Liquid-Liquid Extraction
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OCTOBER 2020 www.processingmagazine.com A BASIC PRIMER ON LIQUID-LIQUID EXTRACTION IMPROVING RELIABILITY IN CHEMICAL PROCESSING WITH PREVENTIVE MAINTENANCE DRIVING PACKAGING SUSTAINABILITY IN THE TIME OF COVID-19 Detecting & Preventing Pressure Gauge AUTOMATIC RECIRCULATION VALVES Failures Schroedahl www.circor.com/schroedahl page 48 LOW-PROFILE, HIGH-CAPACITY SCREENER Kason Corporation www.kason.com page 16 chemical processing A basic primer on liquid-liquid extraction An introduction to LLE and agitated LLE columns | By Don Glatz and Brendan Cross, Koch Modular hemical engineers are often faced with The basics of liquid-liquid extraction the task to design challenging separation While distillation drives the separation of chemicals C processes for product recovery or puri- based upon dif erences in relative volatility, LLE is a fication. This article looks at the basics separation technology that exploits the dif erences in of one powerful and yet overlooked separation tech- the relative solubilities of compounds in two immis- nique: liquid-liquid extraction. h ere are other unit cible liquids. Typically, one liquid is aqueous, and the operations used to separate compounds, such as other liquid is an organic compound. distillation, which is taught extensively in chemical Used in multiple industries including chemical, engineering curriculums. If a separation is feasible by pharmaceutical, petrochemical, biobased chemicals distillation and is economical, there is no reason to and l avor and fragrances, this approach takes careful consider liquid-liquid extraction (LLE). However, dis- process design by experienced chemical engineers and tillation may not be a feasible solution for a number scientists. In many cases, LLE is the best choice as a of reasons, such as: separation technology and well worth searching for a • If it requires a complex process sequence (several quali ed team to assist in its development and design. distillation columns) Figure 1 can be used to gain an understanding of • If the components to be removed or recovered exactly what LLE is. A feed consisting of mostly com- have low volatility ponent A plus component C (solute) is well mixed • If it results in high CapEx and OpEx with solvent B. e goal is to achieve mass transfer • In these instances, LLE may be the best separa- of solute C from feed A into solvent B. After the maxi- tion technology to pursue. mum amount of mass transfer is achieved, the phases 32 Processing | OCTOBER 2020 Figure 1 Figure 2 are separated into an extract phase (solvent C plus In countercurrent extraction, the feed lows in one the extracted solute B) and a rainate phase (feed A direction from stage to stage while the solvent lows plus the residual solute C) and possible the soluble in the opposite direction relative to the feed. Both amount of solvent B. liquid phases are lowing continuously through the Assuming that equilibrium was achieved during extractor. his type of process is shown for a column the mixing phase, this process represents a single type contactor in Figure 3. In Figure 3, the feed is the theoretical stage of extraction. As shown in Figure 1, heavy phase so it is added to the top of the column. It for a single theoretical stage, there are a number of is also the continuous phase, so it essentially ills the parameters identiied at equilibrium, including frac- column. he solvent is the light phase so it is added tion unextracted, distribution coefficient and the to the bottom of the column. It lows as droplets up extraction factor. he key for LLE is to select a solvent through the continuous phase and thus it is the dis- with as high a distribution coeicient as possible for persed phase in the column. Rules of thumb for which the solute to be extracted and as low as possible of all phase should be continuous and which phase should other components present in the feed. be dispersed are provided later. For most LLE processes, a single stage of extrac- An important step in understanding an LLE pro- tion such as this will not provide a suicient amount cess and eventually designing LLE columns is deter- of solute removal from the feed stream. In order to mining the liquid-liquid equilibrium data for the achieve higher levels of extraction, there are two low solvent of choice. he equilibrium data provides the patterns in which LLE can be operated: cross flow equilibrium curve shown in Figure 4. he operating extraction and countercurrent extraction. line in Figure 4 is determined by the actual inlet and Cross low extraction consists of a series of mixing outlet concentrations of solute during steady state and decants using fresh solvent each time. hus, after column operation. hese two lines allow for a graphi- the phase have separated, fresh solvent would be cal determination of the number of theoretical stages. added to the rainate and once again they would be he total number of theoretical stages required can mixed and allowed to decant. his procedure would be stepped of from the operating line to the equilibri- be repeated as many times as necessary to get from um line, as shown in Figure 4, and is analogous to the the feed concentration of solute C to the required raf- method used for absorption and stripping columns. inate concentration, shown as R4 in Figure 2. As an example of this procedure, Figure 5 OCTOBER 2020 | www.processingmagazine.com 33 BUILT TO FILL. BUILT FOR LIFE. Just built beter... READY TO SHIP Figure 3 Mobile Pail Filler This mobile pail iller was created for batch illing operaions at muliple locaions. It is top and sub- surface pail iller that moves around on casters. This iller will handle 4 to 7 gallon containers and only requires 25 lbs. of ineria to move it. Figure 4 Beneits represents the extraction of a carboxylic acid from a great examples of this would are phenol extrac- » Improved Eiciencies & Accuracy fermentation broth using an organic solvent. he red tion using MIBK and acetic acid extraction using » Increase Producion & Maximize Upime line represents the equilibrium data generated using ethyl acetate. Distillation being used as the sole » Heavy-Duty & Long Lasing actual feed and solvent determined via laboratory separation technology for these applications testing. he operating line is drawn by determining would be cost-prohibitive because of the high » User Friendly the material balance required to achieve 95% recov- amount of energy required. For example, if an This soluion has a variety of product opions available to meet ery. In order to achieve 95% recovery of the carboxylic aqueous feed contains < 30% acetic acid, liquid- your needs. To learn more, contact us by calling 833-467-3432. acid, three theoretical stages are required. liquid extraction is usually a more economical Another way to estimate the number of theoreti- solution than distillation for removal and recov- cal stages required for the LLE system is using the ery of acetic acid because the operating costs Kremser Equation. his equation considers the dis- associated with distilling away the water far out- We also provide installaion, parts and ield service tribution coeicient, extraction factor and concentra- weigh the capital costs of the liquid-liquid extrac- 833-467-3432 tion of the solute in the feed, rainate and solvent, all tion process equipment. on a solute-free basis. • LLE is also suited for the removal of hydro- www.specialtyequipment.com A graphical representation of the Kremser equation philic particles from organic streams. For these using diferent extraction factors is shown in Figure 6. applications, water is the solvent. A couple of examples of this type of application would be When is it recommended to use LLE? water extracting DMSO from a polymer solution • LLE is often used for the removal of high boil- and neutralizing & water extracting acids from ing components from dilute aqueous streams organic streams. such as wastewater or fermentation broths. Two • When recovery of non-volatile components is 34 Processing | OCTOBER 2020 BUILT TO FILL. BUILT FOR LIFE. Just built beter... READY TO SHIP Figure 5 Palleized Drum Filler & IBC / Tote Filler The most versaile and widely accepted illing machine is this palleized drum and IBC/tote iller. It is both a top and sub-surface liquid illing machine for illing a pallet of drums or a single IBC/ Figure 6 tote ranging from 5 to 550 gallons. Standard and explosion proof opion available. “The benefits of LLE position it as a powerful separation technol- Beneits ogy able to achieve product purification and recovery, particularly » Improved Eiciencies & Accuracy » Increase Producion & Maximize Upime where distillation is not an economically viable option.” » Heavy-Duty & Long Lasing » User Friendly required, LLE is an excellent choice, particularly LLE can be considered as a cost-efective alter- as compared against distillation. Regular distil- nate if the proper solvent can be identiied. This soluion has a variety of product opions available to meet lation is inefficient because of the high energy your needs. To learn more, contact us by calling 833-467-3432. consumption that is required to boil water away LLE column technology from the non-volatiles. LLE is a better choice As Figure 7 shows, there are three major types of from an operating cost perspective. Extraction extraction equipment: mixer settlers, column contac- and recovery of metals are classically done via tors, and centrifugal extractors. his article will spe- We also provide installaion, parts and ield service LLE processes. ciically focus on LLE columns. 833-467-3432 • If the compound of interest is heat-sensitive and here are two major types of liquid-liquid extrac- www.specialtyequipment.com decomposes with temperature/time, then distil- tion columns: static and agitated. lation may not be a good choice.