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Cover Story
28 Part 1. Crystallization for Ultra-Pure Chemicals
Optimized crystallization units can help address the challenges posed
by product-purity requirements in the battery industry
18
.Departments
4 Editor’s Page A vision for chemical engineering
A recently concluded three-year study offers direction for where chemical
engineers can make the most impact over the next 30 years
48 Economic Indicators
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C
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dzaborski@meritdirect.com hemical engineering is a discipline with far-reaching and di-
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Senior Editor
GEORGE SEVERINE
While the basic principles of chemical engineering remain steadfast,
sjenkins@chemengonline.com Production Manager rapid advances in technology and the evolving needs of society create
gseverine@accessintel.com
MARY PAGE BAILEY new directions and areas of focus for chemical engineers. Recently,
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leaders from the chemical engineering community concluded a three-
GROUP PUBLISHER CHARLES SANDS
year study to outline a vision for the direction of the profession for
Director of Digital Development the next 30 years. This culminated in the report “ New Directions for
MATTHEW GRANT csands@accessintel.com
Vice President and Group Publisher, Chemical Engineering” by the National Academies of Sciences, En-
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CONTRIBUTING EDITORS
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SUZANNE A. SHELLEY
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org). The chair of the committee that wrote the report, Eric Kaler, presi-
DEVELOPMENT dent of Case Western Reserve University, said: “Chemical engineering
PAUL S. GRAD (AUSTRALIA)
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jmcphail@accessintel.com jlepree@chemengonline.com Opportunities for chemical engineering
GEORGE SEVERINE A brief summary from the over 300-page report on areas where chemi-
Fulfillment Manager
gseverine@accessintel.com cal engineers can have the most impact in the coming years follows:
Decarbonization. Chemical engineers are making important con-
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4 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
Chementator
This heat battery is a decarbonized, Edited by:
Gerald Ondrey
‘drop-in’ replacement for industrial boilers
A
s the cost of renewable energy de- do’s technology does not depend on combus- 2D POLYMER
creases, many organizations are tion or phase change, and with its low-cost Chemical engineers at
looking to electrify their operations solid heating media, there is no possibility of the Massachusetts Insti-
to reduce carbon emissions. One gas or liquid being released. “The units are tute of Technology (MIT;
promising area for decarbonization is in- safe and compact, and can tie into existing fa- Cambridge; www.mit.
dustrial heating, which accounts for a large cilities the same way that existing gas- or coal- edu) have synthesized
two-dimensional sheets
fraction of global emissions. However, heat- fired boilers do today,” adds O’Donnell. Fur-
of polyaramide. The
ing networks in plants can be very complex, thermore, Rondo’s system can achieve very achievement, described
making modifications to existing configura- high temperatures (up to 1,000°C), whereas in a February issue of Na-
tions extremely costly. energy-storage systems that employ liquid ture, is said to be the first
Now, a new “heat battery” developed by salts may only reach 570°C, which limits their time a polymer has been
Rondo Energy, Inc. (Oakland, Calif.; www. use for industrial applications. grown in 2D, creating
rondo.energy) aims to provide affordable, de- The company expects to announce its first a material with unusual
carbonized process heat in a drop-in module commercial installations later this year and properties: films of the
that can be easily integrated into an existing was recently awarded $22 million in Series A material have a 2D elas-
boiler network, either to replace aging boil- funding. “We’ve made the transition from the tic modulus of 12.7 GPa
(4–6 times greater than
Variable electricity input High temperature heat storage Continuous, configurable that of bullet-proof glass)
heat output
and a 2D yield strength
Hot air
of 488 MPa (twice that
of steel). Combined with
a density that is one-
sixth that of steel, these
properties could make
Steam the material find appli-
cations as lightweight,
durable coatings for mo-
bile devices and cars, or
as building materials for
bridges and buildings.
Rondo Energy
Feed water The new material,
dubbed 2DPA-1, is made
ers or to complement those still in operation. laboratory to prototypes to first field installa- by the homogenous
“We found a way to use well-proven materials tions. These units are now industrial scale — 2D irreversible polycon-
in a new combination to build a heat battery the standard unit delivers 20 MW of steam, densation of melamine
that uses renewable electricity to deliver high- which is like a boiler that’s burning 85 million — a spontaneous self-
temperature heat by circulating air through a Btu/h,” says O’Donnell. Furthermore, be- assembly process. The
solid material to deliver hot air or high-pres- cause the units are equipped with both con- synthesized material can
then be spin-coated into
sure steam at any condition,” explains John ventional and dynamic outer insulation layers,
thin films. These films are
O’Donnell, CEO of Rondo Energy. To meet the heat losses are minimized, resulting in a 98% not only strong, but also
safety requirements of industrial plants, Ron- heat-delivery efficiency. impermeable to gases,
which would make them
Quantum-inspired computing technology useful as barrier coatings
drastically accelerates materials design for metal structures.
S
Further experiments
emiconductor materials contain nu- fujitsu.com) that is inspired by quantum tech- are underway to learn
merous ingredients in various mixing nology (but not directly using quantum ef- more about the formation
ratios, and high-performance mate- fects). Showa Denko developed an AI model mechanism of 2DPA-1, as
well as changing the mo-
rials are obtained by optimizing the for predicting the properties of semiconductor
lecular makeup to create
formulation. However, more than 1,050 theo- materials. To make the AI model computable other types of materials.
retical combinations of ingredients and mixing on Digital Annealer, Showa Denko expressed Two patents have al-
ratios need to be analyzed, so it would take the AI model as an Ising model, a statistical ready been filed on the
more than dozens of years to explore all pos- mechanical method. By simulating the Ising production process.
sible combinations of these ingredients and model on Digital Annealer, the company says
their mixing ratios with conventional artificial it has reduced the exploration time to dozens
intelligence (AI) methods, according to Showa of seconds, about 72,000 times faster than BIO-HMDA
Denko K.K. (Tokyo, Japan; www.sdk.co.jp). the time required by conventional AI meth- A partnership between
To reduce the time required for the explo- ods. The optimal formulation designed with Genomatica (San Diego,
ration, the company used high-performance the Ising model is expected to obtain semi- Calif.; www.genomatica.
com) and Covestro AG
computing technology, Digital Annealer, a do- conductor materials with 30% higher perfor-
(Leverkusen, Germany;
main-specific computer architecture devel- mance than the formulation designed with
oped by Fujitsu Ltd. (Kawasaki, Japan: www. conventional AI methods, the company says. (Continues on p. 6)
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022 5
Solar clinker produced for the first time
L
www.covestro.com) has
produced the first industri- ast month, Cemex, S.A.B. de C.V. with the Synhelion solar receiver. The pilot
ally significant volumes of a (Cemex; Monterrey, Mexico; www. was installed at the Very High Concentration
plant-based version of hexa- cemex.com) and Synhelion SA (Lu- Solar Tower of IMDEA Energy, located near
methylenediamine (HMDA).
gano, Switzerland; www.synhelion. Madrid, Spain. Synhelion’s solar receiver
HMDA, traditionally derived
from petroleum, is a chemi-
com) successfully connected the clinker consists of a cavity filled with a greenhouse
cal intermediate widely used production process with the Synhelion solar gas (GHG; typically water vapor or mixtures
in the manufacture of Nylon, receiver to produce solar clinker. The mile- of H2O and CO2) flowing from the aperture
as well as in coatings and stone is a first step towards fully solar-driven towards the back of the cavity. Solar radia-
adhesives. Production of cement plants. tion coming from the 1,000-m2 field of 169
ton quantities of bio-based Clinker — a solid material used for making mirrors enters the cavity through a transpar-
HMDA from the fermenta- Portland cement — is produced by fusing ent window and is absorbed by the black
tion of sugar allows those together limestone, clay and other materi- surface of the cavity walls. The energy is
products to be produced als in a rotary kiln at temperatures nearing then thermalized and reradiated back into
more sustainably.
1,500°C. Because fossil fuels are typically the cavity to heat up the GHGs, which is
Highly efficient engineered
bacteria metabolize sugar
used to heat the kiln, they are responsible for then used as a heat-transfer fluid to deliver
and produce, in one step, an approximately 40% of direct CO2 emissions process heat for clinker production. With
aqueous solution of HMDA. of the process. Replacing fossil fuels entirely this design, record-breaking temperatures
This “broth” is worked up in with solar-thermal energy is a gamechanger above 1,500°C are achieved.
a dedicated process to pro- in the industry’s efforts to achieve carbon The pilot, which produced a few kilograms
duce HMDA that is suitable neutrality by 2050. per batch, is the first successful calcination
for polyurethane and nylon The Synhelion and Cemex R&D teams set and, more importantly, the first success-
6,6 applications. up a pilot batch-production unit to produce ful clinkerization ever achieved using only
Genomatica is developing clinker from concentrated solar radiation by solar energy. The next step this year will
the complete, integrated
connecting the clinker production process target continuous production (during day-
process to make HMDA
from renewable feed- Excess CO2 stream Separation unit time), which will be followed by
Synhelion/Cemex
stocks, along with the steps CO2 a dedicated pilot facility with a
needed to build and operate ten-fold increase in capacity. A
Receiver
a production plant, while Preheating
H2O first small-scale industrial plant
Covestro is contributing its tower
Return stream to receiver
is envisioned by 2026 and a
expertise in separating and Thermal energy full-scale industrial plant (150
purifying HMDA and testing
Sensible heat recovery stream
storage (TES) Receiver outlet
stream
MWth solar input power, 900
in polyurethane applications. Precalciner ton/d production capacity) by
Covestro has secured an 2028. The process (diagram)
option to license Genomati-
will use Synhelion’s thermal-
ca’s integrated GENO HMD Kiln
process technology for
energy storage, which will en-
commercial production.
Grate cooler able continuous operation —
Sensible heat recovery stream return even at night.
PSILOCYBIN
Vocan Biotechnologies Inc.
(Victoria, B.C., Canada; A new catalyst for the oxidative dehydration of
www.vocanbiotech.com) propane with CO2
C
has optimized its recom-
binant production system, onverting propane to propylene tivity at 550°C and compared the results
successfully testing its by oxidative dehydrogenation with with existing catalysts. They also performed
proof of concept for the bio- CO2 is an alternative route to con- a mechanistic study to understand the
synthesis of psilocybin suit- ventional propane dehydrogena- functions of the different components and
able for use in future scale- tion, but existing catalysts for this conversion found the catalyst links the propylene-form-
up. A patent application
are not very efficient. Now, in a study de- ing reaction to the deoxygenation of CO2,
has been filed. Psilocybin
is a psychedelic compound
scribed in a recent issue of Nature Cataly- and ensures the catalytic activity is specific
that is showing enormous sis, researchers at the Institute for Catalysis, to propane; water and carbon oxides are
promise in treating addic- Hokkaido University (Sapporo, Japan; www. formed as byproducts. They also found that
tion and depression. cat.hokudai.ac.jp) have developed a highly the catalyst increased the reaction rate ap-
Scientists at Vocan have efficient catalyst — a Pt-Co-In ternary nano- proximately five-fold compared to the typi-
constructed optimized DNA alloy on a ceria (CeO2) support — that exhib- cal values reported from other systems. The
sequences that can pro- its a very high catalytic activity, C3H6 selectiv- reaction produced a higher ratio of propyl-
duce enzymes replicating ity, stability and CO2-utilization efficiency. ene and utilized more CO2 at 550°C com-
the biosynthetic pathway Each of the three metals were chosen pared to previous catalysts. The stability of
used by Psilocybe mush-
for their specific properties: Pt as the main the catalyst is greatly enhanced by combin-
rooms. Vocan’s biosynthetic
process retains the stereo-
active metal due to its ability to break C–H ing the strong CO2 activation ability of the
chemistry of the natural bonds; Co for accelerating CO2 capture and alloy with the oxygen-releasing ability of the
psilocybin molecules found activation; and In to enhance the selectivity. ceria support, which facilitates Mars–van
The researchers tested the catalyst’s ac- Krevelen-type coke combustion.
(Continues on p. 8)
6 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
Dispersion
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T
he presence of per- and polyfluoro- Air cooler
alkyl substances (PFAS) in wastewa- Raw PFAS H2O2
ter and groundwater has garnered Feed tank
Furnace 1
Furnace 2
Furnace 3
Heat Heat
existing PFAS separation technologies, the exchanger exchanger
Concentrated
Battelle Memorial Institute (Columbus, Ohio; PFAS water tank
www.battelle.org) has developed a technol-
ogy, known as the PFAS Annihilator, for de- Sample
stroying both short- and long-chain PFAS location Reactor
eralize a wide range of PFAS species. This Battelle Memorial Institute Heat exchanger
new SCWO technology is related to similar that can concentrate the PFAS before it is destroyed,”
processes used previously to destroy polychlorinated bi- explains Dan Longbrake, director of commercial busi-
phenyls (PCBs), but now has been optimized to destroy ness at Battelle. “To date, our focus for PFAS Annihilator
PFAS molecules. has been on aqueous wastes, such as PFAS-containing
In the process (diagram), an oxidant is introduced into wastewater or landfill leachate, but Battelle is also de-
the supercritical water reactor, and a base (NaOH) is veloping SCWO for destruction of PFAS in solid materi-
added to neutralize the hydrofluoric acid formed by the als, such as contaminated soil,” notes Longbrake. The
reactions. The PFAS Annihilator has demonstrated the technology will also be deployed to reduce or eliminate
ability to destroy 99.99% of total PFAS in various aque- stockpiles of firefighting foams, which contain high lev-
ous feeds, Battelle says, leaving inorganic salts, such as els of PFAS.
NaF and Na2SO4, as inert end-products. The PFAS Annihilator is available as a mobile unit that
“Battelle’s SCWO PFAS-destruction technology can can be transported on a trailer for episodic and demonstra-
be used alone or in combination with another process tion uses. Battelle is also constructing a larger mobile unit.
T
positive effect than the chemi-
cally synthetized counterpart. he transformation of sulfur-con- integrating phosphorus into the metal
taining molecules is an important framework using a technique known as
CARBON FIBERS reaction in organic and pharma- phosphorus-alloying. In doing so, the
The Competence Center Bio- ceutical chemistry. However, the catalytic performance of the precious
polymer Materials of the German sulfur atom strongly coordinates with metal nanoparticles is said to be greatly
Institutes of Textile and Fiber Re- the active sites of metal catalysts, sig- improved. In particular, the ruthenium
search (DITF) Denkendorf (Ger- nificantly decreasing the catalytic per- phosphide nanoparticles (Ru−P/SiO2)
many; www.ditf.de) has devel- formance. Sulfur impurities contained in exhibited a ten-times higher catalytic
oped a sustainable process for
chemical feedstocks also cause catalyst activity than Ru/SiO2. In one of the reac-
the production of carbon fibers.
The HighPerCellCarbon technol-
deactivation. Therefore, the develop- tions studied, the deoxygenation of di-
ogy is a patented process, which ment of a new sulfur-tolerant and highly phenylsulfoxide, (C6H5)2SO, over Ru-P/
has been further developed active catalyst is desired. SiO2 (with 50 bars H2 at 453K) exhibited
under the leadership of Frank To meet this need, researchers at a turnover number of 12,500 — the high-
Hermanutz, that enables carbon Osaka University (Japan; www.osaka- est to date, according to the research-
fibers based on biopolymers to u.ac.jp) have developed a highly active ers — and a yield of more than 99% for
be produced in a sustainable and durable metal-phosphide catalyst diphenyl sulfide, (C6H5)2S.
and particularly environmentally for the deoxygenation of sulfoxides into According to the researchers, this cata-
friendly process. The process in- sulfides. As described in a recent issue lyst shows wide substrate applicability and
volves the wet spinning of cellu-
of the Journal of the American Chemi- can deoxygenate structurally complex
lose fibers using ionic liquids (IL)
as direct solvents. The filament
cal Society Au, the developed catalyst drug intermediates to produce bioactive
spinning-process takes place has a high durability against sulfur-poi- sulfides in high yields. Moreover, Ru−P/
in a closed system, and the IL soning in contrast with the conventional SiO2 can promote sulfoxide deoxygen-
solvent is completely recycled. metal catalysts. ation even in the presence of a lot of sulfur-
The cellulose fibers produced The catalyst — precious metal phos- containing molecules where conventional
(Continues on p. 9) phide nanoparticles — is prepared by Ru/SiO2 is completely deactivated.
8 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
Ultra-rapid production of battery materials in this way are converted
using plasma technology directly into carbon fibers
by a low-pressure stabi-
A
lization process, followed
new ultra-rapid plasma-based pro- span of particle sizes for a single process, while
by a carbonization pro-
cess could significantly expand the also demonstrating many different chemistries cess. Petroleum-based
availability of premium materials for are possible,” notes Trinch. Currently, one of raw materials, which are
battery applications. Developed by industry’s most attractive chemistry blends is usually used in the indus-
6K, Inc. (North Andover, Mass.; www.6kinc. nickel-manganese-cobalt oxide (NMC), and trial production of carbon
com), UniMelt is a single-pass, continuous with the UniMelt process, the stoichiometry of fibers, are substituted by
process that employs a proprietary microwave the blend, as well as the final particle size, can renewable biopolymers.
torch technology to create a ball of plasma at be finely tuned by simply controlling the pro-
6,000K, which can be stretched into a large portions in the aqueous feed, as well as the E-CRACKING
production zone. The base materials for bat- process gases (such as N2 or O2) injected dur- Coolbrook Oy (Hel-
tery cathodes are dissolved in an aqueous so- ing the reaction. Beyond NMC, UniMelt is also sinki, Finland; www.cool
lution, which is sprayed into the plasma reactor expanding the exploration of additional battery brook.fi) and ABB Ltd. (Zu-
using a high-speed droplet sprayer, where the materials, such as lithium titanate (LTO), lithium rich, Switzerland; www.
water from the solution is immediately evapo- lanthanum zirconium oxide (LLZO) and various abb.com) have signed a
memorandum of under-
rated and captured as steam. “Then, over the silicon anodes.
standing (MoU) to com-
next 2–3 s, the battery materials travel through The company is operating two 100-ton/yr mercialize and accelerate
the production zone and the particle is synthe- UniMelt units in Pittsburgh that produce the adoption of Roto Dy-
sized. Depending on the battery chemistry, the powders for additive manufacturing, and namic Reactor (RDR) tech-
particle is either ready for use, or it may need the company is investing $35 million to nology that promises to
a 1–3-h heat treatment to complete the final scale up the process for battery applica- significantly reduce green-
product,” explains Sam Trinch, 6K’s president. tions at a dedicated facility in Massachu- house gas emissions from
This is a vast improvement over current pro- setts. “The new center will have ten manu- steam cracking of olefins.
cesses, such as coprecipitation, which can facturing systems for pilot production. By The agreement will unite
take as long as 3 d. the end of 2022, we should have roughly the two companies’ exper-
tise and create a combined
“We can process materials from 10 nm up to 200 to 300 MWh worth of active cathode
hundreds of micrometers, which is a very large materials capacity,” adds Trinch. (Continues on p. 10)
CHEMSTATIONS.COM/CAKE11
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engineered energy solutions,
new class of electrolyte aims to bridge to-roll manufacturing processes employed in
initially for use in petrochemi-
cal and chemical markets.
the performance gaps between the battery manufacturing. “Compared to other
Coolbrook’s RDR turboma- electrolytes used in conventional electrolytes, rubber electrolytes have a high
chine will be able to replace lithium-ion batteries and solid-state ionic conductivity at room temperature and
a conventional furnace by batteries. The new rubber electrolytes, devel- excellent mechanical toughness. Thus, batter-
directly imparting the rotor oped by a team of researchers from Georgia ies with rubber electrolytes can be more safely
shaft’s mechanical energy to Institute of Technology (Georgia Tech; At- operated at room temperature,” explains Lee.
the hydrocarbon fluid. This is lanta; www.gatech.edu), led by mechanical The rubber electrolyte is composed of
achieved by aerodynamic ac- engineering professor Seung Woo Lee, pro- lithium salt, a cross-linked elastomer ma-
tion through a rotating blade vide several distinctive benefits for batteries in trix (poly butyl acrylate) and a plastic crystal
flow (for more details, see
terms of safety and mechanical stability. (succinonitrile). The materials are synthesized
Chem. Eng., May 2017, p. 9).
When powered by electricity
A major drawback of conventional liquid into a 3D-structured rubber electrolyte ma-
from renewable sources, the electrolytes is their flammability, which has trix. Upon polymerization, the plastic crys-
technology completely elimi- spurred much research into solid-state bat- tal component creates 3D interconnected
nates CO2 emissions in the teries. However, explains researcher Michael pathways for lithium ion transport, enabling
steam-cracking process. Lee, solid electrolyte materials often require high ionic conductivity at room temperature,
ABB will deliver automation, complex manufacturing processes, and the while the elastomer component provides
electrification and digitaliza- materials may decompose at ambient condi- mechanical stability. The team at Georgia
tion to optimize operational tions, potentially releasing toxic chemicals. Tech has fabricated a 4-in. × 7-in. free-
processes and simplify inte- Furthermore, they exhibit low ionic conductivity standing rubber electrolyte, and is working
gration, as well as enhance
at room temperature, meaning that they often on scaling up rubber-electrolyte assembly
the energy efficiency of Cool-
brook’s solution through the
require an elevated temperature to operate, for pouch-type batteries. The team has re-
integration of ABB’s electric which may necessitate thermal management ceived funding from major battery manufac-
motors and variable-speed systems in some applications. The new rub- turer SK Innovation Co. (Seoul, South Korea;
drives. ❐ ber electrolytes are not only flame-retardant, eng.skinnovation.com) to further develop
but also can be fabricated using current roll- next-generation battery materials. n
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IN BRIEF
piping and structural elements is CORROSION
an ongoing problem at chemical KNOWLEDGE BASE
process industries (CPI) facilities ISOLATED AND
because of its potential to contribute to cat- AGGRESSIVE
astrophic failures, safety concerns and in-
CUI-RESISTANT
creased cost and effort for maintenance. The COATINGS
corrosion subcategory known as corrosion
under insulation (CUI) is a particularly difficult COATINGS AS
challenge for plants to address as industrial INSULATION
sites continue to seek efficiency gains and Acuren ALLOYING
avoid heat loss by insulating process equip-
FIGURE 1. Corrosion under insulation (CUI) is a phenom- CUI DETECTION
ment. By its nature, CUI is hidden from view,
enon that can be particularly aggressive when the pres- ADVANCEMENTS
and it can progress quickly under certain ence of moisture is combined with contaminants at a steel
circumstances. The renewed attention on surface, and so it can progress rapidly between asset
CUI has been highlighted by new coating inspection intervals
technologies and detection methods, aimed
specifically at the problem of CUI. Castenada-Lopez says the issue of corro-
sion under insulation (CUI) has been garner-
Corrosion knowledge base ing significant focus recently, because it re-
Professor Homero Castenada-Lopez, the mains a large problem for which there have
director of the National Corrosion and Mate- not generally been efficient solutions. “It’s a
rials Reliability Center at Texas A&M Univer- stubborn problem that is going to be worse
sity (College Station, Tex.; www.tamu.edu), in the future,” he says.
works with companies on improving corro- Steven Reinstadtler, infrastructure mar-
sion performance for their assets, including ket manager at Covestro LLC (Pittsburgh,
testing different materials in various environ- Penn.; www.covestro.com) and committee
ments and identifying which control actions chair with the Association for Materials Pro-
would be most effective at increasing safety tection and Performance (AMMP; Houston;
and reliability. “The ultimate goal is to avoid www.ampp.org), has also seen a renewed
all catastrophic incidents,” Castenada-Lo- focus on CUI. “In the past, any solutions for
pez says, “and when you have aging infra- CUI were extremely limited and individual
structure and assets, it requires that we be components-based,” he says, “Now, while
proactive, rather than reactive, at preventing CUI remains a significant problem, some
corrosion.” In part, that requires closing the solutions are available that do address the
current knowledge gaps and developing a issue, although they tend to be complex
deeper and more widespread understand- and involve multiple components working in
ing of corrosion,” he notes. concert, and so therefore, can be somewhat
“While most people on industrial sites expensive,” Reinstadtler comments.
have a general awareness about corrosion’s
potential impact, there remains a great need Isolated and aggressive
for improving the knowledge base on cor- CUI occurs when moisture mixes with con-
rosion, not only for chemical engineers, but taminants in a “corrosion zone” between
also for mechanical engineers and others,” the interior of the insulation and the coat-
says Castenada-Lopez. ing on the surface of the asset. “Moisture
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CONNECTIONS
ACG
C
hemical process industries matter filter is the N95 filtering face-
(CPI) facilities often present a piece respirator (Figure 1). N95 masks
number of potential respiratory are so-called because they remove
hazards, including airborne particles, 95% of airborne particles 0.3-mi-
toxic chemicals and low-oxygen envi- crons and larger in size. Some N95
ronments, that may require the use of masks have a valve to reduce breath-
respiratory personal-protective equip- ing resistance during exhalation. The
ment (PPE). This reference outlines “N” refers to the mask’s resistance to
the major categories for respiratory oil. N stands for “not resistant to oil.”
protection commonly used in indus- The other two categories are R (resis-
trial production settings. tant to oil) and P (oil-proof).
L
ysine (Figure 1) is an α-amino Pathway A Pathway B
acid used in the biosynthesis Glucose syrup
Fermentation Fermentation
Raw sugar
of proteins. The compound
contains an amino group and
a carboxylic acid group. Under bio- L-Lysine-HCl
logical conditions, the amino group is
protonated (–NH3+) and the carboxylic Pathway C
Raw material(s)
Cyclohexene
acid group is deprotonated (–COO–). Chemical synthesis Pathway
The α-carbon of lysine is a chiral Product under analysis
Other product(s)
center, so two enantiomers of the
compound exist. Only L-lysine is bio- FIGURE 3. Several pathways for making L-lysine exist, including fermentation and chemical synthesis,
logically active. Lysine is an essential which is less common
amino acid that must be supplied comprises three major sections: (1) with an aqueous ammonia solution.
through the diet. It is commercially fermentation; (2) product recovery; Product concentration, drying and
produced as L-lysine monohydrochlo- and (3) product concentration, drying packaging. The L-lysine eluate from
ride (L-lysine·HCl) and L-lysine sulfate. and packaging (Figure 2). ion exchange columns is mixed with
L-lysine·HCl is a yellowish-white, crys- Fermentation. The culture media mother liquor from the product filtra-
talline powder, mainly used as a food used in fermentation is prepared by tion step and concentrated by evapo-
and feed supplement. Other uses re- mixing process water, invert sugar ration. The concentrated lysine solu-
late to cosmetics, human medicine, and nutrients. The fermentation is per- tion is acidified with hydrochloric acid,
culture media and pharmaceuticals. formed in fed-batch mode and under and free L-lysine is converted to L-
Lysine is produced from raw sug- aerobic conditions. To start the batch lysine·HCl. Subsequently, the L-lysine
ar (sucrose) using a conventional phase, the microorganism seed is fed ·HCl solution is sent to the crystallizer,
fermentation process in which raw into the fermenters, which were previ- and lysine salt is filtered. The mother
sugar is hydrolyzed into glucose and ously filled with the fermentation batch liquor is recycled to the evaporator
fructose (invert sugars). The invert medium. After glucose exhaustion, the and the wet cake is conveyed to dry-
sugars are then fermented to pro- batch phase is finished and the fed- ers. Final dry L-lysine·HCl (98.5 wt.%)
duce L-lysine, which is recovered via batch phase is started, during which, is obtained and sent to packaging line
ion-exchange adsorption. glucose and nutrients are continuously before being stored in bags. L-lysine
supplied until the desired L-lysine con- is hygroscopic, so it must be stored in
Process centration is achieved. At the end of tightly sealed containers tightly in dry,
Fermentation-based lysine produc- the fermentation, the broth is sent to cool conditions.
tion from raw sugar is similar to the a buffer tank to provide a continuous
Archer-Daniels-Midland process, and flow in the further process steps. Pathways and uses
Product recovery. The fermenta- The L-lysine·HCl process involving
tion broth is sent to an ultrafiltration sugar fermentation is accomplished by
system for the removal of cell debris modified microorganisms. The sugar
and other suspended solids. Subse- used in the bio-based chemical route
quently, the liquor from ultrafiltration is can be derived from sugarcane, beet
fed to ion-exchange columns, where or corn. L-lysine can also be produced
L-lysine is selectively adsorbed. The from cyclohexene via a chemical path-
FIGURE 1. L-lysine is an essential amino acid with adsorbed L-lysine is then eluted from way. However, only a few plants use
a chiral center
the ion-exchange resins by washing this alternative (Figure 3). n
1. Sugar inversion Editor’s note: The con-
2. Medium vessels tent for this column is de-
3. Fermenters veloped by Intratec Solu-
tions LLC (Houston; www.
4. Buffer tank
intratec.us) and edited by
5. Ultrafiltration unit Chemical Engineering.
6. Ion-exchange unit The analyses and models
7. Evaporator presented are based on
8. Crystallizer publicly available and non-
9. Product filter confidential information.
10. Dryer The content represents the
opinions of Intratec only.
11. Chiller
12. Cooling tower
13. Steam boiler
CW Cooling water
ST Steam
CHW Chilled water
FIGURE 2. The diagram shows the production process for L-lysine
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022 27
Cover Story Part 1
Crystallization for
Ultra-Pure Chemicals
Optimized crystallization units can help address the challenges posed by product-purity
requirements in the battery industry
C
John Warner and rystallization is a key purifica- This article reviews the aspects of crystal-
Nipen Shah tion process that has been used lization technology that particularly impact
JordProxa for decades to refine sugar, pro- the purification of chemicals, and identifies
duce essential pharmaceuticals challenges that operators must overcome,
and recover valuable salts. Producers of as well as key design features that can be
chemicals for applications that demand optimized to overcome these challenges.
IN BRIEF ultra-high purity, such as rechargeable This article uses battery-grade nickel sulfate
CRYSTALLIZATION batteries, which require extremely pure hexahydrate as an example, but the prin-
TECHNOLOGIES nickel, cobalt, manganese and lithium, ciples could be applied to the purification of
PRODUCT PURITY are now turning to crystallization tech- other ultra-pure chemicals as well.
nologies to meet continually increasing
PURITY ENHANCEMENT
purity requirements. Crystallization technologies
FACTORS
In recent years, a rapid increase in de- There are three major types of crystallizers
THE BENEFITS OF LARGE mand for electric vehicles has fueled fast in service today. They are described below:
CRYSTALS product advancements. As a result, the • Forced circulation (FC) crystallizers,
CONTINUAL cost of battery storage decreased by a fac- which rely on crystallization in a mixed sus-
IMPROVEMENT IS KEY tor of six in just five years. pension, may either incorporate mixed prod-
From this period of development, the uct removal or classified product removal
nickel-manganese-cobalt (NMC) chemis- • Fluidized-bed, or Oslo, crystallizers, in
try blend emerged as the top-performing which natural circulation is used to enable
blend for lithium-ion battery performance. fine crystals to be separated by size
Furthermore, automakers learned that • The draft-tube baffle (DTB) crystallizer, in
the key to mass adoption of electric ve- which forced circulation is used to enable
hicles is affordable range. This is best fine crystals to be separated by size
achieved by increasing the energy density
of the batteries through a higher ratio of This article focuses on qualitative insights
nickel in the blend. However, an increased that are or particular relevance to battery
amount of nickel in the batteries comes chemicals. How the configurations of the
with a greater risk of the batteries over- three types of crystallizers impact the for-
heating due to traces of impurity present mation and growth of crystals is discussed
in the nickel-containing battery chemical in Ref. 1. Table 1 provides a high-level
(nickel sulfate hexahydrate; NiSO4·6H2O). comparison of the three different types
To ensure there are no extraneous compo- of crystallizers [2].
nents that will cause the batteries to over- Oslo and DTB crystallizers are both de-
heat, it became critical to use ultra-pure signed to produce larger crystals than the
battery chemicals. FC type by: (a) managing the circulation of
The challenge for the nickel sulfate indus- slurry to avoid excessive supersaturation;
try today, as it strives to meet the rapidly and (b) providing a means of separating
increasing demand for nickel, is to achieve fine crystals, which can then be preferen-
the exceptionally high purity levels that are tially circulated to the heating loop. The first
required for high energy density in batteries. of these features helps prevent nucleation.
A well-designed crystallizer is emerging as The second helps destroy any fine crystals
the critical technology for meeting such pu- that are formed by re-dissolving them into
rity requirements. Figure 1 shows a crystal- the mother liquor as it passes through the
lizer unit that was designed to deliver nickel heating loop. Acting together, these two
sulfate hexahydrate. features narrow the particle-size distribu-
28 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
to be removed.
Fines are returned and will greatly ease the require-
ments imposed upon the upstream
back to the crys-
refining steps.
tal magma
To better understand the role
In the extreme
a crystallizer can play, it is use-
case where high
ful to consider the various ways a
rates of fines
crystal can become contaminated
destruction and
with impurity.
very efficient
A crystal is a three-dimensional
elutriation legs
matrix of atoms arranged in an
are employed
orderly sequence. Theoretically,
to generate very
it should be possible to produce
large crystals
a pure compound by growing the
(greater than 2
crystals from a suitably saturated
mm in diameter),
solution and then separating them.
there is a risk
However, in practice, there are sev-
that the surface
eral ways impurities can be included
FIGURE 1. Due to crystallizers’ unique abilities to deliver high-purity chemi- area of the crys-
either onto or within the crystal ma-
cals, they are being frequently deployed to purify critical battery materials,
such as nickel sulfate hexahydrate tal population will
trix, as shown in Figure 2. These
be insufficient to
were classified in a recent investiga-
tion and increase the mean particle absorb the fresh solids leaving so- tion by Urwin and others [3]. They
size. It is not possible to incorporate lution. Spontaneous nucleation can identified five principal mechanisms
these features into the FC design, occur, resulting in a sudden drop based on the location of the impu-
where the full inventory of slurry is or “crash” of the average crystal rity within the crystallization prod-
well mixed. size. Plant operators have learned
uct: agglomeration; surface de-
The following must also be con- to avoid the population “crashing” position; mother liquor inclusions;
sidered in order to grow and recover by adding mid-sized crystals to the co-crystal formation; and solid
large crystals: crystallizer as “seed” to provide ad-
solution formation.
• Mixing within the crystallizer ditional surface area. Co-crystal formation and solid-
should be as gentle as practically solution formation are controlled by
possible to reduce damage to crys- Product purity the chemistry of the solution, which
tals. Larger crystals will become Since the development of NMC in large part is determined by the
damaged due to momentum chang- batteries with high nickel content, composition of the feed to the crys-
es within the crystallizer. However, there has been increased focus tallizer. We can consider this to be
mixing must be sufficient in order to on the purity of nickel sulfate. In the responsibility of the upstream
suspend the largest of the crystals particular, a de-facto standard of refining process, although it is ac-
and transport them to the boiling four nines purity (99.99% w/w) has knowledged that there is a need to
surface (zone where the highest level been adopted for nickel sulfate provide feedback about the compo-
hexahydrate destined for use in
sition of the concentrated mother li-
of supersaturation exists)
lithium-ion batteries. That allows a
quor, which will be derived from the
• Fines will be generated from
maximum of 100 mg of impurities
feed when the crystallizer reaches
natural breakage (or chipping) of
per kg of nickel sulfate
crystals, as well as by spontaneous hexahydrate product.
nucleation from the supersaturated Nowadays, serious
solution consideration is even
• Although fines destruction in- being given to achiev-
creases the average size of the ing five nines purity. That
crystal population, it significantly would allow just 10 mg of
reduces the available surface area impurity per kg of nickel
for deposition of new solid mat- sulfate hexahydrate
ter. Too little surface area can lead product. Meeting these
to a sudden burst of spontaneous product standards pres-
nucleation ents serious challenges
• Sufficient time must be allowed for nickel refiners. How-
in the magma (semifluid) phase for ever, a properly designed
the growth of large crystals crystallizer can play an
• Classification (or elutriation) of the important role in helping
product removed from the crystal- to achieve four, and then FIGURE 2. There are several inclusion mechanisms for impurities
lizer enables only the largest fraction five nines product purity associated with crystallization
crystallizer will operate with a purge consumer demand. ect references in Australia, Europe and the Middle East.
Prior to the formation of JordProxa, he designed and
flow that is set to no more than 5% When used well, it is clear that crys- sold process plant equipment (often in modular form) for
of the desired product and wash ef- tallization technology achieves the Jord International, and he was instrumental in introduc-
ficiency on the centrifuge that dilutes high degree of purity that is required ing new products into the company’s portfolio to serve
leading global companies. Warner has worked exten-
the entrained mother liquor by a fac- to maximize energy in lithium-ion bat- sively on clean air and clean water projects in both the
tor of five or more. These limiting teries. To stay at the forefront, battery- research and corporate sectors in Australia, the U.S.,
values were used to determine the chemical producers, the minerals Korea, India and Chile. These projects have included the
application of evaporation and crystallization technology
predicted amount of impurity in the processing industry, and their tech- to achieve zero liquid discharge solutions. He holds a
product versus the average diameter nology partners must continue to re- B.S.Ch.E. and a Ph.D. in chemical engineering from the
University of Melbourne in Australia.
of the crystals. The results plotted alize efficiencies that lower costs and
in Figure 5 show that as the crystal deliver increasing value. They must
Nipen Shah is the head of sales at
diameter decreases below 1 mm di- also leverage green energy sources to JordProxa (40 Oxley St, St Leon-
ameter, the amount of impurity in the offer a lower carbon footprint for how ards NSW 2065 Australia; Email:
product increases relatively quickly. to build and operate the plant. ■ nshah@jordproxa.com), a com-
pany specializing in the recovery of
Edited by Mary Page Bailey pure solids from liquid solutions
Continual improvement is key References using evaporation and crystalliza-
Crystallization is critical to meeting 1. Samant, K.D. and O’Young, L., Understanding Crystalliz- tion. Shah oversees the design,
ers and Crystallization, Chem. Eng. Progress, pp. 28–37, costing, proposals, sales and busi-
the benchmark for purity in battery October 2006. ness development activities for the
chemicals. However, if crystallization 2. Shah, N. M., Bradbury, D.S., Rogans, D. M. and Warner, J.J., De- supply of crystallization and evaporation plants for ap-
sign of Battery Grade Purity Nickel and Cobalt Sulphate Crystal- plications involving battery-grade nickel sulfate, cobalt
is to be an acceptable part of the sup- lisation Plants, ALTA Conference Proceedings, May 2019.
sulfate and lithium hydroxide, ammonium sulfate and
ply chain for electric vehicle makers, it 3. Urwin, S.J., Levilain, G., Marziano, I., others, A Structured Ap- zero liquid discharge (ZLD). Shah has a Ph.D. in chemi-
proach to Cope with Impurities during Industrial Crystallization
must also meet the benchmarks for Development, Org. Process Res. Dev., 24, 8, pp. 1,443– cal engineering with specialization in process optimiza-
sustainability and value. Tesla has set 1,456, July 2020. tion from Monash University in Australia.
benchmarks for the industry, which 4. Shah N. M., Bradbury, Warner, J.J., Market Outlook for Bat-
tery Grade Nickel Sulphate and Implications of Varying
have been widely endorsed by other Product Specifications, ALTA Conference Proceedings, Further reading
November 2020.
electric vehicle and battery makers: 5.Warner, J.J., Bradbury, D.S., Shah N. M., The Production of High
For more information on crystallization, please read the
following articles:
• Purity — Battery chemicals must Purity Nickel Sulphate Hexahydrate Suitable for Lithium-Ion Bat-
1. Crystallization: Contributing to Circularity, Chem.
teries by Evaporative Crystallisation, ALTA Conference Proceed-
be free from impurities to allow high ings, May 2018. Eng., March 2021.
2. Moisture Measurement in Solid Materials, Chem.
energy density to be safely achieved. Eng., January 2021.
• Sustainability — The sustainabil- Authors 3. A Simplified Approach to Crystallization Mass Bal-
ity of producing battery chemicals John Warner is the managing di- ances, Chem. Eng., July 2020.
rector at JordProxa (Unit 28/63 4. Nucleation Phenomena in Crystallization, Chem.
must be consistent with the “green” Knutsford Ave, Rivervale WA Eng., May 2020.
credentials of the vehicles that the 6103 Australia; Email: jwarner@ 5. Industrial Crystallization for the CPI, Chem. Eng.,
jordproxa.com). Since the joint November 2017.
chemicals will help power. venture was established in 2018, 6. Confronting Issues in Industrial Crystallization,
• Value — The ratio of perfor- Warner has led JordProxa in its Chem. Eng., November 2017.
mance to cost must increase growth to become a leading sup-
plier of crystallizers to the battery
with time to help drive increased chemical market, with major proj-
32 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
Part 2 Cover Story
Smarter Chemical Recovery
in Pulping Facilities
Evaporation and crystallization technologies have the ability to create advantages for pulping
facilities by improving operational efficiency and reducing waste, while simultaneously
producing high-value product streams
T
Scott Silverstein
he emergence of new prod- and Michael
ucts and markets is driving Begley
a global renaissance of the Veolia Water
pulp-and-paper industry Technologies
due to increased global demand
for cardboard and paper packaging
products, as well as the rise in the
need for hygiene products, such as
IN BRIEF
CHEMICAL RECOVERY
paper towels, tissues and nonwoven
AND ASH TREATMENT
wipes. To adapt to these drivers and
meet this steep demand increase, CHLORIDE REMOVAL
pulp producers and integrated PROCESS
paper manufacturers have been rac- PRODUCING SOP
ing to expand their pulping opera-
tions. In addition to these increased FIGURE 1. A typical chloride-removal process (CRP) in a pulping mill
treats dissolved precipitator ash to remove contaminants and recover
production demands, producers are sodium salts
also feeling pressure from regulatory
agencies, as well as consumers, to con- byproducts, such as high-quality fertilizers.
tinually identify process improvements to Though these sustainability-focused proj-
enhance their sustainability efforts. ects may appear aggressive and require
Pulping facilities require a great deal of investments in new technologies or pro-
water, chemicals and energy, which creates cess changes, in many cases, they can
many challenges when it comes to sustain- significantly improve overall operational
ability. Although the modern pulping process performance within the pulping process
includes sophisticated closed-loop pro- and achieve a quick payback on the capi-
cesses with the ability to recover and reuse tal investment. As a result, both greenfield
water, chemicals and energy, manufacturers and existing pulping facilities can har-
should always keep a keen eye for additional vest the benefits from implementing up-
opportunities that allow companies to lighten grades to their chemical-recovery and
their environmental footprint. One of the key ash-treatment operations.
areas pulping facilities can target is to in-
corporate sustainability projects within the Chemical recovery and ash treatment
plant’s ash-treatment recovery loop. In most modern pulping mills, during the
By enhancing the ash-treatment recov- kraft pulping process, wood is cooked with
ery process with capital improvements, water and chemicals at high temperatures
companies can generate an advantageous in order to separate the cellulose from lignin
proposition. In addition to improving overall and hemicelluloses. The resulting pulp is fur-
plant efficiency, sophisticated ash-treatment ther washed with water. The water used to
projects can significantly reduce discharged wash the pulp, plus the cooking liquor from
waste materials and extend the lifespan of the digester, is called “black liquor.”
critical utility equipment, such as plant boil- Black liquor is concentrated using evapo-
ers — all top-of-mind issues for mill man- ration in order to be combusted as a form
agers. On the sustainability side, enhanced of renewable energy within the recovery
chemical recovery within the ash treatment boiler. Combustion of the black liquor’s
process has the potential to yield valuable solids leads to the generation of energy
A
leading integrated producer, ex- the economics of
porter and recycler of pulp and chemical recovery,
paper in Brazil was looking to ex-
pand its pulping operations.
reducing chemical
discharge and raw
Challenge chemical makeup,
The Kraft process used in the production but also creates
of pulp enables the efficient recovery of challenges for han-
chemicals and heat in a closed-cycle pro- dling and treating
cess. However, it also allows the undesired liquor streams. Non-
buildup of chloride and potassium in the
process elements
recovery cycle, which if left uncontrolled,
can create corrosion and boiler fouling.
(NPEs), including
chloride and potas-
sium entering the FIGURE 2. Glaserite crystals can form during the chloride-removal
process when the crystallization chemistry exceeds solubility limits for
mill through the raw potassium before reaching the chloride solubility limit
wood and chemical
makeup, accumulate in the recovery under-saturated solution feed to the
cycle. Over time, they create condi- CRP system. The CRP system oper-
tions for scaling and plugging in the ates as a true crystallizer, with proper
boiler, leading to lower energy pro- crystal generation, growth and wash-
duction. If left uncontrolled in the ing to maximize the removal of con-
precipitator ash, NPEs can become taminants and recovery of sodium
a significant problem — causing cor- salts. Crystallization occurs through
rosion and boiler fouling — ultimately evaporation of water, causing the
resulting in a reduction in recovery solubility limit of sodium salts to be
boiler capacity and an increase in exceeded. The resulting sodium salt
operating costs. crystals are dewatered and washed
By integrating advanced chloride- in a centrifuge and returned to the re-
and potassium-removal systems to covery cycle via sluicing with black li-
treat the precipitator ash, mills can quor. Chloride and potassium remain
unlock significant operational ben- in solution and are purged from the
Solution
efits and reduced chemical costs, crystallizer in a concentrated stream
After analyzing the composition and per-
forming small-scale pilot testing, it was while simultaneously generating with minimal sodium losses. The CRP
confirmed that the installation of an en- additional revenue streams from system is typically thermally inte-
hanced chloride removal process (ECRP) produced byproducts that also in- grated with a mill’s black-liquor evap-
as a second stage to the site’s existing crease the sustainability of the oration system in order to achieve low
system would be able treat the additional production facility. operational costs.
feed of precipitator ash and prevent signifi- The conventional CRP system
cant boiler-capacity losses and increased
operating costs. With the new system, the
Chloride removal process will achieve a maximum chloride-
site was able to treat up to 10 ton/h of pre- A two-stage crystallization process removal efficiency of 98–99% at a
cipitator ash (equivalent to 240 ton/d). can be used for enhanced removal sodium recovery of 85–95%. For
of NPEs. The first stage consists mills with higher potassium levels,
Creating value from byproducts of a conventional chloride-removal the sodium recovery will be lower.
In this particular case, the SOP produced process (CRP)
from the ECRP system was used by the system (Figure 1)
mill to fertilize its forest reserves to en-
operating close to
hance growth rates for the next genera-
tion of trees. In doing so, the facility was atmospheric pres-
able to close the loop by returning high- sure, followed by
quality nutrient compounds back into a second-stage
the environment. ❑ crystallization pro-
cess designed to
target potassium
and steam, which is used else- within the chemical
where within the plant. Contained recovery process.
in the molten salts (smelt) are most Stage 1 — CRP.
of the needed pulping chemicals, Precipitator ash
which are collected from the re- is dissolved with FIGURE 3. For mills with a particularly high concentration of potassium in
covery boiler and can be reused in condensate, re- the chemical-recovery unit, a second stage can be added to crystallize addi-
the digester. sulting in a slightly tional sodium salts and potentially produce a sulfate of potash (SOP) stream
34 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
For the vast majority of pulp mills, duction of sulfate
the crystallization chemistry will ex- of potash (SOP;
ceed solubility limits for potassium K2SO4) fertilizer.
before reaching the chloride solubil- A portion of the
ity limit. In this case, a portion of the glaserite crystal-
potassium present will crystallize as lizer mother liquor
glaserite (3K2SO4·Na2SO4), which is is purged from
shown in Figure 2. The glaserite will the mill to further
be returned to the mill cycle with the enhance overall
other sodium salts, thereby reducing chloride-removal
the CRP system’s overall potassium- efficiency, with the
removal efficiency. As most pulp mills remainder of the FIGURE 4. SOP is a high-value, crystallized fertilizer product that can create
are more focused on chloride reduc- mother liquor re- an additional revenue stream from pulping mills
tion, the CRP system typically will cycled to the first-
be operated in a way to maximize stage CRP crystallizer. Advanced chemical recovery tech-
chloride removal and soda recovery, Water added to the melter results nologies at pulping facilities can in-
while the potassium removal gener- in selective dissolution of the so- troduce significant benefits for com-
ally ends up in the 70–90% range. dium sulfate and potassium sulfate panies, including reduced operating
Pulp mills with high potassium inputs from the glaserite, leaving purified costs, reduced downtime, and of
may instead wish to maximize potas- potassium sulfate in the solid phase. course the creation of high-value
sium removal and can be limited to The potassium sulfate may then be byproducts, such as SOP fertilizer,
60–80% sodium recovery when op- centrifuged and dried to produce a which can create additional revenue
timal potassium removal is targeted. high-quality SOP byproduct. streams. With respect to sustainabil-
Most high potassium mills must bal- ity, these enhancement projects gen-
ance potassium removal and sodium Producing SOP erally result in reduced water usage,
recovery in order to minimize the cost Crystallized SOP fertilizer (Figure 4) improved energy consumption, less
of sodium losses. is a premium, water-soluble fertil- waste, and in the case of sites that
As a true crystallizer, the conven- izer that is uniquely positioned as a recover nutrients and produce SOP,
tional CRP system is a highly selec- “smart fertilizer” that can allow for these sites can also play a leading
tive purification process to maxi- more consistent results and a higher role in helping secure the global food
mize chloride removal efficiency and quality crop yield. SOP’s enhanced chain, as well as support fertilization
achieve high recovery of sodium water solubility allows the fertilizer to of carbon-capturing forests. ■
salts. Mills that have a high level of be injected into advanced irrigation Edited by Mary Page Bailey
potassium in their chemical recovery systems, which allows for a more ef-
loop have a unique challenge and op- ficient transfer of nutrients to plants. Authors
portunity. By implementing a second SOP fertilizers are also gaining trac- Michael Begley is a senior pro-
stage to the CRP, mills can produce tion over traditional fertilizers be- cess engineer at Veolia Water
Technologies (23563 W Main
additional byproduct streams while cause of their extremely low levels Street, Plainfield, IL 60544; Email:
simultaneously removing high levels of impurities like sodium, chlorine michael.begley@veolia.com) spe-
of chloride and potassium. and heavy metals. These impurities cializing in HPD Evaporation &
Crystallization technologies. His
Stage 2 — Potassium-handling not only can create issues by scal- work involves the design of sys-
enhancements. For mills with high ing and clogging within application tems for thermal evaporation and
crystallization, primarily in the
levels of potassium in the chemical- equipment, but they can also cause pulp-and-paper industry. With more than 33 years of
recovery loop, a second stage can adverse effects to crop quality, es- experience as a chemical engineer, his focus is to de-
be added to complement the initial pecially those sensitive to chlorides. velop new and improved technologies and support busi-
CRP stage (Figure 3). After the CRP Because of these advantages, the ness for the pulp-and-paper sector. He holds a B.S.Ch.E.
from the University of Illinois.
stage, which is operating close to demand for “smart fertilizers,” such Scott Silverstein is a sales man-
atmospheric pressure, sodium salts, as SOP, is expected to significantly ager at Veolia Water Technologies
such as sodium sulfate, burkeite increase. This allows pulping facili- focusing on the commercialization
and distribution of HPD evapora-
(2Na2SO4·Na2CO3) and sodium car- ties to be uniquely positioned as key tion and crystallization technolo-
bonate, are crystallized in the first contributors within the supply chain gies (Same address as above;
stage and returned to the recovery of SOP. With pulping facilities conve- Email: scott.silverstein@veolia.
com). His work involves developing
cycle. The second-stage crystallizer niently positioned across the globe, business projects and managing
acts as an adiabatic flash-crystallizer they can act as decentralized, local accounts for thermal evaporation
unit operating at lower temperature producers of this valuable resource. and crystallization in various water-treatment-related
industries. With more than 17 years of experience as a
to take advantage of the reduced This has the potential to reduce mechanical engineer, project manager and sales man-
glaserite solubility. Crystallized gla- supply-chain logistic costs and en- ager, his focus is to find sustainable water solutions for
serite solids are dewatered in a cen- vironmental impacts by shortening the mining, power generation, lithium-ion battery prod-
ucts, and pulp-and-paper sectors. He holds a B.S. de-
trifuge for subsequent disposal or the distance between the source gree in manufacturing and mechanical engineering from
otherwise further processed for pro- and user. Miami University in Ohio.
C
Robert X. Perez
and Heinz P. entrifugal pumps are widely used the hydraulic minimum flow.
Bloch throughout the chemical process in- Regardless of the reason for pump misap-
Consultants dustries (CPI). Their reliable and effi- plication, the effects of a poor hydraulic fit
cient performance plays a significant will typically be dismal reliability performance
role in plant operations. This article considers and poor overall system efficiency. Figure
the different options on what to do when a 1 shows the numerous adverse effects of
pump begins to operate unreliably or fails. operating too far away from a pump’s BEP
IN BRIEF “sweet spot.” In the field, problems related
PUMP HYDRAULICS Pump hydraulics to off-design operations are typically mani-
HYDRAULIC RERATES
Operation far away from a pump’s best ef- fested by higher than normal vibration levels
ficiency point (BEP) is a common cause of and frequent bearing and seal failures.
PUMP FAILURES pump unreliability. There are a number of rea-
REPAIR OR REPLACE? sons why a centrifugal pump may be found Hydraulic rerates
operating in an off-design condition: The One solution available to avoid problems
REPAIR/SPARE PART
pump may either have originally been mis- caused by an oversized centrifugal pump is
PHILOSOPHIES
applied or the process requirements may to perform a hydraulic rerate on the pump’s
MAKING THE CASE FOR have changed since its initial specification fluid end. The basic idea of a pump hydraulic
UPGRADES and installation. Two minimum flows must rerate is to fit an impeller with a lower flow
PAYBACK TIME be satisfied on the pump curve for reliable rating inside the existing oversized pump
EXAMPLES service: 1) The minimum continuous stable casing. To accommodate a new impeller,
flow (MCSF), which prevents internal recir- case-wear-ring adapters are used to allow
PUMP REPLACEMENT
culation; and
2) the mini-
mum ther-
mal flow, the
point where
rapid inter-
nal heating
begins. The
pump manu-
facturer will
usually state
the MCSF for
its pumps in
its documen-
tation. For
best overall
performance,
it is always
best to keep
the operating
FIGURE 1. The Barringer-Nelson curve shows reliability impact of pump operation away from BEP (Source:
point above Paul Barringer)
36 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
for smaller diameter sets of casing and impeller wear
rings. This would also be a fine opportunity to consider
advanced perfluoralkyl (Vespel CR-6100) stationary
wear parts.
In addition to these modifications, volute throat
area(s) must be matched to the new impeller. This is
done by cutting out the original volute lips and welding
in custom-designed volute lips. This simple, straight-
forward design approach can provide pump users a
cost-effective solution to chronic failures caused by
hydraulic instabilities.
Performing a hydraulic rerate is the task of mechani-
cal engineers, and outside the scope of this article.
More information on how to do this and the benefits
can be found in Ref. 1. We now focus on the decision-
making process for handling a pump failure.
Pump failures
When a centrifugal pump fails, there are several pos-
sible paths forward that a processing facility may con-
sider. The following options are possible:
• Repair the existing pump (Figure 2) at an outside
shop or in-house using replacement parts from stores
• Replace it with a rebuilt pump (in kind) kept in
stores
• Replace it with an identical pump kept in stores or
purchased from a distributor or manufacturer
• Repair it with key upgraded mechanical
component(s) to improve mechanical reliability
• Perform a hydraulic rerate using the existing pump
casing to improve the hydraulic fit (as briefly described
above)
• Replace existing pump with a completely different
model pump that better fits the service
It is important that all centrifugal-pump maintenance
decisions be economically justified, meaning that the
benefits derived from the repair, replacement or modifi-
cation must be of greater value than the base cost. For
maintenance events, such as repairs, the value added
by the repair should exceed the cost of the repair. For
major modifications, economic criteria, such as the in-
vestor rate of return (IRR) and net present value, should
be used to objectively evaluate the benefits of the initial
investment. The benefits of modifications and replace-
ments are typically increased reliability, an improvement
in efficiency, or both. A faithful economic justification
requires that the user understands all the benefits de-
rived by the modification along with all the associated
modification costs.
To decide which path forward makes the most eco-
nomic sense, the reliability professional first needs to
know the following:
1. What is the length of time since the last repair or
the current mean time between failures (MTBF) met-
ric? Best-of-class pumps easily reach MTBF between
six to ten years. Pumps with MTBF of less than two
years should be considered completely unaccept-
able. Therefore, pumps providing MTBF performance
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CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022 37
greater than six years should con- the economic test for deciding if a we see that $1,500 < $4,000. In this
tinue to be repaired as usual and pump should be repaired or replaced case, a repair is not justified since the
pumps providing MTBF performance can be stated as follows: If the value value added by the repair is less than
less than two years should be scruti- added by the repair is greater than the repair cost.
nized for improvement opportunities. the repair cost minus its salvage The reader will note that the lower
Pumps with MTBF between two and value, then it makes more sense to the replacement cost, the more likely
six years should be reviewed on a repair the pump than replace it. This it will make sense to replace a pump
case-by-case basis. can be expressed by Equation (1): than to repair it. Some facilities set
2. What is (are) the root cause(s) of a horsepower limit to define when
the most recent failure? The pump failed pumps are simply replaced,
owners must understand why their (1) which simplifies the decision-making
pump is failing before an upgrade process for a repair shop.
or replacement pump can be evalu- Where:
ated. The most effective modifica- ms = market salvage value Repair/spare part philosophies
tions are those that address the root mpr = market value of the pump after Once a pump is installed, site man-
cause of past failures. repair agement decides its criticality and if
3. How is the pump performing and rva = value added to the pump by the it makes sense to repair it or replace
how close to BEP is it operating? repair it when it fails. Pumps that are fully
4. What is the cost to restore the rc= repair cost spared are considered less critical,
pump back to the manufacturer’s while pumps that are unspared (non-
specifications? From this relationship, we can con- spared) are considered more critical.
5. What is the value of process clude that only repairs that produce There are several cases to consider,
downtime related to an unplanned an added value greater than the cost as follows:
pump failure? of repair makes economic sense. • For smaller, less critical pumps
6. What is the cost of an in-kind re- This statement assumes that the (<5 hp), which are uneconomi-
placement pump and its delivery time. pump in question can be removed cal to repair, either keep complete
7. What is the cost to keep a re- from service and repaired without an pump replacements in stores or
placement pump in stores? economic penalty. order replacement pumps from the
8. What is the cost of design im- Here are a few examples illustrat- manufacturer or distributor when re-
provements being considered? ing how the value-added relation- quired. The decision to either stock
9. What is the total cost of a cen- ship works: a complete spare pump or order it
trifugal pump hydraulic rerate being Example 1. Consider repairing a when required will depend on the
considered? 150-hp centrifugal pump with the expected delivery time.
10. What is the total cost to replace following costs:
• For a fully spared pump that can
an existing pump with one that has a Pump salvage value = $2,000
be removed and repaired because
better hydraulic fit? Post repair pump value= $20,000
the other installed spare is deemed
Value added = $20,000 – $2,000 =
Repair or replace? $18,000 to be reliable and capable of supply-
A common question that comes up Repair cost = $8,000 ing the required flow on its own: In
when pumps fail: Which pump war- Plugging these values into Equation services with medium- to large-size
rants repair and which should simply (1), we see that $18,000 > $8,000. pumps, it makes sense to pull the
be replaced? As described in Ref. 1, Therefore, a repair is justified in this failed pump and repair it — either in
case since the value the shop or off site.
added by the repair is • For a fully spared pump that
greater than the repair can be removed without impacting
cost. the process but takes too long to
Example 2. Consider repair: This might apply to trouble-
repairing a 5-hp cen- some pumps that fail frequently,
trifugal pump with the which may mean that time to repair
following costs: may approach or exceed the time
Pump salvage value = between failures. In these services,
$500 it makes sense to keep a rebuilt or
Post repair pump new pump in stores. When needed,
value = $2,000 the replacement pump can be
Value added = $2,000 removed from the warehouse and
– $500 = $1,500 installed in the field.
Repair cost = $4,000 • For when an unspared pump’s
FIGURE 2. A mechanic inspects a centrifugal pump impeller during a Plugging these val- downtime must be minimized due
repair ues into Equation (1)
38 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM MARCH 2022
TABLE 1. LIKELIHOOD PROJECT WILL BE
APPROVED, BASED ON THE PAYBACK PERIOD • Warehouse spares
other inputs are held fixed, a • Required training and modifica-
Payback Period Range Comment point will eventually be reached tion/updating of operating procedures
< 1 year Sure to be approved at which additions of the input
>1 year but <2 years Likely to be approved yield progressively smaller, or The annualized benefits may include
>2 years but <5 years Difficult project to sell
diminishing, increases in output. the following:
In centrifugal pump applica- • Reduction in repair costs
>5 years Not likely to be approved
tions, the pump’s reliability or • Reduction in production losses
process capability are usually • Increase in process throughput
to its potential economic impact
considered the commodity of inter- • Energy savings
on the plant: These pumps tend
est, while various design improve-
to be more complex and costly, so
ment options can be considered Note that annualized benefits are
it makes sense to store a pump inputs to improve reliability or capa- relative terms. To define an economic
bundle or rotating assembly in the bility to a given economic evaluation. benefit, you need to have a future
warehouse to minimize the repair There is a limit to how many eco- case and a base case. For example,
time in the event of major failures. nomical improvements can be made if a pump is failing twice a year and
Spare seals, bearings and couplings to any given machine. Eventually, costs $10,000 per repair, then the
should also be kept in stores for the nth improvement will no longer base maintenance cost is $20,000/
minor repairs. be economically justified. Here are yr. If you expect the pump failure-rate
An ineffective spare-parts man- some examples of common centrifu- interval to increase to once every 5
agement program can negatively af- gal pump improvements: years, then the future maintenance
fect pump reliability at your site. For • Upgrading mechanical seals and costs are expected to be $10,000/5
this reason, spare parts manage- related sealing systems in a pump or $2,000/yr. In this example, the an-
ment should be an integral part of to improve reliability nualized benefits of the upgrade are
every pump reliability program. How- • Upgrading pump casing metal- expected to be $18,0000 per year.
ever, often spare parts management lurgy to increase useful life The point here is you must always
tends to fly below the radar and is • Installing vibration monitoring consider the future case and the
often given little thought or consider- equipment to prevent catastrophic base case in determining the annual-
ation. To maintain the effectiveness failures ized benefits,
of the program, a team consisting • Rerating a pump to allow op-
of a rotating equipment engineer (or eration closer to its best efficiency
professional), shop foreman, ware-
point (BEP) flow to improve hydrau-
house specialist and a management (3)
lic stability
representative should be involved in
• Installing a spillback line in a
all critical spare part decisions and
tracking. The team should also meet pump’s discharge line to prevent The annualized risk, or simply
regularly to discuss: 1) the status of operation below its minimum contin- risk, is defined here as the sum of
all critical spares; 2) current spare- uous stable flow (MCSF) to prevent all the annualized losses associ-
part stocking levels; 3) changes in internal recirculation at low-flow ated with the failure mode being
stocking levels; 4) decisions to dis- demand conditions analyzed. Therefore, the annualized
pose of obsolete inventory; 5) ad- The payback-period method ex- risk is equal to the annualized main-
dition or deletions of suppliers; 6) plained here is a simple means of tenance costs plus the annualized
stocking upgraded parts, if available, evaluating the benefits of a potential process losses plus the annualized
and so on. After some trial and error, upgrade to management. The pay- environmental fines plus the annu-
an optimal mix of spare parts will be back period is defined as the initial alized demurrage costs and so on.
determined for your given centrifugal investment divided by the expected When evaluating the economics of
pump population. annual revenue realized by the im- reliability projects, we need to know
provement. The payback period of a the differential between the base risk
Making the case for upgrades modification is determined by divid- and the future risk expected from
Rotating machinery professionals are ing the total installation cost of the the improvement. This differential is
always looking for ways to improve upgrade by the annualized benefits: defined as the △Risk, which is the
the reliability or capabilities of their annualized benefit, or revenue, ex-
process pumps. However, there is pected to be realized from a reliability
always a limit to the level of improve- improvement project.
ments that are economically justified. (2) For example, assuming a pump
The economical limit is governed by Installation costs can include, but is failure results in a $20,000 repair,
the law of diminishing returns [2], not limited to, the following items: a $50,000 process loss, and a
which is an economic law stating • Cost of new components and $100,000 demurrage cost, then the
that if one input in the production of equipment losses experienced per seal failure is
a commodity is increased, while all • Demolition and installation costs $170,000. If the pump is failing twice
U
cloth only.
nder the broad umbrella
FIGURE 2. Square weave is the most basic weave
of filter media, there are Common fiber types style used with synthetic materials and wire cloths
many synthetic media ma- As shown in Figure 1, there are sev-
terials, including woven eral common types of fibers used in
filter cloths, woven and non-woven synthetic filter media, as follows:
fabric filter media and filter felts. • Staple fiber fabrics — Yarns made
The term “synthetic” encompasses of many short fibers
cloth materials made of polyeth- • Spun filament fibers — Yarn made
ylene (PE), polypropylene (PP), from multiple discontinuous, small
polyester or nylon, as well as other monofilaments twisted together
specialty materials, such as Saran, • Monofilament fabrics — Fibers
polyamide, Nomex (flame-resistant produced from single extruded
meta-aramid), polyether ether ke- yarns
tone (PEEK), fluoroplastics and other • Multifilament fabrics — Fabric
specially made materials for spe- made from yarns that have several
cific applications. A sub-category of continuous monofilament strands
such media includes wire-cloth filter bundled together FIGURE 3. Square weaves imbue media with high
media. These are woven wire mesh • Woven wire fabrics — Media pro- permeability and stability
made of a variety of metals, the most duced using metallic wires
common being wire mesh made of Also note that combination materi-
stainless steels, such as 316 SS als are available, such as mono/mul-
and 316-L SS. tifilament, mono/staple and multi/
Originally, the materials used for staple combinations.
filter media were silk, cotton and Monofilament fibers offer many
wool. Due to the limitations on the benefits, including excellent diam-
usability of those materials, synthetic eter control for precise fabric open-
materials are used much more often ings, high flowrates, low pressure FIGURE 4. A taffeta weave gives media a rougher
in industrial filtration applications drops, relatively high stiffness and surface that mimics silk cloths
since their introduction around 1945. tensile strength. With these fibers,
Since then, rapid development ac- the filtration mechanism is surface
tivities have widely expanded syn- particle capture, exhibiting excellent
thetic fibers’ applicability in industrial surface particle release. This media
filtration. While cotton and wool are is easy to clean, and also demon-
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(1957–59 = 100) Dec. ’21 Nov. ’21 Dec. ’20 Annual Index: 850
Prelim. Final Final
2013 = 567.3
CE Index_______________________________________________ 776.9 773.1 606.9 800
Equipment _____________________________________________ 979.7 973.8 737.3 2014 = 576.1
Heat exchangers & tanks __________________________________ 832.6 825.7 621.4
Process machinery ______________________________________ 977.6 976.7 737.7 2015 = 556.8 750
Pipe, valves & fittings _____________________________________ 1415.0 1402.1 998.7 2016 = 541.7
Process instruments _____________________________________ 564.0 569.3 433.4 700
Pumps & compressors ____________________________________ 1179.4 1178.8 1086.2 2017 = 567.5
Electrical equipment _____________________________________ 679.0 672.4 571.2 2018 = 603.1 650
Structural supports & misc. ________________________________ 1064.9 1056.6 772.5
Construction labor ________________________________________ 348.0 348.2 336.4 2019 = 607.5
Buildings ______________________________________________ 808.1 796.3 621.0 2020 = 596.2 600
Engineering & supervision __________________________________ 303.3 310.5 311.6
Starting in April 2007, several data series for labor and compressors were converted to accommodate series IDs discontinued by the 550
U.S. Bureau of Labor Statistics (BLS). Starting in March 2018, the data series for chemical industry special machinery was replaced
because the series was discontinued by BLS (see Chem. Eng., April 2018, p. 76–77.)
500
J F M A M J J A S O N D
105
2000 75
100
1900
95 70
1800
90
65
1700
85
60
80 1600
75 1500 55
J F M A M J J A S O N D J F M A M J J A S O N D J F M A M J J A S O N D
*Due to discontinuance, the Index of Industrial Activity has been replaced by the Industrial Production in Manufacturing index from the U.S. Federal Reserve Board.
†For the current month’s CPI output index values, the base year was changed from 2012 to 2017
Current business indicators provided by Global Insight, Inc., Lexington, Mass.
CURRENT TRENDS
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