108 INŻYNIERIA MATERIAŁOWA MATERIALS ENGINEERING ROK XXXVIII

Preparation of mounting massAdrian Krzysztof Antosik*, Zbigniew Czech

Institute of Organic Chemical Technology, West Pomeranian University of Technology Szczecin, *adriankrzysztofantosik@gmail.com

Self-adhesives materials are materials that develop significant adhesive forces upon contact with a substrate without requiring a chemical reaction without leaving residues on the substrate. To exhibit this property, self-adhesives materials should have cohesive strength that is much higher than its adhesion strength to the substrate. Usually they are defined as a viscoelastic material, which in a solvent free state remains permanently tacky at room temperature. Mechanically, they are a soft, sticky substance; consequently, a supporting backing is often required to convert it into commercially useful forms, such as tapes and labels. Mounting mass are a special form of self-adhesives materials usually in similar to modelling clay form plasticizer after warming up in the fingers. They are characterized by the fact that it does not dry out and can be relatively easily peeled off. They are used, inter alia, for fastening light units (in-cluding posters) to dry surfaces (walls, tables). The first company producing them was the company Bostik, the product Blu-tray, the composition of which is the secret of the manufacturer, generally described as a mixture of synthetic rubber, not showing dangerous properties in normal applications. Currently it is known a lot of self-adhesive products in the form of plastic masses produced by industry names “Blu-Tac” (Bostik), “UHU tac patafix” (Uhu GmbH) or “Prott buddies” (Henkel). Preparation of novel mounting mass using composition silicone risen with trimethylopropane triacrylate crosslinking by the use of UV or LED radiation was presented. Their adhesive properties on various substrates and cohesiveness are determined using international standards. Obtained materials are characterized by excellent cohesion and enough adhesion.

Key words: mounting mass, silicone resin, UV-crosslinking, LED-crosslinking.

Inżynieria Materiałowa 2 (216) (2017) 108÷112DOI 10.15199/28.2017.2.9© Copyright SIGMA-NOT MATERIALS ENGINEERING

1. INTRODUCTION

In principle, if the work required separating two dissimilar objects is higher than the work required bringing them into contact, then the objects will cling or stick to each other, that is easily defined phenomenon of adhesion. On the other hand, if the objects are more complex than a pair of well-defined molecules in a well-defined en-vironment, in which attractive forces outweigh repulsion, adhesion is often a highly complex process that involves several mechanisms spanning different length scales. To explain the chemical, physi-cal and mechanical factors governing adhesion the several theories have been developed over time but so far no unified theory has been developed [1÷3].

The UV curing is one of the latest techniques due to its eco-nomical (fast curing) and environmental (low VOCs) advantages, but this technique involve the use of photoinitiators, and also has limitation of penetration (it works only with transparent carrier ma-terials). UV-crosslinking process found interesting application for producing photoreactive PSA systems of high performance used in the coating industry for PVC signed and marked films. The idea of single-component UV-activated PSA became very attractive to manufacturing industries to replacing of the conventional PSA systems crosslinked at room temperature or two-component PSA systems crosslinked at elevated temperature. Crosslinking reac-tion takes place when the polymer layer is exposed to UV radiation where photoinitiator is used to absorb the UV radiation and generate upon cleavage or upon intermolecular reaction the reactive species, free radicals that can initiate the UV-crosslinking. UV-crosslinking technology is providing a precise temporal and spatial control of the setting process which will occur on order, selectively in the il-luminated areas. Such performance, together with cost and environ-mental consideration, are the main reasons why UV-crosslinkable adhesives are being increasingly used and continue to attract atten-tion in various sectors [4÷6].

In the long history of adhesive materials, pressure-sensitive ad-hesives and tapes technology as we know them are a fairly recent concept. However, to trace their origins, one needs to study the his-tory of adhesives as a whole, including the many failures and near misses along the way, as well as the fusion of various technologies,

which eventually led to their development. Since the dawn of his-tory, people learned of the healing powers of certain leaves and plants. There is archaeological evidence indicating that adhesives have indeed been found on primitive tools. More than 6000 years ago, on the arrival of the Egyptian Civilization, the art of healing was already a profession. A primitive tape concept used by Egyp-tians was the use of a paste of starch in water applied to cloth strips. It indicates that surgical bandages, made of a mixture of fat and honey, were in use [7, 8].

Silicones are semi-inorganic polymers (polyorganosiloxanes) that may be fluid, elastomeric, or resinous, depending on the types or organic groups on the silicone atoms and the extent of cross-linkage between polymer chains. The silicone resins owe their high heat stability to the strong silicon–oxygen–silicon bonds. They ex-hibit unique properties, such as high Si–O–Si backbone flexibility, low intermolecular interactions, low surface tension, excellent ther-mal stability and high UV transparency, excellent electrical proper-ties, chemical resistance and outstanding weathering resistance [2, 9÷12].

Silicones are primarily applicable in sealants. They are one-component adhesives, which cure by absorbing moisture from the surrounding air. The polycondensation reaction is isolated with ace-tic acid, recognizable by its characteristic smell. When curing is formed relatively quickly skin, and further curing can proceed by slow moisture absorbs. Silicones have a very high degree of flex-ibility, even at low temperature to –70°C, but they are sensitive to notch. They are resistant to atmospheric conditions effects. They are widely used for construction, the sealing sanitary facilities and bonding glass. Silicones play special role with stand temperature up to 300°C. Then are used to seal heaters on kettles and dryers; fur-naces under construction and the automotive industry. Silicones add do not show wetting paints and lacquers, hence produced in a wide range of colours. They are commonly supplied in packaging (tubes, cartridges) or in foil packs flexible. This allows them to be easily squeezing and dosing using a manual or pneumatic gun [13÷15].

Silicone pressure-sensitive adhesives are high-performance ad-hesives that can be utilized over a wide range of temperature, from –40 to 300°C. The molecular weights of solvent-borne silicones are preferably in the range from 500 000 to 1 500 000 Daltons. They

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bond to both low energy and high-energy surfaces. Silicone poly-mers based on gum contain dimethylsiloxy and diphenylsiloxy groups are adhesives materials with low surface energy (23 N/m), low glass transition temperature (–123°C), and creep (deform). In addition, silicone pressure-sensitive adhesives (Si–PSA) exhibit highly flexible, inert, hydrophobic, non-toxic, and biocompatible in nature. Silicone PSAs crosslinking process can be achieved ther-mally between 120 and 150°C by organic peroxide (because of the small amount of functional groups — methyl or/and phenyl groups). In literature the most common reactive thermally crosslinkers are benzoyl peroxide (BPO) and dichlorobenzoyl peroxide (DClBPO). They allow control of the crosslinking reaction by adjusting per-oxide, which determined degree of crosslinking of the adhesive composition. Peroxide allows control crosslinking reaction by ad-justing the degree of crosslinking of the adhesive composition. In recent years, numerous patents have described and explained the use of addition-cured silicone PSA compositions. The interest in addition-cure silicone chemistry derives primarily from a number of potential benefits this chemistry offers and the increasing avail-ability of functional silicone polymers that may be deployed for such a reaction. To address the VOC emission issue that is inherent with traditional silicone PSA systems high-solids and solvent-less silicone PSAs have been developed. Silicon-bonded vinyl (Si–Vi) functional groups and silicon-bonded hydrogen (SiH) functional groups are containing to silicone polymers in the addition-cure sili-cone PSAs. These silicone polymers are lower in molecular weight than those found in the traditional solvent-borne silicone PSA sys-tems. These silicones adhesives are cured via platinum-catalyzed hydrosilylation reaction of silicon hydride (SiH) with silicon-bonded vinyl (Si–Vi) to form a crosslinked matrix of polymer(s), resin(s) and additives. VOC chemistry is analogous to the solvent-based and solvent-less platinum-catalyzed silicone release coat-ing systems found in silicone release liners for organic PSAs. This type of silicone PSA can be accomplished in a single-zone oven and at a relatively curing in lower temperature (100÷150°C), even though some of these systems are supplied in hydrocarbon solvents. The platinum-catalyzed reaction occurs without any generation of by-products as the solvent evaporates. The key compositional pa-rameters involved in developing addition-curable silicone PSAs include variations in the functional group type (SiH or Si–Vi), the number of functional groups and molecular weights of the polymer, crosslinker and MQ resin. An addition cure silicone PSA composi-tion may also include organic diluents and additives for specific requirements, e.g. for lowering the thermal expansion coefficient, enhancing anchorage with the substrate, or improving high-temper-ature properties. Temperature requirement for curing these silicone PSAs is also lower, thus allowing the use of temperature-sensitive substrates. On the other hand, addition-cured silicone PSA systems do suffer from generally lower heat stability than peroxide systems. Some patents describe improved compositions that utilize peroxide and addition dual-cure mechanisms or the use of antioxidants to im-prove high-temperature performance in overcomes this deficiency [9, 12, 16÷18].

Silicones PSAs have found uses in a variety of applications, over their commercial introduction in the 1960s. Some of the long-established applications for silicone PSAs are found in industrial operations (masking, splicing, roller wrapping) as well as in electri-cal and electronics, medical care and healthcare, and automotive sectors. Over year 2000, there has been continuing interest in it of new uses for silicone PSAs, especially in applications such as medical and industrial tapes. Silicone pressure-sensitive adhesives (PSAs) are widely used in pressure-sensitive tapes and labels when application conditions or the nature of substrate surfaces surpass the performance boundaries of organic-based PSAs. Driven by needs for regulatory compliance and changing performance requirements, silicone PSAs based on new silicone chemistry and cure mecha-nisms have also emerged [2, 19, 20].

In this work the method of preparing novel mounting mass us-ing silicone resin has been presented. Irgacure 2100 and 184 were used as photoinitiators. The effect of crosslinking physicochemical properties of obtained silicone mounting mass was evaluated. Use-ful properties of obtained mass were characterized.

2. MATERIALS

In presented work commercial silicone adhesive Q2-7355 was used, which was product of Dow Corning (USA) and Irgacure 2100 and Irgacure 184 were used as a photoinitiator; product of BASF (Ger-many). TMPTA (trimethylopropane triacrylate) was used as a pho-toreactive monomer; product of BASF (Germany).

3. PREPARATION OF MOUNTING MASS

Silicone resin containing 50 wt. % polymer was mixed with pho-toinitiator and trimethylopropane triacrylate (TMPTA) to obtain homorganic composition (3 wt. % on a base of polymer content Ir-gacaure and 10 wt. % TMPTA). That obtained compositions were exposed to UV or LED (depended which photoinitiator was used) to obtained mounting mass with consistency of modelling clay.

Moreover, for cohesion test compositions before exposed to UV or LED was coated (5 cm/s) on polyester film (36 µm), dried for 10 min at 110°C in drying canal. Thus obtained adhesive film was crosslinked with UV (light source — UV-lamp; wavelength 350±10 nm; intensity of radiation 35 mW/cm2) or LED (light source — LED diodes; wavelength 400±10 nm; intensity of radia-tion 36 mW/cm2) and protected with polyester film (36 µm).

4. METHODS

The cohesion test of mounting mass tape was performed accord-ing to the method of Fédération Internationale des Fabricants et Transformateurs d’adhesifs et thermocollants sur papiers et autres support (FINAT) FTM 8. Mounting mass tape was adhered to steel plates and loaded with 1 kg weight. The contact surface of the ad-hesive layer to the substrate was 6.25 cm2 (2.5×2.5 cm). Samples of adhesive tape were mounted in a machine designed at the Labora-tory for Adhesives and Self-adhesive Materials of the West Pomera-nian University of Technology in Szczecin (Fig. 1.), which enabled automatic time reading of shear strength failure (the time at which an adhesive tape adhesive film falls away from the steel plate). The shear strength was tested at 20°C and 70°C [17, 21, 22]. For each of the tested compositions was carried out 5 measurements.

As well as the cohesion in a combination of materials with dif-ferent surface energy was examined by a modified standard FINAT FTM 8 (taking into account the weight of the material hanging on the ceramic substrate). The modification shear strength was tested at 20°C. During the tests to ceramic tile was glued a piece of mate-rial (paper, polyamide or steel respectively) weighing 10 g using 1 g of mounting mass. The modified test had the task simulations hanging objects (eg. poster) on the wall, in order to determine the application possibilities mounting mass. For each of the tested com-positions was carried out 5 measurements.

Table 1. Mounting mass compositionTabela 1. Skład masy montażowej

SerialNo.

Components weight, g

Silicone risen TMPTAPhotoinitiator

Irgacure 184 Irgacure 2100

1 50 2.5 0.75 0

2 50 2.5 0 0.75

110 INŻYNIERIA MATERIAŁOWA MATERIALS ENGINEERING ROK XXXVIII

Peel adhesion of PSA was tested using Zwick-Roell Z1 machine according to international standard Association des Fabricants Europeens de Rubans Auto-Adhesifs (AFERA) 4001 procedures. A sample of PSA-coated material 1 inch (ca. 2.5 cm) wide and about 5 inch (ca. 12.7 cm) long was bonded to a horizontal target substrate surface of a clean steel test plate at least 12.7 cm in firm contact. A 2 kg hard rubber roller was used to apply the strip. The free end of the coated strip was doubled back nearly touching itself so the angle of removal would be 180°. The free end was attached to the adhesion tester scale. The steel test plate was clamped in the jaws of a tensile testing machine, which was capable of moving the plate away from the scale at a constant rate of 300 mm/min. The scale reading in Newton was recorded as the tape was peeled from the steel surface. The data was reported as the average of the range of numbers observed during the test. The given result was an arith-metic average of three specimens [22]. Adhesion was tested using such substrate as paper, polyamide and steel. For each of the tested compositions was carried out 5 measurements.

5. RESULTS AND DISCUSSION

The cohesion of the mounting mass crosslinking by different light radiation, defined as the time at which the breakage occurred cohe-sive/adhesive were presented in table (Tab. 2). Both compositions were exhibit excellent cohesion at low temperature. Cohesion at 70°C for all composition showed the same effect (adhesion peeling off). This allows the state that the tapes are not resistant at elevated temperature. Comparison cohesive properties at room and elevated temperature show good adhesion and high cohesion to the adhesive layer (adhesive crack at higher temperature).

The cohesion of the mounting mass using to jointed different substrates, defined as the time at which the breakage occurred

cohesive/adhesive were presented in Table 3. Both compositions were exhibit excellent cohesion at low temperature over 30 days. This allows the state that the mounting mass can be used to connec-tion different substrates together at room temperature.

Mounting mass has a low adhesion to various substrates. Among the substrates tested, the adhesion was best in both test composi-tions to steel (about 3 N/25 mm) and the lowest polyamide substrate (approximately 1 N/25 mm). Result of adhesives tests was showed in Figure 2.

Fig. 1. Cohesion tests on the machine designed at the Laboratory for Adhesives and Self-adhesive Materials of the West Pomeranian University of Technology in SzczecinRys. 1. Badanie kohezji na maszynie zaprojektowanej w Laboratorium Klejów i Materiałów Samoprzylepnych na Zachodniopomorskim Uniwersytecie Technologicznym w Szczecinie

Table 2. Cohesion of tested mounting mass at different temperatureTabela 2. Kohezja badanej masy montażowej w różnej temperaturze

SerialNo.

Cohesion, h

20°C 70°C

1 >72 1.7±0.1

2 >72 2.3±0.1

Table 3. Cohesion of various material joint using tested mounting mass in room temperatureTabela 3. Kohezja różnych połączeń materiałowych z użyciem badanej masy montażowej w temperaturze pokojowej

SerialNo.

Cohesion in connection, day

paper/ceramics steel/ceramics polyamide/ceramics

1 >30 >30 >30

2 >30 >30 >30

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6. CONCLUSION

New mounting mass containing silicone resin and trimethylopro-pane triacrylate and crosslinking by UV or LED radiation were ob-tained. The obtained materials are characterized by excellent cohe-sion, white colour. After warming exhibit greater plasticity (can be formed) and highest adhesion.

Obtained mounting mass exhibit low adhesion and high cohe-sion at room temperature compared to other type self-adhesives ma-terials. This can expect that self-adhesives materials can be used to fast sticking light materials (paper, metal or polymer) on different substrates, and then the removal thereof without leaving a trace of adhesive material.

The work research is a prelude to further research on the prop-erties and received of the mounting mass. So far not received the composition characterized as good properties using UV technology.

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[3] Gierens G., Karmann W.: Adhesives and adhesive tape. Wiley (2001) ISBN 3-527-30110-0.

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[6] Czech Z., Kowalczyk A., Kabatc J., Świderska J.: Photoreactive UV-Cros-linkable solvent free acrylic pressure-sensitive adhesives containing copo-lymerizable photoinitiators based on benzophenones. European Polymer Journal 48 (2012) 46÷54.

[7] Czech Z., Kowalczyk A., Świderska J.: Pressure-sensitive adhesives for medical applications. Wide Spectra of Quality Control 17 (2011) 309÷320. ISBN 978-953-307-683-6.

[8] Benedek I.: Pressure-sensitive adhesives and applications. Marcel Dekker (2005) ISBN 0-8247-5059-4.

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[12] Antosik A. K., Czech Z.: Solvent-based pressure-sensitive adhesives. Do-konania Młodych Naukowców 4 (2014) 15÷17.

[13] Antosik A. K., Czech Z.: Solvent-free pressure-sensitive adhesives. Doko-nania Młodych Naukowców 5 (2014) 444÷446.

[14] Mirski Z., Piwowarczyk T. Podstawy klejenia, kleje i ich właściwości. Przegląd Spawalniczy 8 (2008) 12÷21.

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[17] Tolia G., Li S. K.: Study of drug releas and tablet characteristics of silicone adhesive matrix tablets. European Journal of Pharmaceutics and Biophar-maceutics 82 (2012) 518÷525.

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[19] Antosik A. K., Czech Z.: Wpływ ilości barwnika na fizyczne właściwości silikonowych klejów samoprzylepnych. Przemysł Chemiczny 94 (2015) 41÷42.

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[22] Antosik A. K., Bednarczyk P., Czech Z.: Jednostronnie klejące taśmy na bazie samoprzylepnych klejów silikonowych — dobór najlepszej kompo-zycji. Chemik 69 (2015) 95÷97.

[23] Wilpiszewska K., Czech Z.: Citric acid modified potato starch films con-taining microcrystalline cellulose reinforcement — properties and applica-tion. Starch 65 (2014) 1÷8.

Fig. 2. Adhesion of tested mounting mass to different substratesRys. 2. Adhezja badanej masy montażowej do różnych podłoży

112 INŻYNIERIA MATERIAŁOWA MATERIALS ENGINEERING ROK XXXVIII

Otrzymywanie samoprzylepnej masy montażowejAdrian Krzysztof Antosik*, Zbigniew Czech

Instytut Technologii Chemicznej Organicznej, Zachodniopomorski Uniwersytet Technologiczny w Szczecinie, *adriankrzysztofantosik@gmail.com

Inżynieria Materiałowa 2 (216) (2017) 108÷112DOI 10.15199/28.2017.2.9© Copyright SIGMA-NOT MATERIALS ENGINEERING

Słowa kluczowe: masa montażowa, żywice silikonowe, sieciowanie UV, sieciowanie LED.

1. CEL PRACY

Masy montażowe w formie plastycznych mas klejących wielokrot-nego użytku, podobne w konsystencji do plasteliny lub kitu, charak-teryzują się tym, że nie wysychają i dość łatwo można je odkleić. Są używane między innymi do mocowania lekkich elementów (takich jak plakaty) oraz do suchych powierzchni (ściany, tablice). Pierw-szą firmą produkującą je była firma Bostik pod nazwą produktu Blu-Tacka, którego skład stanowi tajemnicę producenta. Jest opisy-wany ogólnie jako mieszanina gum syntetycznych nie wykazująca niebezpiecznych właściwości w normalnych warunkach aplikacji. Obecnie znanych jest wiele produktów samoprzylepnych w posta-ci plastycznych mas produkowanych pod branżowymi nazwami „Blu-Tac” (Bostik), „UHU tac patafix” (Uhu GmbH) czy „Prott buddies” (Henkel), jednak ich skład chemiczny nie jest ujawniony przez producentów.

Celem pracy było otrzymanie mas montażowych na bazie ży-wic silikonowych i triakrylanu trimetylolopropanu wykazujących znakomitą kohezję oraz wystarczającą adhezję do podłoży o zróż-nicowanej energii powierzchniowej. Ponadto zbadano podstawowe właściwości otrzymanych mas montażowych, takie jak adhezja (do stali, polimeru i papieru) oraz kohezja w celu scharakteryzowania otrzymanych nowych materiałów samoprzylepnych oraz określono ich potencjalne możliwości aplikacyjne w porównaniu z istnieją-cymi już na rynku komercyjnymi masami montażowymi wiodą-cych firm.

2. MATERIAŁ I METODYKA BADAŃ

W pracy do uzyskania masy montażowej użyto komercyjnie do-stępnej żywicy silikonowej Q2-7566 firmy Dow Corning (USA), fotoreaktywnego monomeru triakrylanu trimetylolopropanu (TMP-TA) firmy BASF (Niemcy) oraz fotoinicjatorów Irgacure 184 i Ir-gacure 2100 niemieckiej firmy BASF.

W celu otrzymania masy montażowej żywicę silikonową zawie-rającą 50% mas. polimeru mieszano z fotoinicjatorem i triakryla-nem trimetylolopropanu (TMPTA) aż do uzyskania homogenicz-nej kompozycji (odpowiednio 3% mas. fotoinicjatora i 10% mas. TMPTA w przeliczeniu na suchą masę polimeru). Następnie kom-pozycję poddano działaniu promieniowania UV lub LED (w zależ-ności od użytego fotoinicjatora) aż do uzyskania masy montażowej o konsystencji modeliny.

Ponadto w przypadku badań kohezji i adhezji nieusieciowane kompozycje powlekano na folii poliestrowej (36 µm) i suszono przez 10 minut w temperaturze 110°C w kanale suszącym. Otrzy-mane w ten sposób taśmy samoprzylepne sieciowano UV lub LED, a następnie zabezpieczano folią poliestrową (36 µm).

Otrzymane masy montażowe badano zgodnie z międzynarodo-wymi normami Fédération Internationale des Fabricants et Trans-formateurs d’adhesifs et thermocollants sur papiers et autres sup-port (FINAT) FTM 8 i Association des Fabricants Europeens de Rubans Auto-Adhesifs (AFERA) 4001 (odpowiednio kohezja i ad-hezja) oraz ich zmodyfikowanym formom dostosowanym do badań uzyskanej masy montażowej.

3. WYNIKI I ICH DYSKUSJA

Badane kompozycje wykazały wystarczającą adhezję do podłoży o zróżnicowanej energii powierzchniowej. Największą adhezję wykazały obie próbki do podłoża stalowego (około 3 N/25 mm), natomiast najmniejszą do podłoża polimerowego, w tym przypadku poliamidu (około 1 N/25 mm).

Obydwie badane kompozycje wykazały doskonałą kohezje w temperaturze pokojowej (powyżej 72 h). Natomiast w pod-wyższonej temperaturze powstało pęknięcie adhezyjne po około 2 h. Wykazało to, że otrzymane masy montażowe nie są odporne na działanie podwyższonej temperatury i powinny być stosowane w temperaturze pokojowej.

Podczas badań połączeń lekkich materiałów o różnej energii po-wierzchniowej do podłoża ceramicznego uformowany w palcach 1 g masy montażowej utrzymywał 10 g papieru, poliamidu i stali powyżej 30 dni w pozycji prostopadłej do ziemi.

4. PODSUMOWANIE

Otrzymano masy montażowe na bazie kompozycji z żywic sili-konowych i triakrylanu trimetylolopropanu sieciowane za pomo-cą promieniowania UV lub LED. Uzyskane materiały charakte-ryzują się bardzo dobrą kohezją. Mają biały kolor. Po rozgrzaniu w palcach wykazują większą plastyczność (mogą być formowane) oraz przyczepność.

W porównaniu z innymi materiałami samoprzylepnymi otrzy-mane masy montażowe wykazują małą adhezję i dużą kohezje w temperaturze pokojowej. Można oczekiwać, że mogą być uży-wane do przyklejania lekkich materiałów (papieru, metalu lub po-limeru) do różnych podłoży. Można je szybko usuwać bez pozo-stawiania śladów materiału klejowego. Przeprowadzone badania pozwalają stwierdzić, że otrzymane kompozycje po usieciowaniu mogą być z powodzeniem używane do otrzymywania montażo-wych mas o właściwościach samoprzylepnych. Ich właściwości są zbliżone do komercyjnie dostępnych mas montażowych, takich jak „Blu-Tac” (Bostik), „UHU tac patafix” (Uhu GmbH) czy „Prott buddies” (Henkel).