Ashland Performance Materials
Pliogrip Structural Adhesives Acrylic Adhesive for Composite Bonding
November 7, 2012
Michael Barker
Research Fellow
Ashland Performance Materials
2
Commercial
Units
Ashland
Specialty
Ingredients
Ashland
Water
Technologies
Ashland
Performance
Materials
Ashland
Consumer
Markets
Leading
Products &
Services
#1
cellulose ethers,
global leader in
vinyl pyrrolidones
#1
specialty
papermaking
chemicals
#1
unsaturated
polyester resins
and vinyl ester
resins
#2
U.S. franchised
quick-lube chain,
Passenger-car
motor oil
Sales1 $2.7 billion $1.9 billion $1.7 billion $2.0 billion
1 (Pro Forma) for 12 Months Ended Mar. 31, 2012
Four Strong Businesses
Ashland Performance Materials
3
Ashland Performance Materials
Key Benefits to Critical Applications
Composites
Lightweight High Strength
Durability Corrosion Resistance
Adhesives
Strength Durability
Removability Food Safety
Elastomers
Pressure Sensitive
Wear Resistance
Durability
Adhesion
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Our Global Presence
Ashland Performance Materials
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Outline
Adhesive Overview
Acrylic Adhesive Technology
Pliogrip Acrylic Adhesives
Marine Case Studies
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Pliogrip Structural Adhesives
45 years of experience in bonding some of the most
demanding applications i.e. automotive, heavy truck,
marine and general assembly
Trusted and chosen by dozens of leading OEMs for
bonding of composite parts
Today’s overview
Pliogrip 1000 acrylic adhesive & marine case
studies
and many others…
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Definitions
An adhesive is a non-metallic substance that is able to bond the substrates by adhesion (surface forces) and cohesion (internal rigidity)
Structural adhesives represent a class of chemical bonding agents where the strength of the adhesive is greater than the strength of the substrates that are bonded together
The bonded structure must perform under a variety of extreme environmental conditions and load
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Definitions (cont.)
Open Time
The time after mixing a two component adhesive in which the wetting properties of the adhesive are still sufficient to build proper adhesion
Cure time
The time required, after joining
the substrates, to build sufficient strength in the bond line to allow further processing or transportation of the part
Str
ength
Opentime
Handling strength
Operational strength
Final strength
TimeMixing
Str
ength
Opentime
Handling strength
Operational strength
Final strength
TimeMixing
Str
ength
Opentime
Handling strength
Operational strength
Final strength
TimeMixing
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Advantages of Adhesive Bonding
Surface distortion minimized
Stress is distributed uniformly over bond-area
Suitable for bonding a variety of materials
Enables bonding of dissimilar materials
Very strong, age- and crash-resistant bonds
Excellent chemical resistance
Proven technology
Increased productivity
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Definitions
Pot Life
Open Time
Cure Time Time required for the adhesive to reach its ultimate strength (varies with temperature, chemistry and substrate)
Green Strength Time required for the adhesive to achieve green strength allowing further handling of the bonded part (varies with temperature and chemistry) typically 0,35- 0,7 MPa
Time after mixing the two parts in which an adhesive must be applied
Timeframe after adhesive application to achieve good wetting of the second part
2-Part Adhesive Reactive components are kept separate until ready for use
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Adhesive Types Vs. Bulk Mechanical Properties Tensile
Str
ength
[M
Pa]
Elongation [%]
10
20
30
40
100 200 300 400
Phenolics
1-& 2-k Epoxy
2-k-Acrylics
Structural 2-k-Polyurethane
Elastic Adhesives / Structural Sealants
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Adhesion Cure-
type
Adhesive Selection
PLIOGRIP® Structural Adhesives
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Acrylic Adhesive Technology
Common uses – “open mold” composites, gel coats,
bare metals e.g. boats and truck cabs
Very fastest fixture time at RT but cannot be heat
accelerated
Resists corrosion in bare-metal bonding
Bondable open time from 5 to 80 min
Very high elongation
6 month shelf life
Flammable with acrylic odor / VOCs
Tensile: 21- 28 MPa
Elongation: ~ 70-150%
Modulus: ~365- 410 MPa
Viscosity: 225 – 250 Pa s
Mechanical Properties
+
Free Radical Monomer
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Pliogrip Acrylic Adhesives
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PLIOGRIP®
Adhesive
PLIOGRIP®
Curative
Open
Time
(minutes
at 22C)
Fixture
Time
(minutes
at 22C)
Features & Benefits
1000 MARINE
(drum only)
1000
1040 40 80
High-body, long open-time, low-
boil product for stringer & deck-to-
hull bonding. For use on FRP and
gel coat surfaces.
1060 60 120
1080 80 160
1100 140 280
1000c GENERAL
INDUSTRIAL
(drum or
490ml
cartridges)
1005c (1003LV/1202) 5 - 8 10 – 15 Faster fixture times for smaller
jobs. Exceptional performance
on FRP, aluminum, stainless steel,
CRS, ABS, PC, and other
substrates.
1010c (1003LV/1202) 8 – 13 20 – 25
1020c (1002LV/1201) 16 – 24 40 – 50
1035c (1001LV/1201) 30 – 40 70 – 80
• Significantly less boil than competitive acrylic adhesives
• Increased productivity through long open times yet faster fixture times
• Reduces bond-line read through
Pliogrip 1000 10:1 Acrylic Adhesive
Pliogrip Acrylics have a 6 month shelf life from date of shipping
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Pliogrip Acrylic in Marine Applications
16
Stringer Bonding, Deck-to-Hull, Liner, Bulkhead
Replaces “glassing in” (lamination) or bonding paste
significant time savings (no sanding / prep)
higher elongation, flexibility,
better fatigue properties
Pliogrip 1000
Very long open times (up to 140 min +)
High body and gap-filling
Pliogrip 1000c
Faster cure times
Cartridges available
Enhanced performance on bare metals
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20
40
60
80
100
120
140
160
0 30 60 90 120 150 180 210 240
Tem
pera
ture
(C
)
Time (minutes)
Pliogrip 1000 Cure vs. Mix Ratio
Pliogrip Adhesive
8:1 by volume 10:1 by volume 12:1 by volume
Open
Time
Fixture
Time
Open
Time
Fixture
Time
Open
Time
Fixture
Time
Pliogrip 1000/1040 47 min 70 min 57 min 81 min 74 min 103 min
Pliogrip 1000/1060 61 min 87 min 75 min 103 min 98 min 134 min
Pliogrip 1000/1080 82 min 109 min 102 min 133 min 143 min 181 min
Pliogrip technologies are
adaptable to meet various
processing needs, thus
eliminating demand for different
adhesive systems
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Pliogrip 1000c Bonding Vs. Substrate
5,3 MPa 15,3 MPa
Pliogrip 1020c Structural
Acrylic Cartridge Adhesive
Lap Shear Samples
Fiber Tear on FRP and Cohesive
Failure on Metal with
No Surface Preparation
FRP to Gelcoat
Fiber Tear
765 psi (avg)
5,3 MPa
Stainless Steel 304
Cohesive Failure
2217 psi (avg)
15,3 MPa
FRP to FRP
Fiber Tear
500 psi (avg)
3,45 MPa
Aluminum 6061-T6
Cohesive Failure
2157 psi (avg)
14,9 MPa
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19
Pliogrip 1000c Has Better Sag Resistance
1,0 cm 0,13 cm 0,38 cm
Pliogrip has less sag on vertical applications. The adhesive will not move out of
the glue line and cause excess clean up or result in bondline starvation
Competitor A
Competitor B
B A
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20
-40ºC Cold Side Impact Performance
Standard - GM9751P • 60 in-lb is “perfect score” • achieving a rebound
60
53
60
15
56
22
48
23
0 10 20 30 40 50 60
Energy Absorbed (in-lb)
FRP
CRS
SS-304
AL 6061 T6
Su
bstr
ate
Teste
d
PG 1005c Competitor XX420
Excellent bond performance on a variety of metal and
composite substrates, exceeded competitive products
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Pliogrip 1000 in FRP Bonding
PLIOGRIP Exhibited 100% Fiber Tear In All Cases
PLIOGRIP
Competitor 1
Competitor 2
Competitor 3
Lap
Sh
ear
Str
eng
th
MPa
Tested on standard composites used in the marine market -
Lap shear performance meets or exceeds the competitor products
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Adhesive
Test Temperatures
At 20C At 31C
Open Time
of a 5 cm
Bead
(min)
Time to
Strength
Build in a
0,32 cm
Bond (min)
Open Time
of a 5 cm
Bead
(min)
Time to
Strength
Build in a
0,32 cm
Bond (min)
Pliogrip
1000/1060 78 97 30 54
Competition 80 200 30 110
Pliogrip 1000/1060 has a dramatic advantage over Competition
Improved Cycle Time & Ability to Process the Part Sooner
Pliogrip 1000 Vs. Competition Strength Build
1. As measured side-by-side in Ashland Inc. laboratory
2. Strength build is defined as when .7 MPa cross peel is reached
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23
Pliogrip 1000 - Shrinkage & Boil
PLIOGRIP 1000
Bulk
Cartridge
Less Boil and Shrinkage with PLIOGRIP 1000 – Pliogrip has more durability within
the bond line resulting from the lack of voids and stress cracks, also may help
reduce bond line read through
Competitor 1
Competitor 2 PLIOGRIP 1000
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Pliogrip Acrylic Application Methods
2-part “catalyzed” structural adhesives must be mixed
together to start the cure process
Meter Mix Dispense Equipment
(Used with drums, or pails) Cartridges
Or HAND-MIX
With pallet & spatula
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Case Studies
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Advantages of Acrylic Adhesive
Stronger and better adhesive than bonding paste
Modulus and elongation result in tougher more fatigue-resistant joints
Acrylic bonds to FRP and gelcoat without sanding or abrasion
Cost of sandpaper
Reduce labor
Reduce dust from sanding
Reduce cleanup of dust
Faster application if using mix-dispense equipment
Faster cure than bonding paste
Cycle time in molds
Acrylic Adhesive vs UPR Bonding Paste
26
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Acrylic Adhesive is Stronger than UPR Bonding
Paste on FRP
Room Temp
Lap Shear
Petrol/Gasoline Immersion
Lap Shear
Strength
(MPa)
Fiber Tear
(%)
Strength
(MPa)
Fiber Tear
(%)
PG1000 6,0 97% 6,5 100%
UPR ISO Marine
Bonding Paste 3,4 19% 2,7 14%
1. Surface preparation: dry wipe / no sanding
2. Substrate UPR FRP
3. Immersion in petrol/gasoline for 1 week at 23ºC
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Case Study 13 Meter Fishing Boat
Miami, FL USA
Liner to Hull-Stringer Attachment
Change from UPR
bonding paste to Pliogrip
1000/1080
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Case Study 13 Meter Fishing Boat – Miami, FL USA
Liner to Hull-Stringer Attachment
Change from UPR Bonding Paste to Pliogrip
Boat builder changed to Pliogrip 1000/1080 acrylic adhesive
for longitudinal stringer-to-liner joints and reduced extent of laminating reinforcement
50kg – 57 kg per boat @ 1,27 cm bond line thickness
Saved an average of 8 labor hours per boat Faster application of acrylic adhesive using GS Manufacturing TM mix-
dispense unit vs. bonding paste
Reduction of areas reinforced with lamination
Elimination of sanding and prep steps on adhesive joints
Stronger, tougher joints
Boat builder subsequently converted all product lines to Pliogrip
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Case Study 10 Meter sport fishing boats, Brasil
Stringer, Bulkhead, Deck-to-Hull
Stringer and bulkhead (existing models): boat builder uses 6-layer
lamination.
Deck-to-hull (existing models): boat builder uses combination of
lamination, 1-part MCU sealer, and screw fasteners.
Lamination
Prep consists of sanding and cleanup
Manual preparation of glass matt and tedious application of multi-layer
mat and laminating resin
Dust from sanding and unnecessary VOC in solvent wipe
Boat builder sought new attachment methods for it’s new model
Background
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Boat builder used Pliogrip 1010c and 1035c 490ml cartridges for
prototypes
Pliogrip 1010c used on deck-to-hull joint, eliminating 1-part MCU, and
reducing lamination on interior of joint and screw fasters on exterior of
joint
Cycle time reduced from 2 days to 40 minutes
Pliogrip 1035c used on stringer attachment, completely eliminating
lamination
Cycle time reduced from 5 days to 3 hours
Cycle would be further improved using drums and mix-dispense
equipment
Case Study 10 Meter sport fishing boats, Brasil
Stringer, Bulkhead, Deck-to-Hull
Solution
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Case Study 10 Meter sport fishing boats, Brasil
Stringer, Bulkhead, Deck-to-Hull
27 PG1035c carts &
6 PG1010c carts
were used for
stringer (approx 15
kg)
Adhesive application
time 30 minutes,
plans to get faster
on next boat
IPA wipe employed
as prep-step (dust)
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Pliogrip 1000 Summary
Fast Fixture Times
Low Boil
Over 13,8 MPa lap shear strength with cohesive failure on bare aluminum, stainless steel, CRS
Achieves fiber tear on FRP and gel coat without prep
Excellent bare metal performance (Pliogrip 1000c)
Commercial applications in marine, bus/coach, and heavy truck
Displaces “glassing in” or bonding paste
Significant time savings (no sanding / prep)
High elongation, flexibility, excellent fatigue properties
Available in cartridge & bulk
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Ashland – Produtos para Náutica
GEL COAT
RESINAS POLIÉSTER
& VINIL-ÉSTER
Beneteau, France
Chaparral, USA
Sea Ray, USA
ADESIVOS
ESTRUTURAIS
RESINAS COM
RETARDÂNCIA Á CHAMA
Ashland Performance Materials
David Britto – 07/11/2012
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MaxguardTM LE/33LE com tecnologia LE baixa emissão de estireno com superior qualidade.
Ashland Performance Materials
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MAXGUARD® LE/33LE com Patente da Tecnologia LE
Gelcoat MAXGUARD premiado
MAXGUARD NP
com a tecnologia LE foi eleito
como gelcoat mais importante
para o sucesso futuro
da indústria plástico reforçado!
INDUSTRY
AWARDS
Valores dos testes informados nesta apresentação são valores médios de diversos testes.
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MAXGUARD® LE/33LE com Patente da Tecnologia LE
INDUSTRY
AWARDS
Tecnologia de baixa emissão
de estireno
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MAXGUARD® LE/33LE com Patente da Tecnologia LE
INDUSTRY
AWARDS
Tecnologia de baixa emissão
de estireno
Gelcoat normal
• Polímero normal com
baixa compatibilidade
com estireno, resulta
em gelcoat com
excesso de estireno
= estireno
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MAXGUARD® LE/33LE com Patente da Tecnologia LE
INDUSTRY
AWARDS
Tecnologia de baixa emissão
de estireno
Gelcoat com a tecnologia LE
• Polímero normal com
baixa compatibilidade
com estireno, resulta
em gelcoat com
excesso de estireno
= estireno
• O novo polímero de alta
compatibilidade com
estireno, significa baixo
teor de estireno no
gelcoat.
= estireno
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MAXGUARD® LE/33LE com Patente da Tecnologia LE
INDUSTRY
AWARDS
Tecnologia de baixa emissão
de estireno
Emissão de estireno medido em cabine de pintura
• Polímero normal com
baixa compatibilidade
com estireno, resulta
em gelcoat com
excesso de estireno
= estireno
• O novo polímero de alta
compatibilidade com
estireno, significa baixo
teor de estireno no
gelcoat.
= estireno
1200
Gelcoat com 1000
Tecnologia LE
800
gelcoat normal Q
ua
ntid
ade
ap
lica
da
(m
g/s
)
600
400
200
0
0 10 20 30 40 50 60 70
Tempo (min)
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MAXGUARD® LE/33LE com Patente da Tecnologia LE Emissão de estireno e rendimento medido na cabine de pintura.
Gelcoat com Gelcoat Standard
Tecnologia LE
Teor de estireno 28% 39%
Tempo de aplicação 194 sec 187 sec
Massa pulverizada* 3.0 kg / 6.6 lb 3.0 kg / 6.6 lb
Massa no molde* 2.7 kg / 5.9 lb 2.4 kg / 5.3 lb
*escala Eficiência na Transferência 90% 80%
Emissão durante a Pulverização** 3.6% 7.0% **IR
Emissão Total** 6.7% 13.6%
Redução de 50% na emissão de estireno.
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MAXGUARD® LE/33LE com Patente da Tecnologia LE Emissão de estireno medido na produção de um barco de 36 pés.
100
80
60
40 M
ed
içã
o d
e E
stire
no
no
du
to d
e
20
exa
ustã
o (
pp
m)
0
0 10 20 30 40 50 60 70
Tempo (min)
Gelcoat com Tecnologia LE gelcoat normal
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MAXGUARD® LE/33LE com Patente da Tecnologia LE Resistência ao amarelamento medido pela QUV-A na FMC II
5
4
3
2
1 Am
are
lam
en
to (
DY
B)
0
0 250 500 750 1000
Tempo (h)
Gelcoat com tecnologia LE gelcoat normal
Redução de 50% no amarelamento
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MAXGUARD® LE/33LE com Patente da Tecnologia LE Retenção de brilho medido pela QUV-A com ângulo de 20°
100
80
60
40
20
Brilh
o (
%)
0
0 250 500 750 1000
Tempo (h)
Gelcoat com tecnologia LE gelcoat normal
Aumento de 15% na retenção de Brilho
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MAXGUARD® LE/33LE com Patente da Tecnologia LE Contração linear medida de acordo com a norma ASTM D 2566
100
80
60
40
20
Brilho (%)
0
0 250 500 750 1000
Tempo (h)
Gelcoat com tecnologia LE gelcoat normal
2.5
2.0
1.5
1.0
0.5
Co
ntr
açã
o (
%)
0
Gelcoat com tecnologia LE gelcoat normal
Redução de 30% na Contração
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David Britto
Ashland Performance Materials
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David Britto
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MAXGUARD® LE/33LE com Patente da Tecnologia LE
100
80
60
40
20
Brilho (%)
0
0 250 500 750 1000
Tempo (h)
Gelcoat com tecnologia LE gelcoat normal
2.5
2.0
1.5
1.0
0.5
Co
ntr
açã
o (
%)
0
Gelcoat com tecnologia LE gelcoat normal
Beneteau, France
Chaparral, USA
Sea Ray, USA
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Soluções em resina para o mercado náutico
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Soluções em resina para o mercado náutico
• Resinas de Laminação • Resinas de Infusão
AME 5100 (Resina Premium para Cascos e Skin Coat) AME 6100 INF (Vinil-Éster Premium)
AME 2100 AME 5100 INF
AROPOL Q65471 AME 2100 INF
ENVIREZ L 86300 (“Green” – Fonte de Recurso Renovável) AROPOL Q 65471 INF
• Solução para Skin Coat (Superfície isenta de marcações)
• Peças Pequenas (RTM)
AROPOL NLN 71500 INF AME VPRO AME 5001 + ARAZYN 13.0 (Gel VE Barreira Química) (Resina VE para Skin Coat)
ENVIREZ Q 11500 (Green)
• Resinas para Off-Shore & Tanques de Combustíveis
DERAKANE 510 N e 510 C
Hetron™LB 6806-182
MODAR 814A
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Resinas para Laminação / Skin Coat
•Escolha dos produtos depende das necessidades requeridas por cada cliente. P
reço
•All MACT Compliant
•Uso em qualquer parte da embarcação.
AME 5100 T25 Premium VE. Grande combinação
de força e aparência
AME 2100 T25 Resina VE modificada para uso geral. Excelentes
propriedades mecânicas
AROPOL Q 65471 T25 Blenda de resinas com alto HDT, baixíssima contração
e excelente acabamento superficial
Desempenho
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Resinas para Infusão
•Escolha dos produtos depende das necessidades requeridas por cada embarcação P
reço
•Uso em qualquer parte da embarcação
AME 6100 INF Premium VE, altíssimas propriedes físicas e HDT
Excepcional resistência á fadiga.
Indicada para barcos de alto desempenho
AME 5100 INF Premium VE. Grande combinação
de força e aparência
AME 2100 INF Resina VE modificada para uso geral. Excelentes
propriedades mecânicas
AROPOL Q 65471 INF Blenda de resinas com alto HDT, baixíssima contração
e excelente acabamento superficial
Desempenho
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AME 2100 / AME 5100 / AME 6100 - Resinas Vinil-Éster
• Características
– Oferecer aos nossos clientes resinas Vinil-Éster com flexibilidade de opções,
atendendo todos os níveis de exigência técnica.
– Podem ser utilizadas em Laminação, Infusão e Skin Coat.
– Baixa emissão de estireno.
– Disponíveis também nas versões de INFUSÃO.
• Vantagens
– Melhores Propriedades que resinas disponíveis no mercado.
– Variados níveis de Desempenho e Custo, adequando-se as necessidades de
cada cliente.
– Longa história de sucesso em Náutica.
– Alto HDT e Propriedades Mecânicas.
– Elevada Resistência á Fadiga.
Disponível em estoque
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Solução de Alto Desempenho para Skin Coat
Skin Coat
AME V-PRO Vantagens
(Gel Coat Barreira Química) –100% Vinil-Éster – Uso acima ou abaixo
da linha d’água + – Elevada Resistência ao Blistering
– Excelente Acabamento Superficial AME 5100 – Eliminação Print Thru em Infusões
(Resina Vinil-Éster) – Contração Superficial Reduzida
– Aplicação com Gelcoteadeira e “Caneca”
– Baixa Emissão de Estireno
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AROPOL Q 65471 – Resina UPR Spray/Infusão Premium
• Características – Blenda de Resinas Otimizadas para Aplicações Náuticas.
– Baixa Emissão de Estireno.
– Reduzida Contração.
– Disponível também na versão de INFUSÃO.
• Vantagens
– Melhores propriedades mecânicas que resinas Ortoftálicas Covencionais.
– Acabamento superficial melhorado e duradouro, devido á Baixa Contração e
ao alto HDT.
– Indicada para clientes que desejam um upgrade de desempenho sobre resina
de laminação usada atualmente.
– Processamento mais rápido devido ao rápido desenvolvimento de Dureza
Barcol.
Disponível em estoque
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Resinas Low Profile para RTM
• Gama variada de produtos P
reço
• Todas as pequenas partes acima da linha d’água
AROPOL NLN 71500 INF Acabamento Superficial Premium
ENVIREZ Q11500 INF Excelente Acabamento Superficial – “Opção Green”
Fonte de Recurso Renovável
AROTRAN 6500 Low Profile Standard. Necessita de aquecimento do molde
Performance
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AROPOL NLN 71500 INF
• Características AROPOL NLN 71500
– Resina para RTM Low Profile (“Contração Zero”).
– Versões para 12 e 22 minutos.
– Cura à temperatura ambiente.
– Indicada peças pequenas acima da linha d’água.
• Vantagens
– Acabamento “Classe A” – acabamento com nível automotivo.
– Menor pico exotérmico, limitando danos nos moldes.
– Aplicável a grande variedade de processos e peças.
– Preço competitivo.
– Permite excelente acabamento para peças com Gel Coat aplicado em ambas as
faces.
Caso de sucesso em fabricantes como Tiara, Viking Grady White
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Resinas para Tanques de Combustíveis
• Ainda há confusão sobre o uso de tanques de combustíveis
em compósitos, quando expostos á presença de Etanol.
• Ashland possui duas resinas disponíveis e testadas
– Ambas foram certificadas sob a norma UL1316 para armazenamento de
combustíveis.
– Derakane 510N (INF)
Resina Premium que não requere pós-cura
– Hetron™LB 6806-182
Menor custo, mas requer pós-cura
– Disponíveis nas versões de Infusão e Laminação
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60
Bus/Coach Application Example Cargo Doors, Large Coach Manufacturer in
Canada Mixed material cargo doors
• RTM, RTM lite, FRP, Stainless Steel, Bare Aluminum, and Bare Steel
Customer desired to reduce # of adhesives and improve cold impact
results
Pliogrip 1003LV/ 1202 acrylic tested on substrates
• GM 9751P -40⁰C cold side impact testing
Pliogrip acrylic bested competition and secured this cargo door
application
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Experimental Details
1.Open time determined by time for 100g mass in a 5 cm jar to reach 40ºC; 5 cm jar simulates
a 5 cm diameter bead
2.Fixture time determined by time to peak temperature in a 0,3 cm thick bond line, which correlates with strength build in cross-peel testing.
3.Smaller quantities would result in a slower cure rate, larger quantities would result in faster cure rate
4.Data measured at 23ºC conditions, hotter or colder ambient conditions will affect result
Ashland Performance Materials
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MARINE PRODUCTS
Ashland Performance Materials
David Britto – 07/11/2012