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Productivity Improvements Through Recovery of Pickle Liquors with the APU Process

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Productivity Improvements Through Recovery of Pickle Liquors with the APU Process Continuous recovery of pickle liquors saves acid and reduces waste treatment expense as well as providing a means of decreasing pickling times and ellml- nating downtimes for bath replacement and tank clean out. Reductions In ener- gy consumption and fume emissions are also possible. Productivity improvements through recovery of pickle liquors with the APU process Craig J. Brown, Executive Vice President, Eco-Tec Ltd., Pickering, Ont., Canada I Reprinted from IRON AND STEEL ENGINEER 0 Copyright, Association of Iron and Steel Engineers Continuous recovery of pickle liquors saves acid and reduces waste treatment expense as well as providing a means of decreasing pickling times and ellmi- nating downtimes for bath replacement and tank clean out. Reductions in ener- gy consumptlon and fume emissions are also possible. Productivity improvements through recovery of pickle liquors with the APU process Craig J. Brown, Executive Vice President, Eco-Tec Ltd., Pickering, Ont., Canada PICKLING is the chemical removal of surface oxides or ing metallic salts of those acids. The process is reversible, in scale from steel by immersion in an aqueous acid solution. that the acid can be readily desorbed from the resin with While wide variations are possible in the type, strength and water. It is thus possible, by alternately passing contaminat- temperature of the acid solutions used, sulfuric and hydro- ed acid and water through a bed of this resin, to separate the chloric acids are the most common pickling acids for carbon free acid from the metal. steel. Mixtures of nitric and hydrofluoric acids are generally Unfortunately, only small volumes of solution can be pro- used for stainless steel. cessed each cycle. The difficult part of the process is finding Pickle liquors become contaminated with dissolved met- a way to efficiently elute purified acid from the resin without als through use. As the metal concentration increases, the contaminating it with the impure feed acid and without ex- free acid concentration decreases and pickling efficiency cessively diluting it. drops. Additions of fresh concentrated acid are made from A novel ion exchange technique called Recoflo, which has time to time to rejuvenate the bath but eventually it be- been extensively used for recovery of metals from metal fin- comes spent and must be discarded. Pickling speed varies ishing wastewater,2 has proven ideal for this application. continually throughout the life of the bath and it is difficult Through the use of short resin beds, fine mesh resins, coun- to avoid either under or over-pickling. terflow regeneration and various other features, the Recoflo While most pickle acids are relatively inexpensive, the in- technique provides the necessary tool with which to achieve direct costs associated with pickling go well beyond the cost the required separation efficiency. The resulting system is of the acid consumed. Some of these indirect costs include: called an acid purification unit or APU. There are two steps in the basic APU process-the up- Labor to make up fresh acid. stroke and downstroke (Fig. 1).During the upstroke, con- Labor for removal and disposal of spent acid. taminated acid is pumped into the bottom of the resin bed. Cost of neutralizing chemicals. Acid is sorbed by the resin particles and the remaining de- Ultimate disposal of resulting solid waste. acidified metallic salt solution, called the by-product, is col- Reduction in productivity resulting from the inhibit- lected from the top of the bed. Next, during the downstroke, ing action of dissolved metals. Lost production time that occurs while spent acid is removed and replaced. Flg. 1 - APU operating cycle. Quality control problems due to over and under-pick- ling as bath composition changes. UPSTROKE Recovery of spent pickle liquors can potentially reduce METALLIC SALT WATER BYPRODUCT (WASTE) many of these costs. I Various techniques have been employed to recover waste 4 pickle liquors. These systems are based on a variety of unit operations including evaporation, crystallization, roasting and solvent extraction. Unfortunately, most are expensive and generally not suitable for any but the largest and most technically sophisticated operations. water A simple, low cost unit, called the acid purification unit reservoir (APU), was introduced in 1978 in North America for recov- ering spent mineral acids. Since that time, several hundred of these systems have been installed around the world, pri- marily in metal finishing applications such as sulfuric acid DOWNSTROKE aluminum anodizing, sulfuric/peroxide brass and copper et- SPENT ACID chants and various aluminum, brass, copper and nickel et- I m chants employing nitric acid.l I Recovery of pickle liquors with the APU has recently at- tracted considerable attention in the steel industry and a large number of units have been installed over the past cou- ple of years for this application. The APU process water PURIFIED Operating principle - Certain ion exchange resins have ACID PRODUCT the ability to sorb strong acids from solution, while exclud- January 1990 Iron and Steel Engineer 55 water is pumped into the top of the bed, desorbing the puri- fied acid from the resin so that a purified acid product is 1 F I collected from the bottom of the bed. The total cycle typical- ly takes approximately 5 min to complete and continuously repeats itself. Equipment and layout - The heart of the APU is the res- in bed which is typically 30 to 60 cm (12 to 24 in.) in height, depending on the application. Scale-up is accomplished by increasing the diameter of the bed. Units are constructed in a range of capacities. Small units with bed diameters from 15 to 50 cm (6 to 20 in.) utilize hy- dropneumatic reservoirs to pump the feed acid and elution water through the resin bed. Larger units, up to 180 cm (72 in.), utilize electronic measurement of flows and are I I equipped with external holding tanks and pumps. I I A typical unit equipped with a 107-cm (42-in.) dia bed is )WASTE shown in Fig. 2. This particular unit will process 8760 litres (2310 gal)/hr of stainless steel pickle liquor. Fig. 3 - Typical APU installation configuration. Because of its compact size, the unit can be shipped fully assembled and pretested so that installation and start-up costs are minimal. The basic mechanics of the system are Typical results for steel and stainless steel pickling are simple. Consequently, reliability is high and maintenance shown in Table I and 11. costs are low. Removal of suspended solids from the acid prior to pro- For most pickling applications, the system is operated in a cessing is essential. Depending on the nature of the solids bypass arrangement directly on the pickling tank (Fig. 3). and the acid solution, a variety of filters have been em- Operation in this manner maintains the tank at a consistent, ployed. Excellent success has been achieved utilizing a depth low level of metal contamination. Through regular bath filter similar to the multimedia sand filter employed in water analysis and acid makeup, the acid concentration can also be treatment facilities. held at a constant value. In this way, the pickling process can be optimized. Sulfuric acid pickling Contaminated acid flows through a filter directly to the Sulfuric acid is usually limited to batch pickling operations, unit. The acid is retained in the unit and the metal-bearing although there are still some continuous sulfuric pickling by-product or waste stream exits from the unit. The waste lines in operation. stream flows from the unit on a near continuous basis To achieve satisfactory pickling rates it is necessary to op- throughout the day. For the plant waste treatment system, a erate sulfuric acid pickle baths hot. This does not present a small continuous flow such as this is much easier to handle problem for the APU since the resins are stable up to 100°C. than the large instantaneous load that is normally generated Systems have been in continuous service at 80°C in excess of when a whole bath is dumped. four years with no significant drop in performance. Water is used to elute the acid from the unit and this acid Appreciable improvements can be achieved in terms of product flows directly back to the process tank. Regular ad- improved productivity, acid savings and pollution abate- ditions of concentrated makeup acid are required to replace ment with the APU. acid neutralized through metal dissolution. Where several process tanks are in use, the system may be Productivity improvements - Generally, at least 10% used on all tanks continuously or in rotation. sulfuric acid must be maintained in the pickling bath to in- As a rule of thumb, it is possible to easily remove close to sure minimum pickling rates. The acid becomes spent when 60% of the metal from the acid in one pass and recover ap- the dissolved iron level reaches 6 to 8% by weight. At higher proximately 90% of the free acid. Although it is usually feasi- levels, the sulfate will crystallize out of solution. Care must ble to achieve a 90% separation by adjusting operating condi- be taken to not allow either the free acid level to get too high tions, production of high purity acid is usually not necessary. or the bath temperature too low, as this will depress the solu- bility of the ferrous sulfate and cause crystallization. The TABLE I Acid recovery Flg. 2 - Typical APU. Concentrations Pickling Feed, Product By-product, application Component g/iitre g/iltre g/iitre Sulfuric acld H2SOs 150 137 9.9 Fe 50 14.3 29.9 Hydrochloric acid HCI 140 142 10.3 Fe 45.6 33.5 20.4 TABLE I1 Typical APU field results: stalnless steel plckllng Composition Fe, gl Free HF, Free HN03, Relative APU stream litre Normal Normal flow rate Feed 27.0 0.83 1.59 1.00 Product 3.0 0.65 1.51 1.00 Bv-Droduct 20.0 0.15 0.08 1.20 56 iron and Steel Engineer January 1990 sulfate crystals tend to clog transfer pipes and pumps, inter- dragout is neglected, the amount of 93% sulfuric acid re- fering with bath replacement schedules.
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