Eur. J. Wood Prod.
(2015) 73:697–700
DOI 10.1007/s00107-015-0942-9
BRIEF ORIGINAL
Wet adhesion durability improvement of polyurethane wood
adhesives with primer
Carlos Amen-Chen1 • Joseph Gabriel1
Received: 3 October 2014 / Published online: 26 June 2015
Ó Springer-Verlag Berlin Heidelberg 2015
Abstract Southern yellow pine and Douglas fir were
glued with two different 1C PUR adhesives and evaluated
by means of the vacuum-pressure and delamination tests
according to the Canadian Standard CSA O112.9 and the
European Standard EN 391, method B, respectively. By
using a water-based primer before application of the
adhesive, wet wood failure percentage and delamination
resistance of the polyurethane adhesives dramatically
increased compared to matched samples glued under the
same conditions without primer. Standard requirements
were achieved when primer was used.
1 Introduction
The North American structural wood market is divided into
groups of wood species having similar working and gluing
properties. Douglas fir and southern yellow pine are the
most representative species, each representing one category
of commercial wood.
Adhesion durability for structural wood purposes in the
North American market is regulated by a set of standards by
the American Society for Testing Materials (ASTM) and
Canadian Standard Association (CSA). Standard ASTM
D2559 for wet resistance to delamination and block shear
after vacuum-pressure soak by CSA O112.9 are key tests
used to prove the wet adhesion quality of wood adhesives.
Delamination test EN 391 is a similar test applied in Europe.
& Carlos Amen-Chen
carlos.amen@henkel.com
1
Purbond AG, Industriestrasse 17a, 6203 Sempach Station,
Switzerland
It has been shown that the dry adhesion strength of
moisture curing one component polyurethane adhesives
(1C PUR) to wood is comparable to other adhesive che-
mistries, however, the amount of wood failure percentage
after humidity exposure is markedly lower when tested in
the wet state and delamination higher (Vick and Okkonen
2000). Wood failure percentage is an important require-
ment included in the CSA O112.9 (Canadian Standards
Association 2004) for structural wood adhesives intended
for exterior exposure use.
An aqueous urea solution primer together with 1C PUR
adhesives gave good results on southern yellow pine,
meeting the requirements set by ASTM D2559 on wood
delamination, but was not effective on Douglas fir (Gillis
et al. 2003). Wood had to be additionally sanded prior to
application of urea. No other results were reported
regarding the wet adhesion strength and wood failure
percentage.
Sheng et al. (2007) used diluted aqueous solutions of
polyethylene imines with a strong alkaline pH of
11.5–12.5. Wood was sanded first and the primer required a
drying time of 1–4 h before gluing with a 1C PUR or a
urea–formaldehyde adhesive. Dry tensile strength of native
Australian woods improved, but no results were reported
regarding wet adhesion strength, wet wood failure per-
centage or delamination resistance.
A formaldehyde-based hydroxymethylated resorcinol
(HMR) primer improves the wet adhesion of a variety of
adhesives including 1C PUR (Vick and Okkonen 2000).
The solution has to be left for 4 h for the reaction to take
place and must be used within 3–8 h.
In this work, enhancement of adhesion durability of 1C
PUR wood adhesives by aqueous primer compositions is
reported. Vacuum pressure soak and delamination resistance
tests according to the CSA O112.9 and the former European
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698 Eur. J. Wood Prod. (2015) 73:697–700

Standard EN 391, method B (European Committee for
Standardization 2001), respectively, are presented.
2 Materials and methods
The following materials were used:
Primer A was an aqueous solution of polyethoxylated
(20) sorbitan ester based on lauric acid. It has an average
hydroxyl value of 100 mg KOH g-1, a hydrophilic lipo-
philic balance (HLB) of 16.7, and is available under the
commercial name TweenÒ 20 from Croda Europe, Eng-
land. Primer A was used as a 5 % wt solution in deionized
water.
The primer was applied with a paint brush at a quantity
of 10–20 g m-2 on both wood sides and allowed to pen-
etrate the surface for 5–15 min prior to the application of
the adhesive.
Two 1C PUR wood adhesives from the company Pur-
bond AG, Sempach Station, Switzerland were used.
Adhesive K1 was formulated with an experimental
methylene diphenyl diisocyanate (MDI) based prepolymer
with 20 % by weight NCO content; a Brookfield viscosity of
25,000 mPa s-1 as measured at 20 °C, an average isocyanate
functionality of 2.8 and an open assembly time of 60 min.
Adhesive K2 was based on a methylene diphenyl
diisocyanate (MDI) prepolymer and is commercially
available under the brand PURBONDÒ. It had 16 % by
weight NCO; a Brookfield viscosity of 24,000 mPa s-1 at
20 °C, an average isocyanate functionality of 2.2 and an
open assembly time of 30 min.
Adhesive was applied one-sided on samples at a quan-
tity of 160–180 g m-2 and pressed at 0.8 MPa pressure for
4 h. Glued samples were stored for at least 7 days at 20 °C
and 65 % relative humidity prior to testing.
Freshly planed Douglas fir and southern yellow pine
lamellas in dimensions 350 9 70 9 40 mm3 with a mois-
ture content of 11–12 % and a density between 0.56 and
0.59 with a growth ring angle of \45° were used in the
vacuum pressure soak testing according to the CSA O112.9
standard. Matched samples, corresponding to glued wood
substrates with and without primer were also used in this
test. Seven specimens in dimensions 50 9 50 9 40 mm3
were cut from the samples. The specimens were submerged
in water at room temperature and subjected to a vacuum of
20–30 kPa absolute pressure for 30 min followed by a
period under 550 kPa pressure for 120 min. The specimens
were then immediately tested while wet under shear with a
50 kN universal testing machine at a shearing speed of
5 mm/min (Zwick-Roell, Ulm, Germany). The averaged
results are shown in Table 1.
Freshly planed Douglas fir (Pseudotsuga menziesii) and
southern yellow pine (Pinus taeda L.) boards
350 9 150 9 30 mm3 with a moisture content of 11–12 %
and a density between 0.55–0.70 g cm-3 with a growth
ring angle of <45° were used for delamination test
according to the European Standard EN 391, method B.
Matched samples were glued with and without the primer.
Four specimens cut from the samples in dimensions
75 9 135 9 120 mm3 were submerged in water at room
temperature and subjected to a vacuum of 20–30 kPa
absolute pressure for 30 min in a pressure-resistant vessel

Table 1 Vacuum-pressure test of Douglas fir and southern yellow pine with and without the use of primer A
Southern yellow pine glued with Douglas fir glued with adhesive K2
adhesive K1
Shear strength Wood failure Shear strength Wood failure
(MPa) (%) (MPa) (%)

Specimen 1 6.7 (7.0) 100 (75) 9.3 (8.7) 100 (90)

Specimen 2 7.1 (6.7) 100 (80) 9.3 (9.0) 65 (65)
Specimen 3 6.9 (6.8) 75 (40) 9.3 (9.0) 80 (60)
Specimen 4 6.7 (6.5) 85 (60) 8.9 (9.2) 100 (40)
Specimen 5 6.7 (6.5) 85 (50) 9.2 (8.9) 100 (60)
Specimen 6 6.7 (6.5) 100 (70) 9.4 (8.8) 100 (35)
Specimen 7 6.7 (6.3) 85 (40) 9.4 (8.9) 100 (60)
Average 6.8 (6.6) 90 (59) 9.2 (8.9) 90 (60)
Difference in the average results with and without primer 0.20 31 0.30 30
Pooled standard deviation 0.19 13 0.14 12
Standard error of the difference in the average 0.101 7 0.079 6
T-statistic value 1.69 4.46 3.75 4.57
2-tailed, 95 % confidence interval of the difference in the 0.20 ± 0.22 31 ± 15 0.30 ± 0.17 30 ± 14
average
Values in parentheses are without primer

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Table 2 Delamination results Delamination (%) Average delamination/bond line

of Douglas fir and southern
yellow pine with and without Specimen 1 Specimen 2 Specimen 3 Specimen 4
the use of primer A
Southern yellow pine glued with adhesive K1 ? primer
Bond line 1 0.0 (25.9) 0.0 (35.7) 0.0 (11.3) 1.9 (24.4) 0.5 (24.3)
Bond line 2 1.9 (15.8) 0.0 (24.4) 0.0 (20.3) 0.0 (5.6) 0.5 (16.5)
Bond line 3 5.6 (34.2) 0.0 (21.4) 0.0 (50.0) 9.8 (37.6) 3.9 (35.8)
Bond line 4 5.6 (62.0) 0.0 (56.4) 0.0 (31.6) 6.4 (51.5) 3.0 (50.4)
Average 3.3 (34.5) 0.0 (34.5) 0.0 (28.3) 4.5 (29.8) 2.0 (31.8)
Douglas fir glued with adhesive K2 ? primer
Bond line 1 0.0 (31.5) 0.0 (44.2) 0.0 (31.5) 0.0 (28.8) 0.0 (34.0)
Bond line 2 0.0 (28.8) 0.0 (30.8) 0.0 (26.9) 0.0 (40.8) 0.0 (31.8)
Bond line 3 7.7 (48.8) 7.7 (46.2) 1.9 (59.6) 8.5 (55.8) 6.4 (52.6)
Average 2.6 (36.4) 2.6 (40.4) 0.6 (39.3) 2.8 (41.8 2.1 (39.5)
Values in parentheses are without primer

after which a period under 550 kPa pressure for 120 min
followed. Specimens were exposed to a hot airflow in a
drying chamber (2–3 ms-1, 65–70 °C, 8–10 % relative
humidity) until initial mass was reached. The averaged
results are shown in Table 2.
3 Results and discussion
Previous findings on polyurethane wood adhesives have
shown wet shear strength comparable to those of resorcinol
formaldehyde (Vick and Okkonen 2000). However, wood
failure percentage of polyurethane glued wood after water
exposure is poor, with most of the failure loci located
where latewood rings meet or in general, when gluing high
density wood species. It is also in these high density late-
wood regions where delamination of glued wood tends to
occur.
The phenomenon of poor wet wood failure percentage
of 1C PUR wood adhesives is reversible and depends on
the exposure conditions. When wet specimens are dried
again to standard conditions, wood strength and wood
failure percentage closely match those found in the dry
state before water immersion, showing that wet exposure
does not permanently damage the bond line (Klaeusler
et al. 2014).
Polyethoxylated sorbitan esters are primarily emulsifiers
available with different hydrophilic-lipophilic balances
(HLB). A product with a HLB value of 16.7 (oil-in-water)
was chosen and evaluated for its effect on polyurethane wet
adhesion on wood. Although 1C PUR adhesives cure with
humidity in wood, these adhesives are rather hydrophobic.
Therefore, it was hypothesized that by choosing a high
HLB value emulsifier as primer, the adhesive and wood
interface could become more compatible with each other,
and that the adhesive could penetrate and diffuse into the
wood cell wall better, especially when gluing high density
species. Use of emulsifiers has previously been tested when
gluing water-based phenolic resins to less polar acetylated
wood (Youngquist et al. 1988).
The importance of the wood-adhesive interface region
for the durability of adhesives has been stated earlier by
Frihart (2007), who believes that the durability of an
adhesive lies primarily on its ability to penetrate the wood
cell walls. The adhesive-filled wood cell walls in this zone
are then stabilized when exposed to humidity. Although
this theory may support the approach used here, more work
has to be done to unambiguously assess the mechanism of
adhesion enhancement of the primer used.
Table 1 shows the results obtained for the use of primer
A on Douglas fir and southern yellow pine after vacuum-
pressure testing. Comparison of results with the same wood
without primer shows that wood failure percentage has
been increased clearly. The shear strength was just slightly
higher with primer but the wood failure percentage almost
doubled. A statistical unpaired t-Student test of the samples
bonded with and without primer reveals that the difference
in the average in wood failure percentage is significant with
95 % confidence.
Primer A was also tested on both woods for delamina-
tion resistance and results are shown in Table 2. Gluing
without primer was also carried out. Delamination was
drastically reduced to levels below 5 % in comparison to
over 30 % on matched samples with no primer.
4 Conclusion
The use of hydrophilic emulsifier solutions as primers
clearly improved the adhesion durability of 1C PUR on two
major North American wood species. Delamination resis-
tance and vacuum-pressure test requirements were met by

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applying low amounts of the primers before adhesive
application. These simple aqueous solutions of a non-toxic,
safety label-free, biodegradable emulsifier have shown to
be very versatile and effective in enhancing the durability
of polyurethane adhesives on several wood species. Further
examination of the primer should be carried out in order to
clarify its improvement effect.
References
Canadian Standards Association (2004) Evaluation of adhesives for
structural wood products (exterior exposure). O112.9-2004.
Vacuum-pressure test. Ontario, Canada
European Committee for Standardization (2001) Glued laminated
timber. Delamination test of glue lines. Standard EN 391.
Brussels, Belgium
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Eur. J. Wood Prod. (2015) 73:697–700
Frihart C (2007) Model for understanding the durability performance
of wood adhesives. In: Proceedings of 30th annual meeting of
the Adhesion Society, Tampa Bay, FL, 18–21 Feb 2007,
pp 222–224
Gillis HR, Parker AA, Teachey PY, Marcinko JJ (2003) Lignocel-
lulosic composites, adhesive systems, and process. International
application number PCT/US03/13931
Klaeusler O, Hass P, Amen C, Schlegel S, Niemz P (2014)
Improvement of tensile shear strength and wood failure
percentage of 1C PUR bonded wooden joints at wet stage by
means of DMF priming. Eur J Wood Prod 72:343–354
Sheng L, Wei DY, Gutowski W, Molenaar S, Spicer M (2007)
Method and composition for priming wood and natural fibre. Eur
Pat 1989261:B1
Vick CB, Okkonen A (2000) Durability of one part polyurethane
bonds to wood improved by HMR coupling agent. For Prod J
50(10):69–75
Youngquist JA, Sachs IB, Rowell RM (1988) Adhesive bonding of
acetylated aspen flakes, Part 2. Effect of emulsifiers on phenolic
resin bonding. Int J Adhes Adhes 8(4):197–200