Download - Case Study: API Recovery Process
Consultancy.
Project Delivery.
Innovation.
Case Study: API Recovery Process
Process Design leads to £10m/year savings
Client: Multinational Pharmaceutical Manufacturer
Who are we?
Process engineering consultancy
Specialising in advanced modelling techniques, to give answers that
are more accurate, reliable and robust
Decades of process and mechanical engineering experience
Combine cutting edge simulation with real world understanding, to
provide you with solutions that are effective and practical.
Experience in Pharmaceutical / Fine Chemicals
Page 2
Project Background
FDA Approved Process
Manufacture of valuable API, recovered through filter dryer
10% of product lost as 0.7% solution in aqueous mother liquor,
representing ~£15m/year
Lab scale trials had demonstrated 90% recovery of this when extracted
with acidified MTBE in a stirred batch vessel
Caustic added to MTBE solution, API forms the soluble sodium salt in
the aqueous phase in concentrated form.
MTBE removed by batch vacuum distillation
Calcium added to aqueous phase to precipitate out the API
API re-filtered and spent mother liquor sent for further effluent treatment
Page 3
Our Responsibilities
Work within constraints fixed by pilot trials and FDA application and
three possible locations on site
Complete survey and feasibility to determine best location, that:
Minimises cycle time, does not restrict main production of API
Minimises capital cost
Can be sufficiently automated
Will not result in more solvent emissions from the site
Write up feasibility work and produce flow diagram of proposed option
Develop Front End Design
Develop Detailed Design
Page 4
Final Process Flow Diagram
Page 5
+5°C HTF
Vent
Condenser
E6-3010
VOC
Abatement
FIQ
Pure
Water
+5°C HTF
Vent
Condenser
E6-0984
VOC
Abatement
GN2
FIQ
Pure
Water
E6-0700
Feed
Vessel10m3
1500, 1600 & 2000
Mother Liquors
Salt Soln to Heel Recovery
Retreat
Material or
NaCL
E6-3003
GN2
GN2
GN2
GN2
PRODUCT
+5°C HTF
Condenser
1M HCl
YI
3rd Floor
1st Floor
Ground Floor
2rd Floor
E6-0500E6-0800
E6-0600
E6-0400
YI
Dedicated
Filter Dryer
Calcium Chloride
(Ex-E6-1829)
MTBE Solvent
(ex Bulk)
+5°C HTF +5°C HTF
Vent
Condenser
Vent
Condenser
FIQ
1M
HCl
0.25M
NaOH
Decant
Decant
pH
pH
+5°C HTFDistillation
Condenser
E6-3003 (Spent MTBE)
4m3
E6-3003 (Waste
Distillate)
FIQ
Pure Water
10m3
10m310m3
6.3m3
E6-1320
E6-1300
SOLID PRODUCT
to Matcon Bins
Precipitator
E6-3101 Waste Tank
(Grand Mother Liquors)
Dedicated
Filtrate
Receiver
Aqueous
Receiver
Extract
Receiver
Extraction
Vessel
Vacuum
Distillation
10m3
VOC
Abatement
+5°C HTF
-20°C HTF
Condenser
Condenser
E6-3003
E6-3005
3005
E6-3003/5
E6-0200
E6-3005
E6-0207
E6-0204
E6-0201
E6-0507
0.25M
NaOH
Pures Charging
Booth
E6-0420
E6-0520E6-0505
Organic
Aqueous
Waste
E6-3001
E6-0208
4" S
elf V
en
t - Lin
ed
6" S
elf V
en
t - Lin
ed
3" S
elf V
en
t - Lin
ed
E6-0613
E6-0511
Venting
Manifold
E6 – 0825
(coarse filtration)
SP
E6
-02
05
SP
HCC Pump
E6-0203
Vent
E6-0206
+5°C HTF
Vent
E6-0605 E6-0405
E6 – 3505
(fine filtration)
E6-0211
Vac Pump
E6-0980
VOC
Abatement
+5°C HTF
Vent
Condenser
VOC
Abatement
E6-0512
VOC
Abatement
E6-1200
Precipitator
Filters 1520,
1620, 2020
Glove
Bag
E6-0982
(Ex E6-0613)
Backventing Line
E6-3003
GN2
SI-01
SI-02
SI-03
FCV
Waste
Receiver
INVENTORY 11
INVENTORY 08
INVENTORY 09
INVENTORY 10
INVENTORY 07
INVENTORY 02
INVENTORY 01 INVENTORY 04
INV
EN
TO
RY
03
INV
EN
TO
RY
05
INV
EN
TO
RY
06
Including all
Services/
Utilities &
Relief Streams
INVENTORY 12
INVENTORY 13
MTBE
Storage F120
& Transfer
Line to E6
E6-0713E6-0413
1st Floor
Ground Floor
2rd Floor
E6-0202
(Ex E6-0511)
Part of Inventory 12
Inside E6
Cycle Time Evaluation – Software Tools
Page 6
Using Aspentech’s Batch Plus Simulation Software to:
Develop process recipe and run as a script
Quickly identifies pinch points and conflicts
Optimise process step timings and use as basis for sizing equipment
Obtain outline heat and mass balance and utility consumptions
Support the design from concept to commissioning
Develop first draft Standard Operating Procedures
Develop OQ Protocols
Process Design Activities – Part 1
Process changes on P&IDs
HAZOP
Checking suitability of existing equipment (e.g. pumps, lines)
New line sizing (pumped and gravity) for new plant configuration
New equipment specifications (e.g. vessel, agitator, heat exchangers)
Full materials of construction review, particularly as strong acids used
Consideration of MTBE vapours when moving liquids between vessels,
quantifying simultaneous vapour losses to assess impact on CATOX.
Specification of high efficiency knock-back vent condensers
Page 7
Process Design Activities – Part 2
Full utility assessment, particularly on chiller system, to understand
instantaneous demands and impact on other building users.
Balancing heat transfer fluid systems to route to new locations.
Assessment using network flow software such as AFT Arrow/Fathom
Two phase reacting relief studies for vessels and jackets
Development of IQ/OQ protocols and briefing of production staff on new
process design
Overseeing mechanical design to ensure that process requirements are
met
Page 8
Outcomes
Predicted cycle time and product recovery proved on commissioning
Design made the best use of existing equipment and maximised gravity
transfers to avoid purchase of additional pumps
Project budget and timescales met
Minimal required changes at commissioning
Client reported years of trouble free operation since commissioning
Page 9
Summary
Led FEED and oversaw Detailed Design to deliver process providing
client with ~£10m/ year savings
Used a combination of simulation expertise and design experience to
minimise capital costs (including re-use of existing equipment) and
optimise operations
Fully evaluated all the production risks with sharing the facility, including
ease of construction, risk of cross contamination and automating needs
Provided a full design package with supporting process calculations and
documentation, including two-phase reacting relief
Process was implemented with minimal start-up changes, and predicted
cycle time was validated
Page 10
Summary
Page 11
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Project Delivery.
Innovation.
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