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Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups
Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
1 Contents lists available at ScienceDirect 2 3 4 5 6 journal homepage: www.elsevier.com/locate/dib 7 8 9 Data Article 10 11 12 13 14 15 16 17 Jakob Manhart a, Santhosh Ayalur-Karunakaran a, 18 Simone Radl a, Andreas Oesterreicher b, Andreas Moser c, 19 Christian Ganser d,e, Christian Teichert d, Gerald Pinter c, 20 a,f b,f a 21 Q1 Wolfgang Kern , Thomas Griesser , Sandra Schlögl 22 Q2 a Polymer Competence Center Leoben GmbH, Roseggerstraße 12, A-8700 Leoben, Austria b 23 Christian Doppler Laboratory for Functional and Polymer based Ink-Jet Inks, Otto Glöckel-Straße 2, A-8700 Leoben, Austria 24 c Chair of Materials Science and Testing of Plastics, University of Leoben, Otto Glöckel-Straße 2, A-8700 25 Leoben, Austria 26 d Institute of Physics, University of Leoben, Franz Josef – Straße 18, A-8700 Leoben, Austria e 27 Christian Doppler Laboratory for Fiber Swelling and Paper Performance, Graz University of Technology, Inffeldgasse 23, 8010 Graz, Austria 28 f Chair of Chemistry of Polymeric Materials, University of Leoben, Otto Glöckel-Straße 2, A-8700 Leoben, 29 Austria 30 31 32 a r t i c l e i n f o abstract 33 34 Article history: The photo-reversible [4πs þ 4πs] cycloaddition reaction of pen35 Received 31 August 2016 dant anthracene moieties represents a convenient strategy to 36 Received in revised form impart wavelength dependent properties into hydrogenated 37 9 September 2016 carboxylated nitrile butadiene rubber (HXNBR) networks. The Accepted 16 September 2016 38 present article provides the 1H NMR data on the reaction kinetics 39 of the side chain functionalization of HXNBR. 2-(Anthracene-9-yl) Keywords: 40 oxirane with reactive epoxy groups is covalently attached to the Photoreversible networks Q5 41 polymer side chain of HXNBR via ring opening reaction between Reaction kinetics the epoxy and the carboxylic groups. Along with the 42 Thermo-mechanical properties identification, 1H NMR data on the quantification of the attached 43 functional groups are shown in dependence on reaction time and 44 concentration of 2-(anthracene-9-yl)oxirane. Changes in the 45 modification yield are reflected in the mechanical properties and 46 DMA data of photo-responsive elastomers are illustrated in 47 dependence on the number of attached anthracene groups. DMA 48 49 DOI of original article: http://dx.doi.org/10.1016/j.polymer.2016.08.106 50 E-mail address: [email protected] (S. Schlögl). 51 52 http://dx.doi.org/10.1016/j.dib.2016.09.023 53 2352-3409/& 2016 The Authors. Published by Elsevier Inc. This is an open access article under the CC BY license 54 (http://creativecommons.org/licenses/by/4.0/).
Data in Brief
Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
2
55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108
curves over repeated cycles of UV induced crosslinking (λ 4 300 nm) and UV induced cleavage (λ ¼254 nm) are further depicted, demonstrating the photo-reversibility of the thermomechanical properties. Interpretation and discussion of the data are provided in “Design and application of photo-reversible elastomer networks by using the [4πs þ 4πs] cycloaddition reaction of pendant anthracene groups” (Manhart et al., 2016) [1]. & 2016 The Authors. Published by Elsevier Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Specifications Table Subject area More specific subject area Type of data How data was acquired Data format Experimental factors
Experimental features
Data source location Data accessibility
Chemistry Polymer Photochemistry Table, graphs H NMR spectra were recorded with a Varian 400-NMR operating at 399.66 MHz and DMA measurements were performed with a SDTA861E DMA analyzer from Mettler-Toledo. Analyzed 1 H NMR spectra were acquired by using a relaxation delay of 10s and 45° pulse. CDCl3 was used as solvent and spectra were referenced to Si(CH3)4 as internal standard. For DMA measurements, an amplitude of 20 mm and a measurement frequency of 1 Hz were used. The test specimen were heated from 60 °C to þ40 °C with a heating rate of 2 K/min. Functional rubber materials were synthetized and 1H NMR experiments were performed to verify and quantify the attachment of 2-(anthracene-9-yl)oxirane. Loss factor and storage modulus of photo-reversible rubber materials are provided in dependence on the modification yield and UV exposure dose. Leoben, Austria 1
Data are provided with this article
Value of the data
1H NMR data enables an easy assigning of the proton peaks, which is relevant to determine the modification yield of side chain modified rubber and polymer materials.
Comparison of the reaction kinetics with other epoxy based systems can help to understand the
influence of key parameters on the ring-opening reaction between epoxy moieties and carboxylic acid groups. DMA data allow a deeper understanding of the role of bulky aromatic side chains on the structuralproperty relationship of elastomer materials.
1. Data 1
H NMR data on the verification and quantification of HXNBR materials with pedant anthracene groups are provided. DMA data on side chain functionalized HXNBR materials are shown in dependence on the modification yield. Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
2. Experimental design, materials and methods 2.1.
1
H NMR experiments of side chain functionalized HXNBR
The synthesis procedure is provided in Ref. [1]. For the characterization of the reaction kinetics, small amounts of the reactions solution were taken out at selected reaction times of one batch that was stirred at room temperature for 72 h. The reaction solution was immediately precipitated to stop the ongoing reaction and subsequently two purification steps were carried out in which the samples were dissolved in chloroform again and precipitated in cold methanol. After removing the supernatant from the precipitate, the latter was dried at room temperature under vacuum and analyzed regarding its modification yield. For the quantification of the modification yield, 1H NMR spectra were referenced to a residual chloroform signal of 7.27 ppm (corresponding to Si(CH3)4 with a shift of 0.0 ppm) after Fourier transformation. In order to quantify the anthracene signal, the isolated peak at 4.05 ppm was integrated including its complete shoulders on both sides after an appropriate baseline subtraction. For reference purposes, the signal from 2.95 to 0.2 ppm was integrated as it originates from the polymer chain. The modification yield was then calculated according to Eq. (1), wherein the average number of protons per repeating unit was calculated to be 6.033. modification yield ¼
single proton0 s signal of attached anthracene signal of polymer chain average number of protons per repeating unit
ð1Þ
Fig. 1 provides the 1H NMR spectra of HXNBR prior to and after side chain modification with 2(anthracene-9-yl)oxirane together with the 1H NMR spectrum of 2-(anthracene-9-yl)oxirane. Fig. 2 shows the reaction kinetics of the side chain modification of HXNBR, which was carried out at room temperature. The number of attached anthracene groups is plotted against the reaction time. The influence of the concentration of 2-(anthracene-9-yl)oxirane in the reaction mixture on the modification yield is displayed. 2.2. DMA experiments of side chain functionalized HXNBR Sample preparation and DMA experiments are detailed in Ref. [1]. Table 1 illustrates the storage modulus at 23 °C of side chain modified HXNBR materials in dependence on the modification yield that ranges from 0 to 1.30 mol%.
normalized signal (-)
109 110 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138 139 140 141 142 143 144 145 146 147 148 149 150 151 152 153 154 155 156 157 158 159 160 161 162
3
2-(anthracene-9-yl)oxirane detail
5,7
HXNBR
detail
5,4
5,1
detail
8,5
8,0
7,5
5,6
4,8
4,0
3,2
modified HXNBR
12
10
8
6
4
2
chemical shift (ppm) Fig. 1. 1H NMR spectra of 2-(anthracene-9-yl)oxirane, HXNBR and their reaction product (arrows indicate peaks that emerged and decreased upon side chain functionalization).
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
1,8 1,6 (5)
1,4 1,2
(4)
1,0
(3)
0,8 0,6
(2)
0,4
(1)
0,2 0,0 0
10
20
30
40
50
60
70
Reaction time (h) Fig. 2. Modification yield of photo-responsive rubber materials versus reaction time in dependence on the 2-(anthracene-9-yl) oxirane concentration; (1) 10, (2) 30, (3) 60, (4) 100 and (5) 150 phr (parts per hundred rubber). (The line is a guide to the eye). Table 1 Storage modulus (E0 ) of photo-responsive rubber materials after UV induced crosslinking. Sample
Modification yielda/mol.%
E0 at 23 °C after UV exposure (260 J/cm2)b/MPa
Rubber-0 Rubber-1 Rubber-2 Rubber-3 Rubber-4
0 0.19 0.49 0.86 1.30
2.7 2.7 2.9 3.1 3.3
a b
Determined by 1H NMR experiments. Determined by DMA measurements.
1,7
1,7 1,6 1,5
tan(δ) (-)
1,6
tan(δ) (-)
163 164 165 166 167 168 169 170 171 172 173 174 175 176 177 178 179 180 181 182 183 184 185 186 187 188 189 190 191 192 193 194 195 196 197 198 199 200 201 202 203 204 205 206 207 208 209 210 211 212 213 214 215 216
Modification yield (mol.% of repeating units)
4
1,5
1,4 1,3 1,2 1,1
1,4 -21
-20
-19
-18
-17
-16
-15
-14
temperature (°C)
-13
-12
-11
-14
-12
-10
-8
-6
-4
-2
0
temperature (°C)
Fig. 3. DMA curves of photo-responsive rubber materials upon prolonged UV exposure (λ4 300 nm); (a) (♦) rubber-0, (■) rubber-1, (▲) rubber-2 and (b) () rubber-3.
Fig. 3a and b provide the DMA curves of photo-responsive rubber materials with different modification yields, which have been photochemically crosslinked (λ 4300 nm) at different exposure doses. In addition, Fig. 4 details the DMA curves of rubber-4 in a broad temperature range over prolonged UV exposure (λ4 300 nm). Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
5
tan δ (-)
2,0 217 218 1,8 219 + 1,6 220 1,4 221 222 1,2 223 1,0 224 0,8 225 0,6 226 227 0,4 228 0,2 229 0,0 230 -60 -50 -40 -30 -20 -10 0 10 20 30 40 231 temperature (°C) 232 233 Fig. 4. DMA curves of rubber-4 upon prolonged UV exposure (λ 4300 nm) over a temperature range from 60 to þ 40 °C. 234 Details of the DMA curves in a narrow temperature range are also given in Ref. [1]. 235 236 237 238 239 240 241 242 243 244 245 246 247 248 249 250 251 252 253 254 Fig. 5. DMA curves of rubber-4 over repeated cycles of UV induced crosslinking with 46 J/cm2 (λ 4300 nm, N2) and UV induced 255 cleavage with 9.72 J/cm2 (λ¼ 254 nm, N2) over a temperature range from 60 to þ 40 °C. Details of the DMA curves in a narrow temperature range are also given in Ref. [1]. 256 257 In Fig. 5 the DMA curves of rubber-4 are provided in a broad temperature range over three cycles 258 of photochemical crosslinking and subsequent photochemical cleavage upon deep UV exposure. 259 260 261 Acknowledgments 262 263 The research work of this paper was performed at the Polymer Competence Center Leoben GmbH 264 (PCCL, Austria) within the framework of the COMET-program of the Federal Ministry for Transport, 265 266 Q3 Innovation and Technology and Federal Ministry for Economy, Family and Youth with contributions by the Chair of Chemistry of Polymeric Materials (University of Leoben, Austria). The PCCL is funded 267 by the Austrian Government and the State Governments of Styria, Lower and Upper Austria. 268 T. Griesser and A. Oesterreicher thank the Christian Doppler research association and the Austrian 269 270 Ministry for Economy, Family and Youth (BMWFJ) for financial support.
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
6
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
271 Transparency document. Supporting information 272 273 Q4 Transparency data associated with this article can be found in the online version at http://dx.doi. 274 org/10.1016/j.dib.2016.09.023. 275 276 277 Reference 278 279 [1] J. Manhart, S. Ayalur-Karunakaran, S. Radl, A. Oesterreicher, A. Moser, C. Ganser, et al., Design and application of photoreversible elastomer networks by using the [4πsþ 4πs] cycloaddition reaction of pendant anthracene groups, Polymer 280 (2016), http://dx.doi.org/10.1016/j.polymer.2016.08.106.
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
1 Contents lists available at ScienceDirect 2 3 4 5 6 journal homepage: www.elsevier.com/locate/dib 7 8 9 Data Article 10 11 12 13 14 15 16 17 Jakob Manhart a, Santhosh Ayalur-Karunakaran a, 18 Simone Radl a, Andreas Oesterreicher b, Andreas Moser c, 19 Christian Ganser d,e, Christian Teichert d, Gerald Pinter c, 20 a,f b,f a 21 Q1 Wolfgang Kern , Thomas Griesser , Sandra Schlögl 22 Q2 a Polymer Competence Center Leoben GmbH, Roseggerstraße 12, A-8700 Leoben, Austria b 23 Christian Doppler Laboratory for Functional and Polymer based Ink-Jet Inks, Otto Glöckel-Straße 2, A-8700 Leoben, Austria 24 c Chair of Materials Science and Testing of Plastics, University of Leoben, Otto Glöckel-Straße 2, A-8700 25 Leoben, Austria 26 d Institute of Physics, University of Leoben, Franz Josef – Straße 18, A-8700 Leoben, Austria e 27 Christian Doppler Laboratory for Fiber Swelling and Paper Performance, Graz University of Technology, Inffeldgasse 23, 8010 Graz, Austria 28 f Chair of Chemistry of Polymeric Materials, University of Leoben, Otto Glöckel-Straße 2, A-8700 Leoben, 29 Austria 30 31 32 a r t i c l e i n f o abstract 33 34 Article history: The photo-reversible [4πs þ 4πs] cycloaddition reaction of pen35 Received 31 August 2016 dant anthracene moieties represents a convenient strategy to 36 Received in revised form impart wavelength dependent properties into hydrogenated 37 9 September 2016 carboxylated nitrile butadiene rubber (HXNBR) networks. The Accepted 16 September 2016 38 present article provides the 1H NMR data on the reaction kinetics 39 of the side chain functionalization of HXNBR. 2-(Anthracene-9-yl) Keywords: 40 oxirane with reactive epoxy groups is covalently attached to the Photoreversible networks Q5 41 polymer side chain of HXNBR via ring opening reaction between Reaction kinetics the epoxy and the carboxylic groups. Along with the 42 Thermo-mechanical properties identification, 1H NMR data on the quantification of the attached 43 functional groups are shown in dependence on reaction time and 44 concentration of 2-(anthracene-9-yl)oxirane. Changes in the 45 modification yield are reflected in the mechanical properties and 46 DMA data of photo-responsive elastomers are illustrated in 47 dependence on the number of attached anthracene groups. DMA 48 49 DOI of original article: http://dx.doi.org/10.1016/j.polymer.2016.08.106 50 E-mail address: [email protected] (S. Schlögl). 51 52 http://dx.doi.org/10.1016/j.dib.2016.09.023 53 2352-3409/& 2016 The Authors. Published by Elsevier Inc. This is an open access article under the CC BY license 54 (http://creativecommons.org/licenses/by/4.0/).
Data in Brief
Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
2
55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108
curves over repeated cycles of UV induced crosslinking (λ 4 300 nm) and UV induced cleavage (λ ¼254 nm) are further depicted, demonstrating the photo-reversibility of the thermomechanical properties. Interpretation and discussion of the data are provided in “Design and application of photo-reversible elastomer networks by using the [4πs þ 4πs] cycloaddition reaction of pendant anthracene groups” (Manhart et al., 2016) [1]. & 2016 The Authors. Published by Elsevier Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Specifications Table Subject area More specific subject area Type of data How data was acquired Data format Experimental factors
Experimental features
Data source location Data accessibility
Chemistry Polymer Photochemistry Table, graphs H NMR spectra were recorded with a Varian 400-NMR operating at 399.66 MHz and DMA measurements were performed with a SDTA861E DMA analyzer from Mettler-Toledo. Analyzed 1 H NMR spectra were acquired by using a relaxation delay of 10s and 45° pulse. CDCl3 was used as solvent and spectra were referenced to Si(CH3)4 as internal standard. For DMA measurements, an amplitude of 20 mm and a measurement frequency of 1 Hz were used. The test specimen were heated from 60 °C to þ40 °C with a heating rate of 2 K/min. Functional rubber materials were synthetized and 1H NMR experiments were performed to verify and quantify the attachment of 2-(anthracene-9-yl)oxirane. Loss factor and storage modulus of photo-reversible rubber materials are provided in dependence on the modification yield and UV exposure dose. Leoben, Austria 1
Data are provided with this article
Value of the data
1H NMR data enables an easy assigning of the proton peaks, which is relevant to determine the modification yield of side chain modified rubber and polymer materials.
Comparison of the reaction kinetics with other epoxy based systems can help to understand the
influence of key parameters on the ring-opening reaction between epoxy moieties and carboxylic acid groups. DMA data allow a deeper understanding of the role of bulky aromatic side chains on the structuralproperty relationship of elastomer materials.
1. Data 1
H NMR data on the verification and quantification of HXNBR materials with pedant anthracene groups are provided. DMA data on side chain functionalized HXNBR materials are shown in dependence on the modification yield. Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
2. Experimental design, materials and methods 2.1.
1
H NMR experiments of side chain functionalized HXNBR
The synthesis procedure is provided in Ref. [1]. For the characterization of the reaction kinetics, small amounts of the reactions solution were taken out at selected reaction times of one batch that was stirred at room temperature for 72 h. The reaction solution was immediately precipitated to stop the ongoing reaction and subsequently two purification steps were carried out in which the samples were dissolved in chloroform again and precipitated in cold methanol. After removing the supernatant from the precipitate, the latter was dried at room temperature under vacuum and analyzed regarding its modification yield. For the quantification of the modification yield, 1H NMR spectra were referenced to a residual chloroform signal of 7.27 ppm (corresponding to Si(CH3)4 with a shift of 0.0 ppm) after Fourier transformation. In order to quantify the anthracene signal, the isolated peak at 4.05 ppm was integrated including its complete shoulders on both sides after an appropriate baseline subtraction. For reference purposes, the signal from 2.95 to 0.2 ppm was integrated as it originates from the polymer chain. The modification yield was then calculated according to Eq. (1), wherein the average number of protons per repeating unit was calculated to be 6.033. modification yield ¼
single proton0 s signal of attached anthracene signal of polymer chain average number of protons per repeating unit
ð1Þ
Fig. 1 provides the 1H NMR spectra of HXNBR prior to and after side chain modification with 2(anthracene-9-yl)oxirane together with the 1H NMR spectrum of 2-(anthracene-9-yl)oxirane. Fig. 2 shows the reaction kinetics of the side chain modification of HXNBR, which was carried out at room temperature. The number of attached anthracene groups is plotted against the reaction time. The influence of the concentration of 2-(anthracene-9-yl)oxirane in the reaction mixture on the modification yield is displayed. 2.2. DMA experiments of side chain functionalized HXNBR Sample preparation and DMA experiments are detailed in Ref. [1]. Table 1 illustrates the storage modulus at 23 °C of side chain modified HXNBR materials in dependence on the modification yield that ranges from 0 to 1.30 mol%.
normalized signal (-)
109 110 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138 139 140 141 142 143 144 145 146 147 148 149 150 151 152 153 154 155 156 157 158 159 160 161 162
3
2-(anthracene-9-yl)oxirane detail
5,7
HXNBR
detail
5,4
5,1
detail
8,5
8,0
7,5
5,6
4,8
4,0
3,2
modified HXNBR
12
10
8
6
4
2
chemical shift (ppm) Fig. 1. 1H NMR spectra of 2-(anthracene-9-yl)oxirane, HXNBR and their reaction product (arrows indicate peaks that emerged and decreased upon side chain functionalization).
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
1,8 1,6 (5)
1,4 1,2
(4)
1,0
(3)
0,8 0,6
(2)
0,4
(1)
0,2 0,0 0
10
20
30
40
50
60
70
Reaction time (h) Fig. 2. Modification yield of photo-responsive rubber materials versus reaction time in dependence on the 2-(anthracene-9-yl) oxirane concentration; (1) 10, (2) 30, (3) 60, (4) 100 and (5) 150 phr (parts per hundred rubber). (The line is a guide to the eye). Table 1 Storage modulus (E0 ) of photo-responsive rubber materials after UV induced crosslinking. Sample
Modification yielda/mol.%
E0 at 23 °C after UV exposure (260 J/cm2)b/MPa
Rubber-0 Rubber-1 Rubber-2 Rubber-3 Rubber-4
0 0.19 0.49 0.86 1.30
2.7 2.7 2.9 3.1 3.3
a b
Determined by 1H NMR experiments. Determined by DMA measurements.
1,7
1,7 1,6 1,5
tan(δ) (-)
1,6
tan(δ) (-)
163 164 165 166 167 168 169 170 171 172 173 174 175 176 177 178 179 180 181 182 183 184 185 186 187 188 189 190 191 192 193 194 195 196 197 198 199 200 201 202 203 204 205 206 207 208 209 210 211 212 213 214 215 216
Modification yield (mol.% of repeating units)
4
1,5
1,4 1,3 1,2 1,1
1,4 -21
-20
-19
-18
-17
-16
-15
-14
temperature (°C)
-13
-12
-11
-14
-12
-10
-8
-6
-4
-2
0
temperature (°C)
Fig. 3. DMA curves of photo-responsive rubber materials upon prolonged UV exposure (λ4 300 nm); (a) (♦) rubber-0, (■) rubber-1, (▲) rubber-2 and (b) () rubber-3.
Fig. 3a and b provide the DMA curves of photo-responsive rubber materials with different modification yields, which have been photochemically crosslinked (λ 4300 nm) at different exposure doses. In addition, Fig. 4 details the DMA curves of rubber-4 in a broad temperature range over prolonged UV exposure (λ4 300 nm). Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
5
tan δ (-)
2,0 217 218 1,8 219 + 1,6 220 1,4 221 222 1,2 223 1,0 224 0,8 225 0,6 226 227 0,4 228 0,2 229 0,0 230 -60 -50 -40 -30 -20 -10 0 10 20 30 40 231 temperature (°C) 232 233 Fig. 4. DMA curves of rubber-4 upon prolonged UV exposure (λ 4300 nm) over a temperature range from 60 to þ 40 °C. 234 Details of the DMA curves in a narrow temperature range are also given in Ref. [1]. 235 236 237 238 239 240 241 242 243 244 245 246 247 248 249 250 251 252 253 254 Fig. 5. DMA curves of rubber-4 over repeated cycles of UV induced crosslinking with 46 J/cm2 (λ 4300 nm, N2) and UV induced 255 cleavage with 9.72 J/cm2 (λ¼ 254 nm, N2) over a temperature range from 60 to þ 40 °C. Details of the DMA curves in a narrow temperature range are also given in Ref. [1]. 256 257 In Fig. 5 the DMA curves of rubber-4 are provided in a broad temperature range over three cycles 258 of photochemical crosslinking and subsequent photochemical cleavage upon deep UV exposure. 259 260 261 Acknowledgments 262 263 The research work of this paper was performed at the Polymer Competence Center Leoben GmbH 264 (PCCL, Austria) within the framework of the COMET-program of the Federal Ministry for Transport, 265 266 Q3 Innovation and Technology and Federal Ministry for Economy, Family and Youth with contributions by the Chair of Chemistry of Polymeric Materials (University of Leoben, Austria). The PCCL is funded 267 by the Austrian Government and the State Governments of Styria, Lower and Upper Austria. 268 T. Griesser and A. Oesterreicher thank the Christian Doppler research association and the Austrian 269 270 Ministry for Economy, Family and Youth (BMWFJ) for financial support.
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i
6
J. Manhart et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
271 Transparency document. Supporting information 272 273 Q4 Transparency data associated with this article can be found in the online version at http://dx.doi. 274 org/10.1016/j.dib.2016.09.023. 275 276 277 Reference 278 279 [1] J. Manhart, S. Ayalur-Karunakaran, S. Radl, A. Oesterreicher, A. Moser, C. Ganser, et al., Design and application of photoreversible elastomer networks by using the [4πsþ 4πs] cycloaddition reaction of pendant anthracene groups, Polymer 280 (2016), http://dx.doi.org/10.1016/j.polymer.2016.08.106.
Please cite this article as: J. Manhart, et al., Data on synthesis and thermo-mechanical properties of stimuli-responsive rubber materials bearing pendant anthracene groups, Data in Brief (2016), http: //dx.doi.org/10.1016/j.dib.2016.09.023i