Members: Ryan Foringer : Team Leader & Process Design

John Miller : Procurement Specialist & Process Design

Curtis Williamson : Engineering Manager & Process Design

Stephen Heisler : Process Automation & Programming Specialist

Emulsion Polymerization

Reactor Group (13622)

Sponsor: RIT Department of Chemical and Biomedical Engineering

Agenda

Project Description

Concept Summary

System Architecture

Design Summary

Complications in Design

System Testing and Results

Project Evaluation

Suggestions for Future Work

Acknowledgements

Project Description

Customer

Need # Priority Description

CN1 1

A mixing vessel with ability to perform temperature control of contents

(i.e. jacket for steam flow, or, jacket for hot water flow, or, electrical

heater.

CN2 1 One outlet of mixed, homogenous, emulsion.

CN3 1

Port, window or lid that allows visual inspection of the mixing vessel

(higher surface area such as the visualization of the top of the entire

vessel might enable better visual assessment).

CN4 1 The ability to see the outlet flow, i.e. the stream lines if dye is added

visible through transparent tubing.

CN5 1 A mechanical mixer/stirrer, designed for emulsion preparation, or other

mixing solution the rate of which can be adjusted.

CN6 1 The ability to control mixer stir rate

CN7 1 Characterization of the emulsion homogeneity in time by taking sequential

samples of the effluent and measuring their viscosity.

CN8 1

Design must include the capacity for temperature control or includes a

strategy by which the temperature control capability could be added in

future projects without the significant alteration of the existing apparatus.

CN9 1 200 g/min coater rate

CN10 1 60 minute batch time with 5 minute CIP

CN11 1 Cost per batch less than $10

CN12 1 Particle size must be visible by optical microscope for product evaluation.

Assumption Room temperature operation

Assumption Viscometers will be provided

Project Description

Specification

Number Importance

Customer

Needs Description

1 Emulsion Characteristics

1.1 1 2 The emulsion shall have a 10micon range particle size distribution.

1.2 1 2

The emulsion shall have a particle growth no more than 5% the original size after 1

hour.

1.3 2 2,7 The emulsion shall have a transmission above .8.

1.4 1 12 The emulsion must have particle sizes between 500 to 5microns.

2 Emulsion Process

2.1 1 10

The entire emulsion batch process shall be 60 minutes with a 5 minute CIP

included

2.2 1 11 The emulsion process shall have a chemical cost under 10$ for each batch tested.

2.3 1 9 The emulsion batch size shall deviate no larger than 5% of a 10L batch.

3 Reproducibility

3.2 1 2

The emulsion shall have a batch to batch particle sizes with no more 5micron

deviation.

4 Flowing Fluids

4.1 2 10 The oil feed shall be sub-fed at a rate of 146mL/s to 66mL/s.

Concept Summary

Lab application for future chemical engineering

students

Visual insight into emulsion creation

Designed for process parameter variability

Low budget batch runs

Future project expansion

System Architecture

97-31 ml/s

200 ml/s

500 ml/s 3 hp

Design Summary

Vessel – jacketed glass reactor

High shear Cowles mixing blade

3 Hp VSD electrical motor

Water, canola oil and sodium dodecyl sulfate

system

Subsurface oil feeding

Complications in Design

Weight of the motor - 61 lbs

Shaft Stability (Chuck Design) - above 1500 RPM

Motor Power Supply - 240V

Subsurface Flow Rate Assumptions

2 minor losses in elbow

1 minor loss from valve

Longer than anticipated discharge

System Testing and Results

Sample Oil (%)

SDS

(wt%)

Avg. Size

(um)

Concentrati

on RPM Shakes

Time

(min)

1 10 0.5 59.75 30100 - 100 5

2 10 1 57.5 52500 - 100 5

3 10 2 45.5 60000 - 100 5

4 10 5 53.5 57500 - 100 5

5 20 0.5 69.25 48200 - 100 5

6 20 1 37 65400 - 100 5

7 20 2 43.75 58800 - 100 5

8 20 5 48.25 65700 - 100 5

9 30 0.5 54 31300 - 100 5

10 30 1 56.25 52500 - 100 5

11 30 2 78.5 56300 - 100 5

12 30 5 69 50000 - 100 5

13 20 6.75E-05 63 33400 1300 - 3

14 20 6.25E-04 57 39000 1300 - 5

15 20 1.25E-03 49.25 42000 1300 - 6

16 20 1.88E-03 27.75 87300 1300 - 7

17 20 1.88E-03 25 92400 1400 - 10

18 20 1.88E-03 25 93600 1500 - 10

19 20 1.88E-03 25 - 1500 - 10

20 20 1.88E-03 25 - 1500 - 10

Compilation of Results

System Testing and Results

System Testing and Results

System Testing and Results Spec

Number Importance CN # Description Target Goal

Pass/

Fail Test #

1 Emulsion Characteristics

1.1 1 2 The emulsion shall have a 10micon range particle size distribution. +/- 10microns from average Pass 10

1.2 1 2

The emulsion shall have a particle growth no more than 5% the original size

after 1 hour. Under 5% growth Fail 11

1.3 2 2,7 The emulsion shall have a transmission above .8. Transmission Value > .8 Fail -

1.4 1 12 The emulsion must have particle sizes between 500 to 5microns.

Particle Diameter between 5-

500microns Pass 4,5,6,9,10

2 Emulsion Process

2.1 1 10

The entire emulsion batch process shall be 60 minutes with a 5 minute CIP

included 60min run time Pass 12,13

2.2 1 11

The emulsion process shall have a chemical cost under 10$ for each batch

tested. $10 batch Pass 7,8,9,10

2.3 1 9 The emulsion batch size shall deviate no larger than 5% of a 10L batch. 5% volume fluctuation Fail All Tests

3 Reproducibility

3.2 1 2

The emulsion shall have a batch to batch particle sizes with no more

5micron deviation. +/- 5microns from average

Pass/

Fail 12

4 Flowing Fluids

4.1 2 10 The oil feed shall be sub-fed at a rate of 146mL/s to 66mL/s. Flow rates between 146-66mL/s Fail 13

CN # Physical Characteristics Equipment Acquired Pass/

Fail

1 A mixing vessel with the ability to control temperature Glass Jacketed Mixing Vessel Pass

3 Reactor allows for visual inspection of the mixing process Glass Jacketed Mixing Vessel Pass

4 Ability to see the outlet flow Glass Jacketed Mixing Vessel Pass

5,6

Mechanical mixer designed for preparation of emulsions and variable

control.

3hp VSD motor, high shear

Cowles blade Pass

8

Heat compatability and ability to add heating element without significant

changes Glass Jacketed Mixing Vessel Pass

Project Evaluation

Successes

Exceeded expectations for particle size

Successful gravity subsurface oil feed

Vessel design exceed expectations

Successful management of obstacles

Failures

Max 1500 RPM

Subsurface feeding flow rate

Particle stabilization

Volume change not taken into consideration

Suggestions for Future Work

Addition of a salt into the process – Particle stability

Chuck Redesign – Shaft stability

In-line measurements – Accuracy

Ensure closed volume system – Fixed Volume

More accurate form of measurement – Precision

Pump installation – Flow rate dependence

Automation Valves Pump Motor Labview Temperature control

Acknowledgements We would like to thank the Rochester Institute of Technology Department of

Chemical and Biomedical Engineering in funding the Emulsion Reactor.

A thank you to Christiaan Richter for the opportunity to develop the Emulsion Reactor .

A special thanks to Neal Eckhaus and Steve Possanza for their guidance in project management and expert advice in engineering design.

We would also like to thank Kevin Penfield from Croda Inc, whom had helped us narrow down our range of variables and provided insight into stable emulsions.

Many thanks to Gabriel Zajia and Mike Sanchez for lending their expertise on emulsion generation techniques.

Thank you Karuna Koppula for your assistance with the flow systems design.

Thank you Ken Ruschak and Evident Technologies for the donation of chemicals for our tesing.

QUESTIONS