scale-up of a reactive chemical process utilising cobr technology · 2018. 7. 3. · specific heat...

Innovation you can build on™Innovation you can build on

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Name, DateJames Birbeck, Manufacturing Manager, 27 June 2018

Scale-Up of a Reactive Chemical Process

Utilising COBR Technology


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Agenda / Contents About Croda

Project Vision and Problem

Why Use COBR Technology?

Laboratory Work

Project Video

Pilot Trials

Takeaway Messages

Questions

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Who We Are & What We Do

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We are the name behind the high performance ingredients and technologies

in some of the biggest, most successful brands in the world: developing,

making and supplying speciality chemicals that are relied on by industries

and consumers everywhere.

Our Business Model

Engage Create SellWe work in close

partnership with

customers and develop

emerging technologies

around the world

We design innovative

ingredients that

enhance everyday

products

We manufacture to

consistently high

standards across the

world

We generate revenue

by selling our

ingredients directly to

customers

Make


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Where We Operate

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Our glo

bal te

am

37 Countries 68 Operating Sites 4,309 Employees


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The Vision

To deliver a manufacturing process that could:

Produce consistent high quality material, at least as

good as the existing process

Be flexible enough to efficiently switch products of

similar chemistries

Have a significantly smaller footprint, thereby reducing

capital costs spent on infrastructure

Increase our operating efficiency and reduce our

carbon footprint

Enable high levels of service to our customers through

increasing capacity without limiting agility

Deliver an innovative process that could set a

benchmark by which other processes measured

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The Problem

Croda was becoming capacity constrained on a critical

asset

The cost of replacing the asset was high largely due to

infrastructure costs

Alternative technologies were sought and COBR was

identified as likely to yield success

Successfully applied for funding from Innovate UK to

support this development project

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Issues With Scale-up

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Kinetics

Heat transfer

Physical properties Mixing different phases

Mass transfer

Thermodynamics


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Why Flow Chemistry?

Mixing

Heat Transfer

Mass Transfer

Gas Dispersion

Particle Suspension

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Mixing is at the heart of chemical process industries


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Traditional Routine of Scaling Up

Lab Pilot Full scale

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Kinetic reaction

time e.g. 30 mins

Overall process

time e.g. >30 hours


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Specific Heat Transfer Area Decreases

Significantly with Scale

It takes much longer time to heat or cool industrial scale stirred tank vessels

NiTech’s COBR technology gives the same specific surface area for heat transfer at full scale as in the laboratory

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Diameter (m)

Height (m)

Volume (m3)

Surface area (m2)

Surface area / volume (m2/m3)

0.001 m3 STR 0.05 0.5 0.001 0.08 80

1 m3 STR 0.75 2.3 1 5.33 5.33

10 m3 STR 1.50 5.6 10 8.44 0.844

50 m long DN50 NiTech

Reactor0.05 50 0.098 7.85 80

Diameter (m)

Height (m)

Volume (m3)

Surface area (m2)

Surface area / volume (m2/m3)

0.001 m3 STR 0.05 0.5 0.001 0.08 80

1 m3 STR 0.75 2.3 1 5.33 5.33

10 m3 STR 1.50 5.6 10 8.44 0.844


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Demonstration of Radial Mixing

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Reo = 1250 (xo = 4 mm, f = 1 Hz)

Real system 3-D CFD simulation


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Demonstration of Plug Flow

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Oscillation

Out

Tracer

liquid

Conductivity probes

Probe 13.7 meters away from injectionProbe 27.9 meters away from injectionProbe 310.1 meters away from injection

No. of CSTR = 550 for a RT of 60 mins

E ~ 10-3 10-4 m2 s-1


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Why is COBR Technology of

Interest to Croda

• Provides opportunities for more streamlined processing

Smaller footprint

• Necessary when manufacturing speciality chemicals

High throughput

• Better for higher viscosity oleochemicals

Low pressure

drop

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How Does Our Business Need to

Adapt?

Workshops with Cambridge IFM highlighted ways each organisation needed to adapt to move forward with this type of technology

For Croda these included:

How do we ensure a smooth transition for our customers onto this technology, e.g. re-approval

Gain a realistic understanding of readiness levels for technologies like COBR

Understand how disruptive process technology fits into Croda’s strategy

Understand the true value of any quality improvements for our customers

Aiding acceptance of new technologies and the value that they can bring to our business

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What Could This Deliver for Our Business?

Better ability for us to locate manufacturing processes closer to our

customers or raw materials

Equipment can be designed and built in the UK but shipped globally as

required due to footprint reduction

Reduce the need for large storage tanks, and better ability to meet

supply chain requirements

Allows Croda to be more agile and more quickly meet changing market

demands

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Mobile COBR Plant


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How We Started

As a collaborative project team offering their own skills: Croda, CPI, NiTech and University of Cambridge IFM

Initially laboratory work was used to identify fundamental reaction parameters

Although Croda had been running the process a number of years some of these parameters were not known

Our initial discoveries paved the way for designing an effective reaction process on COBR

But also allowed us to better optimise our existing asset, allowing us more time to develop this technology

Business modelling to understand how we to adapt to fully utilise this type of technology

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Laboratory Work

Started with small batch OBR

Used to identify key reaction parameters

To prove the concept

Transferred processonto a continuousglass OBR

Proved the reactor capabilities

Synthesised sufficientmaterial for testing

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Laboratory Results

Full kinetics of each of the reactions identified

Enabled us to understand the chemistry and not the existing process

Gained a better understanding of factors that affected kinetics

Proved the potential for COBR technology to be utilised

Understood the likely scaleup outcomes

Allowed rough reaction window to be identified

Reactor design scope derived from this

Better understanding of the reactor allowed us to improve our batch process

Allowed it to run faster and increased capacity

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Project Video

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Pilot Plant Delivered

A fully operational COBR pilot unit capable of

producing materials in specification

Plant trials to determine the operating window for the

process and optimisation

Ability to produce all of the materials under

investigation

Flexible design to allow modifications during the trials

Full scale plant design now underway

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Pilot Trials

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Pilot trials took place at Croda’smanufacturing site

Fed directly from the plant

Three products manufactured

Over 70 tons of material was made, almost all in specification

Some design modifications were made during the trials

Important lessons learned to take forward to final design


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Use of Inline Analysis for Self-Optimising

Process

•CoA

•Offline

•Measurement

•20 samples

Input

•Process parameters

•Data logging

•6M data points

Process•Specification testing

•200 samplesOutput

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Importance

for quality

Importance

for efficiency

High High Low

High MediumMedium


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Use of Inline Analysis for Self-Optimising

Process

Inline RM analysis

Input• Process

parameter

• DCSProcess

• Inline analysisOutput

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Control parameters

Optimise based on parameters and output quality - continuously


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What Did We Learn?

1. A significant amount about our process!

2. Using genuine raw materials is important, otherwise

this can lead to false results

3. Ensure you have suitable lab equipment and do not

underestimate the challenges of continuous synthesis

4. Analytical methods for testing mid-reaction are critical

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What Did We Learn?

5. The transition to continuous is much easier with a

thorough batch study, use DoE methodology to test all

areas of the possible reaction window

6. Scale-up was easier than expected, the reactors

performed better through the scale-up process

7. Cleaning needs to be understood before full scale

design

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Takeaway Messages

COBR technology can transform industrial processes

But this may not currently be possible for all

process

The fundamentals will guide the possibility and final

design

Without this the processes is not well enough

understood to transfer to continuous

Have a vision of what the future looks like

Without this it will be difficult to break down the

barriers of tradition and fear of change


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Any Questions?

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scale-up of a reactive chemical process utilising cobr technology · 2018. 7. 3. · specific heat...

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