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"Utilization of Bio-Energy Waste in Bioplastic Formulations to
Manufacture Biodegradable Packaging and Recyclable
Electrical devices ”
FAPESP Week 2012 – Symposiums in Canada & US
Toronto, ON/Canada – October 17, 2012
Carlos A. Correa
Recycling and Bioplastics
Plasmacro / Brazil
André Leclerc
Green Solutions
Ingredion Inc. (Casco) / Canada
ISTP-FAPESP Cooperation program 2010-2012
Organization chart
André Leclerc
Project leader
Casco
Allison Sprague
Consultant
Emersa
Dr Roman Blaszczyk
Process engineer
Casco
Dr Michael Sills
Consultant
Ms Colleen Lytton
Assistant Coordinator
Casco
Dr Mohini Sain
Professor & Director
CBBP
Dr Robert Jeng
Fungi taxonomy
Specialist
Dr Lynn He
Senior Researcher
Dr Arturo Rodriguez
Researcher Assistant
Biomaterial
Dr. Carlos Correa
Project leader
Plasmacro
Lucio Mannosso
Business Manager
Corn Products Brazil
Dra Vanessa Alves
ID Specialist
Corn Products Brazil
Lucas Menegatti
Trainee/Process
Plasmacro
Dr. Cristiano de Santi
Assistant Coordinator
Plasmacro
Companies Academic Research Centers
Dr. Alcides Leão
UNESP/Botucatu
Sivoney Souza
Researcher
Dr. Elias Hage
Academic partner
UFSCar
Technical Support
CCDM/IIFQ
INDUSTRIAL PARTNERS
Plasmacro is based in São Carlos in the state of Sao
Paulo in Brazil and is part Polikem group. The group
has been on the recycling business over 10 years and
has large experience in reprocessing scrapped plastics
from various sources.
Mission
Find solutions for environmental issues generated by
post-consumer and industrial scraps through innovative
process and products.
22°04'06.54"S 47°53'01.03"O
Brazil
Sao Paulo State (Pop 41.2 Millions in 2010
GDP 34% of the Brazilian’s GDP
Sao Carlos
Google Street View Image
Plasmacro’s Location
Level of Complexity
• L= Number of locations (6): São Carlos, Toronto, Trois-
Reviéres/Chicago, Mogi Guaçu, Botucatu and São Paulo.
• P= Number of participants (7): Plasmacro (R&D), UofT
(R&D), Corn Products Brasil (R&D), Casco/Ca (Marketing),
Corn Products International (Higher management), UNESP
(R&D), FAPESP and ISTP (Funding and advisory).
• T= number of processes involved in the project (4): Starch
modification; Starch processing with glycerol; PVC dry
blending; Starch/PVC compounding.
Level of complexity,   TLPC exp! 
PROJECT OBJECTIVES
- Recovery of bioenergy waste;
- Use of o crude glycerol as a plasticizer for
thermoplastic starches;
- Compounding thermoplastic starches with
recycled PVC for application in injection
molding of electrical parts;
- Compounding thermoplastic starches with
bioplastics for applications as disposable
packaging.
THE GREEN DRIVE TO SUSTAINABILITY
Growth of glycerol waste from biodiesel
production in Brazil
Biodiesel production in last decades Projections
In cubic meters
In billion
liters
5% of Brazilian diesel is biodiesel
25% of Brazilian petrol is ethanol from sugar cane
USES FOR GLYCEROL
(Propane – 1,2,3 triol)
Medicines
Formula and Packaging
of drugs
Food and cosmetics
Humectant
Fabrics
Softener for fibers
Paper
Plasticizer for strenght
And flexibility
Explosives
Fabrication of
Nitrogliceryn (TNT)
Lubricants
Paints and
varnishes
Traditional
New applications - biorefinery
Animal feed
Dust supressor
Fuel for
electricity
generation
Propene for
plastics
Bioadditives
Fuel antifreeze
& antioxidants
Ethylene glycol
antifreeze for car
radiators
Propanediol
Building block for
Polyesters (PTT)
Ethanol from
biotechnology
processes
Starch plasticizer
THERMOPLASTIC STARCHES
Starch fragmentation and gelatinization
can be produced by either single or
twin screw extrusion in presence of a
suitable plasticizer (glycerol or/and
water) under controlled temperature,
processing time, shear rate and
lubricants.
Challenge is to optimizing gelatinization
process for modified starches with
crude glycerol for further
compounding with PVC formulations
and other thermoplastics.
A = Amylose (linear)
B = Amylopectine (branched)
PVC MARKET
• The global installed capacity for PVC
production is currently about 47.5
million metric tons per year and
expected to grow to 59.1 million
metric tons by 2020.
• Braskem is producing more than one
million tons of PVC resin a year in
Brazil.
• The building sector consumes ¾ of the
whole PVC production and has been
growing at double digits owing to
large incentives in Brazil.
Types of Pipe Waste
• Degassing powders: unwanted by recyclers
owing to it’s difficult to handle, - represents
about 1-2% of the overall production;
• Extrusion purguing: hard to reprocess
owing to unknown variations in chemical
composition and degraded material;
• Chips from pipe sawing, hard to recycle
owing to its “fluffy” low density.
• Non-complied pipe connectors from
injection molding (higher quality scrap)
In Brazil, there’s an estimate amount of
500 metric tons/month from pipe waste
PROPOSED INNOVATION CONCEPT
FOR G-PVC
(i) 100% recycled material from PVC industrial
waste (mostly pipes);
(ii) Formulations containing thermoplastic starch
from renewable resources;
(iii) Starch plasticized with a residue from
bioenergy (glycerol from biodiesel).
Changes in Brazilian regulations on regard to
electrical/electronic devices was seen as an opportunity to
test a new concept in green/biobased innovation.
Prospective Application
Electrical devices in compliance with new Brazilian
Regulations – NBR 14136
Devices in current use to be replaced after 2010
2 and 3 pins plugs and socket according to NBR 14136
Technical Challenges to Match Product
Specifications
• Mixing capability of different compounds in the
formulations;
• Matching chemical compatibility and melt rheology;
• Thermal stability during processing;
• Dimensional stability and rigidity of end products;
• Moisture absorption;
• Dielectric strength and inflammability properties.
Technologies
starch
Crude glycerol
(Brazil biodiesel)
Injection molding of electric parts & othersDisposable Packaging
bioreactorfungus
PHB + DDGs
(Canadian/Brazil sources)
DDGs: Distillers Dried Grains solubles
PHB: Polyhydroxybutyrate
PVC: Polyvinylchloride
Recycled PVC
(Canadian/Brazil sources)
Modified Starch
Proprietary UofT
Thermoplastic
Starch (GPS)
Plasmacro LtdaUNESP/Plastitech
Coffee cup lid
Other
pictures
Base trophy
Electric plate
3 components
electric
socket diagram
Plasticizing
CBBP/CPBrazil
Preparation of PVC Dry Blend*
Homogenization
4 tons batches
Pipe scrap
from
processors
Sieving
20 Mesh screen
High Speed
Mixer/cooler
*As processed at Plasmacro recycling site in Sao Carlos, Brazil
Thermal Processing of Starch + Glycerol
The glycerol plasticized starch (GPS) was produced by Corn Products
International in a pilot plant in Conchal/Brazil using a co-rotating twin-screw
extruder (72mm and L/D40).
Z1 Z2 Z3 Z4 Z5 Z6 Z7 Z8 Z9 Z10
50 110 115 120 120 120 120 120 120 120
Temperature profile
Twin screw co-rotating extruder (Coperion 35mm L/D 44) employed for
compounding the glycerol plasticized starch (GPS) with recycled PVC.
Z1 Z2 Z3 Z4 Z5 Z6 Z7 Z8 Z9 Z10
150 160 170 160 155 155 150 150 150 150
Temperature profile
Die: 160 oC - 200 RPM
PVC COMPOUNDING WITH GPS
Mechanical Properties
ASTM D638
Captions: R=Regular Starch; M=Modified Starch; BB=Biobased content; PG=Pure
Glycerol; CG=Crude Glycerol; *Single screw and **Twin screw extruder
0
500
1000
1500
2000
2500
R
ecycled
P
VCR
_BB
21-C
G
*R
_BB
21-PG
**R
_BB
36-PG
**R
_BB
21-C
G
**R
_BB
36-C
G
**M
_B
B21-PG
**
M
_B
B21-C
G
**
G-PVC Formulation
Young's
Modulus(MPa)
0
5
10
15
20
25
30
35
40
R
ecycled
P
VCR
_BB
21-C
G
*
R
_BB
21-PG
**
R
_BB
36-PG
**R
_BB
21-C
G
**
R
_BB
36-C
G
**
M
_B
B21-PG
**
M
_B
B21-C
G
**
G-PVC Formulations
TensileStrenght
(MPa)
Moisture Absorption
-6,00
-4,00
-2,00
0,00
2,00
4,00
6,00
8,00
0 20 40 60 80 100
Relative Humidity (%)
%Moisturecontent
Sample 1 R-PVC/Dop Sample 2 R-PVC/Drapex
Sample 3 G-PVC/Dop Sample 4 G-PVC/Drapex
R-PVC = Recycled PVC without starch
Dop= Phthalate plasticizer – Drapex = Soya oil based plasticizer
Phase morphology affects G-PVC end properties
after
extraction
with HCl
after
extraction
with water
after
extraction
with HCl
Compressed G-PVC with modified
starch
Compressed G-PVC with regular starch
Compressed samples for scanning electron
Microscopy observations
Holes caused by dissolution
of starch lumps and/or
carbonate fillers in recycled PVC
INJECTION MOLDING PROTOTYPES
Tooling, Process and molded parts
Market Issues
• G-PVC can be regarded as a “technology push” (a new product
and technology in search for new markets);
• The proposal was initially focused on injection molding of
electrical devices but PVC market is huge and other markets
are being prospected.
• A clearer picture of how companies deal with disposal of PVC
residues, recycling policies and green approaches in both
countries is required*
*Ecotigre: PVC resin from ethanol
CONCLUSIONS
• Dealing with a multi-disciplinary research team
and conciliate academic and industrial interests in
a international environment is not a small
undertake;
• R&D still required on formulation and customized
processing before end products are considered
ready for market;
• Clearer picture on company policies for vinyl
(PVC) waste is a key issue;
• Expand market for long-term applications.
MERCI BEAUCOUP
THANK YOU
OBRIGADO!
Questions?
• Plasmacro will be responsible for marketing the products using
the existing customers’ network from Polikem group in Brazil.
For the proposed products it’s a new market to be developed.
• Plasmacro does not intend to sell the product directly into the
retail market. This should be done in association thru wholesale
business.
• Price formation for compound formulations is aimed to be kept
below R$1,20 to be competitive on injecton molding market
• For a projection of 50ton/month, a cash flow of around R$
170,000 would be required based on Plasmacro current expenses.
From this amount 70% should be ready available and the
remaining taken from short term loans
G-PVC Project Scope

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FAPESP_WEEK_TORONTO

  • 1. "Utilization of Bio-Energy Waste in Bioplastic Formulations to Manufacture Biodegradable Packaging and Recyclable Electrical devices ” FAPESP Week 2012 – Symposiums in Canada & US Toronto, ON/Canada – October 17, 2012 Carlos A. Correa Recycling and Bioplastics Plasmacro / Brazil André Leclerc Green Solutions Ingredion Inc. (Casco) / Canada
  • 2. ISTP-FAPESP Cooperation program 2010-2012 Organization chart André Leclerc Project leader Casco Allison Sprague Consultant Emersa Dr Roman Blaszczyk Process engineer Casco Dr Michael Sills Consultant Ms Colleen Lytton Assistant Coordinator Casco Dr Mohini Sain Professor & Director CBBP Dr Robert Jeng Fungi taxonomy Specialist Dr Lynn He Senior Researcher Dr Arturo Rodriguez Researcher Assistant Biomaterial Dr. Carlos Correa Project leader Plasmacro Lucio Mannosso Business Manager Corn Products Brazil Dra Vanessa Alves ID Specialist Corn Products Brazil Lucas Menegatti Trainee/Process Plasmacro Dr. Cristiano de Santi Assistant Coordinator Plasmacro Companies Academic Research Centers Dr. Alcides Leão UNESP/Botucatu Sivoney Souza Researcher Dr. Elias Hage Academic partner UFSCar Technical Support CCDM/IIFQ
  • 3. INDUSTRIAL PARTNERS Plasmacro is based in São Carlos in the state of Sao Paulo in Brazil and is part Polikem group. The group has been on the recycling business over 10 years and has large experience in reprocessing scrapped plastics from various sources. Mission Find solutions for environmental issues generated by post-consumer and industrial scraps through innovative process and products.
  • 4. 22°04'06.54"S 47°53'01.03"O Brazil Sao Paulo State (Pop 41.2 Millions in 2010 GDP 34% of the Brazilian’s GDP Sao Carlos Google Street View Image Plasmacro’s Location
  • 5. Level of Complexity • L= Number of locations (6): São Carlos, Toronto, Trois- Reviéres/Chicago, Mogi Guaçu, Botucatu and São Paulo. • P= Number of participants (7): Plasmacro (R&D), UofT (R&D), Corn Products Brasil (R&D), Casco/Ca (Marketing), Corn Products International (Higher management), UNESP (R&D), FAPESP and ISTP (Funding and advisory). • T= number of processes involved in the project (4): Starch modification; Starch processing with glycerol; PVC dry blending; Starch/PVC compounding. Level of complexity,   TLPC exp! 
  • 6. PROJECT OBJECTIVES - Recovery of bioenergy waste; - Use of o crude glycerol as a plasticizer for thermoplastic starches; - Compounding thermoplastic starches with recycled PVC for application in injection molding of electrical parts; - Compounding thermoplastic starches with bioplastics for applications as disposable packaging.
  • 7. THE GREEN DRIVE TO SUSTAINABILITY
  • 8. Growth of glycerol waste from biodiesel production in Brazil Biodiesel production in last decades Projections In cubic meters In billion liters 5% of Brazilian diesel is biodiesel 25% of Brazilian petrol is ethanol from sugar cane
  • 9. USES FOR GLYCEROL (Propane – 1,2,3 triol) Medicines Formula and Packaging of drugs Food and cosmetics Humectant Fabrics Softener for fibers Paper Plasticizer for strenght And flexibility Explosives Fabrication of Nitrogliceryn (TNT) Lubricants Paints and varnishes Traditional New applications - biorefinery Animal feed Dust supressor Fuel for electricity generation Propene for plastics Bioadditives Fuel antifreeze & antioxidants Ethylene glycol antifreeze for car radiators Propanediol Building block for Polyesters (PTT) Ethanol from biotechnology processes Starch plasticizer
  • 10. THERMOPLASTIC STARCHES Starch fragmentation and gelatinization can be produced by either single or twin screw extrusion in presence of a suitable plasticizer (glycerol or/and water) under controlled temperature, processing time, shear rate and lubricants. Challenge is to optimizing gelatinization process for modified starches with crude glycerol for further compounding with PVC formulations and other thermoplastics. A = Amylose (linear) B = Amylopectine (branched)
  • 11. PVC MARKET • The global installed capacity for PVC production is currently about 47.5 million metric tons per year and expected to grow to 59.1 million metric tons by 2020. • Braskem is producing more than one million tons of PVC resin a year in Brazil. • The building sector consumes ¾ of the whole PVC production and has been growing at double digits owing to large incentives in Brazil.
  • 12. Types of Pipe Waste • Degassing powders: unwanted by recyclers owing to it’s difficult to handle, - represents about 1-2% of the overall production; • Extrusion purguing: hard to reprocess owing to unknown variations in chemical composition and degraded material; • Chips from pipe sawing, hard to recycle owing to its “fluffy” low density. • Non-complied pipe connectors from injection molding (higher quality scrap) In Brazil, there’s an estimate amount of 500 metric tons/month from pipe waste
  • 13. PROPOSED INNOVATION CONCEPT FOR G-PVC (i) 100% recycled material from PVC industrial waste (mostly pipes); (ii) Formulations containing thermoplastic starch from renewable resources; (iii) Starch plasticized with a residue from bioenergy (glycerol from biodiesel). Changes in Brazilian regulations on regard to electrical/electronic devices was seen as an opportunity to test a new concept in green/biobased innovation.
  • 14. Prospective Application Electrical devices in compliance with new Brazilian Regulations – NBR 14136 Devices in current use to be replaced after 2010 2 and 3 pins plugs and socket according to NBR 14136
  • 15. Technical Challenges to Match Product Specifications • Mixing capability of different compounds in the formulations; • Matching chemical compatibility and melt rheology; • Thermal stability during processing; • Dimensional stability and rigidity of end products; • Moisture absorption; • Dielectric strength and inflammability properties.
  • 17. starch Crude glycerol (Brazil biodiesel) Injection molding of electric parts & othersDisposable Packaging bioreactorfungus PHB + DDGs (Canadian/Brazil sources) DDGs: Distillers Dried Grains solubles PHB: Polyhydroxybutyrate PVC: Polyvinylchloride Recycled PVC (Canadian/Brazil sources) Modified Starch Proprietary UofT Thermoplastic Starch (GPS) Plasmacro LtdaUNESP/Plastitech Coffee cup lid Other pictures Base trophy Electric plate 3 components electric socket diagram Plasticizing CBBP/CPBrazil
  • 18. Preparation of PVC Dry Blend* Homogenization 4 tons batches Pipe scrap from processors Sieving 20 Mesh screen High Speed Mixer/cooler *As processed at Plasmacro recycling site in Sao Carlos, Brazil
  • 19. Thermal Processing of Starch + Glycerol The glycerol plasticized starch (GPS) was produced by Corn Products International in a pilot plant in Conchal/Brazil using a co-rotating twin-screw extruder (72mm and L/D40). Z1 Z2 Z3 Z4 Z5 Z6 Z7 Z8 Z9 Z10 50 110 115 120 120 120 120 120 120 120 Temperature profile
  • 20. Twin screw co-rotating extruder (Coperion 35mm L/D 44) employed for compounding the glycerol plasticized starch (GPS) with recycled PVC. Z1 Z2 Z3 Z4 Z5 Z6 Z7 Z8 Z9 Z10 150 160 170 160 155 155 150 150 150 150 Temperature profile Die: 160 oC - 200 RPM PVC COMPOUNDING WITH GPS
  • 21. Mechanical Properties ASTM D638 Captions: R=Regular Starch; M=Modified Starch; BB=Biobased content; PG=Pure Glycerol; CG=Crude Glycerol; *Single screw and **Twin screw extruder 0 500 1000 1500 2000 2500 R ecycled P VCR _BB 21-C G *R _BB 21-PG **R _BB 36-PG **R _BB 21-C G **R _BB 36-C G **M _B B21-PG ** M _B B21-C G ** G-PVC Formulation Young's Modulus(MPa) 0 5 10 15 20 25 30 35 40 R ecycled P VCR _BB 21-C G * R _BB 21-PG ** R _BB 36-PG **R _BB 21-C G ** R _BB 36-C G ** M _B B21-PG ** M _B B21-C G ** G-PVC Formulations TensileStrenght (MPa)
  • 22. Moisture Absorption -6,00 -4,00 -2,00 0,00 2,00 4,00 6,00 8,00 0 20 40 60 80 100 Relative Humidity (%) %Moisturecontent Sample 1 R-PVC/Dop Sample 2 R-PVC/Drapex Sample 3 G-PVC/Dop Sample 4 G-PVC/Drapex R-PVC = Recycled PVC without starch Dop= Phthalate plasticizer – Drapex = Soya oil based plasticizer
  • 23. Phase morphology affects G-PVC end properties after extraction with HCl after extraction with water after extraction with HCl Compressed G-PVC with modified starch Compressed G-PVC with regular starch Compressed samples for scanning electron Microscopy observations Holes caused by dissolution of starch lumps and/or carbonate fillers in recycled PVC
  • 24. INJECTION MOLDING PROTOTYPES Tooling, Process and molded parts
  • 25. Market Issues • G-PVC can be regarded as a “technology push” (a new product and technology in search for new markets); • The proposal was initially focused on injection molding of electrical devices but PVC market is huge and other markets are being prospected. • A clearer picture of how companies deal with disposal of PVC residues, recycling policies and green approaches in both countries is required* *Ecotigre: PVC resin from ethanol
  • 26. CONCLUSIONS • Dealing with a multi-disciplinary research team and conciliate academic and industrial interests in a international environment is not a small undertake; • R&D still required on formulation and customized processing before end products are considered ready for market; • Clearer picture on company policies for vinyl (PVC) waste is a key issue; • Expand market for long-term applications.
  • 28. • Plasmacro will be responsible for marketing the products using the existing customers’ network from Polikem group in Brazil. For the proposed products it’s a new market to be developed. • Plasmacro does not intend to sell the product directly into the retail market. This should be done in association thru wholesale business. • Price formation for compound formulations is aimed to be kept below R$1,20 to be competitive on injecton molding market • For a projection of 50ton/month, a cash flow of around R$ 170,000 would be required based on Plasmacro current expenses. From this amount 70% should be ready available and the remaining taken from short term loans G-PVC Project Scope