A 2 L glass reactor conventional for free-radical polymerizations was charged with 8 g of acrylic acid, 272 g of 2-ethylhexyl acrylate, 120 g of isobornyl acrylate and 266 g of 1:1 acetone:special-boiling-point spirit 60/95. After nitrogen gas had been passed through the reactor for 45 minutes with stirring, the reactor was heated to 58° C. and 0.2 g of azoisobutyronitrile (AIBN, Vazo 64™, DuPont) in solution in 10 g of acetone was added.
Subsequently the external heating bath was heated to 75° C. and the reaction was carried out constantly at this external temperature. After a reaction time of 1 h a further 0.2 g of AIBN in solution in 10 g of acetone was added. After a reaction time of 5 hours 0.8 g of bis(4-tert-butylcyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 6 hours the batch was diluted with 100 g of special-boiling-point spirit 60/95. After a reaction time of 7 hours 0.8 g of bis(4-tert-butyl-cyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 10 hours the batch was diluted with 150 g of special-boiling-point spirit 60/95. After a reaction time of 24 h the reaction was discontinued and the product cooled to room temperature. Subsequently the polyacrylate was blended with 0.6% by weight of aluminum(IIII) acetylacetonate (3% strength solution, acetone) and the blend was diluted to a solids content of 30% with special-boiling-point spirit 60/95 and then coated from solution onto a PET film. After drying at 120° C. for 30 minutes, the application rate was 50 g/m2. The technical adhesive properties were analyzed by carrying out test methods A, B and C.
A 2 L glass reactor conventional for free-radical polymerizations was charged with 8 g of acrylic acid, 312 g of 2-ethylhexyl acrylate, 80 g of isobornyl acrylate and 170 g of 1:1 acetone:special-boiling-point spirit 60/95. After nitrogen gas had been passed through the reactor for 45 minutes with stirring, the reactor was heated to 58° C. and 0.2 g of azoisobutyronitrile (AIBN, Vazo 64™, DuPont) in solution in 10 g of acetone was added. Subsequently the external heating bath was heated to 75° C. and the reaction was carried out constantly at this external temperature. After a reaction time of 1 h a further 0.2 g of AIBN in solution in 10 g of acetone was added. After a reaction time of 5 hours 0.8 g of bis(4-tert-butylcyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 6 hours the batch was diluted with 100 g of special-boiling-point spirit 60/95. After a reaction time of 7 hours 0.8 g of bis(4-tert-butyl-cyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 10 hours the batch was diluted with 150 g of special-boiling-point spirit 60/95. After a reaction time of 24 h the reaction was discontinued and the product cooled to room temperature. Subsequently the polyacrylate was blended with 0.6% by weight of aluminum(IIII) acetylacetonate (3% strength solution, acetone) and the blend was diluted to a solids content of 30% with special-boiling-point spirit 60/95 and then coated from solution onto a PET film. After drying at 120° C. for 30 minutes, the application rate was 50 g/m2. The technical adhesive properties were analyzed by carrying out test methods A, B and C.
A 2 L glass reactor conventional for free-radical polymerizations was charged with 8 g of acrylic acid, 312 g of 2-ethylhexyl acrylate, 80 g of stearyl acrylate and 266 g of 1:1 acetone:special-boiling-point spirit 60/95. After nitrogen gas had been passed through the reactor for 45 minutes with stirring, the reactor was heated to 58° C. and 0.2 g of azoisobutyronitrile (AIBN, Vazo 64™, DuPont) in solution in 10 g of acetone was added. Subsequently the external heating bath was heated to 75° C. and the reaction was carried out constantly at this external temperature. After a reaction time of 1 h a further 0.2 g of AIBN in solution in 10 g of acetone was added. After a reaction time of 5 hours 0.8 g of bis(4-tert-butylcyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 6 hours the batch was diluted with 100 g of special-boiling-point spirit 60/95. After a reaction time of 7 hours 0.8 g of bis(4-tert-butyl-cyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 10 hours the batch was diluted with 150 g of special-boiling-point spirit 60/95. After a reaction time of 24 h the reaction was discontinued and the product cooled to room temperature. Subsequently the polyacrylate was blended with 0.6% by weight of aluminum(IIII) acetylacetonate (3% strength solution, acetone) and the blend was diluted to a solids content of 30% with special-boiling-point spirit 60/95 and then coated from solution onto a PET film. After drying at 120° C. for 30 minutes, the application rate was 50 g/m2. The technical adhesive properties were analyzed by carrying out test methods A, B and C.
A 2 L glass reactor conventional for free-radical polymerizations was charged with 8 g of acrylic acid, 352 g of 2-ethylhexyl acrylate, 40 g of isobornyl acrylate and 170 g of 1:1 acetone:special-boiling-point spirit 60/95. After nitrogen gas had been passed through the reactor for 45 minutes with stirring, the reactor was heated to 58° C. and 0.2 g of azoisobutyronitrile (AIBN, Vazo 64™, DuPont) in solution in 10 g of acetone was added. Subsequently the external heating bath was heated to 75° C. and the reaction was carried out constantly at this external temperature. After a reaction time of 1 h a further 0.2 g of AIBN in solution in 10 g of acetone was added. After a reaction time of 5 hours 0.8 g of bis(4-tert-butylcyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 6 hours the batch was diluted with 100 g of special-boiling-point spirit 60/95. After a reaction time of 7 hours 0.8 g of bis(4-tert-butyl-cyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 10 hours the batch was diluted with 150 g of special-boiling-point spirit 60/95. After a reaction time of 24 h the reaction was discontinued and the product cooled to room temperature. Subsequently the polyacrylate was blended with 0.6% by weight of aluminum(IIII) acetylacetonate (3% strength solution, acetone) and the blend was diluted to a solids content of 30% with special-boiling-point spirit 60/95 and then coated from solution onto a PET film. After drying at 120° C. for 30 minutes, the application rate was 50 g/m2. The technical adhesive properties were analyzed by carrying out test methods A, B and C.
A 2 L glass reactor conventional for free-radical polymerizations was charged with 8 g of acrylic acid, 372 g of 2-ethylhexyl acrylate, 20 g of isobornyl acrylate and 170 g of 1:1 acetone:special-boiling-point spirit 60/95. After nitrogen gas had been passed through the reactor for 45 minutes with stirring, the reactor was heated to 58° C. and 0.2 g of azoisobutyronitrile (AIBN, Vazo 64™, DuPont) in solution in 10 g of acetone was added. Subsequently the external heating bath was heated to 75° C. and the reaction was carried out constantly at this external temperature. After a reaction time of 1 h a further 0.2 g of AIBN in solution in 10 g of acetone was added. After a reaction time of 5 hours 0.8 g of bis(4-tert-butylcyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 6 hours the batch was diluted with 100 g of special-boiling-point spirit 60/95. After a reaction time of 7 hours 0.8 g of bis(4-tert-butyl-cyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 10 hours the batch was diluted with 150 g of special-boiling-point spirit 60/95. After a reaction time of 24 h the reaction was discontinued and the product cooled to room temperature. Subsequently the polyacrylate was blended with 0.6% by weight of aluminum(IIII) acetylacetonate (3% strength solution, acetone) and the blend was diluted to a solids content of 30% with special-boiling-point spirit 60/95 and then coated from solution onto a PET film. After drying at 120° C. for 30 minutes, the application rate was 50 g/m2. The technical adhesive properties were analyzed by carrying out test methods A, B and C.
A 2 L glass reactor conventional for free-radical polymerizations was charged with 8 g of acrylic acid, 192 g of 2-ethylhexyl acrylate, 200 g of isobornyl acrylate and 170 g of 1:1 acetone:special-boiling-point spirit 60/95. After nitrogen gas had been passed through the reactor for 45 minutes with stirring, the reactor was heated to 58° C. and 0.2 g of azoisobutyronitrile (AIBN, Vazo 64™, DuPont) in solution in 10 g of acetone was added. Subsequently the external heating bath was heated to 75° C. and the reaction was carried out constantly at this external temperature. After a reaction time of 1 h a further 0.2 g of AIBN in solution in 10 g of acetone was added. After a reaction time of 5 hours 0.8 g of bis(4-tert-butylcyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 6 hours the batch was diluted with 100 g of special-boiling-point spirit 60/95. After a reaction time of 7 hours 0.8 g of bis(4-tert-butyl-cyclohexanyl) peroxydicarbonate (Perkadox 16™, Akzo Nobel) in solution in 10 g of acetone was added. After 10 hours the batch was diluted with 150 g of special-boiling-point spirit 60/95. After a reaction time of 24 h the reaction was discontinued and the product cooled to room temperature. Subsequently the polyacrylate was blended with 0.6% by weight of aluminum(IIII) acetylacetonate (3% strength solution, acetone) and the blend was diluted to a solids content of 30% with special-boiling-point spirit 60/95 and then coated from solution onto a PET film. After drying at 120° C. for 30 minutes, the application rate was 50 g/m2. The technical adhesive properties were analyzed by carrying out test methods A, B and C.
A 2 L glass reactor conventional for free-radical polymerizations was charged with 8 g of acrylic acid, 352 g of 2-ethylhexyl acrylate, 40 g of isobornyl acrylate and 170 g of 1:1 acetone:special-boiling-point spirit 60/95. After nitrogen gas had been passed through the reactor for 45 minutes with stirring, the reactor was heated to 58° C. and 0.2 g of azoisobutyronitrile (AIBN, Vazo 64™, DuPont) in solution in 10 g of acetone was added. Subsequently the external heating bath was heated to 75° C. and the reaction was carried out constantly at this external temperature. After a reaction time of 1 h a further 0.2 g of AIBN in solution in 10 g of acetone was added. After 6 hours the batch was diluted with 100 g of special-boiling-point spirit 60/95. After 10 hours the batch was diluted with 150 g of special-boiling-point spirit 60/95. After a reaction time of 24 h the reaction was discontinued and the product cooled to room temperature. Subsequently the polyacrylate was blended with 0.6% by weight of aluminum(IIII) acetylacetonate (3% strength solution, acetone) and the blend was diluted to a solids content of 30% with special-boiling-point spirit 60/95 and then coated from solution onto a PET film.
aBS = bond strength to steel at 23° C. and 50% atmospheric humidity, measured after bonding.
bBS = bond strength to steel at 23° C. and 50% atmospheric humidity after 72 hours of bonding.
cBS = bond strength to steel at 23° C. and 50% atmospheric humidity after bonding; the PSA tapes were stored at 60° C. for 3 months beforehand. 50 g/m2 application rate to PET film 25 μm thick.
From the figures from table 1 it can be inferred that the inventive examples, even under very extreme storage conditions, possess only a very low peel increase. In contrast, the examples R1 and R2 already exhibit a much greater peel increase, since in the case of R1 the adhesive is already very soft and is therefore able to flow out very well over a prolonged period of time. Reference example R2, by contrast, is very hard and therefore exhibits—especially at high temperatures—an improved flow-out and hence a high peel increase in test C. For use for the bonding of printing plates it is preferred to use pressure-sensitive adhesives having a low peel increase preferably, in order that the PSA tape can be removed again easily after the printing process. The bonds may extend from several days through to several months, so that test C in particular is very informative as regards the suitability of a pressure-sensitive adhesive for bonding printing plates. Here, the inventive adhesives produced according to the method show themselves to be very advantageous as compared, for example, with the systems containing only a very low fraction (R1) or a very high fraction (R2) of isobornyl acrylate.
A PET film 25 μm thick and etched on both sides with trichloroacetic acid was coated with examples 1, 2, 3, 4, R1 or R2. Following crosslinking and drying, the application rate was 20 g/m2. For this purpose the film was coated directly from solution with the examples and dried at 100° C. for 30 minutes. The specimens thus coated were lined with a double-sidedly siliconized release paper. Subsequently, a commercially customary acrylate PSA was laminated via a transfer carrier onto the uncoated side of the existing assembly, with an application rate of 20 g/m2.
In the following step, a EVA foam with a thickness of 500 μm and a density of 270 kg/m3 was laminated on. Then, again via a transfer carrier, a commercially customary acrylate PSA is laminated onto this foam carrier, onto the uncoated side of the existing assembly, at an application rate of 50 g/m2.
The double-sided PSA tapes described above with the adhesive side lying open (see
After 7-day storage at 23° C. and 50% atmospheric humidity, the edge lifting of the printing plate from the double-sided PSA tape was ascertained. The values are reported in mm, are averaged from three measurements, and are summarized in table 2.
A PSA tape suitable for printing-plate bonding ought to exhibit edge lifting of less than 30 mm. The boundary is a function of the fact that, at higher values, the printing process is severely impaired.
Examples 1 to 4 meet this requirement on the one hand as a result of the production method, which allows the formation of graft copolymers. Example R3, without a graft initiator, demonstrates that the edge lifting deteriorates markedly. On the other hand, examples 1 to 4 in combination with the inventive method show that edge lifting can be reduced to the degree necessary.
Number | Date | Country | Kind |
---|---|---|---|
103 03 538.9 | Jan 2003 | DE | national |
103 14 898.1 | Apr 2003 | DE | national |
Filing Document | Filing Date | Country | Kind | 371c Date |
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PCT/EP04/00093 | 1/9/2004 | WO | 00 | 10/4/2006 |