CN107429491A - 高光泽金属效应纸和板 - Google Patents
高光泽金属效应纸和板 Download PDFInfo
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- CN107429491A CN107429491A CN201680019701.7A CN201680019701A CN107429491A CN 107429491 A CN107429491 A CN 107429491A CN 201680019701 A CN201680019701 A CN 201680019701A CN 107429491 A CN107429491 A CN 107429491A
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- base material
- phenyl
- alkyl
- compound
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 29
- 239000002184 metal Substances 0.000 title claims abstract description 29
- 230000000694 effects Effects 0.000 title description 3
- 239000000203 mixture Substances 0.000 claims abstract description 71
- 239000000463 material Substances 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 49
- 239000011248 coating agent Substances 0.000 claims abstract description 28
- 238000000576 coating method Methods 0.000 claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 238000007711 solidification Methods 0.000 claims abstract description 9
- 230000008023 solidification Effects 0.000 claims abstract description 9
- -1 oxime ester compound Chemical class 0.000 claims description 100
- 150000001875 compounds Chemical class 0.000 claims description 43
- 229920000642 polymer Polymers 0.000 claims description 25
- 150000002576 ketones Chemical class 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 22
- 239000011347 resin Substances 0.000 claims description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 239000012965 benzophenone Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 229920006317 cationic polymer Polymers 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 6
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052753 mercury Inorganic materials 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 4
- 125000002252 acyl group Chemical group 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 3
- 230000009885 systemic effect Effects 0.000 claims description 3
- 239000002537 cosmetic Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 239000005022 packaging material Substances 0.000 claims description 2
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 2
- 241000208125 Nicotiana Species 0.000 claims 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims 1
- 238000007639 printing Methods 0.000 abstract description 33
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- 238000003475 lamination Methods 0.000 abstract description 3
- 238000012856 packing Methods 0.000 abstract description 2
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 42
- 239000000049 pigment Substances 0.000 description 40
- 239000000976 ink Substances 0.000 description 33
- 150000002148 esters Chemical class 0.000 description 25
- 239000001257 hydrogen Substances 0.000 description 24
- 229910052739 hydrogen Inorganic materials 0.000 description 24
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 22
- 239000002904 solvent Substances 0.000 description 20
- 229910052736 halogen Inorganic materials 0.000 description 19
- 150000002367 halogens Chemical class 0.000 description 19
- 150000002431 hydrogen Chemical class 0.000 description 16
- 125000001624 naphthyl group Chemical group 0.000 description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 15
- 239000002253 acid Substances 0.000 description 15
- 229920001577 copolymer Polymers 0.000 description 15
- 229910052740 iodine Chemical class 0.000 description 14
- 239000011630 iodine Chemical class 0.000 description 14
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical class [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 13
- 238000006467 substitution reaction Methods 0.000 description 13
- 125000004642 (C1-C12) alkoxy group Chemical group 0.000 description 11
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 11
- 239000000178 monomer Substances 0.000 description 11
- 125000006552 (C3-C8) cycloalkyl group Chemical group 0.000 description 10
- 239000000853 adhesive Substances 0.000 description 10
- 230000001070 adhesive effect Effects 0.000 description 10
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 10
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 9
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- 125000000217 alkyl group Chemical group 0.000 description 8
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 239000003973 paint Substances 0.000 description 8
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 8
- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 229920002554 vinyl polymer Polymers 0.000 description 8
- 239000003999 initiator Substances 0.000 description 7
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
- 239000002966 varnish Substances 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000012752 auxiliary agent Substances 0.000 description 6
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 6
- 238000005240 physical vapour deposition Methods 0.000 description 6
- 239000004814 polyurethane Substances 0.000 description 6
- 230000005855 radiation Effects 0.000 description 6
- 229920006305 unsaturated polyester Polymers 0.000 description 6
- 125000006710 (C2-C12) alkenyl group Chemical group 0.000 description 5
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 5
- 239000000020 Nitrocellulose Substances 0.000 description 5
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 5
- 239000004305 biphenyl Substances 0.000 description 5
- 235000010290 biphenyl Nutrition 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 5
- 229920001220 nitrocellulos Polymers 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
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- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 4
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- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical class C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 4
- 125000005428 anthryl group Chemical group [H]C1=C([H])C([H])=C2C([H])=C3C(*)=C([H])C([H])=C([H])C3=C([H])C2=C1[H] 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
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- 239000000460 chlorine Substances 0.000 description 4
- 229920001519 homopolymer Polymers 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 4
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 150000002924 oxiranes Chemical class 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 4
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- 125000004765 (C1-C4) haloalkyl group Chemical group 0.000 description 3
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- 239000005864 Sulphur Substances 0.000 description 3
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
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- ZWPWLKXZYNXATK-UHFFFAOYSA-N bis(4-methylphenyl)methanone Chemical class C1=CC(C)=CC=C1C(=O)C1=CC=C(C)C=C1 ZWPWLKXZYNXATK-UHFFFAOYSA-N 0.000 description 3
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- 125000000538 pentafluorophenyl group Chemical group FC1=C(F)C(F)=C(*)C(F)=C1F 0.000 description 3
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 3
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Abstract
本发明涉及一种在纸或板基材上产生明亮光泽的金属涂层的方法。本发明的其他方面是可通过使用该方法获得的纸或板制品,以及该纸或板用于装饰或包装目的的用途。特别地,本发明涉及一种方法,其中将可UV固化的组合物施加/印刷在纸或板基材上,并通过UV/可见光从背面透过纸或板固化。在固化步骤的同时,将涂覆/印刷的纸或板的涂覆/印刷面压在镜面状垫片上。垫片不具有结构,且应具有镜面质量。在第二步骤中,用铝层涂覆/加印该上光和固化的表面。结果是展示出优异的光泽和亮度的金属化表面。
Description
本发明涉及一种在纸或板基材上产生明亮光泽的金属涂层的方法。本发明的其他方面为可通过使用该方法获得的纸或板制品,以及该纸或板用于装饰或包装目的的用途。
目前,纸或板上的金属效应印刷通过例如直接在纸或卡纸板上印刷含溶剂的铝油墨且随后用高光泽UV清漆加印而进行。结果是光泽的表面,然而这与金属镜面状表面的明亮光泽相距甚远。另一方面,明亮光泽是包装行业以及装饰用途的一个重要方面。因此,这些行业中强烈需要非常高光泽的明亮金属化的纸和板。
本发明满足了这一要求,并且为纸和板提供了明亮的金属光泽。
WO 2012/176126涉及一种在纸基材上形成表面浮雕微结构,特别是光变图像(光变装置)的方法。
通过使用该方法,可以在纸基材上快速且精确地复制微结构,例如全息图。
WO 2012/176126中描述的方法用可UV固化的组合物(清漆)进行,将所述组合物施加在纸基材上并且用微结构压印,其中所述组合物在进行压印时用可透过纸固化。
在第二步骤中,任选在UV固化的组合物的至少一部分上沉积透明的高折射率材料层和/或金属层。用于固化的UV灯在UV-A范围内,优选在近VIS范围内表现出发射峰,且所述可UV固化的组合物包含至少一种在UV-A区,优选额外在近VIS范围内吸收的光引发剂。
本发明涉及一种方法,其中将可UV固化的组合物施加/印刷在纸或板基材上,并通过UV/可见光从背面透过纸或板固化。在固化步骤的同时,将涂覆/印刷的纸或板的涂覆/印刷面压在镜面状垫片上。垫片不具有结构,且应具有镜面质量。在第二步中,将该压制和固化的表面用铝层覆盖/加印。结果是展示出优异光泽和亮度的金属化表面。
本发明的一个方面为一种在纸或板基材上形成显示出光泽的光滑表面涂层的方法,包括以下步骤:
A)将可固化组合物施加至纸或板基材的正面的至少一部分上;
B)使所述可固化组合物与垫片接触,同时通过使用设置在纸基材背面的至少一个UV灯固化所述组合物;和
C)在固化的组合物上沉积铝层,
其中所述灯具有处于UV-A范围和近VIS范围内的发射峰,并且所述可固化组合物包含至少一种在UV-A区域且此外在近VIS范围内吸收的光引发剂。
例如在上述方法中,所述可固化组合物包含选自单-和双酰基氧化膦化合物、α-氨基酮型化合物或肟酯化合物及其混合物的光引发剂。
优选地,光引发剂选自单-和双酰基氧化膦化合物及其混合物。
例如,所述可固化组合物包含单-或双酰基氧化膦化合物与二苯甲酮类化合物、α-羟基酮、α-烷氧基酮或α-氨基酮化合物的混合物。
所述灯通常为镓或铁掺杂的中压汞灯。
在另一实施方案中,所述灯为聚焦反射型二极管阵列(FRDA)系统,其具有处于UVA范围的发射,此外还具有400nm以上的发射峰。
本发明通常在印刷装置上进行。
本发明的印刷装置包括:
a)用于将纸基材供应通过该装置的机构,
b)包括液体可UV固化组合物源的涂覆站和用于将液体组合物从所述源施加至基材表面的装置,
d)压光/固化站,其包括用于将涂覆的表面压在镜面状垫片上的装置和用于固化树脂的装置。所述装置设置成使得所述组合物施加至基材的上表面;用于压光表面的装置包括例如安装在金属筒上的镜面状镍板和接触基材的背面并且具有沿与筒旋转轴相同的轴旋转的轴的两个夹紧辊,且用于固化树脂的装置为位于纸基材背面的UV源。
在本发明的上下文中,术语“压光”或“上光”作为同义词使用。其含义是在涂覆的基材上提供非常光滑的表面。
非常重要的是垫片的表面不具有微结构。垫片材料选自镍套筒;安装在金属筒上的镍板或其他金属材料。
优选地,垫片为安装在金属筒上的镍板。
在一个实施方案中,本发明的装置可为离线或独立的单元,或者在替代的优选实施方案中,其可为在线的或者集成体系,其具有其他常规印刷、层压、切割、撕裂和其他转换站作为集成生产工艺的一部分。
在本发明的另一方面中,所述装置可进一步包括具有或不具有加热单元的UV后固化单元,或者仅包括IR加热单元或组合的UV/IR,出于辅助和加速清漆体系固化的目的,这可能是特别推荐的。当离开印刷/固化单元的涂覆基材未完全固化时,可使用该后固化单元。后固化单元确保涂层完全固化。在几乎所有情况下,后固化单元都并非是必需的。
根据本发明,固化透过纸基材,而不是透过垫片进行(位于中空石英筒的孔中的UV源等)。
典型的可固化组合物包含:
(a)1.0-20.0重量%,特别是1.0-15.0重量%,非常特别是3.0-10.0重量%的光引发剂,
(b)99.0-80.0重量%,特别是99.0-85.0重量%,非常特别是97.0-90.0重量%的树脂,
其中组分a)和b)的总和加起来为100%。
在本发明的方法中,使用一种光引发剂或两种或更多种光引发剂的混合物。
在本发明的优选实施方案中,光引发剂选自α-羟基酮型化合物、α-烷氧基酮型化合物、α-氨基酮型化合物、单-和双酰基氧化膦化合物、苯基乙醛酸类化合物、肟酯化合物和盐化合物(锍盐化合物和碘盐化合物)及其混合物。
目前最优选的光引发剂为单-和双酰基氧化膦化合物。单-和双酰基氧化膦化合物可单独使用。或者,可使用单-和双酰基氧化膦化合物的混合物,或者单-和双酰基氧化膦化合物可与其他光引发剂混合使用,所述其他光引发剂例如为二苯甲酮型、α-氨基酮型、α-羟基酮型、缩酮化合物、苯基乙醛酸类化合物、肟酯化合物或盐化合物,特别为二苯甲酮类化合物、α-羟基酮、α-烷氧基酮或α-氨基酮化合物,非常特别为二苯甲酮化合物、α-羟基酮或α-烷氧基酮化合物。如果黄化不是问题,则可单独或与其他光引发剂混合使用α-氨基酮化合物。
光引发剂的实例是本领域技术人员所已知的,例如由Kurt Dietliker在“Acompilation of photoinitiators commercially available for UV today”,SitaTechnology Textbook,Edinburgh,London,2002年中公开。
合适的酰基氧化膦化合物的实例具有式XII:
其中:
R50为未取代的环己基、环戊基、苯基、萘基或联苯基;或者为被一个或多个卤素、C1-C12烷基、C1-C12烷氧基、C1-C12烷硫基或NR53R54取代的环
己基、环戊基、苯基、萘基或联苯基;或者R50为未取代的C1-C20烷基;或者为被一个或多个卤素、C1-C12烷氧基、C1-C12烷硫基、NR53R54或-(CO)-O-C1-C24烷基取代的C1-C20烷基;
R51为未取代的环己基、环戊基、苯基、萘基或联苯基;或者为被一个或多个卤素、C1-C12烷基、C1-C12烷氧基、C1-C12烷硫基或NR53R54取代的环己基、环戊基、苯基、萘基或联苯基;或者R51为-(CO)R’52;或R51为未取代或被一个或多个卤素、C1-C12烷氧基、C1-C12烷硫基或NR53R54取代的C1-C12烷基;
R52和R’52彼此独立地为未取代的环己基、环戊基、苯基、萘基或联苯基;或者为被一个或多个卤素、C1-C4烷基或C1-C4烷氧基取代的环己基、环戊基、苯基、萘基或联苯基;或R52为包含S原子或N原子的5或6元杂环;
R53和R54彼此独立地为氢、未取代的C1-C12烷基或被一个或多个OH或SH取代的C1-C12烷基,其中烷基链任选被1-4个氧原子间隔;或者R53和R54彼此独立地为C2-C12链烯基、环戊基、环己基、苄基或苯基;
具体实例为双(2,4,6-三甲基苯甲酰基)苯基氧化膦(819);2,4,6-三甲基苯甲酰基二苯基氧化膦(TPO);(2,4,6-三甲基苯甲酰基苯基)次膦酸乙酯;(2,4,6-三甲基苯甲酰基)-2,4-二戊氧基苯基氧化膦;双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基戊基氧化膦。
此外,感兴趣的还有式XII化合物与式XI化合物的混合物以及不同式XII化合物的混合物。
实例为双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基戊基氧化膦与1-羟基环己基苯基酮的混合物,双(2,4,6-三甲基苯甲酰基)苯基氧化膦与2-羟基-2-甲基-1-苯基丙-1-酮的混合物,双(2,4,6-三甲基苯甲酰基)苯基氧化膦与(2,4,6-三甲基苯甲酰基苯基)次膦酸乙酯的混合物等。
合适的二苯甲酮类化合物的实例具有式X的化合物:
其中:
R65,R66和R67彼此独立地为氢、C1-C4烷基、C1-C4卤代烷基、C1-C4烷氧基、Cl或N(C1-C4烷基)2;
R68为氢、C1-C4烷基、C1-C4卤代烷基、苯基、N(C1-C4烷基)2、COOCH3、
Q为具有2-6个羟基的多羟基化合物的残基;
x为大于1但不大于Q中可用羟基数的数;
A为-[O(CH2)bCO]y-或-[O(CH2)bCO](y-1)-[O(CHR71CHR70)a]y-;
R69为氢、甲基或乙基;如果N大于1,则基团R69可彼此相同或不同;
a为1-2的数;
b为4-5的数;
y为1-10的数;
n为1-5的数;且
m为2-10的整数。
具体实例为BP(=二苯甲酮),可获自Lamberti的Esacure(2,4,6-三甲基二苯甲酮和4-甲基二苯甲酮的混合物),4-苯基二苯甲酮,4-甲氧基二苯甲酮,4,4'-二甲氧基二苯甲酮,4,4'-二甲基二苯甲酮,4,4'-二氯二苯甲酮,4,4'-二甲氨基二苯甲酮,4,4'-二乙氨基二苯甲酮,4-甲基二苯甲酮,2,4,6-三甲基二苯甲酮,4-(4-甲硫基苯基)二苯甲酮,3,3'-二甲基-4-甲氧基二苯甲酮,2-苯甲酰基苯甲酸甲酯,4-(2-羟基乙硫基)二苯甲酮,4-(4-甲苯硫基)二苯甲酮,4-苯甲酰基-N,N,N-三甲基氯化苯甲铵,2-羟基-3-(4-苯甲酰基苯氧基)-N,N,N-三甲基-1-氯化丙铵一水合物,4-(13-丙烯酰基-1,4,7,10,13-五氧杂十三烷基)二苯甲酮,4-苯甲酰基-N,N-二甲基-N-[2-(1-氧代-2-丙烯基)氧基]乙基氯化苯甲铵;[4-(2-羟基乙硫基)-苯基]-(4-异丙基苯基)甲酮;联苯基-[4-(2-羟基乙硫基)-苯基]甲酮;联苯-4-基苯基甲酮;联苯-4-基对甲苯基甲酮;联苯-4-基间甲苯基甲酮;[4-(2-羟基乙硫基)-苯基]对甲苯基甲酮;[4-(2-羟基乙硫基)-苯基]-(4-异丙基苯基)甲酮;[4-(2-羟基乙硫基)-苯基]-(4-甲氧基苯基)甲酮;1-(4-苯甲酰基苯氧基)丙-2-酮;[4-(2-羟基乙硫基)-苯基]-(4-苯氧基苯基)甲酮;3-(4-苯甲酰基苯基)-2-二甲氨基-2-甲基-1-苯基丙-1-酮;(4-氯苯基)-(4-辛硫基苯基)-甲酮;(4-氯苯基)-(4-辛硫基苯基)甲酮;(4-氯苯基)-(4-十二烷硫基苯基)甲酮;(4-溴苯基)-(4-辛硫基苯基)甲酮;(4-十二烷硫基苯基)-(4-甲氧基苯基)甲酮;(4-苯甲酰基苯氧基)乙酸甲酯;联苯基-[4-(2-羟基乙硫基)-苯基]甲酮;1-[4-(4-苯甲酰基苯硫基)-苯基]-2-甲基-2-(4-甲基苯基磺酰基)丙-1-酮(可由Lamberti获得的1001)。
合适的α-羟基酮、α-烷氧基酮或α-氨基酮化合物的实例具有式(XI):
其中:
R29为氢或C1-C18烷氧基;
R30为氢、C1-C18烷基、C1-C12羟烷基、C1-C18烷氧基、OCH2CH2-OR34、吗啉代、S-C1-C18烷基,基团-HC=CH2、C(CH3)=CH2、
d,e和f为1-3;
c为2-10;
G1和G2彼此独立地为聚合物结构的端基,优选为氢或甲基;
R34为氢、
R31为羟基、C1-C16烷氧基、吗啉代、二甲氨基或-O(CH2CH2O)g-C1-C16烷基;
g为1-20;
R32和R33彼此独立地为氢、C1-C6烷基、C1-C16烷氧基或-O(CH2CH2O)g-C1-C16烷基;或者为未取代的苯基或苄基;或者为被C1-C12烷基取代的苯基或苄基;或者R32和R33与它们所连接的碳原子一起形成环己基环;
R35为氢、OR36或NR37R38;
R36为氢、任选被一个或多个非连续O原子间隔的C1-C12烷基,且未被间隔或被间隔的C1-C12烷基任选被一个或多个OH取代;或者R36为
R37和R38彼此独立地为氢或未取代或被一个或多个OH取代的C1-C12烷基;
R39为任选被一个或多个非连续O间隔的C1-C12亚烷基,-(CO)-NH-C1-C12亚烷基-NH-(CO)-或
条件是R31、R32和R33并不全部一起为C1-C16烷氧基或-O(CH2CH2O)g-C1-C16烷基。
具体实例为1-羟基环己基苯基酮(184)或500(184与二苯甲酮的混合物),2-甲基-1-[4-(甲硫基)苯基]-2-吗啉代丙-1-酮(907),2-苄基-2-二甲氨基-1-(4-吗啉代苯基)-丁-1-酮(369),2-二甲氨基-2-(4-甲基苄基)-1-(4-吗啉-4-基苯基)-丁-1-酮(379),(3,4-二甲氧基苯甲酰基)-1-苄基-1-二甲氨基丙烷,1-[4-(2-羟基乙氧基)苯基]-2-羟基-2-甲基-1-丙-1-酮(2959),2,2-二甲氧基-1,2-二苯基乙-1-酮(651),2-羟基-2-甲基-1-苯基丙-1-酮(1173),2-羟基-1-{4-[4-(2-羟基-2-甲基丙酰基)-苄基]-苯基}-2-甲基丙-1-酮(127),2-羟基-1-{4-[4-(2-羟基-2-甲基丙酰基)-苯氧基]-苯基}-2-甲基丙-1-酮,由Lamberti提供的Esacure KIP,2-羟基-1-{1-[4-(2-羟基-2-甲基丙酰基)-苯基]-1,3,3-三甲基茚满-5-基}-2甲基-丙-1-酮。
和产品可从BASF SE获得。
合适的苯基乙醛酸化合物的实例具有式XIII:
其中:
R60为氢、C1-C12烷基或
R55,R56,R57,R58和R59彼此独立地为氢,未取代的C1-C12烷基或被一个或多个OH、C1-C4烷氧基、苯基、萘基、卤素或CN取代的C1-C12烷基;其中烷基链任选被一个或多个氧原子间隔;或R55,R56,R57,R58和R59彼此独立地为C1-C4烷氧基、C1-C4烷硫基或NR52R53;
R52和R53彼此独立地为氢,未取代的C1-C12烷基或被一个或多个OH或SH取代的C1-C12烷基,其中烷基链任选被1-4个氧原子间隔;或R52和R53彼此独立地为C2-C12链烯基、环戊基、环己基、苄基或苯基;且
Y1为任选被一个或多个氧原子间隔的C1-C12亚烷基。
式XIII化合物的具体实例为氧代苯基乙酸2-[2-(2-氧代-2-苯基乙酰氧基)-乙氧基]乙基酯(754),α-氧代苯乙酸甲酯。
合适的肟酯化合物的实例具有式XIV:
其中:
z为0或1;
R70为氢、C3-C8环烷基;未取代或被一个或多个卤素、苯基或CN取代的C1-C12烷基;或者R70为C2-C5链烯基;未取代或被一个或多个C1-C6烷基、卤素、CN、OR73、SR74或NR75R76取代的苯基;或者R70为C1-C8烷氧基,苄氧基;或未取代或被一个或多个C1-C6烷基或卤素取代的苯氧基;
R71为苯基、萘基、苯甲酰基或萘甲酰基,其各自被一个或多个卤素、C1-C12烷基、C3-C8环烷基、苄基、苯氧基羰基、C2-C12烷氧基羰基、OR73、SR74、SOR74、SO2R74或NR75R76取代,其中取代基OR73、SR74和NR75R76任选经由基团R73、R74、R75和/或R76与苯基或萘基环上的其他取代基形成5或6元环;或者其各自被苯基或被一个或多个OR73、SR74或NR75R66取代的苯基取代;或者R71为噻吨基,或
R72为氢;未取代的C1-C20烷基或被一个或多个卤素、OR73、SR74、C3-C8环烷基或苯基取代的C1-C20烷基;或者为C3-C8环烷基;或者为未取代或被一个或多个C1-C6烷基、苯基、卤素、OR73、SR74或NR75R76取代的苯基;或者为未取代或被一个或多个C1-C6烷基、苯基、OR73、SR74或NR75R76取代的C2-C20烷酰基或苯甲酰基;或者为C2-C12烷氧基羰基、苯氧基羰基、CN、CONR75R76、NO2、C1-C4卤代烷基、S(O)y-C1-C6烷基或S(O)y-苯基;
y为1或2;
Y2为直接键或无键;
Y3为NO2或
R73和R74彼此独立地为氢,C1-C20烷基,C2-C12链烯基,C3-C8环烷基,被一个或多个,优选2个O间隔的C3-C8环烷基,苯基-C1-C3烷基;或者为被OH、SH、CN、C1-C8烷氧基、C1-C8烷酰基、C3-C8环烷基或间隔有一个或多个O的C3-C8环烷基取代的C1-C8烷基,或者所述C1-C8烷基被未取代或被一个或多个C1-C8烷基、卤素、OH、C1-C4烷氧基或被C1-C4烷硫基取代的苯甲酰基取代;或者为苯基或萘基,其各自未取代的或被卤素、C1-C12烷基、C1-C12烷氧基、苯基-C1-C3烷氧基、苯氧基、C1-C12烷硫基、苯硫基、N(C1-C12烷基)2,二苯基氨基或取代;
R75和R76彼此独立地为氢、C1-C20烷基、C2-C4羟烷基、C2-C10烷氧基烷基、C2-C5链烯基、C3-C8环烷基、苯基-C1-C3烷基、C1-C8烷酰基、C3-C12链烯酰基、苯甲酰基;或者为苯基或萘基,其各自未取代或者被C1-C12烷基、苯甲酰基或C1-C12烷氧基取代;或者R75和R76彼一起为任选被O或NR73间隔并且任选被羟基、C1-C4烷氧基、C2-C4烷酰氧基或苯甲酰氧基取代的C2-C6亚烷基;
R77为C1-C12烷基、噻吩基或苯基,其未取代或被C1-C12烷基、OR73、吗啉代或N-咔唑基取代。
具体实例为1,2-辛二酮1-[4-(苯硫基)苯基]-2-(O-苯甲酰肟)(OXE01),乙酮1-[9-乙基-6-(2-甲基苯甲酰基)-9H-咔唑-3-基]-1-(O-乙酰肟)(OXE02),9H-噻吨-2-甲醛-9-氧代-2-(O-乙酰肟),乙酮1-[9-乙基-6-(4-吗啉代苯甲酰基)-9H-咔唑-3-基]-1-(O-乙酰肟),乙酮1-[9-乙基-6-(2-甲基-4-(2-(1,3-二氧代-2-二甲基环戊-5-基)乙氧基)-苯甲酰基)-9H-咔唑-3-基]-1-(O-乙酰肟)(Adeka N-1919),乙酮1-[9-乙基-6-硝基-9H-咔唑-3-基]-1-[2-甲基-4-(1-甲基-2-甲氧基)乙氧基)苯基]-1-(O-乙酰肟)(Adeka NCI831)等。
还可加入阳离子光引发剂,例如过氧化苯甲酰(其他合适的过氧化物描述在US4950581第19栏第17-25行中),或芳族锍,或碘盐,例如如US4950581第18栏第60行至第19栏第10行所述。
合适的锍盐化合物具有式XVa,XVb,XVc,XVd或XVe:
其中:
R80,R81和R82各自独立地为其他未取代的苯基或被-S-苯基、取代的苯基;
R83为直接键,S,O,CH2,(CH2)2,CO或NR89;
R84,R85,R86和R87彼此独立地为氢、C1-C20烷基、C3-C8环烷基、C1-C20烷氧基、C2-C20链烯基、CN、OH、卤素、C1-C6烷硫基、苯基、萘基、苯基-C1-C7烷基、萘基-C1-C3烷基、苯氧基、萘氧基、苯基-C1-C7烷氧基、萘基-C1-C3烷氧基、苯基-C2-C6链烯基、萘基-C2-C4链烯基、S-苯基、
(CO)R89、O(CO)R89、(CO)OR89、SO2R89或OSO2R89;
R88为C1-C20烷基、C1-C20羟烷基、
R89为氢、C1-C12烷基、C1-C12羟烷基、苯基、萘基或联苯基;
R90,R91,R92和R93彼此独立地具有对R84所给的含义之一;或R90和R91连接,从而与它们所连接的苯环形成稠合环体系;
R95为直接键、S、O或CH2;
R96为氢、C1-C20烷基;被一个或多个O间隔的C2-C20烷基;或者为–L-M-R98或-L-R98;
R97具有对R96所给的含义之一或者为
R98为单价敏化剂或光引发剂结构部分;
Ar1和Ar2彼此独立地为未取代或被C1-C20烷基、卤素或OR99取代的苯基;或者为未取代的萘基、蒽基、菲基或联苯基;或者为被C1-C20烷基、OH或OR99取代的萘基、蒽基、菲基或联苯基;或者为-Ar4-A1-Ar3或
Ar3为未取代的苯基、萘基、蒽基、菲基或联苯基;或者为被C1-C20烷基、OR99或苯甲酰基取代的苯基、萘基、蒽基、菲基或联苯基;
Ar4为亚苯基、亚萘基、亚蒽基或亚菲基;
A1为直接键、S、O或C1-C20亚烷基;
X为CO、C(O)O、OC(O)、O、S或NR99;
L为直接键、S、O、C1-C20亚烷基或被一个或多个非连续O间隔的C2-C20亚烷基;
R99为C1-C20烷基或C1-C20羟烷基;或者为被O(CO)R102取代的C1-C20烷基;
M1为S、CO或NR100;
M2是直接键、CH2、O或S;
R100和R101彼此独立地为氢、卤素、C1-C8烷基、C1-C8烷氧基或苯基;
R102为C1-C20烷基;
R103为且
E为阴离子,特别为PF6、SbF6、AsF6、BF4、(C6F5)4B、Cl、Br、HSO4、CF3-SO3、F-SO3、CH3-SO3、ClO4、PO4、NO3、SO4、CH3-SO4或
锍盐化合物的具体实例例如为270(BASF SE);UVI-6990,UVI-6974(Union Carbide),KI 85(Degussa),SP-55,SP-150,SP-170(Asahi Denka),GE UVE 1014(General Electric),KI-85(=三芳基锍六氟磷酸盐;Sartomer),CD 1010(=混合三芳基锍六氟锑酸盐;Sartomer);CD 1011(=混合三芳基锍六氟磷酸盐;Sartomer)。
合适的碘盐化合物具有式XVI:
其中:
R110和R111各自独立地为氢、C1-C20烷基、C1-C20烷氧基、OH取代的C1-C20烷氧基、卤素、C2-C12链烯基、C3-C8环烷基,特别为甲基、异丙基或异丁基;且
E为阴离子,尤其为PF6、SbF6、AsF6、BF4、(C6F5)4B、Cl、Br、HSO4、CF3-SO3、F-SO3、CH3-SO3、ClO4、PO4、NO3、SO4、CH3-SO4或
碘盐化合物的具体实例例如为甲苯基枯基碘四(五氟苯基)硼酸盐,4-[(2-羟基十四烷氧基)苯基]苯基碘六氟锑酸盐或六氟磷酸盐,甲苯基枯基碘六氟磷酸盐,4-异丙基苯基-4'-甲基苯基碘六氟磷酸盐,4-异丁基苯基-4'-甲基苯基碘六氟磷酸盐(250,BASF SE),4-辛氧基苯基苯基碘六氟磷酸盐或六氟锑酸盐,双(十二烷基苯基)碘六氟锑酸盐或六氟磷酸盐,双(4-甲基苯基)碘六氟磷酸盐,双(4-甲氧基苯基)碘六氟磷酸盐,4-甲基苯基-4'-乙氧基苯基碘六氟磷酸盐,4-甲基苯基-4'-十二烷基苯基碘六氟磷酸盐,4-甲基苯基-4'-苯氧基苯基碘六氟磷酸盐。
在提及的所有碘盐中,具有其他阴离子的化合物当然也是合适的。碘盐的制备是本领域技术人员已知的并且例如描述在文献US 4151175,US 3862333,US 4694029,EP562897,US 4399071,US 6306555,WO 98/46647;J.V.Crivello,“PhotoinitiatedCationic Polymerization”,UV Curing:Science and Technology,编辑S.P.Pappas,第24-77页;Technology Marketing Corporation,Norwalk,Conn.1980,ISBN号0-686-23773-0;J.V.Crivello,J.H.W.Lam,Macromolecules,10,1307(1977)和J.V.Crivello,Ann.Rev.Mater.Sci.1983,13,第173-190页和J.V.Crivello,Journal of PolymermerScience,Part A:Polymer Chemistry,第37卷,4241-4254(1999)中。
卤素为氟、氯、溴和碘。
可能的话,C1-C24烷基(C1-C20烷基,尤其是C1-C12烷基)通常为直链或支化的。实例为甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、正戊基、2-戊基、3-戊基、2,2-二甲基丙基、1,1,3,3-四甲基戊基、正己基、1-甲基己基、1,1,3,3,5,5-六甲基己基、正庚基、异庚基、1,1,3,3-四甲基丁基、1-甲基庚基、3-甲基庚基、正辛基、1,1,3,3-四甲基丁基和2-乙基己基、正壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基或十八烷基。C1-C8烷基通常为甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、正戊基、2-戊基、3-戊基、2,2-二甲基丙基、正己基、正庚基、正辛基、1,1,3,3-四甲基丁基和2-乙基己基。C1-C4烷基通常为甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基。
C2-C12链烯基(C2-C5链烯基)基团为直链或支化链烯基,例如乙烯基、烯丙基、甲代烯丙基、异丙烯基、2-丁烯基、3-丁烯基、异丁烯基、正戊-2,4-二烯基、3-甲基-丁-2-烯基、正辛-2-烯基或正十二碳-2-烯基。
C1-C12烷氧基(C1-C8烷氧基)为直链或支化烷氧基,例如甲氧基、乙氧基、正丙氧基、异丙氧基、正丁氧基、仲丁氧基、叔丁氧基、戊氧基、异戊氧基或叔戊氧基、庚氧基、辛氧基、异辛氧基、壬氧基、癸氧基、十一烷氧基和十二烷氧基。
C1-C12烷硫基(C1-C8烷硫基)为直链或支化烷硫基,且具有与烷氧基相同的优选方案,除了氧与硫交换之外。
C1-C12亚烷基为二价C1-C12烷基,即具有两个(而不是一个)自由价态的烷基,例如三亚甲基或四亚甲基。
环烷基通常为C3-C8环烷基,例如环戊基、环己基、环庚基或环辛基,其可为未取代的或取代的。
在数种情况下,有利的是除了光引发剂之外使用敏化剂化合物。合适的敏化剂化合物的实例公开在WO 06/008251第36页第30行至第38页第8行中,其公开内容通过引用并入本文。作为敏化剂,尤其可使用上文所述的二苯甲酮类化合物。
本发明方法和装置中使用的灯具有处于UV-A范围(400-320nm)和短波长可见光谱(400-450nm)内的发射峰。即,灯的发射峰处于320-450nm的范围内。
本发明前文和权利要求中使用的术语“近VIS范围”意指短波长可见光谱(400-450nm)。
UV辐射通常分为UV-A、UV-B和UV-C,如下所示:UV-A:400-320nm;UV-B:320-290nm;UV-C:290-100nm。
可使用任何紫外光源作为辐射源,例如高压或低压汞灯、冷阴极管、黑光、紫外LED、紫外激光和闪光。
可用于本发明方法中的灯的实例如下所示:
-通过以小比例引入金属卤化物来改变光谱输出的中压汞弧:
-铁掺杂的—光谱输出偏移至350-450nm;
-镓掺杂的—发射非常少的UV;在紫色和蓝色光谱区域中发射(通过用金属碘化物掺杂汞弧来在如下波长(nm)处获得预期的额外UV线:镓(Ga)403、417;铁(Fe)358、372、374/5、382、386、388);和
-聚焦反射型二极管阵列(FRDA)系统(igb-tech GmbH),例如具有约400nm发射峰的FRDA 202。也可使用多光谱灯。
有利地,在本发明的方法和装置中使用镓或铁掺杂的中压汞弧来更有效地产生UV-A(315-400nm)或UV-B(280-315nm),并提供更好的辐射效率范围和更高的固化。这些灯还在近VIS范围内表现出一部分发射。
各辐射器由铝壳体组成,其包含具有椭圆形(或根据应用,为抛物线形)横截面的线性反射器。与辐照器壳体相连的反射器由特殊的铝制成,其具有高UV反射率以及耐晦暗性和耐腐蚀性。
所用的光引发剂或光引发剂混合物和灯必须根据特定纸张类型进行优化,以达到最佳印刷速度。
所述可UV固化的组合物(通常为涂料或漆)通常可通过凹版印刷、柔性版印刷、喷墨印刷、胶版印刷和丝网印刷方法以及通过涂覆方法沉积。可固化漆通过紫外(UV)光固化。UV固化漆可由BASF SE获得。本发明所用的暴露于光化辐射的漆需要在它们再次与垫片分离时达到固化阶段。特别适用于所述漆组合物的是工业涂装和印刷领域的可辐射固化工业中使用的化学物质。特别合适的是含有一种或数种光潜催化剂的组合物,所述催化剂引发暴露于UV辐射的漆层聚合。特别适用于快速固化和转化成固态的组合物是包含一种或数种对自由基聚合敏感的单体和低聚物,例如丙烯酸酯、甲基丙烯酸酯或含有至少一个烯属不饱和基团的单体或/和低聚物的组合物。
不饱和化合物可含有一个或多个烯属双键。它们可具有低(单体)或高(低聚)分子量。包含双键的单体的实例为烷基、羟烷基或氨基丙烯酸酯,或烷基、羟烷基或氨基甲基丙烯酸酯,例如丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯或丙烯酸2-羟乙酯、丙烯酸异冰片酯、甲基丙烯酸甲酯或甲基丙烯酸乙酯。硅酮丙烯酸也是有利的。其他实例为丙烯腈,丙烯酰胺,甲基丙烯酰胺,N-取代的(甲基)丙烯酰胺,乙烯基酯如乙酸乙烯酯,乙烯基醚如异丁基乙烯基醚,苯乙烯,烷基-和卤代苯乙烯,N-乙烯基吡咯烷酮,氯乙烯或偏二氯乙烯。
含有两个或更多个双键的单体的实例为乙二醇、丙二醇、新戊二醇、六亚甲基二醇或双酚A的二丙烯酸酯和4,4'-双(2-丙烯酰氧基乙氧基)二苯基丙烷,三羟甲基丙烷三丙烯酸酯,季戊四醇三丙烯酸酯或四丙烯酸酯,丙烯酸乙烯酯,二乙烯基苯,琥珀酸二乙烯基酯,邻苯二甲酸二烯丙基酯,磷酸三烯丙基酯,异氰脲酸三烯丙基酯或三(2-丙烯酰基乙基)异氰脲酸酯。
较高分子量(低聚物)的多不饱和化合物的实例为丙烯酸酯化的环氧树脂,含丙烯酸酯、乙烯基醚或环氧基的聚酯,以及聚氨酯和聚醚。不饱和低聚物的其他实例为不饱和聚酯树脂,其通常由马来酸、邻苯二甲酸和一种或多种二醇制备且分子量为约500-3000。此外,还可使用乙烯基醚单体和低聚物,以及具有聚酯、聚氨酯、聚醚、聚乙烯基醚和环氧主链的马来酸酯封端的低聚物。特别合适的是WO90/01512中所述的带有乙烯基醚基团的低聚物与聚合物的组合。然而,乙烯基醚和马来酸官能化的单体的共聚物也是合适的。该类不饱和低聚物也可称为预聚物。
特别合适的实例为烯属不饱和羧酸和多元醇或聚环氧化物的酯,以及在链或侧基中具有烯属不饱和基团的聚合物,例如不饱和聚酯、聚酰胺和聚氨酯及其共聚物,在侧链中含有(甲基)丙烯酸基团的聚合物和共聚物,以及一种或多种该类聚合物的混合物。
不饱和羧酸的实例为丙烯酸、甲基丙烯酸、巴豆酸、衣康酸、肉桂酸和不饱和脂肪酸如亚麻酸或油酸。优选丙烯酸和甲基丙烯酸。
合适的多元醇是芳族的,特别是脂族和脂环族多元醇。芳族多元醇的实例为氢醌、4,4'-二羟基联苯、2,2-二(4-羟基苯基)丙烷,以及线型酚醛清漆和甲阶酚醛树脂。聚环氧化物的实例为基于上述多元醇,特别是芳族多元醇和表氯醇的那些。其他合适的多元醇为在聚合物链或侧基中含有羟基的聚合物和共聚物,例如聚乙烯醇及其共聚物或聚甲基丙烯酸羟烷基酯或其共聚物。合适的其他多元醇为具有羟基端基的低聚酯。
脂族和脂环族多元醇的实例为优选具有2-12个碳原子的亚烷基二醇,例如乙二醇,1,2-或1,3-丙二醇,1,2-、1,3-或1,4-丁二醇,戊二醇,己二醇,辛二醇,十二烷二醇,二甘醇,三甘醇,分子量优选为200-1500的聚乙二醇,1,3-环戊二醇,1,2-、1,3-或1,4-环己二醇,1,4-二羟基甲基环己烷,甘油,三(β-羟乙基)胺,三羟甲基乙烷,三羟甲基丙烷,季戊四醇,二季戊四醇和山梨糖醇。
多元醇可用一种羧酸或不同的不饱和羧酸部分或完全酯化,而在偏酯中,游离羟基可被改性,例如醚化或用其他羧酸酯化。
酯的实例为:三羟甲基丙烷三丙烯酸酯,三羟甲基乙烷三丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、三羟甲基乙烷三甲基丙烯酸酯、四亚甲基二醇二甲基丙烯酸酯、三甘醇二甲基丙烯酸酯、四甘醇二丙烯酸酯、季戊四醇二丙烯酸酯、季戊四醇三丙烯酸酯、季戊四醇四丙烯酸酯、二季戊四醇二丙烯酸酯、二季戊四醇三丙烯酸酯、二季戊四醇四丙烯酸酯、二季戊四醇五丙烯酸酯、二季戊四醇六丙烯酸酯、三季戊四醇八丙烯酸酯、季戊四醇二甲基丙烯酸酯、季戊四醇三甲基丙烯酸酯、二季戊四醇二甲基丙烯酸酯、二季戊四醇四甲基丙烯酸酯、三季戊四醇八甲基丙烯酸酯、季戊四醇二衣康酸酯、二季戊四醇三衣康酸酯、二季戊四醇五衣康酸酯、二季戊四醇六衣康酸酯、乙二醇二丙烯酸酯、1,3-丁二醇二丙烯酸酯、1,3-丁二醇二甲基丙烯酸酯、1,4-丁二醇二衣康酸酯、山梨糖醇三丙烯酸酯、山梨糖醇四丙烯酸酯、季戊四醇改性的三丙烯酸酯、山梨糖醇四甲基丙烯酸酯、山梨糖醇五丙烯酸酯、山梨糖醇六丙烯酸酯、低聚酯丙烯酸酯和甲基丙烯酸酯、甘油二丙烯酸酯和三丙烯酸酯、1,4-环己烷二丙烯酸酯、分子量为200-1500的聚乙二醇的双丙烯酸酯和双甲基丙烯酸酯,或其混合物。
还适合作为可聚合组分的是相同或不同的不饱和羧酸与优选具有2-6个,特别是2-4个氨基的芳族、脂环族和脂族多胺的酰胺。该类多胺的实例为乙二胺,1,2-或1,3-丙二胺,1,2-、1,3-或1,4-丁二胺,1,5-戊二胺,1,6-己二胺,辛二胺,十二烷基二胺,1,4-二氨基环己烷,异佛尔酮二胺,苯二胺,双苯二胺,二-β-氨基乙基醚,二亚乙基三胺,三亚乙基四胺,二(β-氨基乙氧基)-或二(β-氨基丙氧基)乙烷。其他合适的多胺为聚合物和共聚物,优选在侧链中具有额外的氨基,和具有氨基端基的低聚酰胺。该类不饱和酰胺的实例为亚甲基双丙烯酰胺、1,6-六亚甲基双丙烯酰胺、二亚乙基三胺三甲基丙烯酰胺、双(甲基丙烯酰胺基丙氧基)乙烷、甲基丙烯酸β-甲基丙烯酰胺基乙基酯和N-[(β-羟基乙氧基)乙基]丙烯酰胺。
合适的不饱和聚酯和聚酰胺例如衍生自马来酸和二醇或二胺。一些马来酸可被其他二羧酸代替。它们可与烯属不饱和共聚单体,例如苯乙烯一起使用。聚酯和聚酰胺也可衍生自二羧酸和烯属不饱和二醇或二胺,尤其是衍生自具有例如6-20个C原子的较长链的那些。聚氨酯的实例为由饱和或不饱和二异氰酸酯和不饱和或分别地饱和二醇组成的那些。
在侧链中具有(甲基)丙烯酸酯基团的聚合物同样是已知的。它们可例如为基于线型酚醛清漆的环氧树脂与(甲基)丙烯酸的反应产物,或者可为乙烯醇或用(甲基)丙烯酸酯化的其羟烷基衍生物的均聚物或共聚物,或者可为用(甲基)丙烯酸羟烷基酯酯化的(甲基)丙烯酸酯的均聚物或共聚物。
在侧链中具有丙烯酸酯或甲基丙烯酸酯基团的其他合适的聚合物例如为溶剂可溶性或碱可溶性聚酰亚胺前体,例如具有与分子中的主链或酯基连接的可光聚合侧基的聚(酰胺酸酯)化合物,即根据EP624826。该类低聚物或聚合物可与任选的反应性稀释剂如多官能(甲基)丙烯酸酯一起配制,以制备高度敏感的聚酰亚胺前体抗蚀剂。
可聚合组分的实例还有在分子结构内具有至少两个烯属不饱和基团和至少一个羧基官能团的聚合物或低聚物,例如通过饱和或不饱和多元酸酐与环氧化合物和不饱和一元羧酸的反应的产物反应获得的树脂,例如JP 10-301276中所述的光敏化合物和商业产品如EB9696,UCB Chemicals;Nippon Kayaku Co.,LTD.的KAYARAD TCR1025,获自Shin-Nakamura Chemical Co.,Ltd.的NK OLIGO EA-6340、EA-7440;或在含羧基的树脂和具有α,β-不饱和双键和环氧基的不饱和化合物之间形成的加成产物(例如ACA200M,DaicelIndustries,Ltd.)。作为可聚合组分实例的其他商业产品是获自Daicel ChemicalIndustries,Ltd.的ACA200、ACA210P、ACA230AA、ACA250、ACA300、ACA320。
可光聚合化合物可单独使用或以任何所需的混合物使用。优选使用多元醇(甲基)丙烯酸酯的混合物。优选的组合物包含至少一种具有至少一个游离羧基的化合物。
作为稀释剂,单或多官能烯属不饱和化合物或数种所述化合物的混合物可以以基于组合物的固体部分为至多70重量%的量包含在上述组合物中。
可聚合组合物可额外包含溶剂。溶剂可为酯/醇混合物,优选为乙酸正丙酯和乙醇。更优选地,酯/醇混合物的比例为10:1-40:1,甚至更优选为20:1-30:1。所用溶剂可包含任何一种或多种酯,例如乙酸正丙酯、乙酸异丙酯、乙酸乙酯、乙酸丁酯;醇,如乙醇、工业用甲醇变性酒精、异丙醇或正丙醇;酮,如甲基乙基酮或丙酮;芳族烃,如甲苯;和水。
尽管水可单独用作稀释剂,但是在大多数情况下,其与有机溶剂如醇一起使用。
本发明还提供了包含至少一种乳化或溶解在水或有机溶剂中的烯属不饱和的可光聚合化合物作为可聚合组分的组合物。
不饱和可聚合组分也可与不可光聚合的成膜组分混合使用。这些可例如为有机溶剂中的物理干燥聚合物或其溶液,例如硝化纤维素或乙酰丁酸纤维素。然而,其也可为可化学和/或热固化的树脂,例如多异氰酸酯、聚环氧化物和三聚氰胺树脂,以及聚酰亚胺前体。同时使用可热固化的树脂对用于称为混杂体系的体系中是重要的,其在第一阶段中光聚合,在第二阶段中通过热后处理来交联。
将光引发剂或光引发剂的混合物引入配制剂中以引发UV固化过程。
例如,可固化组合物(UV漆)包含:
(a)1.0-20.0重量%,特别是1.0-15.0重量%,非常特别是3.0-10.0重量%的光引发剂,
(b)99.0-80.0重量%,特别是99.0-85.0重量%,非常特别是97.0-90.0重量%的树脂(可聚合的组分),
其中组分a)和b)的总和加起来为100%。
可固化组合物可包含各种添加剂。其实例包括热抑制剂、光稳定剂、荧光增白剂、填料和颜料,以及白色和彩色颜料、染料、抗静电剂、粘合增进剂、润湿剂、流动助剂、润滑剂、蜡、抗粘剂、分散剂、乳化剂、抗氧化剂;填料,例如滑石、石膏、硅酸、金红石、炭黑、氧化锌、铁氧化物;反应促进剂、增稠剂、消光剂、消泡剂、流平剂和通常用于例如漆、油墨和涂料技术中的其他助剂。
UV漆可包含Sartomer Europe系列或BASF SE(10-60%)的系列的环氧丙烯酸酯(10-60%)和一种或数种获自Sartomer Europe或BASF SE的丙烯酸酯(单官能和多功能)单体(20-90%)和一种或数种光引发剂(1-15%),例如819(BASF SE),和流平剂如获自BYK Chemie的361(0.01-1%)。
在本发明的另一实施方案中,紫外涂料可着色。即,可固化组合物可包含颜料和/或染料。颜料可为透明有机彩色颜料或无机颜料。
合适的彩色颜料尤其包括选自如下的有机颜料:偶氮、偶氮甲碱、次甲基、蒽醌、酞菁、培利酮(perinone)、苝、二酮吡咯并吡咯、硫靛、二嗪亚氨基异吲哚啉、二嗪、亚氨基异吲哚啉酮、喹吖啶酮、黄烷士酮、阴丹酮、蒽素嘧啶和喹酞酮颜料,或其混合物或固溶体;尤其是二嗪、二酮吡咯并吡咯、喹吖啶酮、酞菁、阴丹酮或亚氨基异吲哚啉酮颜料,或其混合物或固溶体。
特别感兴趣的彩色颜料包括C.I.颜料红202、C.I.颜料红122、C.I.颜料红179、C.I.颜料红170、C.I.颜料红144、C.I.颜料红177、C.I.颜料红254、C.I.颜料红255、C.I.颜料红264、C.I.颜料棕23、C.I.颜料黄109、C.I.颜料黄110、C.I.颜料黄147、C.I.颜料橙61、C.I.颜料橙71、C.I.颜料橙73、C.I.颜料橙48、C.I.颜料橙49、C.I.颜料蓝15、C.I.颜料蓝60、C.I.颜料紫23、C.I.颜料紫37、C.I.颜料紫19、C.I.颜料绿7、C.I.颜料绿36、WO08/055807中所述的片状2,9-二氯喹吖啶酮,或其混合物或固溶体。
片状有机颜料,如片状喹吖啶酮、酞菁、fluororubine、二嗪、红色苝或二酮吡咯并吡咯可有利地用作组分B。
合适的彩色颜料还包括常规无机颜料;尤其是选自如下组的那些:金属氧化物、锑黄、铬酸铅、铬酸硫酸铅、钼酸铅、群青蓝、钴蓝、锰蓝、氧化铬绿、水合氧化铬绿、钴绿和金属硫化物,例如硫化铈或硫化镉,硫硒化镉,铁酸锌,钒酸铋,普鲁士蓝,Fe3O4,炭黑和混合金属氧化物。可商购获得的无机颜料的实例为3920、920、645T、303T、110、110M、CHROMOXIDGRUEN GN和CHROMOXIDGRUEN GN-M。
可用于着色可固化组合物的染料的实例选自偶氮、偶氮甲碱、次甲基、蒽醌、酞菁、二嗪、黄烷士酮、阴丹酮、蒽素嘧啶和金属络合物染料。优选单偶氮染料、钴络合染料、铬络合物染料、蒽醌染料和铜酞菁染料。
印刷方法可高速进行,并且用正在印刷的文档或标签上的任何常规印刷物套准。典型的印刷速度为50-300m/分钟或者甚至更快。
基材可呈一个或多个片或网的形式。基材优选是能在12-300微米厚度下透射UV光的不透明基材,例如纸。纸基材选自普通纸、钞票纸、合成纸或聚合物钞票。普通纸由木浆制成。钞票纸通常由棉花制成。合成纸含有大部分衍生自石油的合成树脂作为其主要材料。合成纸有三个主要子类:
-薄合成纸,如(PPG Industries;微孔,高度填充的,单层,聚烯烃合成材料)或(Covert-All,Inc.;不透明的白色多层双轴取向的聚丙烯(BOPP)产品);
-纤维合成纸(聚合物纤维而不是木纤维);和
-膜层压的合成纸:纸/膜/纸,例如(Landquart);膜/纸/膜,例如混杂钞票基材(Giesecke&Devrient;围绕棉纤维芯的保护性聚酯膜的组合)。
术语纸基材还包括聚合物钞票,例如Guardian(Securency;双轴取向的聚丙烯(BOPP)芯,其具有通过凹版印刷施加的白色底漆)。
纸张的厚度根据ISO 534测量。
纸或板基材的重量通常为30-300g/m2。
优选地,根据ISO 8791-4(PPS 10)测量,纸或板基材在涂覆和上光之前具有小于1.5μm,优选小于1.1μm的粗糙度。
铝金属颗粒通常通过物理气相沉积制造(PVD金属颜料)。真空沉积的操作范围可为5-50nm,金属颗粒的厚度可为8-21nm。优选地,金属颜料颗粒的厚度小于50nm。
在McBeth光密度计上测量,光密度可为0.046-1,尤其为0.09-0.8。在另一实施方案中,在McBeth光密度计上测得的范围为0.2-0.8,尤其为0.5-0.8。
平均粒径可为8-15微米,通过Coulter LS130激光衍射粒度计测量。
在本发明的上下文中,术语平均直径还包括矩形颗粒的长度。
例如,气相沉积铝颗粒的平均直径为8.0-12μm,厚度为11-18nm。
例如,气相沉积铝颗粒的平均直径为8.0-12μm,厚度为12-14nm。
PVD铝颗粒的生产例如描述在Peter Wissling等,Metalleffekt-Pigmente,Herausgeber,U.Zorll,Vincentz Verlag 2005,第53-63页中。颗粒的厚度通过光学方法在生产过程中控制。在沉积期间,测量沉积颗粒的光密度,从而可以以高精度调节厚度。用于各种应用的PVD铝颗粒例如可以以商品名Metasheen(RTM)由BASF SE商购获得。
PVD薄片的生产是本领域所公知的。例如,WO0024946公开了一种制备薄片的方法,其包括:提供气相沉积室;将输送设备放置在气相沉积室中;在真空沉积室中提供指向输送设备的剥离涂层源和真空沉积源,其中沉积源沉积薄片材料层;对室施加真空,并且在室抽真空时,依次将来自剥离涂层源的剥离涂层和来自真空沉积源的气相沉积薄片层交替施加至输送设备,从而构成交替的薄片材料层和中间剥离涂层的多层夹心结构,所述剥离涂层包含形成光滑连续阻隔层的可溶性材料和可在其上形成薄片材料层的支撑表面,从而将夹心结构从抽真空的室中取出,得到多层夹心结构,其可通过用基本上完全溶解中间剥离涂层以从薄片中除去它们的材料进行后续处理而容易地分离成细粒度的薄片。
根据WO0024946,用于制备金属薄片的另一种方法是Avery DennisonCorporation的用于制备以商品名Metalure(RTM)销售的薄片的方法。在该方法中,将聚酯载体的两面用溶剂基树脂溶液进行凹版涂覆。然后将干燥的涂覆幅材输送到金属化设备,在其中用气相沉积铝的薄膜将涂覆片材的两面金属化。然后将具有薄金属膜的片材返回到涂覆设备,在其中用溶剂基树脂溶液的第二膜涂覆铝的两面。然后将干燥的涂覆/金属片材再次输送到金属化设备中,以将气相沉积铝的第二膜施加至片材的两面。然后将得到的多层片材输送进一步加工的设备,在其中在溶剂如丙酮中将涂层从载体上剥离。剥离操作将连续层破碎成包含在浆料中的颗粒。溶剂将浆料中的金属层之间的聚合物溶出。然后对浆料进行声处理和离心以除去溶剂和溶解的涂层,从而留下约65%固体的浓缩铝片的饼。然后将该饼在合适的载体中静置,并通过均化进一步调整尺寸成为用于油墨、油漆和涂料的受控尺寸的薄片。通过该方法制得的用于可印刷应用如油墨的金属薄片的特征在于粒度为约4-12μm,厚度为约15-约25nm。
本发明方法提供的最终金属化涂层的光泽度值高于500°相对光泽度单位,在20°几何下测量。
在本发明的一个具体实施方案中,在将可固化组合物(清漆)施加至纸基材的正面的至少一部分之前,在正面上用阳离子聚合物对纸或板进行处理。
本发明的上下文中的“处理”包括将聚合物溶液施加至纸基材的表面的所有合适的方法;特别是印刷或涂覆。
在本发明中用于处理纸张的阳离子聚合物包含能形成阳离子胺盐的胺重复单元。含胺基的阳离子聚合物可为均聚物或共聚物。所述均聚物或共聚物可呈碱形式,也可部分或完全呈阳离子胺盐形式。该阳离子聚合物例如描述在US 2008/0318150第3-4页中。
优选地,阳离子聚合物为聚乙烯胺,其优选水解至至少90%。
聚乙烯胺或部分或完全水解的聚乙烯基甲酰胺可通过聚合N-乙烯基甲酰胺且随后水解和消去甲酰基以获得胺基而获得。水解度可为1-100%,优选≥50%,更优选≥90%。特别优选完全水解的聚乙烯基甲酰胺。
N-乙烯基甲酰胺聚合物的制备和随后的水解例如详尽描述在US 6,132,558第2栏第36行至第5栏第25行中。聚乙烯胺和部分或完全水解的聚乙烯基甲酰胺可由BASF SE以商品名和商购获得。
例如,这些聚合物的平均分子量Mw为20 000-2 000 000g/mol,例如为50 000-1000 000g/mol,特别为100 000-500 000g/mol。
例如,聚乙烯胺含有0.1-22毫当量(meq),例如5-18meq阳离子基团/每克聚乙烯胺。聚乙烯胺聚合物通常呈分散体或溶液的形式,例如固含量为10-40%,例如为15-30%,优选为20-25%。其通常由该类溶液或分散体施加至纸或板上。
上述聚合物溶液的施加量例如为2-20g/m2纸基材,例如为2-15g/m2纸基材,优选为4-12g/m2纸基材。随后通过红外干燥器和/或热空气干燥器将聚合物溶液干燥。
还可与阳离子聚合物一起施加其他天然聚合物如淀粉,特别是支链淀粉。混入阳离子聚合物中的量通常为5-50%,基于阳离子聚合物的重量。
金属油墨可通过常规的印刷机如凹版印刷、轮转凹版印刷、柔性版印刷、平版印刷、胶版印刷,凸版印刷和/或丝网方法或其他印刷方法施加至基材上。然后可将基材重新卷绕以用于随后步骤的离线印刷,或者替代地,可将基材预先在线印刷或离线印刷或随后在线印刷。
金属基油墨可包含金属颜料颗粒、粘合剂和任选的着色剂,例如颜料或染料,其中可用于着色UV清漆的颜料和染料也可用于着色金属基油墨。
油墨优选包含低固体、高粘度的粘合剂。优选地,颜料与粘合剂的重量比为10:1-1:10。更优选地,颜料与粘合剂的重量比为6:1-1:6,甚至更优选为4:1-1:4。最优选地,颜料与粘合剂的比例为3:1-1:3。
所述组合物的金属颗粒重量含量可小于10%。优选地,所述组合物的颗粒含量小于6重量%,更优选为0.1-6重量%,甚至更优选为0.1-3重量%,仍更优选为0.2-2重量%。在本发明的另一实施方案中,油墨的金属颜料含量可为2-4重量%,优选为3重量%。
适用于本发明方法和装置的金属油墨的实例公开在WO05/051675、WO2005049745和PCT/EP2009/066659中。
如在普通印刷油墨的情况下那样,所述油墨包含铝薄片、粘合剂、助剂等。
就粘合剂树脂而言,可使用热塑性树脂,其实例包括聚乙烯基聚合物[聚乙烯(PE)、乙烯-乙酸乙烯酯共聚物(EVA)],氯乙烯-乙酸乙烯酯共聚物,乙烯醇-乙酸乙烯酯共聚物,聚丙烯(PP),乙烯基聚合物[聚氯乙烯(PVC)、聚乙烯醇缩丁醛(PVB)、聚乙烯醇(PVA)、聚偏二氯乙烯(PVdC)、聚乙酸乙烯酯(PVAc)、聚乙烯基缩甲醛(PVF)],聚苯乙烯基聚合物[聚苯乙烯(PS)、苯乙烯-丙烯腈共聚物(AS)、丙烯腈-丁二烯-苯乙烯共聚物(ABS)],丙烯酸基聚合物[聚甲基丙烯酸酯)(PMMA)、MMA-苯乙烯共聚物],聚碳酸酯(PC),纤维素[乙基纤维素(EC)、乙酸纤维素(CA)、丙基纤维素(CP)、乙酸丁酸纤维素(CAB)、硝化纤维素(CN)],氟基聚合物[聚氯氟乙烯(PCTFE)、聚四氟乙烯(PTFE)、四氟乙烯-六氟乙烯共聚物(FEP)、聚偏二氟乙烯(PVdF)],氨基甲酸酯基聚合物(PU),尼龙[6型、66型、610型、11型],聚酯(烷基)[聚对苯二甲酸乙二醇酯(PET)、聚对苯二甲酸丁二醇酯(PBT)、聚对苯二甲酸环己烷酯(PCT)],线型酚醛清漆型酚醛树脂等。此外,还可使用热固性树脂如甲阶酚醛树脂型酚醛树脂、尿素树脂、三聚氰胺树脂、聚氨酯树脂、环氧树脂、不饱和聚酯等,以及天然树脂如蛋白质、树胶、紫胶、王古王巴树脂(copal)、淀粉和松香。
此外,可根据需要在粘合剂中添加用于稳定印刷膜的柔性和强度的增塑剂和用于调节其粘度和干燥性质的溶剂。溶剂可包含任何一种或多种酯,例如乙酸正丙酯、乙酸异丙酯、乙酸乙酯、乙酸丁酯;醇,如乙醇、工业用甲基变性酒精、异丙醇或正丙醇;酮,如甲基乙基酮或丙酮;芳族烃,如二甲苯和甲苯。根据印刷方法的类型,可使用具有约100℃低沸点温度的溶剂和250℃或更高的高沸点温度的石油溶剂。例如,可使用烷基苯等作为具有低沸点温度的溶剂。溶剂的实例为乙氧基丙醇、甲基乙基酮、甲氧基丙基乙酸酯,二丙酮醇等。
此外,可适当地添加助剂,包括用于改善干燥性质、粘度和分散性的各种反应性试剂。助剂用于调节油墨的性能,例如可使用改善油墨表面的耐磨性的化合物和加速油墨干燥的干燥剂等。
也可使用不使用溶剂的可光聚合固化树脂或可电子束固化树脂作为载体主要成分的基料树脂。其实例包括丙烯酸类树脂,下文显示了可商购获得的丙烯酸类单体的具体实例。
可使用的单官能丙烯酸酯单体包括例如丙烯酸2-乙基己酯、2-乙基己-EO加合物丙烯酸酯、乙氧基二甘醇丙烯酸酯、丙烯酸2-羟基乙酯、丙烯酸2-羟基丙酯、丙烯酸2-羟乙酯-己内酯加合物、丙烯酸2-苯氧基乙基酯、苯氧基二甘醇丙烯酸酯、壬基酚-EO加合物丙烯酸酯、(壬基酚-EO加合物)-己内酯加合物丙烯酸酯、丙烯酸2-羟基-3-苯氧基丙酯、丙烯酸四氢糠基酯、糠醇-己内酯加合物丙烯酸酯、丙烯酰吗啉、丙烯酸二环戊烯基酯、丙烯酸二环戊基酯,丙烯酸二环戊烯氧基乙酯、丙烯酸异冰片酯、(4,4-二甲基-1,3-二烷)-己内酯加合丙烯酸酯、(3-甲基-5,5-二甲基-1,3-二烷)-己内酯加合物丙烯酸酯等。
可使用的多官能丙烯酸酯单体包括己二醇二丙烯酸酯、新戊二醇二丙烯酸酯、聚乙二醇二丙烯酸酯、三丙二醇二丙烯酸酯、新戊二醇羟基新戊酸酯二丙烯酸酯、(新戊二醇羟基新戊酸酯)-己内酯加合物二丙烯酸酯、(1,6-己二醇二缩水甘油醚)-丙烯酸加成物、(羟基新戊醛-三羟甲基丙烷乙缩醛)二丙烯酸酯、2,2-双[4-(丙烯酰氧基二乙氧基)苯基]丙烷、2,2-双[4-(丙烯酰氧基二乙氧基)苯基]甲烷、氢化双酚A-氧化乙烯加合物二丙烯酸酯、三环癸烷二甲醇二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、季戊四醇三丙烯酸酯、(三羟甲基丙烷-氧化丙烯)加合物三丙烯酸酯、甘油-氧化丙烯加合物三丙烯酸酯、二季戊四醇六丙烯酸酯和五丙烯酸酯的混合物、二季戊四醇与低级脂肪酸和丙烯酸的酯、二季戊四醇-己内酯加合物丙烯酸酯,三(丙烯酰氧基乙基)异氰脲酸酯、2-丙烯酰氧基乙基磷酸酯等。
包含上述树脂的油墨不含溶剂,且如此构成从而在通过电子束或电磁波辐照时在链反应中聚合。
就这些油墨中的紫外线辐照型油墨而言,可向其中加入光聚合引发剂,并根据需要,可以加入敏化剂、助剂如阻聚剂和链转移剂等。
就光聚合引发剂而言,存在(1)直接光解型引发剂,包括芳基烷基酮、肟酮、酰基氧化膦等,(2)自由基聚合反应型引发剂,包括二苯甲酮衍生物、噻吨酮衍生物等,(3)阳离子聚合反应型引发剂,包括芳基重氮盐、芳基碘盐、芳基锍盐和芳基苯乙酮盐等,和此外的(4)能量转移型引发剂,(5)光致氧化还原型引发剂,(6)电子转移型引发剂等。就可电子束固化型油墨而言,不需要光聚合引发剂,并且可使用与紫外线辐照型油墨相同类型的树脂,并且可根据需要向其中添加各种助剂。
所述油墨包含总含量为0.1-20重量%,优选0.1-10重量%的铝颜料,基于油墨总重量。
优选地,当沉积在基材上时,金属油墨的厚度足够薄,从而允许光透过。
粘合剂可包括选自如下组中的任意一种或多种:聚乙烯醇缩丁醛、硝基纤维素、氯乙烯、乙酸乙烯酯共聚物、乙烯基、丙烯酸类、氨基甲酸酯、聚对苯二甲酸乙二醇酯、萜烯酚、聚烯烃、硅酮、纤维素、聚酰胺、聚酯、松香酯树脂。优选的粘合剂为50%硝化纤维素(ID硝化纤维素DHL120/170和硝化纤维素DLX30/50,由Nobel Industries提供)和50%聚氨酯(IDNeorez U335,由Avecia提供)。溶剂可为酯/醇混合物,优选比例为20:1-30:1的乙酸正丙酯和乙醇。
本发明还涉及可通过使用本发明的方法获得的纸制品。纸制品可为钞票,识别文件如护照、身份证、驾驶执照,包装材料如标签,折叠纸盒,用于药品、服装、软件、化妆品、烟草或任何其他需要装饰的产品的纸袋。优选方案和解释同样适用于本发明的所有方面。
以下实施例说明本发明。
实施例
金属油墨(D50,8.0-12.0μm,厚度13nm):
金属油墨的制备程序:将铝颜料浆料以使得将颜料和粘合剂比例调节为2.7:1的比例添加至上述硝化纤维素清漆中,加入乙酸乙酯以将油墨调节至印刷粘度(20秒,Zahn 2号杯)。将所得分散体用Dispermat以800rpm搅拌10分钟。
基材:白板,Invercote T 220g/m2,275μm m(高品质涂覆纸,IggesundPaperboard Europe)。将印刷面完全涂覆并修饰至消光水平。表面粗糙度1.1μm。
UV漆如WO 2012/176126的实施例所述,使用光引发剂3。
UV漆和金属油墨使用Moser印刷机施加,其包括UV凹版印刷机单元和在线溶剂型凹版印刷单元。
印刷速度30m/分钟,UV固化强度50瓦/cm2,溶剂油墨干燥温度80℃,
UV凹版印刷滚筒70L/cm丝网,溶剂油墨凹版印刷滚筒70L/cm丝网。结果列于表1中。
表1通过Zehntner光泽计ZGM 1110测量印刷样品的光泽度
光泽单位/基材 | 20°角 | 60°角 | 85°角 |
Invercote T | 2 | 11 | 60 |
金属油墨 | 18 | 108 | 90 |
3微米UV漆 | 88 | 97 | 101 |
UV和金属油墨 | 730 | 580 | 143 |
当首先透过基材在镜面镍垫片上固化UV清漆且加印包含细等级铝颜料的金属油墨时,纸和板上的金属油墨的光泽度显著提高。
Claims (19)
1.一种在纸或板基材上形成展示出光泽的光滑表面涂层的方法,包括以下步骤:
A)将可固化组合物施加至纸或板基材的正面的至少一部分上;
B)使所述可固化组合物与垫片接触,同时通过使用设置在纸基材背面上的至少一个UV灯固化所述组合物;和
C)在固化的组合物上沉积铝层,
其中所述灯具有处于UV-A范围和近VIS范围内的发射峰,并且所述可固化组合物包含至少一种在UV-A区域且此外在近VIS范围内吸收的光引发剂。
2.根据权利要求1所述的方法,其中所述可固化组合物包含选自单-和双酰基氧化膦化合物、α-氨基酮型化合物或肟酯化合物及其混合物的光引发剂。
3.根据权利要求1或2所述的方法,其中所述灯为镓或铁掺杂的中压汞灯。
4.根据权利要求1或2所述的方法,其中所述灯为聚焦反射型二极管阵列(FRDA)系统,其具有处于UVA范围的发射,此外还具有400nm以上的发射峰。
5.根据权利要求1-4中任一项所述的方法,其中所述光引发剂选自单-和双酰基氧化膦化合物及其混合物。
6.根据权利要求1-5中任一项所述的方法,其中所述可固化组合物包含单-或双酰基氧化膦化合物与二苯甲酮类化合物、α-羟基酮、α-烷氧基酮或α-氨基酮化合物的混合物。
7.根据权利要求1-6中任一项所述的方法,其中所述可固化组合物包含:
(a)1.0-20.0重量%,特别是1.0-15.0重量%,非常特别是3.0-10.0重量%的光引发剂,
(b)99.0-80.0重量%,特别是99.0-85.0重量%,非常特别是97.0-90.0重量%的树脂,
其中组分a)和b)的总和加起来为100%。
8.根据权利要求1-7中任一项所述的方法,其中所述垫片的表面不具有微结构,并且垫片材料选自镍套筒;安装在金属筒上的镍板或其他金属材料。
9.根据权利要求8所述的方法,其中所述垫片为安装在金属筒上的镍板。
10.根据前述权利要求中任一项所述的方法,其中所述纸基材选自普通纸、钞票纸、合成纸和聚合物钞票基材。
11.根据前述权利要求中任一项所述的方法,其中最终金属化涂层的光泽度值高于500相对光泽度单位,在20°几何下测量。
12.根据前述权利要求中任一项所述的方法,其中气相沉积的铝颗粒的平均直径为8.0-12μm,厚度为11-18nm。
13.根据前述权利要求中任一项所述的方法,其中气相沉积的铝颗粒的平均直径为8.0-12μm,厚度为12-14nm。
14.根据前述权利要求中任一项所述的方法,其中所述纸或板基材的粗糙度小于1.5μm,优选小于1.1μm。
15.根据前述权利要求中任一项所述的方法,其中所述纸或板基材的重量为30-300g/m2。
16.根据前述权利要求中任一项所述的方法,其中在将可固化组合物施加至纸基材的正面的至少一部分之前,所述纸或板已在正面上用阳离子聚合物处理。
17.根据权利要求16所述的方法,其中所述阳离子聚合物为聚乙烯胺。
18.可使用权利要求1-17中任一项所述的方法获得的纸或板制品。
19.根据权利要求18所述的纸或板制品,其为钞票,识别文件如护照、身份证、驾驶执照,包装材料如标签,折叠纸盒,用于药品、服装、软件、化妆品、烟草或任何其他需要装饰的产品的纸袋。
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CN103608183A (zh) * | 2011-06-21 | 2014-02-26 | 巴斯夫欧洲公司 | 在纸或纸板上印刷衍射光栅 |
WO2013176729A1 (en) * | 2012-05-24 | 2013-11-28 | Amcor Group Gmbh | Multi-layer printing process |
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CN111944406A (zh) * | 2020-08-20 | 2020-11-17 | 山东沃丰新材料有限公司 | 一种抗静电彩铝板及其生产工艺 |
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