WHY IS PILOT PLANT IMPORTANT ?

PROCESS ENGINEERING – BCT 403

MAYURI DUTTA
01016100416
BIOCHEMICAL ENGINEERING
B.TECH – 4TH YEAR
PURPOSE OF PILOT PLANTS

 In the development of commercial chemical processes to manufacture new

products or to use new feedstocks to produce existing products, a number of steps
are needed before the commercial plant is built and operated. These steps begin
with initial laboratory experiments that establish the necessary unit operations for
the process flow sheet and end with the design of the commercial plant.
 A pilot plants acts as a bridge between the initial laboratory development work
and the design, construction, and operation of the commercial plant. It is usually
operated to provide engineering data, demonstrate technical feasibility for the
commercial design, thereby reducing the inherent risks attached with developing
a new process and allowing for a more economic assessment of the process.
 GOALS OF A PILOT PLANT
Following are goals that are commonly required from a pilot plant program. However, because
each pilot plant program has unique requirements, not all of them may apply to all pilot plants : -

 confirm the technical feasibility of a proposed process, either on a continuous basis or larger scale batch operation
 confirm the range of operating parameters such as temperatures, pressures, and feedstock composition that will produce
acceptable product quality and recovery
 generate prefeasibility and feasibility engineering data for the commercial design
 produce sufficient quantities of product for market evaluation or clinical trials representative of what will be made in the
commercial plant
 demonstrate the process using commercial-grade reagents and recycle streams
 confirm the composition of intermediate streams
 confirm the expected product yields and purity from the commercial plant
 generate data to confirm the commercial mass and energy balance
 determine reagent consumptions expected in the commercial plant
 provide data to determine the economic feasibility of a new process, including capital and operating costs
 identify unwanted side reactions and demonstrate control of these reactions
 determine materials of construction for the commercial plant
 obtain environmental data for permitting
 determine waste stream compositions from the commercial plant and required treatment operations
 determine the potential for scale buildup in processing equipment and methods to minimize scaling
 develop standard operating procedures for the commercial operation
 develop and test the operability of the process control scheme planned for the commercial plant
 produce small-scale quantities of specialty chemicals for smaller niche markets
PILOT PLANT PLANNING
 Appropriate planning is key to a successful pilot plant program. All successful piloting
projects start with a clear understanding of and alignment with the business needs of the
company. The consequences of overlooking this first step can range from significant delays
to project failure. These different needs should include :-
 Marketing needs
 Commercialization needs
 Technological needs

 During the pilot program planning, it should be kept in mind that pilot plant operations
generate data in four general forms:
 Plant operating conditions, principally temperature, pressure, retention time, and flow rates
 Assay results of stream samples
 Physical properties of streams, such as specific gravity, slurry density, particle sizes, and
viscosity
 Observations by the pilot plant personnel
CASE STUDY : BASE-CATALYZED
DEGRADATION DUE TO RECYCLED SOLVENT
USE

 The United States Pharmacopeia-National Formulary (USP-NF) is a book of public

pharmacopeial standards that defines the allowable impurity level in the manufacturing of Active
Pharmaceutical Ingredients (API).
 For cases when biomass is used as the feedstock, the extraction and purification of the API
compound results in a purified product with very small amounts of a family of molecules having
very similar structure and behaviour. Due to which the manufacturing process is then designed to
target these specific impurities. The dilemma arises in deciding on how much impurity can be
removed from the product without sacrificing the yield.
 In the following example, the process as delivered to the pilot design team used a marker
compound to make impurity-based process decisions. Because of the extremely low level of
select impurities, the analytical method in use was unable to fully resolve the product
impurity profile until almost the last purification step.
 It was determined at the bench scale that this marker compound would predict the behavior of all
impurities roughly 80% of the time. All of the unit operations in the purification process were
designed to remove specific product analogues based on polarity, and the marker compound
correlation was the basis of a validation of the process.
 During the pilot operation of the API process, the first production batch appeared
to be within USP–NF specification during in-process testing. However, at the
final purification stage, an unknown impurity was detected at levels exceeding
the default of 100 ppm.
 After much deliberation, it was determined that the unknown impurity was a
degradation product of a known impurity, and that the process was incapable
of removing it. As a result, the pilot batch was destroyed, and the process was
sent back to the bench scale to address this new impurity.
 It was the discovered that the unknown impurity was created early in the process
due to the buildup of residual weak base in the primary solvent used in the
process, which was recycled. All the compounds in the family of the API are
subject to base-catalyzed epimerization, and the epimer of the API was an
expected impurity.
 Process steps had been designed to accommodate the gradual degradation of the
API to its epimer in small amounts. What had not been considered was that
some of the key impurities would also undergo this degradation, and these
degradants had not been included in the correlation study with the marker
compound.
 The development of the process at the bench scale had used technical-grade
solvent that did not contain enough of the base to affect the epimerization of the
impurities.
 When the switch was made to the recycled solvent at pilot, the process
effectively created a new family of impurities that had not been addressed.
 To overcome this problem, the pilot plant was stopped and the process
development program returned to the laboratory to alter the process to handle
these impurities.
 This required that the pilot plant be redesigned, delaying the implementation of
the commercial process and greatly increasing the development costs.

This case study is a great example of highlighting the significance of pilot plant. Had
the manufacturing process been shifted straight from the bench scale to commercial
scale, it would have led to a colossal loss of raw materials, economy, energy and
time, due to a crucial flaw in the process, that was discovered in the pilot scale. It is
therefore extremely important to realize that a pilot plant should be a scaled-down
version of the commercial operation, not a scaled-up version of the laboratory
apparatus.
REFERENCES

1. Gertenbach, D. (2018). Pilot Plants. Kirk-Othmer Encyclopedia of Chemical

Technology, 1–21.
2. Gertenbach, D., & Cooper, B. (2009, November). Scaleup issues from bench to
pilot. In American Institute of Chemical Engineers National Meeting, Nashville,
TN (Vol. 8).