emulsion polymerization reactor

Members: Ryan Foringer

John Miller Curtis Williamson Stephen Heisler

Emulsion Polymerization Reactor Group (13622)

Agenda   LabVIEW analysis   Updated Customer needs/P&ID/PFD   Test Plan   System Architecture   Updated Engineering Specifications   BOM and Gant Chart   Risk Assessment

Changes To Customer Needs

  Changed  Two Inlets no longer required  Control of the inlet flow rates is only open close  Automated process no longer required  Automated overflow protection no longer required

  New  Tank must feed downstream coater at 200 g/min   60 min batch time with 5 min CIP  Cost per batch is less than $10   Particle Size must be visible via optical microscope for product

evaluation

Updated Block Diagram

Updated PFD

Test Plan

Test Plan Example Format

Test Plan Example Testing Steps

Feasibility Analysis - Vessel

Glass Vs Stainless Steel •  Cost •  Heat Loss •  Durability •  Reaction Visibility •  Use in Lab setting

Feasibility Analysis – Mixing Blade   Cowles Mixer vs Propeller Blade type mixers

  Emulsification ability   Propeller blade testing   Expert Opinion

 Availability

Feasibility Analysis- Particle Size

S

O

SO

t

t

MMRatiio

RV

V

RRP

xnVn

=

=

−+=

+=

+=−

30

33max

3max

34

)(34

10)9.264.27(

)1265.154(.

π

π

CMC Calculations and Equations

Symbol Value Units n 12 atoms R 25000 nm Lmax 1.672 nm Vt 0.3502 nm3 P 3.75E+10 Par@cles Mols (SDS) 6.23E-‐14 mol Mass (SDS) 1.8E-‐11 g Volume (Oil) 6.54E-‐08 cm3 Mass (Oil) 6.02E-‐08 g Ra@o (O/S) 3353.089

R

Feasibility Analysis- Particle Size Inputs

Par@cle Diameter 50 microns Volume of DI Water 18 L

Outputs Volume of Canola Oil 2 L

Mass Ra@o of Oil to SDS 3353.089 O/S Mass of SDS 0.548748 g Batch Cost 4.688747 $

Inputs Par@cle Diameter 50 microns

Volume of DI Water 10 L Outputs

Volume of Canola Oil 10 L Mass Ra@o of Oil to SDS 3353.089 O/S

Mass of SDS 2.743739 g Batch Cost 23.44373 $

Condition 90% DI-Water 10% Oil



Volume of DI Water 15.73447 L Outputs

Volume of Canola Oil 4.265533 L Mass Ra@o of Oil to SDS 3353.089 O/S

Mass of SDS 1.170351 g Batch Cost 10 $

Condition Converged Volume to meet Customer Need 11












Volume of DI Water 18.07175 L Outputs

Volume of Canola Oil 1.928252 L Mass Ra@o of Oil to SDS 335.1071 O/S


Condition Converged Volume to meet Customer Need 11

Feasibility Analysis- Particle Size   Assumptions

  The cost of DI Water is negligible   The CMC theory equations are applied

  Desired Parameters   Batch Cost is $10.00   Oil to DI Water ratio varies from 10% to 50%   Vessel Size needs to meet a 200g/min continuous flow rate to the

coater

  All Three conditions cannot be simultaneously met   Optimum parameter to be changed: Coater Flow Rate

  All three parameters could be achieved simultaneously   Overall cost of reactor will decrease

Feasibility Analysis- Sub-Feed Flow Calculations

h0 h2

h3

h1

P2

Tank 1

P1

Tank 2

P1 =!oilgh1

P2 =!oilg h2 " h0( )+!h2ogh0

#V2#t

= A2#h2#t

=m

#V1#t

= A1#h1#t

= "m

m =$D4!128µL

P1!oil

+gh3%

&''

(

)**"

P2!oil

+

,--

.

/00


  Flow Rate Analysis Assumptions   Incompressible liquid   Fully developed flow   Laminar flow  Discharge is to bottom of tank (h=0)

  Optimized Dimensions  Oil vessel height above reactor vessel   Pipe Diameter  Oil Vessel Diameter


  Oil vessel height above reactor vessel   Higher h3, more constant flow rate

  Slight decrease in discharge time

  h3>1m is unrealistic for apparatus dimensions

  Diameter of pipe

Pipe Dia Approx. Flow rate Tank 1 emp6es?

in ml/s Worst Case (50% oil)

0.25 6.08 N

0.5 97.29 Y

0.75 492.5 Y


  Percentage Oil to Aqueous Analysis

Oil % Discharge Time Start Flow Rate Final Flow Rate

s m3/s m3/s

10 181 0.0126 0.0081

20 302 0.0172 0.0082

30 392 0.0219 0.0084

40 464 0.0264 0.0085

50 523 0.0311 0.0087


0

20

40

60

80

100

120

140

160

180

0 10 20 30 40 50 60

Flow

Rat

e (m

l/s)

Percentage Oil

Discharge Time vs. Oil Percentages


0

20

40

60

80

100

120

0 10 20 30 40 50 60

Flow

Rat

e (m

l/s)

Percentage Oil

Flow Rates vs Oil Percentage

Starting Flow Rate

Final Flow Rate


  10% Oil, 2in Dia

-0.01

0

0.01

0.02

0.03

0.04

0.05

0.06

0.07

0 10 20 30 40 50 60 70 H

eigh

t In

Tank

1 (m

)

Time (s)

Height In Tank 1 vs Time

0.00003

0.000032

0.000034

0.000036

0.000038

0.00004

0.000042

0.000044

0.000046

0 10 20 30 40 50 60 70

Volu

met

ric

Flow

Rat

e (m

3/s)

Time (s)

Volumetric Flow Rate vs Time


  50% Oil, ½ in Dia

-0.1

-0.05

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0 50 100 150 200 250

Hei

ght I

n Ta

nk 1

(m)

Time (s)

Height In Tank 1 vs Time

0

0.00002

0.00004

0.00006

0.00008

0.0001

0.00012

0 50 100 150 200 250

Volu

met

ric

Flow

Rat

e (m

3/s)

Time (s)

Volumetric Flow Rate vs Time

Engineering Specifications Specifica6on Number Importance Customer

Needs Descrip6on 1 Emulsion Characteris6cs 1.1 1 2 The emulsion shall have a 10% standard devia@on par@cle size distribu@on. 1.2 1 The emulsion shall have a par@cle growth no more than 5% the original size per hour. 1.3 2 2,7 The emulsion shall have a transmission above .8. 1.4 1 The emulsion must have par@cle sizes that are easily observale by means of op@cal imaging. 2 Emulsion Process 2.1 1 10 The emulsion batch dura@on shall be within 60 minutes to perform desired specifica@ons. 2.2 1 11 The emulsion process shall have a chemical cost under 10$ per batch. 2.3 2 10 The emsulsion process shall end with a 5 minute CIP as part of the process dura@on. 2.4 1 9 The emulsion batch size shall be large enough to compensate for a coater feed rate of 200g/min 3 Motor Proper6es 3.1 2 6 The motor shall have a rmp ramp rate of 100rpm/s. 3.2 3 5,6 The motor shall have max rmp of 6000rpm. 3.3 1 7 The motor shall have a rpm that corresponds to a shear rate. 4 Flowing Fluids 4.1 2 2 The solvent/surfactant flow rate shall be 500mL/s into the vessel. 4.2 2 The emulsion fluid shall drain out of the vessel at a rate of 250mL/s. 4.3 2 The oil feed shall be sub-‐fed at a rate of 25mL/s

Bill of Materials

Risk Assessment ID Risk Item Effect Cause Likelihood Severity Importance Ac6on to Minimize Risk Owner

Describe the risk briefly

What is the effect on any or all of the project deliverables if the cause actually happens

What are the possible causes of this risk L*S

What ac=on(s) will you take (and by when) to prevent, reduce the impact of, or transfer the risk of this occurring

Who is responsible for following through on mi=ga=on?

1 Customer Needs Requires For Expensive Vessel

Budget Surpassed, Customer Need 1 not met

Ideal reactor vessel material is Stainless Steel and calls for jacked vessel both of which are expensive.

3 3 9

Sacrifice energy savings, and use less conduc@ve glass vessel. If jacket is too expensive to implement, disregard need *approved by customer*

Ryan

2 Subfeeding doesn’t complete emptying of the oil vessel

Process fails, Emulsion not created. Customer Need 2 not met.

Assump@ons on flow rate feasability analysis were too lenient. 3 3 9

If subfeeding fails and cannot be fixed, we will revert to a top feeding system.

Ryan

3 Flow from Oil Tank exceeds Predic@ons

Unrealis@c flow rate, improper emulsifica@on Flow Calula@ons inaccurate 3 2 6

If flow rate is too high, poten@al correc@on with valve opening, change of pipe size possible

John

4 Par@cle is not visible by op@cal means

Customer Need 12 is not met and analysis of par@cle cannot be determined

Mixng @me and rate may not be at op@mum values 2 3 6

If aher chemical tes@ng op@miza@on, desired par@cles are not achieved, poten@ally a new surfactant or oil could be used.

Cur@s

5 Unable to achieve stable, repeatable par@cle size.

Customer Need 2 not met Theore@cal CMC calcula@ons were inacurate. 2 3 6

If aher chemical tes@ng op@miza@on, desired par@cles are not achieved, poten@ally we could add thickening agent or mixed surfactants.

Cur@s

6 Tes@ng Facili@es Not available

Cannot test chemical combina@ons, process configura@ons

closed, booked 2 2 4 Prevent; schedule tes@ng ahead of @me to ensure availability Cur@s

7 Chemicals Not Available Tes@ng is delayed Backordered, delayed in shipment 1 3 3 Prevent: Order chemicals in advance,

check availibility John

8 Defec@ve Equipment Delayed project comple@on, budget exceeded

improper construc@on, structural integrity comprimised 1 3 3 Purchase equipment in advance. Stephen

9 Insufficient mixing of the oil water solu@on

Target par@cles not achieved/ batched lost. Motor failure 1 3 3

Ensure motor is func@onal prior to batch run, and ensure motor is in spec.

John

10 Blade doesn’t provide proper shear mixing

Target par@cles not achieved within max batch @me

Current blade is not appropriate dispite expert guidance. 1 3 3 Back up informa@on from experts

with blade company website info. Stephen

11 Valve Fails Loss of batch Poor Manufacture 1 1 1 Inspect valve before purchase, if fails, purchase new valve. John

Satisfaction of Customer Needs Customer Need # Process used to sa@sfy specific customer need

1 The vessel that will be purchased for this emulsion will be a jacketed glass wall vessel with an inlet and outlet port for temperature controlling flow.

2 This need will be sa@sfied through the par@cle size tes@ng plan.

3 The vessel that will be purchased for this emulsion will be a glass walled vessel, so every part of the emulsion will be visible to the viewer.

4 The exit of the vessel will be made of glass, so the outlet port will have a visible fluid flow.

5 The motor that will be used to make the emulsion and do par@cle tes@ng will have a variable RPM control.

6 The motor that will be used to make the emulsion and do par@cle tes@ng will have a variable RPM control.

7 This need will be sa@sfied through the par@cle size tes@ng plan and the motor tes@ng plan.

8 The vessel that will be purchased for this emulsion will be a jacketed glass wall vessel with an inlet and outlet port for temperature controlling flow.

9 The size of the vessel will be large enoguh to compensate a con@nuous flow rate of 200g/min.


11 This need has been sa@sfied by use of the CMC calcula@ons.


QUESTIONS & IDEAS

emulsion polymerization reactor

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