International Journal of Innovation and Applied Studies

ISSN 2028-9324 Vol. 8 No. 4 Oct. 2014, pp. 1836-1841

© 2014 Innovative Space of Scientific Research Journals
http://www.ijias.issr-journals.org/

Synthesis and Optimization of PVA based paper lamination adhesives

1 2 2
Ruhul Amin , Rashedul Alam Adnan , and Md. Rubaiyat Islam
1
Assistant professor,
Department of Chemical Engineering,
Bangladesh University of Engineering & Technology (BUET), Dhaka-1000, Bangladesh
2
Department of Chemical Engineering,
BUET, Dhaka, Bangladesh

Copyright © 2014 ISSR Journals. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

ABSTRACT: Polyvinyl alcohol (PVA) and polyvinyl acetate (PVAc) are the polymers of great interest because of many desirable
characteristics. They can be used for many purposes. One of the major uses of these polymers is they can be used to produce
adhesives for paper converting, packaging and laminating. The purpose of this work is to develop a suitable process for
producing PVA based adhesives. In this work, both polyvinyl acetate and polyvinyl alcohol adhesives were prepared.
Adhesives were prepared by the polymerization and alcoholysis of vinyl acetate monomer (VAM). Different performance
tests were conducted after preparing these adhesives. In this study it was found that better quality adhesives can be
prepared from polyvinyl alcohol. Different performance tests were conducted on the adhesives prepared. It was found from
the performance tests that polyvinyl alcohol adhesive is the best adhesive that can be used for lamination. Drying time for
polyvinyl alcohol was found 12.9 minutes which was better than polyvinyl acetate adhesives. Moreover, pull-off test shows
that maximum allowable pressure for PVA adhesive is higher than PVAc adhesives and the value is 195 psi.

KEYWORDS: Polyvinyl alcohol, polyvinyl acetate, Vinyl acetate monomer, Adhesive, Polymer.

1 INTRODUCTION

An adhesive is any substance applied to the surfaces of materials that binds them together and resists separation [1]. The
importance of using paper lamination adhesive is increasing day by day. In Bangladesh, all the adhesives used for different
purposes such as, paper lamination, book binding, book cover preparing is imported from different countries. Using imported
adhesive is costly. This study work is based on producing foreign quality adhesive at low cost.
The use of adhesives offers many advantages over other binding techniques such as sewing, mechanical fastening,
thermal bonding, etc. These include the ability to bind different materials together, to distribute stress more efficiently
across the joint, the cost effectiveness of an easily mechanized process, an improvement in aesthetic design, and increased
design flexibility [2]. Properties of adhesive and applications may vary depending on the raw materials used to prepare those
adhesives. Vinyl ester family is the most important polymers that can be used to produce different adhesives [3]. Vinyl ester
is a synthetic polymer. PVA adhesives are water based adhesives [4]. They are mainly used for mounting paper, paper
products canvas etc. Polyvinyl acetate latexes were the first synthetic polymer latexes made on an industrial scale, beginning
in Germany in the 1930s [5]. With the addition (and/or generation in situ) of PVA as an emulsifier, PVA latexes became one of
the major products of the adhesive and surface coating industries.
PVA based adhesive preparation is a complex process. It shows complexity of polymerization reaction such as initiation,
propagation, termination and is time consuming [6]. It is, therefore, an object of this invention to provide a practical and
economical process for producing polyvinyl acetate adhesives having a lower degree of crystallizability. A further object is to
provide an improved method of polymerizing vinyl acetate to yield polyvinyl acetate that may be converted to polyvinyl

Corresponding Author: Ruhul Amin 1836

 Ruhul Amin, Rashedul Alam Adnan, and Md. Rubaiyat Islam

alcohol having a low degree of crystallizability. Optimization of different methods of adhesive preparation and the selection
of most cost effective method is another motto of this study.

2 MATERIALS AND METHODS

2.1 MATERIALS

The main materials used here are Polyvinyl Alcohol and Vinyl acetate monomer. Sodium Hydrogen Carbonate was used as
a buffer solution and Potassium persulfate as initiator. Detergent was used surfactant solution and all of these were found
from local market.

2.2 METHODOLOGY

Different types and grades of binders can be produced from polyvinyl Alcohol (PVA) and polyvinyl acetate (PVAc). Paper
converting, packaging wood, tile and home handyman adhesive can be produced from polyvinyl Acetate. On the other hand
polyvinyl alcohol binders are mainly used for paper applications and in textile industries. Synthesis processes of these
adhesives are different depending on the use of the adhesives. Our goal is to study a process for producing commercial
grade paper lamination binder. To achieve this goal, we have prepared both PVA and PVAc based adhesives.

2.3 POLYVINYL ACETATE PREPARATION

Two different tests were conducted to prepare polyvinyl acetate adhesive. The basic difference between the two
experiments was in the use of raw materials. In the first experiment no polyvinyl alcohol was used while polyvinyl alcohol
was used in the second experiment. Adhesives of two different grades have been found from two different experiments.
Polyvinyl alcohol is a water soluble polymer and it was used to partially hydrolyze polyvinyl acetate. Thus, adhesive prepared
in the second experiment has better bonding characteristics than the one prepared from the first experiment.

2.4 METHOD 1

The raw materials used for this method was vinyl acetate monomer (VAM), potassium persulfate, sodium bicarbonate
and surfactant solution. Potassium persulfate was used as the initiator of the polymerization reaction. Sodium persulfate was
used as buffer solution. 0.12 g sodium bicarbonate and 0.12 g potassium persulfate was dissolved in 5ml water respectively.
0.2 g surfactant solution was dissolve in 20 ml water. 40 ml water was added to 30 ml vinyl acetate monomer solution. All the
prepared solutions were mixed together in a polymerization bottle. Then the solution it was heated using magnetic stirrer for
o
8 hours. The temperature was kept at 70-80 C. After 8 hours of heating, polyvinyl acetate was found. The problem with this
method is plastic was formed with prepared adhesive and this plastic formation was found as precipitation. The quality of the
prepared adhesive was decreased because of the plastic formation. Another problem of this plastic formation is that it
hindered the movement of magnetic stirrer and thus the proper mixing of the solution.

2.5 METHOD 2

Method 2 is a modification of the first method as; plastic was formed in the first method. In this method additional
polyvinyl alcohol was used in the solution. 0.2 g PVA was dissolved in water and added to the polymerization bottle. PVA
partially hydrolyzes polyvinyl acetate and the adhesive produced in this method has a better binding quality. All procedures
are same as the previous method. The adhesive found in this process has no plastic precipitation, has a better binding quality
than the previous one. The reason behind this better quality is polyvinyl alcohol was used in this method. But still, the
desired quality couldn’t be achieved. So, another experiment was conducted to produce polyvinyl alcohol (PVA) adhesive.

2.6 POLYVINYL ALCOHOL PREPARATION

Polyvinyl alcohol cannot be prepared directly from vinyl alcohol monomer [7]. So, it was prepared from vinyl acetate
monomer. PVAc was prepared from vinyl acetate monomer. The procedure is just as discussed in the previous section. Then
PVA was prepared by the alcoholysis of PVAc. Methanol was used for the alcoholysis of PVAc. NaOH was used as the catalyst.
The solution was refluxed for 1 hour at 80℃. PVA was found as precipitate. It was separated by filtration and the PVA binder
was prepared by hydrolyzing the solid PVA. The adhesive prepared in this method has very good binding characteristics. Its
quality is almost same as the imported adhesives used in the local market.

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Synthesis and Optimization of PVA based paper lamination adhesives

3 PERFORMANCE TESTS

After preparing adhesives using three different methods, different performance tests were conducted to measure their
strengths. The tests we have conducted were:
1. Pull-off test
2. Peel test
3. Drying time test
The results found from these tests have shown the strength and quality of the different adhesives prepared. The tests
were conducted to conclude whether the adhesives prepared in this work is good or not.

3.1 PULL OFF-TEST

Pull-off adhesion testers measure the force required to pull a specified diameter of coating away from its substrate [8].
This test provides a direct indication of the strength of adhesion between the coating and the substrate. Equipments
required for this test were pressure source, pressure gauge and actuator. The flat surface of a paper is adhered to the coating
to be evaluated. A coupling connector from the actuator was attached to the paper, after allowing for the bonding adhesive
to cure. Pressure is slowly increased to the actuator within the system. Separation occurs when the pressure in the actuator
becomes greater than the bond strength between the coating and the substrate. The pressure at which separation occurs is
the maximum allowable pressure for the adhesive used.

3.2 DRYING TIME

Drying time is the period of time recommended for the adhesive to set after it is covered with the substrate. Drying time
was calculated manually. A stop clock was used to measure the drying time of the adhesives. The time required for each
sample to complete drying is observed.

3.3 T-PEEL TEST

Peeling is the most important test conducted for adhesives [9]. Because, paper lamination binders are applied in a way
that papers can be separated by peeling easily rather than tearing. An Admet eXpert 7600 series machine was used for the t-
peel test. High frequency data points were captured by the tester and a characteristic curve was found for each of the
samples. Each end of the sample was loaded into opposite tensile grips. The grips were separated at a constant rate and the
average load and the peak load were noted.

4 RESULTS AND DISCUSSION

4.1 PULL OFF-TEST

Maximum allowable pressures found from the pull-off test were different for all the samples. Maximum pressures for all
the samples are shown in table-1.

Table-1: Pull-off test result for different samples

Name of the sample Sample 1 Sample 2 Sample 3 Market product

Maximum pressure 55 80 195 210
(psi)

The maximum allowable pressure is different for different samples (Figure 1).

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 Ruhul Amin, Rashedul Alam Adnan, and Md. Rubaiyat Islam

Maximum pressure, psi 220

170

120

70

20

1 2 3 4
-30

Figure 1: Graphical representation of pull-off test result

From the bar diagram it can be said clearly that the adhesive prepared in the third experiment has the best adherent
quality and the maximum allowable pressure is nearly equal to that of the market product.

4.2 DRYING TIME

The drying time was calculated manually. Using the stop clock, the drying time for the adhesive to set after it is covered
with the substrate. Drying time for different samples is shown in table-2.

Table-2: Drying time for different samples

Sample name Sample1 Sample 2 Sample 3 Market

product
Drying time (min) 23.4 21.1 12.9 10.1

The drying time is noted for different samples and market product and it is found that Sample 3 is close to market
adhesive (Figure-2)

30
Drying time(min)

20

10

0
Sample 1
Sample 2
Sample 3
Market product

Figure 2: Drying time of various samples

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Synthesis and Optimization of PVA based paper lamination adhesives

4.3 T-PEEL TEST

In T-peel test, laminating films are detached by the pneumatic tension grip. Different loads need to separate the films and
displacements of the arms were observed.

Table-3: T-peel test result for different samples

Sample 1 Sample 2 Sample 3 Market product

Displacement Load (N) Displacement Load (N) Displacement Load (N) Displacement Load (N)
(mm) (mm) (mm) (mm)
0 10 0 10 0 10 0 10
2 55 2 75 2 129 2 168
4 41 4 32 4 67 4 72
6 25 6 28 6 76 6 70
8 31 8 28 8 64.5 8 68
10 25 10 27.5 10 65 10 68

The grips were separated at a constant rate and the average load and the peak load were noted (figure-3).

180 Sample 1
160
140
Maximum load (N)

120
Sample 2
100
80
60
Sample 3
40
20
0
0 4 8 12 Market
Displacement (mm) Product

Figure 3: T-peel test for various samples

From analyzing all the results it is clearly stated that market product is still better than ours. Some reasons are liable for
that such like: Using local detergent instead of AMA, AOT which caused foam during PVA synthesis, using Vinyl acetate
monomer in fist two sample tests which formed plastic during operation, running semi batch instead of batch system,
presence of air bubble in the final product etc.

5 CONCLUSION

It can be stated that the synthesis and optimization of PVA based adhesive constitutes a mature field of research with
commercial opportunities and a promising future in the forthcoming years. The objective of this study was to establish a
simplified and economically feasible process for PVA adhesive production. From analyzing the results it is concluded that
method 3 is the optimized method. It is clearly mentioned that using polyvinyl acetate will not be feasible for this study. PVA
adhesive has less drying time of 87s which confirms that it dries faster. From pull off test it is proved that PVA adhesive can
tolerate up to a pressure of 195 psi which is approximate to existing market adhesive. Drying time and T peel test also proved

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 Ruhul Amin, Rashedul Alam Adnan, and Md. Rubaiyat Islam

its properties as a fine quality adhesive. Experimental study showed that it was a time consuming process and needs great
inspection.

REFERENCES

[1] A. J. Kinloch Adhesion and Adhesives: Science and Technology, illustrated, reprint Ed. Springer Science & Business Media,
1987.
[2] Allen, J.P. Biophysical Chemistry: John Wiley & Sons, 2009.
[3] Kim, J.K. and Pal, K, Recent Advances in the Processing of Wood-Plastic Composites, Springer, 2010.
[4] T.E. Rolando, Solvent-Free Adhesives, Ismithers Rapra Publishing, 1998.
[5] J.C. Salamone, Polymeric Material Encyclopedia, CRC Press, 1996.
[6] Fried, J.R. Polymer Science and Technology, 2nd, illustrated, reprint Ed. Prentice Hall Professional Technical Reference,
2003.
[7] Sakurada, I. Polyvinyl Alcohol Fibers, illustrated Ed. CRC Press, 1985.
[8] Silva, L., Dillard, D., Blackman, B. and Adams, R. Testing Adhesive Joints: Best Practices, John Wiley & Sons, 2012.
[9] Benedek, I. Pressure-Sensitive Adhesives and Applications, 2nd, illustrated, revised Ed. CRC Press, 2004.

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