly recover precious metals Figure 1.4.: Lewatit ion exchangers as bagged goods at the warehouse of the production plant in Bitterfeld (Germany). LANXESS has more than 70 years of experience with the production and application of ion exchange materials. 4. purify wastewater before it is discharged into the environment (final exchange principle) and here too to possibly recover precious metals In this brochure, the listed options are discussed in the above order. Reading this brochure will give you an idea of the manifold application fields of polymer adsorbent materials. The Lewatit brand stands for innovative filtration media and, at the same time, also for innovative and highly efficient technologies, such as the fluidized bed or multistep process. LANXESS is investing globally in new production facilities for ion exchangers and other products that are key to water treatment. Figure 1.6.: Reaction container for the functionalization of ion exchange beads in Bitterfeld. Figure 1.5.: The most state-of-the-art production facility for monodisperse ion exchangers in the world can be found in Bitterfeld. It was commissioned in Keep metals and the environment at its best by using Lewatit -filtered water and process solutions! 4

5 1.2. METAL PROCESSING INDUSTRY The metal processing and metal refining industry includes many different trade groups. One major group is the so-called electroplating branch, which takes on commission orders e.g. by the automotive industry to coat mainly small-type semifinished products. There are more than 4,000 such businesses in Germany alone. Jewelry industry, coinage facilities, mirror manufactories But the metal processing industry group does not only encompass these types of subcontractors. In general, it can be said that all production areas are of relevance that process metals that are used for producing goods. The following list provides an overview: Production of precision products, such as clocks, precision instruments, model railways, music instruments, optical devices etc. Production of semi-finished products, such as screws, nails, wires, cables, pipes, steel springs, sectional strips, ball bearings, axles etc. Construction of any type of vehicles Production of electronic components, such as conductor plates, computer chips, solar cells and other electronic components Production of fixtures, hinges, locks, handles, mountings etc. Production of tools, household appliances, machines and other commodities Production of construction elements for the construction industry and much more! 5

6 1.3. WHAT ARE ION EXCHANGERS? Ion exchangers consist of superfine synthetic beads with a diameter of 0.3 to 1.2 mm. They are added in bulk to filter devices. If mixed with an aqueous suspension, they can be easily filled into the filter device or rinsed out, if desired. selectivity). On the other hand, you can also see concentration effects: the higher the concentration in the solution, the more readily will a weaker binding ion sort displace a stronger binding species ( law of mass action). polymerbackbone functional group + + Figure 1.9.: The so-called ion exchange reaction at the functional groups fixed in the pores is the basis of all filtration processes described in the present brochure. Interaction between exchanged particles and functional group takes place via electrostatic forces. Figure 1.7.: Ion exchangers are filled into filter devices in bulk. Filtration takes place in the filter bed. After saturation of the ion exchanger with the filtered-out impurities, the filters can be chemically regenerated on site, so that they can be reused. The concentrates can then be used for recovering materials or they can be disposed of in a costefficient and environmentally friendly manner. Charge The capability to filter out material from aqueous solutions is based on so-called functional groups that rest on the surface of fine pores that homogenously run through the polymer beads, reaching their innermost depths. Regenerate Rinse Figure 1.8.: View of the inside of an ion exchange bead: it is permeated with fine pores that are filled with water. This way, material that is dissolved in the water can diffuse in and out. Material contained in water can penetrate the beads through their pores. Likewise, material stored in the resin can diffuse out of the beads and can be released to the surrounding medium. If particles are absorbed and dispensed at the same time, we speak of an exchange. Preferably, charged particles socalled ions are exchanged. Exchange at the functional groups follows two driving forces: on the one hand, different ion sorts have different binding capabilities, i.e. stronger binding ions displace the weaker binding ones (chemical driving force = Figure 1.10.: Charging of an ion exchange filter bed, removal of the charge with a regenerant solution and rinse-out of the regenerant solution. After that, the filter is ready to be used again. 6

7 Ion-exchange active filter materials differ mainly in terms of the following properties: Type of functional group SO 3 Na strongly acidic IAT (SAC) (e.g. Lewatit SP 112) CO 2 H Monomer basis of the polymer structure Degree of cross-linking of the polymer Gel-type or macro-porous structure of the polymer Particle size distribution Monodispersity or heterodispersity Average grain size Fines Charged form of the functional group Material s chemical purity weakly acidic IAT (WAC) (e.g. Lewatit CNP 80) CH 2 -N(CH 3 ) 2 H Cl weakly basic IAT (WBA) (e.g. Lewatit MP 62) CH 2 -N(CH 3 ) 2 HCl CH 2 -N(CH 3 ) 3 Cl medium basic IAT (e.g. Lewatit MonoPlus MP 64 WS) Tabelle CH 2 -N(CH 3 ) 3 1.1, Cl S.6 strongly basic IX type 1 (SBA1) (e.g. Lewatit K 6362) CH 2 -N(CH 3 ) 2 CH 2 -CH 2 -OH Cl strongly basic IX type 2 (SBA2) (e.g. Lewatit K 6363) CH 2 -N(CH 2 -CH 2 -CH 3 ) 3 Cl The type of functional group is the most important distinctive criterion and it determines, in essence, the chemical properties of the exchanger material. I.e., it defines what chemical substances can be preferably eliminated and with what water composition this will be achieved. Table 1.1. provides an overview of the various functional groups and states important pertinent products from the Lewatit portfolio. What is important to know are the following conventional names of ion exchangers and certain resin types: IX: SAC: Ion Exchange Resin Strongly Acidic Cation Exchanger WAC: Weakly Acidic Cation Exchanger SBA: Strongly Basic Anion Exchanger WBA: Weakly Basic Anion Exchanger CR: AR: Chelating Resin Adsorber Resin strongly basic IX type 3 (e.g. Lewatit Monoplus SR 7) CH 2 -CO-O-Na -Na CH 2 -N CH 2 -CO-O-Na -Na IDA-chelating resin (e.g. Lewatit MonoPlus TP 207) O CH 2 -P-O -Na CH 2 -N O- Na H AMPA-chelating resin (e.g. Lewatit MonoPlus TP 260) SH C=NH CH 2 -N... H thiurea chelating resin (e.g. Lewatit Monoplus TP 214) CH 3 OH H OH OH CH 2 -N -CH 2 - C - C - C - CH 2 OH H OH H H Methylglucamine IX (e.g. Lewatit MK 51) CH 2 -N(CH 3 ) 2 FeO(OH) hybrid adsorber (e.g. Lewatit FO36) CH 3 -CH 2 CH 3 -CH 2 -CH 2 -CH 2 -CH 2 -CH 2 -O CH 3 -CH 2 -CH 2 -CH 2 -CH 2 -CH 2 -O CH 3 -CH 2 Levextrel resin D2EHPA-saturated (Lewatit OC 1026) P O OH adsorber resin (e.g. Lewatit VP OC 1064 PH) Table 1.1.: Various functional groups of Lewatit ion exchangers. 7

8 1.4. IDEAL PRODUCTS AND PROCESSES The performance of ion-exchange active filters can be rated based on the following criteria: 1. Duration of the filtration cycle until next regeneration 2. Consumption of regeneration chemicals and rinse water per volume of purified water 3. Slip of substances running through the filter unhindered 4. Release of impurities by the exchanger material 5. Mechanical and osmotic stability 6. Lifetime of the resin until it has to be exchanged Premium products of the Lewatit brand have been optimized in terms of the aforementioned characteristics. Our customers can always expect the best when it comes to these criteria. At this point it must also be pointed out, however, that performance does not only depend on the filter material s quality but also on the concept of the overall facility, its mode of operation and on structural features of the filter device: The aforementioned criteria are not the responsibility of the resin producer. Therefore, it is important to select an as qualified as possible manufacturer to build your plant. LANXESS will name qualified plant manufacturers upon request. Ion exchangers will show the following advantages under suitable process conditions: Small, compact systems that can be easily automated and require little monitoring Robust filter material that, depending on utilization, will last up to ten years Relatively low investment costs for the filter bed High competitiveness compared to other technologies Easy to maintain and clean if soiled Easy to replace in case of damage Use of selective exchangers allows for highly efficient procedures and the possibility to recover material Most often, ion exchangers are aggregates that work in combination with other treatments, e.g. with prior deferrization or heavy metal precipitation. Therefore, the mode of operation must be adjusted accordingly. What is also very important is proper water management: the water that is fed into the ion exchanger must be specified. Partial flows must not be added randomly. In order to ensure longevity of the ion exchanger it needs to be maintained on a recurring basis: e.g., the filter bed must be backwashed in ascending flow on a regular basis in order to wash out impurities and resin breakage and to loosen the bed and even it out. When constructing filter devices, one of the most important things is to achieve optimum distribution of the liquid above and within the resin bed. Figure 1.11.: Water softening system using ion exchange technology. 8

9 2. RAW WATER TREATMENT Water is used for different purposes in production: Feeding of cooling water circuits Rinsing of work pieces Preparing and diluting solutions Vapor generation Operating sanitary facilities Preparing drinking water for own staff Different requirements on the quality of water are made depending on the process, selection of device types, and treated or produced products. These quality requirements include the following: Hardness (permanent, temporary, overall hardness ) Iron and manganese content Salinity as indicated by conductivity or electrical resistance Suspended matter content (TS) Corrosiveness ph level Dissolved gases (for example CO 2, O 2...) Dissolved organic matter (TOC, DOC) Odor and possibly taste Sterility and others Raw water may originate from the most various sources, including the following: Public supply network Own well Withdrawal from a body of surface water Rainwater Condensates Wastewater of a neighboring production plant that shows only minor contamination Different treatment methods must be applied depending on the quality of the raw water and the required quality of the water used in production, including the following: When selecting the suitable method or a combination of methods, economic aspects play an important role (investment and operating costs), but practical aspects, such as logistics, user friendliness, availability, reliability and space requirements are also taken into consideration. Raw Water Water Treatment Process Process Water Water Quality A Quality C Process Water Quality B Production Figure 2.1.: Normally, production will require water of various qualities, which is produced with the help of separate processing lines. Ion exchangers are used mainly in three areas when turning raw water into high-quality production water: Coagulation/precipitation Wet oxidation Gas stripping Sedimentation Sand filtration Ion exchange Membrane filtration Activated carbon filtration Water softening Partial or complete desalination Ultra desalination The following plays a minor role: Deferrization and demanganization TOC removal 9

10 Water softening is aimed at removing the minerals that cause hardness, such as calcium, magnesium and carbonate. There are two different water softening methods that use ion exchangers: During so-called decarbonization with weakly acidic cation exchangers (e.g. Lewatit CNP 80 WS) in H form, calcium and magnesium are bound. The released H + unites with carbonates and releases carbonic acid. By eliminating calcium, magnesium and the associated bicarbonate you will achieve partial desalination. Regeneration takes place using acid. During water softening with strongly acidic cation exchangers (e.g. Lewatit MonoPlus S 1567 or Lewatit C 249), the resin is used in sodium form. Hardness is eliminated in exchange with sodium ions. This keeps the salt level in the water at a constant level. Regeneration takes place using a concentrated NaCl solution. Because of the reaction between the released ions H + and OH - under formation of water (H + + OH - H 2 O), the discharge of the filter system is almost free of charged particles and hence called demineralized water. This way, residual water conductivities of less than 1 μs/cm can be easily achieved. Through the combined use of strongly and weakly acidic or rather strongly and weakly basic resins as a composite, investment costs and the cost of regenerants can be reduced ( so-called composite beds). CO 2 stripping after the cation exchanger stage also shows advantages, as it saves the anion exchanger capacities for the absorption of carbonate (see also figure 2.2.). Regeneration of the acidic resins takes place with acid and regeneration of the basic resins with leach. For complete desalination, series-connected cation exchangers and anion exchangers are used. The cation exchanger removes all cations and replaces them with protons (H + ). The anion exchanger then removes all anions and replaces them with (OH - ). K +, A - air, CO 2 H +, A - κ < 1 µs/cm R > 18 MΩ Salt containing rinse water WAC SAC WBA H + + OH - -> H 2 O SBA MB Fully desalinated water Luft H +, A - Figure 2.2.: Flowchart of a more complex complete desalination system with cation-exchanger column as a WAC/SAC composite bed, gas washer, anion-exchanger column with a WBA/SBA composite bed and mixed bed for achieving ultrapure water qualities with a resistance value of up to 18 MΩ. 10

11 If the water is to be desalinated even more to achieve even lower conductivities, so-called mixed bed filters (e.g. Lewatit MonoPlus S 108 H / MonoPlus M 500 MB) are installed downstream of the conventional complete desalination system. This way, it is possible to achieve ultrapure water (UPW) qualities of up to 18 MΩ in specific electrical resistance. If not by conventional means, iron and manganese can be removed from raw water (deferrization/demanganization) through adsorption to a strongly acidic resin through exchange against sodium. Organic matter measured as TOC or rather DOC can be mainly found where surface water is used as a source of raw water. Organic matter originates mainly from natural sources and belongs to the group of humins, building blocks and fulvic acids, among others. Since these substances are mainly of an anionic nature, they can be adsorbed to a great extent, at strongly or weakly basic resins. Regeneration takes place using neutral or alkaline brines. Ion exchangers used for removing the TOC / DOC are usually installed upstream of the desalination system to protect it against organic impurities. Therefore, they are also called scavengers. Figure 2.4.: The purity of water is shown by indicating the specific conductivity or rather the specific electrical resistance. For applications in the area of microelectronics, ultrapure water qualities of up to 18 MΩ in specific electrical resistance are required. Products for raw water treatment Softening, decarbonization Lewatit CNP 80 Lewatit MonoPlus S 100 Lewatit MonoPlus SP 112 Lewatit MonoPlus S 108 Lewatit C 249 Lewatit S 1667 Cation exchange Lewatit C 267 Lewatit MonoPlus SP 112 Lewatit MonoPlus S 108 Anion exchange Lewatit MP 64 Lewatit MP 62 WS Lewatit MonoPlus MP 68 Lewatit MonoPlus MP 500 Lewatit MonoPlus M 500 Lewatit MonoPlus M 800 Mixed beds Lewatit NM 60 Lewatit NM 91 Lewatit UltraPure 1292 MD Deferrization, demanganization Lewatit MonoPlus SP 112 TOC scavenger Lewatit MonoPlus MP 64 Lewatit MonoPlus MP 62 WS Lewatit S 6268 Lewatit 6328 A Lewatit A 8071 Figure 2.3.: Complete desalination system with cation exchanger, CO 2 stripper and anion exchanger. 11

12 3. TREATMENT OF PROCESS BATHS One of the main application areas of electrochemical coating of metal surfaces is corrosion prevention. Apart from that, hardness, wear resistance, aging and temperature resistance as well as decoration also play an important role. Electrochemical coating of surfaces (e.g. chromizing, galvanizing, nickel coating etc.) Chemical and mechanical polishing (CMP) of silicon wafers In all these cases, the process solution will change over time. The active agent will be partially consumed and at the same time byproducts or rather impurities will build up in the process bath. The consumed portion of the active agents can be replenished. This way, for example a pickling acid can be regenerated by adding concentrated acid. Likewise, the zinc that is consumed during the plating of steel can be topped up by adding chemicals. Nevertheless, byproducts and impurities will increasingly build up in the bath. a) Electrochemical metal separation + - b) Chemical metal separation Red e - Red e - Figure 3.1.: Various aqueous-based metallic salt solutions (electrolytes) are used for treating surfaces. Me 2+ Me 0 Me 2+ Me 0 The necessary electrolyte a process stream in terms of this brochure is a liquid stream containing a relatively highly concentrated active agent that is dissolved in water. This active agent is then reacted against a metallic surface or against a surface consisting of another material. In addition to that, materials can also be prepped for a further process step by using other process baths. In that case, the process stream acts as a reactant in a chemical reaction. Examples include the following: Etching of surfaces with an acid or brine (e.g. electropassivation of aluminum in sulfuric acid baths or derusting / slight etching of steel surfaces in hydrochloric acid) Figure 3.2.: Electrochemical and chemical coating of surfaces. In the left-hand image the metal is reduced from the circuit through electrodes and in the right-hand image through a chemical reducing agent. The reduced metal deposits on the surface. The higher the concentration, the more easily can these impurities impair the surface treatment result. This lesser quality shows in form of discolorations, stains or reduced corrosion protection. Creating fine structures through etching (e.g. during production of conductor plates, in micromechanics and other areas) Chemical passivation of surfaces with brines (e.g. chemical nickel, phosphating ) 12

13 A) Complete disposal after consumption W W N Me 2+ if Me 2+, N exceed the limit W, N, Me 2+ Figure 3.3.: A brand new galvanizing system just after its installation (with the friendly permission of Gerhard Weber Kunststoff-Verarbeitung GmbH, Minden) So, in the past it was often common practice to completely dispose of the process baths after a certain time, which led to the following consequences: The active agent contained in the process bath (acid, metallic salt, reagent) was lost for good and had to be completely replaced. Waste disposal B) Continuous recycling W A relatively large volume of process solution had to be treated at once in a relatively large-scale wastewater treatment facility. This led to a relatively large amount of secondary waste (e.g. heavy metal sludge, salt) that had to be further disposed of. W N Me 2+ Thanks to the ion exchanger technology, it is now possible in some cases to selectively remove the byproducts and impurities from the bath while experiencing only a very minor loss in active agents. The following provides some examples of how this technology works: Alternatives A) Complete disposal and B) Recycling of the electrolyte solution are further explained in figure 3.4. W, N, Me 2+ W Recycling filter N, Me 2+ Waste disposal Figure 3.4.: When using process baths, active agent (W) is consumed and replenished accordingly. At the same time, byproducts (N) and metal (e.g. Me 2+ ) build up. Me 2+ is formed by corrosion of the working piece. If the critical concentration of N and Me 2+ is exceeded, the bath can no longer be used. It then has to be disposed of (case A) or recycled (case B). 13

14 3.1. REGENERATION OF ACIDIC PROCESS SOLUTIONS Unless acidic process solutions show high concentrations in hydrogen ions, cationic impurities, such as Fe 2+, Zn 2+, Al 3+ etc. that have built up can be removed with the help of strongly acidic cation exchangers in H form. If such a process bath is continuously run over an ion exchanger, impurities can be kept at a tolerable concentration level, which will considerably prolong the bath s lifetime. The relevant exchange reaction will effect a true regeneration, since the take-up of foreign metals will at the same time release an equivalent in hydrogen ions into the solution. One example of how the lifetime of an acidic process bath can be prolonged is to remove cationic metal ions from a phosphoric acid bath. In this case, the ion exchanger Lewatit MonoPlus SP 112 in H form can remove cations, such as Fe 2+, Zn 2+, and/or Al 3+. Another example is the etching of steel with hydrochloric acid. Here, Fe 2+ ions will build up over time. By adding H 2 O 2 in a side stream, the Fe 2+ can be oxidized to Fe 3+, which forms the anionic and very dark colored [FeCl 4 ] - complex in the acid. This complex attaches in an extremely selective manner to strongly basic anion exchangers, such as Lewatit K By letting the acid pass over the anion exchanger, the iron can be removed to the largest extent to leave behind a residual concentration of less than 1 ppm. In this case, regeneration takes place simply by letting water pass over. The previously absorbed iron-chloro complex will break down under these conditions. The anion exchanger will repel the cationic iron and the latter will be washed out by the water. This procedure is so efficient that it can also be used for purifying hydrochloric acid RECYCLING OF CHROME BATHS Depending on the base material to be treated (iron, messing) or already existing coatings (nickel, copper), chromium (VI) electrolytes can be contaminated by foreign metals, such as copper, zinc, iron and chromium (III). The built up of these impurities result from surface corrosion and by cathodic reduction of C(VI). While small amounts of chromium (III) and especially an iron content of 2-3 g/l will have a positive effect on current yield, larger amounts of foreign metals will result in poorer conductivity of the electrolyte, reduced current yield and a poorer visual appearance of the chrome coating. Therefore, when it comes to recycling, the bath is diluted to a concentration of approx. 100 g/l CrO 3 and cooled to room temperature, because otherwise it would result in oxidative damage to the ion exchanger. In order to remove iron, chromium and other heavy metal cations, a strongly acidic cation exchanger of the type Lewatit MonoPlus SP 112 H is used. Under the given circumstances it can be charged with up to 20 g Fe/Cr per liter resin. Regeneration takes place using 10% sulfuric acid. After purification, the treated chromium (VI) electrolyte is brought back to its original concentration by means of evaporation and then added to the bath RECYCLING OF SULFURIC ACID Large amounts of sulfuric acid are used during the anodization of aluminum. Aluminum builds up increasingly in the process bath and is tolerated only up to a certain concentration. Such baths are recycled using the so-called acid retardation process. This method is basically based on that a strongly basic ion exchanger can absorb acids while repelling metallic salts. This phenomenon is caused by the effect of charge, also called Donnan effect. The acid will normally enter from below into a lean column filled with special resin, such as, e.g., Lewatit K At the top of the column, various fractions will leave the column one after the other. First of all, clean water that has remained in the column from the previous cycle will be released. It can be temporarily stored and then reused in the next cycle. Then follows the fraction with the saltcomprising impurities in this case aluminum sulfate. This fraction is disposed of through the wastewater. Finally, there is a stage in which the acid starts to break through. Feeding of the column is stopped at the beginning of this stage. Now it is time for regeneration: to that end, demineralized water is simply added from above i.e. in opposite direction to the charge. The water will completely absorb the acid adsorbed by the ion exchange beads and wash it back into the process bath. 14

15 The name acid retardation has been derived from the fact that, during this process, first the salt and then the acid will leave the column with retardation. + Al + H 2 O for regeneration During charging as well as during regeneration relatively low flow speeds are applied. The acid will break through already after approx. one filter bed volume. The cycle comprising charging and regeneration will take less than an hour. H 2 SO 4 anodization bath 10 % H 2 SO 4, 5 g/l Al 2 (SO 4 ) 3 H 2 O+ recycled H 2 SO 4 SBA This procedure is most efficient when using acids with a concentration of between 10 and 20 percent. Normally, it will be possible to keep the concentration of metal cations in the process bath at a level of 5 g/l to 10 g/l. But this method is not suitable for the precision cleaning of acids. Residual concentrations in the mg/l range cannot be achieved with acid retardation. IX Al 2 (SO 4 ) 3 + H 2 O Wastewater LANXESS has developed the acid retardation resin Lewatit 6387, which thanks to its superfine beads (0.39 mm in diameter) allows for a particularly high degree of separation between the fraction with impurities and the fraction with acid. And there are numerous other applications apart from the aforementioned ones, where a process bath can be purified in a similar way and its lifetime considerably prolonged. Table 3.1. provides an overview of the most important known methods. Figure 3.5.: Schematic diagram of the acid retardation process and a technical system made by GOEMA. Impurity Area of application Ion exchanger Fe 2+, Zn 2+, Al 3+, Cu weakly acidic process solutions, e.g. phosphoric acid, tartaric acid Lewatit MonoPlus SP 112 Fe 3+, Zn 2+, Cd 2+, Sn 2+ complexes concentrated hydrochloric acid Lewatit K 6362 Fe 3+, Cr 3+, Cu 2+, Zn 2+ Chrome (VI) acid < 10 % Lewatit MonoPlus SP % - 20 % H 2 SO 4, HNO 3, HF, H 3 PO 4, Al 3+, Fe 3+ Lewatit K 6387 by means of retardation Fe 3+, Zn 2+ from Cr (III) passivation bath Lewatit OC 1026 Fe 3+ from Zn galvanization bath Lewatit MonoPlus TP 207 Zn 2+ from Ni galvanization bath Lewatit OC 1026 TOC from Cr (III) passivation bath Lewatit VP OC 1064 PH Cu 2+ from CMP suspensions Lewatit MonoPlus TP 207 Cu 2+ from NH 4 Cl etchants Lewatit MonoPlus TP 207 Table 3.1.: Application examples for the recycling of process baths or production streams. 15

16 4. RECYCLING OF RINSE WATER Rinsing is an important and frequent intermediate step when treating surfaces. Its goal is to remove any process solution residues from the prior treatment stage. This prevents the process solution from being carried to the subsequent process step. In order to save water and chemicals, many modern production plants have optimized their rinse processes. Nowadays, they use so-called dip and flow rinse tanks, as shown in below figure Transport system + The recirculation system used for desalinating the rinse water works similar to an ion exchange system used in raw water treatment. It basically consists of a series-connected cation exchanger and anion exchanger. Despite their similarity, recirculation systems differ in the following respects from raw water treatment systems: Complex composition of rinse waters: heavy metals, complexing agents, detergents, oils and fats Risk of substances accumulating in the recirculation system Risk of microbial contamination of the entire installation Process bath Clean water Risk of damage to the ion exchanger caused by certain substances, such as detergents or deposition of insoluble salts Dip rinse tank Contaminated water Flow rinse tank Figure 4.1.: State-of-the-art rinse process. Rinsing takes place by dipping the work piece into several series-connected tanks. In the flow rinse tank water cascades onto the work piece. Normally, a macro-porous strongly acidic resin (such as Lewatit MonoPlus SP 112) is combined with a weakly basic resin (such as Lewatit MonoPlus MP 64) when used in recirculation systems. Should the rinse water, however, contain salts of weak acids, such as CN -, H 2 BO 3 -, HSiO 3 - or bicarbonate, the weakly basic resin must be followed by a strongly basic resin (such as Lewatit K 6362). A weakly basic resin alone would not be able to absorb the aforementioned ions. Where applicable, the concentrated rinse water from the dip rinse tank is returned to the upstream process after evaporation. The water discharged from the lowest container of the flow rinse tank is collected and can be disposed of as wastewater or recycled. Many rinse processes will generate water that is contaminated only slightly with salt and often has a lower salt content than the raw water used for fresh water production. In these cases it makes sense to desalinate the water in a recirculation system and to return the recovered and fully desalinated water to the rinse process. Figure 4.2.: Surface rinsing is necessary between each and every process step. 16

17 If the rinse water contains not only salts but also detergents (soaps, surfactants), a protective filter ( scavenger ) should be installed upstream of the desalination system, e.g. an activated carbon filter or adsorber resin. Cationic tensides can form an irreversible coating on cation exchangers and anionic tensides an irreversible coating on anion exchangers. Therefore, they should be removed before reaching the ion exchanger. If a strongly basic resin is used downstream, as mentioned above, one must pay close attention that the upstream weakly basic ion exchanger is not passed over, because otherwise the strongly basic resin might be irreversibly charged with metal cyanide complexes, chromate or other components. Various organic complexing agents acting on the basis of monovalent or multivalent carboxylic acids or amino or phosphoric acid are also absorbed by the ion exchangers. They also adsorb metals in complexed form: for example, a heavy metal complexed with EDTA would attach to the anion exchanger because the metal complex is anionic i.e. negatively charged. One must pay attention that the water is largely free from particulate matter before it is treated with ion exchangers and that drops of oil or emulsified oils are also not carried into the ion exchange bed. I.e., the water should be pretreated by way of demulsification, light liquid separation or possibly membrane filtration. One should also refrain from introducing strong oxidants, such as peroxides or chlorine to the water. These oxidants can cause irreversible damage to the ion exchanger through degradation of functional groups and dewetting of the polymer structure. A widespread problem in connection with recirculation systems is microbial contamination and uncontrolled growth of algae in pipelines, stackable containers and the filter bed of ion exchangers. The growth of algae in stackable containers can be reduced by using UV lamps, and ion exchangers can be disinfected with various methods, including increased backwashing, use of acid and brine and even controlled use of biocides. K +, A - 1, A 2 organic K +, A - 1, A - 2 H +, A - 1, A - 2 Salt containing rinse water ( ) ( ) AR or GAC SAC WBA SBA Organic K + A - 1 A - 2 Recycled rinse water Demineralized water Figure 4.3.: Schematic diagram of a recirculation system: the first and last filter is optional and required only for certain water qualities. The scavenger removes dissolved organic matter, the cation exchanger removes cations, the weakly basic anion exchanger the anions of strong acids (A 1 - ) and the strongly basic anion exchanger the anions of weak acids (A 2 - ). 17

18 An easy but still very efficient way to reduce algae growth is to use opaque construction material and container covers. If the objective is to produce quality water with a residual conductivity of less than 1 µs/cm, a mixed bed, e.g. Lewatit UltraPure 1292 MD, may have to be installed downstream of the combination of Lewatit MonoPlus SP 112 and Lewatit MonoPlus MP 64. If the rinse water contains precious metals, it may be possible to recover them from the pure regenerants. If you are dealing with a mixture of materials and if you are interested only in recovering a subcomponent, it makes sense to use a selective exchanger in the regenerant stream. Scavenger Lewatit VP OC 1064 PH Cation exchanger Lewatit MonoPlus SP 112 Lewatit MonoPlus S 108 Anion exchanger (for A - 1 ) Lewatit MP 62 WS Lewatit MonoPlus MP 64 Lewatit MonoPlus MP 68 Anion exchanger (for A 2- ) Lewatit K 6362 Mixed bed Lewatit UltraPure 1211 MD Table 4.1.: Products that are suited for rinse water recycling. Figure 4.4.: Recirculation system made by Decker VT. 18

19 5. TREATMENT OF WASTEWATER All water that has come into contact with metallic components or electrolyte solutions during production contains potentially toxic metallic salts. This water must undergo treatment in accordance with legal provisions before it is discharged into the environment. For wastewater from the metal processing industry in Germany the limits prescribed in Annex 40 of the German Wastewater Ordinance apply. That is why in metal processing plants the respective system is called detoxification system (see figure 5.1.). Normally, detoxification takes place in a multistage system and has the following tasks: Oxidative destruction of free cyanides and cyanide-metal complexes Oxidative destruction of organic complexing agents (such as EDTA, NTA...) Electrochemical recovery of precious metals Precipitation of heavy metal ions through transformation into sparingly soluble hydroxides, carbonates or sulfides When performing precision cleaning of wastewater, it is beneficial to use selective ion exchangers. In this position they are also called polishing filters. They make it possible to safely keep the residual concentration of metals below a value 0.1 mg/l. Since final exchangers also provide protection against accidental release of metals in the upstream treatment stages as a result of operating errors, they are sometimes also referred to as police filters. The working mechanism of ion exchangers in the final exchange position is shown in detail in figure 5.2. especially the interaction between ion exchanger and upstream precipitation stage. The main load of heavy metals, such as copper, nickel, chromium (III), cobalt, iron etc. is separated during the precipitation stage. Caustic soda or lime milk is preferably used for precipitation. If final exchangers are employed, one can do without adding sulfidic precipitants. The heavy metals are transformed into sparingly soluble hydroxides in the precipitation reactor and can then be separated, for example with a filter press. Separation and thickening of the heavy metal sludge Precision cleaning of wastewater to ensure compliance with the limits Process water Production Recovered metal Detoxification system Wastewater contaminated with heavy metals Chemical oxidation (e.g. of cyanides and organic ligands) Chem. reduction (e.g. of Cr (VI)) Extraction electrolysis Precipitation / filtration IX Polishing filter Heavy metal sludge Purified wastewater Figure 5.1.: Principle of the working mechanism of a detoxification system used in the metal processing industry. The wastewater is first treated in partial streams and then precipitated. The ion exchanger as a final exchanger is the final barrier before the wastewater is discharged into the environment. 19

20 Normally, precipitation and subsequent solids separation will make it possible to eliminate more than 99% of the pollutants from the water. However, given an initial concentration of 1000 mg/l and 99% separation, one will still be dealing with a residual concentration of 10 mg/l, which in the case of most heavy metals means that the limit is still clearly exceeded. In order to ensure that the wastewater to be discharged complies with the discharge requirements, one can install an ion exchanger downstream which will further reduce the concentration of pollutants through precision cleaning. The combination of high-performance stage and precision-cleaning stage will lead to an overall elimination of more than 99.9% of pollutants. The spent regenerant solution is normally returned to the precipitation tank where it is admixed to the main wastewater stream. I.e., it needs no special treatment and as a result heavy metals will only be released through one single outlet namely the filter press. The heavy metal sludge is then either disposed of at a dump site or used as a resource in extractive metallurgy, e.g. at a copper smelting plant. The application described herein is mainly about removing heavy metal ions, such as copper, nickel, chromium, cobalt etc. in case they are present as cations. This is the traditional area of application for a chelation exchanger, such as Lewatit MonoPlus TP 207. Most systems that are being used in practice work according to this principle. However, the wastewater produced in the metal processing industry sometimes also contains other pollutants that cannot be absorbed by Lewatit MonoPlus TP 207. But there are ion exchangers that can fulfill this task through selective binding: Precious metals, such as gold, silver, platinum, palladium, rhodium, iridium etc. can if present as anionic complexes be bound with Lewatit K 6362 or Lewatit MonoPlus TP 214. Mercury can be reliably removed using Lewatit TP 214. Anionic chromate, molybdate and tungstate is best bound by Lewatit MonoPlus MP 62 WS or Lewatit K 6362 in a weakly acidic to acidic solution. When it comes to removing arsenate or antimonate, Lewatit FO 36 works selectively. Heavy metal > 1000 ppm Heavy metal < 10 ppm Heavy metal < 0.1 ppm Heavy metal wastewater Precipitant (CaO, NaOH) Regenerant (HCl) Conditioner (NaOH) Rinse water Precipitation reactor Filter press ph adjustment Polishing filter Purified wastewater Heavy metal hydroxides Sludge Dump Regenerant stream Figure 5.2.: Cooperation between polishing filter and upstream precipitation system. While heavy metal precipitation can normally reduce heavy metals to residual concentrations of less than 10 ppm, ion exchangers can achieve a further reduction to more than 0.1 ppm. Given an initial concentration of more than 1,000 ppm this means an elimination of more than 99.9% of pollutants. 20

21 Perfluorinated tensides (e.g. PFOS) can be reduced to the ppb or even ppt range using weakly or strongly basic resins, such as Lewatit MP 62 or Lewatit K Boron is selectively separated using Lewatit MK 51, and fluoride selectively attaches to aluminum-loaded Lewatit MonoPlus TP 260. If the wastewater contains several impurities at the same time, which cannot be bound by one and the same type of selective exchanger, it is recommended to combine several suitable resin filters. The advantages of using ion exchangers as final exchangers can be summarized as follows: Very low residual concentrations, which ensures compliance with limits through multistage effect in the filter column Selectivity allows for targeted absorption of trace impurities, leaving behind harmless components, such as calcium, magnesium, chloride etc. No use of expensive and polluting organosulfur precipitants Relative tolerance of suspended solids, such as gypsum and limestone precipitations Recovery of recyclable fractions Products that can be used as polishing filters Adsorption of cationic heavy metals, such as Cu 2+, Zn 2+, Cd 2+, Cr 3+, Ni 2+ Lewatit MonoPlus TP 207 Adsorption of quicksilver and precious metals (Au, Ag, Pd...) Lewatit MonoPlus TP 214 Adsorption of precious metal cyanide complexes ([Au(CN) 2 ] -, [Ag(CN) 2 ] - ) Lewatit MP 62 WS / Lewatit K 6362 Adsorption of anionic heavy metals (CrO 2-4, MoO 2-4 ) Lewatit MP 62 WS / Lewatit K 6362 Adsorption of PFT (PFOS ) Lewatit K 6362 Adsorption of As, Sb, CN- Lewatit FO 36 Adsorption of boron (B(OH) 3 ) Lewatit MK 51 Adsorption of fluoride (F-) Lewatit TP 260 (Al form) Table 5.1. Lewatit products that can be used as polishing filters. 21

22 6. OUTLOOK This brochure shows how versatilely and effectively ion exchangers can be used in the metal processing industry. But this brochure describes only a limited selection of the many different types of use. As a matter of fact, there are numerous other technical applications. For more detailed technical information, please contact our team of experts here at LANXESS. Comprehensive product descriptions and safety data sheets can be downloaded at Ion exchangers have great innovative potential and should always be checked for their suitability when developing new technologies. Please also take advantage of our expertise when conducting research projects. Our team of application engineers and researchers will gladly support you in your efforts to develop new tailored solutions. 7. CONTACTS Lenntech info@lenntech.com Tel Fax The above information and our technical advice whether verbal, in writing or by way of trials is give in good faith but without any warranty. This also applies where proprietary rights of third parties are involved. Our advice does not release you from the obligation to check its current validity and, in particular, the validity of our safety data sheets and technical information and to test our products for suitability for your intended procedures and purposes. The application, use and processing of our products and of the products manufactured by you on the basis of our technical advice is beyond our control and, therefore, entirely your own responsibility. Our products are sold in accordance with the current version of our General Terms and Conditions of Sale and Delivery. The above formulation is intended solely as a guide for our business partners and other parties interested in our products. As the concrete areas of use and application of the suggested formulations are beyond our control, it is imperative to test them at least under technical, environmental, health and safety aspects to see whether they meet your specific requirements and whether they are suitable for the intended use and application. Although the ingredients, dosages and compound and article properties indicated herein reflect our recommendation at the time of publication, the formulations are not subject to continuous review and/or updating, and you agree that use is undertaken at your own risk. We cannot be held liable for any changes to ingredients and their processing behavior that may occur at a later point in time or for their effects on the properties of the articles/products that are produced using these suggested formulations All Rights Reserved LANXESS Deutschland GmbH 22

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