TT 136 Pure Monomer Resins TT136

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Pure monomer resins

Extending hydrogenated hydrocarbon resins with

pure monomer resins in SIS-based nonwoven

construction pressure sensitive

adhesive formulations

Technical tip

Introduction

Nonwoven construction adhesives based on SIS-type

polymers traditionally use hydrogenated hydrocarbon

resins such as Eastotac™ resins as the tackifier of choice

due to their compatibility, thermal stability, and high-

temperature properties. Eastman has investigated the

possibility of extending hydrogenated hydrocarbon resins

in these types of formulations with pure monomer resins

(PMRs), with results that indicate PMRs can be added up to

13% by resin volume without negatively affecting adhesive

performance or thermal aging properties.

Data

Pure monomer resins offer excellent thermal stability,

high-temperature resistance, and low molecular weight.

Traditionally used to selectively modify the styrenic end

blocks to balance cohesion and viscosity, PMRs can be

effectively used in synergy with hydrogenated hydrocarbon

resins in SIS-based adhesives without negatively affecting

performance.

Typical properties of selected hydrogenated hydrocarbon

resins and PMRs are given in Table 1. Values shown are an

average of typical samples and should not be interpreted as

product specifications.

Pure monomer resins

Extending hydrogenated hydrocarbon resins with pure

monomer resins in SIS-based nonwoven construction

pressure sensitive adhesive formulations

Table 1. Typical properties of resinsa

Resins Type

Ring & ball

softening

point (°C)

Mn/Mw/Mz

(Daltons) Tg (°C)

Gardner

color/YIDb

Eastotac™

H-100W

Hydrogenated

hydrocarbon resin 100 450/1000/2150 41 <1/8

Kristalex™ 3085 PMR 85 650/1150/1900 41 <1/4

Piccotex™ LC PMR 91 750/1350/2200 46 <1/8

Piccolastic™ A75 PMR 74 700/1300/2250 35 1/-

a Obtained from Eastman publication WA-86A, Spectrum of Hydrocarbon Resins; WA133, Eastman Hydrocarbon resins

b YID = Yellowness Index

An SIS-based disposable diaper construction adhesive

formulation was prepared with Eastotac™ H-100W

hydrogenated hydrocarbon resin as the control. Effects of three

different PMRs (Kristalex 3085, Piccotex LC, and Piccolastic

A75) as extenders for Eastotac H-100W were evaluated at two

different levels; 4% and 8% by weight (in formulation) or 7%

and 13% extension with respect to the total hydrogenated

hydrocarbon resin amount (Eastotac H100W:PMR, 93:7 and

87:13 ratios). Table 2 shows the formulations used in this study.

aKRATON Polymers LLC (polymer)

bEastman Chemical Company (resins)

cCalumet Specialty Products (naphthenic oil)

dBASF (antioxidant)

Table 2. Disposable diaper construction adhesive formulations with PMRs (shown in weight %)

Formulation

ingredient

Eastotac™

H-100W

control

Kristalex™ 3085 Piccotex™ LC Piccolastic™ A75

93:7

H100W:3085

87:13

H100W:3085

93:7

H100W:LC

87:13

H100W:LC

93:7

H100W:A75

87:13

H100W:A75

Kraton™

1165a20 20 20 20 20 20 20

Eastotac™

H-100Wb59.5 55.5 51.5 55.5 51.5 55.5 51.5

Kristalex™

3085b– 4 8 – – – –

Piccotex™

LCb– – – 4 8 – –

Piccolastic™

A75b– – – – – 4 8

Calsol™

5550c20 20 20 20 20 20 20

Irganox™

1010d0.5 0.5 0.5 0.5 0.5 0.5 0.5

Study formulations were prepared using a Brabender mixer

and evaluated for the following properties:

• Viscoelastic properties—Using Dynamic Mechanical

Analysis (DMA)

• Viscosity profiles at different temperatures (before and

after aging [177°C for 72 h])—Brookfield Viscometer

• Adhesive property evaluation—1-mil-thick adhesive

coating on Mylar™

– 180 degree peel on stainless steel substrate (peel rate

@ 4 inches/min)

– Loop tack on stainless steel substrate

The viscoelastic performance analysis (DMA) of the PMR

extended formulations at two different levels, along with the

control formulation is shown in Figure 1.

1.E+10

1.E+09

1.E+08

1.E+07

1.E+06

1.E+05

1.E+04

10

1

0.1

0.01

Eastotac H100W control 87:13 H100W:3085

87:13 H100W:LC 87:13 H100W:A75

G' (dynes/cm2)

Tan delta

−50 −30 −10 10 30 50 70 90 110 130

Temperature (°C)

4° to 6°C change in

3rd crossover temp.

With 8% by weight PMR (87:13 H100W:PMR)

Figure 1. Viscoelastic properties of formulations extended with PMRs.

10

1

0.1

0.01

Tan delta

−50 −30 −10 10 30 50 70 90 110 130

Temperature (°C)

1.E+10

1.E+09

1.E+08

1.E+07

1.E+06

1.E+05

1.E+01

G' (dynes/cm2)

Tg and Tan d peak value

3rd crossover temp.

Tan d min. value and Tan d min. temp.

With 4% by weight PMR (93:7 H100W:PMR)

Eastotac H100W control 93:7 H100W:3085

93:7 H100W:LC 93:7 H100W:A75

As shown in Figure 1, the viscoelastic characteristics, Tg, and

elastic modulus are not significantly affected by the addition

of PMRs to the control formulation. The single Tg exhibited

by the extended formulations is also an indication of good

compatibility between the polymer and tackifiers. The only

notable exception is a slightly lower melting temperature

(approximately 4° to 6°C) when the formulation is extended

with PMRs at the highest loading level weight (8%).

Figure 2 illustrates the absolute values of important

parameters such as Tg, Tan d minimum value at Tan

d minimum temperature (an indication of cohesive

property), 3rd crossover temperature (indication of melting

temperature), and Tan d peak value at Tg (indication of tack).

The only significant difference noted is for the 3rd crossover

temperature with the 8% PMR extended formulations (87:13)

with Eastotac™ H-100W. All other properties are comparable.

Figure 2. Viscoelastic property comparison values from DMA.

4.37

0.17

3rd crossover Tan d min. temp.

2nd crossover Tg

Different DMA temperature properties

Temperature (°C)

120

100

80

60

40

20

0

Estotac H100W control

93:7 H100W:3100

93:7 H100W:A75

87:13 H100W:3100

87:13 H100W:LC

87:13 H100W:A75

93:7 H100W:LC

98.3 72.4 38.4 16.4

16.4

18.4

16.4

38.4

40.4

72.4

72.4

68.492.4

92.3 70.4 38.4 16.4

14.434.4

70.4

94.4

36.4 16.4

94.4

98.3

38.4

70.3

94.3

Tan d peak value @ Tg

Tan d min. value @ Tan d min. temp.

Tan d value comparisons

Tan d value

4.22 4.19 4.33

4.46 4.57 4.49

0.17 0.19 0.19 0.18 0.20 0.20

5.00

4.00

3.00

2.00

1.00

0.00

Estotac H100W control

93:7 H100W:3100

93:7 H100W:A75

87:13 H100W:3100

87:13 H100W:LC

87:13 H100W:A75

93:7 H100W:LC

Figure 4. Loop tack on stainless steel

Figures 3 and 4 summarize the adhesive property evaluation

results, which were performed with 0.9–1-mil-thick Mylar™-

coated films on a stainless steel substrate. While most

extended formulations exhibit similar performance to the

control, a notable exception is Piccotex™ LC at 7% loading

with Eastotac™ H100W. Improvement is shown in both

adhesive peel and loop tack. The higher loop tack shown for

Piccolastic™ A75 extended formulations can be attributed

to the slightly lower softening point characteristics of

Piccolastic™ A75 compared to the other PMR resins.

Figure 5 illustrates there are no significant differences above

150ºC in the viscosity profiles at 5 different temperatures

between the control formulation and PMR extended

formulations, even after aging at 177°C for 72 h.

Temperature (°C)

Initial viscosity profiles before aging

Eastotac H100W control

87:13 H100W:3085

87:13 H100W:LC

87:13 H100W:A75

93:7 H100W:3085

93:7 H100W:LC

93:7 H100W:A75

Brookfield viscosity (cps)

12,000

10,000

8,000

6,000

4,000

2,000

0

130 150 170 190 210

lb/inch

4.74

4.27

5.26

4.16

4.89

4.65

3.78

6.00

5.00

4.00

3.00

2.00

1.00

0.00

93:7

H100W:LC

93:7

H100W:A75

87:13

H100W:3085

87:13

H100W:LC

87:13

H100W:A75

Eastotac

H100W

control

93:7

H100W:3085

lb

10.00

9.00

8.00

7.00

6.00

5.00

4.00

3.00

2.00

1.00

0.00

Figure 3. 180 degree peel on stainless steel

(peel rate at 4 inches/min)

93:7

H100W:LC

93:7

H100W:A75

87:13

H100W:3085

87:13

H100W:LC

87:13

H100W:A75

Eastotac

H100W

control

93:7

H100W:3085

6.80

6.39

7.60

8.28

7.57

6.96

7.37

Figure 5. Brookfield viscosity (cps) profiles of

formulations at different temperatures.

Figure 4. Loop tack on stainless steel

Depicted in Figure 6 are the before and after color-aging

characteristics for both the control and PMR extended

formulations, which also exhibit similar or better performance.

Initial (before aging)

Figure 6. Aging studies of the formulations at 177°C for 72 h.

Aged pictures of formulations extended with 7% PMRs

(93:7 H100W:PMRs)

Initial (before aging)

Aged pictures of formulations extended with 13% PMRs

(87:13 H100W:PMRs)

Conclusion

SIS-based nonwoven adhesive formulations that utilize

hydrogenated hydrocarbon resins can be extended with

pure monomer resins from 7%–13% (with respect to

hydrogenated resin level) without negatively affecting the

adhesive performance and thermal aging properties.

Benefits include:

• Improved adhesive peel and loop tack

• Higher amount of PMRs gives a slightly lower viscosity

and melt transition (4° to 6°C from DMA)

• Good thermal stability (color and viscosity) on aging

Eastman Chemical Company

Corporate Headquarters

P.O. Box 431

Kingsport, TN 37662-5280 U.S.A.

Telephone:

U.S.A. and Canada, 800-EASTMAN (800-327-8626)

Other Locations, (1) 423-229-2000

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2909 VA Capelle aan den IJssel

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Commercial Company, Ltd. Jingan Branch

1206, CITIC Square

No. 1168 Nanjing Road (W)

Shanghai 200041, P.R. China

Telephone: (86) 21 6120-8700

Fax: (86) 21 5213-5255

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2-11-16 Minami Aoyama

Minato-ku, Tokyo 107-0062 Japan

Telephone: (81) 3-3475-9510

Fax: (81) 3-3475-9515

Eastman Chemical Asia Pacific Pte. Ltd.

#05-04 Winsland House

3 Killiney Road

Singapore 239519

Telephone: (65) 6831-3100

Fax: (65) 6732-4930

www.eastman.com

Material Safety Data Sheets providing safety precautions that should be

observed when handling and storing Eastman products are available online or

by request. You should obtain and review the available material safety

information before handling any of these products. If any materials mentioned

are not Eastman products, appropriate industrial hygiene and other safety

precautions recommended by their manufacturers should be observed.

Neither Eastman Chemical Company nor its marketing affiliates shall be

responsible for the use of this information or of any product, method, or apparatus

mentioned, and you must make your own determination of its suitability and

completeness for your own use, for the protection of the environment, and for the

health and safety of your employees and purchasers of your products. NO

WARRANTY IS MADE OF THE MERCHANTABILITY OR FITNESS OF ANY PRODUCT,

AND NOTHING HEREIN WAIVES ANY OF THE SELLER’S CONDITIONS OF SALE.

Eastman, Eastotac, Kristalex, Piccolastic, and Piccotex are trademarks of

Eastman Chemical Company.

All other brands are the property of their respective owners.

© Eastman Chemical Company, 2012.

TT-136 10/12