CN104263063B - The optical fiber coloring ink of radiation-hardenable - Google Patents

The optical fiber coloring ink of radiation-hardenable Download PDF

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Publication number
CN104263063B
CN104263063B CN201410535049.7A CN201410535049A CN104263063B CN 104263063 B CN104263063 B CN 104263063B CN 201410535049 A CN201410535049 A CN 201410535049A CN 104263063 B CN104263063 B CN 104263063B
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acrylate
optical fiber
radiation
fiber coloring
coloring ink
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CN104263063A (en
Inventor
黄星
余晓梦
皮亚斌
桂振东
皮广
宋文勇
崔丽云
吴雅
廖学明
万欢
王龙
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Wuhan Changying Xin Technology Co. Ltd.
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WUHAN YANGTZE OPTICAL ELECTRONIC CO Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • C09D11/103—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds of aldehydes, e.g. phenol-formaldehyde resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/10—Printing inks based on artificial resins
    • C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • C09D11/104—Polyesters

Abstract

The present invention relates to the optical fiber coloring ink of a kind of radiation-hardenable, it is characterized in that by weight percentage, the content of its each component is: mill base 1-20%, reactive diluent 20-40%, auxiliary agent A 0.5-4%, UV resin 40-60%, light trigger and aided initiating 3-10%, each component sum meets 100%. The curing rate of the optical fiber coloring ink of radiation-hardenable of the present invention is fast, and solidification effect is good, use its painted rear optical fiber bright not fade, smooth surface sense of touch good, can also effectively make a distinction under dark light.

Description

The optical fiber coloring ink of radiation-hardenable
Technical field
Patent of the present invention relates to optical fiber and fibre coating field, and described ink is suitable for the coating of optical fiber coloring layer.
Background technology
Optical fiber coloring ink is used exclusively for a kind of ultraviolet radiant light cured printing ink of optical fiber coloring, and its Main Function is to manufacture colored optical fiber to make optical fiber still can effectively make a distinction after being prepared to optical cable. High performance optical fiber coloring ink on the performance such as intensity, reliability of optical fiber, stability, decay, micro-curved all without impact. The ink being coated in outside of fiber may also operate as the iris action to environment, particularly to the iris action of dust and water clearly, thus reducing the environmental activity impact on optical fiber serviceability.
Traditional optical fiber coloring speed is at 500-2400m/min, and so coating at a high speed makes ink must have the curing rate being exceedingly fast and quick levelability. Do not fade for 100 times, curing degree and the solvent resistance of ink are had strict requirement by this by resistance to butanone wiping for painted good optical fiber needs. Painted good optical fiber can be invaded bubble by fine cream for a long time when preparing into optical cable, so the compatibility experiments of ink and fine cream just seems extremely important. Current Ge great optical cable factory requires that painted good optical fiber soaks 1 month dyed layer without obscission at 85 DEG C of fine cream, and the ageing-resistant performance of dyed layer is had strict requirement by this, and common UV ink cannot meet the requirement of optical fiber coloring ink completely.
Summary of the invention
The technical problem to be solved is the deficiency existed for above-mentioned prior art and the optical fiber coloring ink providing a kind of radiation-hardenable, can be used for the coating of optical fiber coloring layer, and improve the speed of optical fiber coloring, make painted after optical fiber undamped, solvent resistance good, resistance to oil product soaks.
The present invention solves that the technical scheme that problem set forth above adopts is:
A kind of optical fiber coloring ink of radiation-hardenable, by weight percentage, the content of its each component is: mill base 1-20%, reactive diluent 20-40%, auxiliary agent 0.5-4%, UV resin 40-60%, light trigger and aided initiating 3-10%, each component sum meets 100%.
By such scheme, described reactive diluent is the reactive diluent that pigment wetting is good. preferably, described reactive diluent is 4-tert-butylcyclohexyl acrylate, decyl acrylate, ethoxyethoxyethyl acrylate, 2-phenoxy group acrylate, ring trimethylolpropane dimethoxym ethane acrylate, trimethylolpropane trimethacrylate, two-trimethylolpropane tetra-acrylate, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, double pentaerythritol methacrylate, propylene glycol diacrylate, tripropylene glycol diacrylate, 1, 6-hexanediyl ester, neopentylglycol diacrylate, (2) third oxidation neopentylglycol diacrylates, (3) third oxidation trimethylolpropane trimethacrylates, (3) ethoxyquin trimethylolpropane trimethacrylate, glycerol propoxylate triacrylate, isobornyl acrylate, one or more in glycol phthalate mixture in any proportion.More preferably, described reactive diluent is one or more mixture in any proportion in 4-tert-butylcyclohexyl acrylate, ring trimethylolpropane dimethoxym ethane acrylate, propylene glycol diacrylate, tripropylene glycol diacrylate, 1,6-hexanediyl ester, glycerol propoxylate triacrylate, (2) third oxidation neopentylglycol diacrylate, tetramethylol methane tetraacrylate, double pentaerythritol methacrylates.
By such scheme, by weight percentage, its each constituent content is described mill base: pigment 10-50%, reactive diluent 30-70%, urethane acrylate 3-20%, defoamer 1-2%, wetting dispersing agent 3-10%, and each component sum meets 100%. The present invention need first adding portion reactive diluent etc. be uniformly dispersed by pigment, adding in described optical fiber coloring ink formulations with the form of mill base, therefore the reactive diluent in the above-mentioned optical fiber coloring ink being applied to radiation-hardenable enumerated is equally applicable to the dispersion of described mill base again.
Specifically, described pigment can apply to the pigment of UV ink, and its granule should be less than 10 ��m, and be capable of withstanding and radiated by UV, adds in described optical fiber coloring ink formulations with the form of mill base. Preferably, described pigment be titanium dioxide white (titanium dioxide), white carbon black, Phthalocyanine Blue BGS, Phthalocyanine Green G, benzidine yellow G, permanent yellow GR, benzimidazolone yellow, forever solid orange, forever solid palm fibre, permanent violet, quinacridone is red, naphthol reds, benzimidazolone are red, anthraquinone is red, one or more mixture in any proportion in lithol that fuchsin.
Specifically, wetting dispersing agent described in mill base is the high molecular polymer containing pigment affinity groups, it is possible to selected from commercially available BKY company BYK-111, BKY-163, BKY-168; EFKA-4450, EFKA-4620, EFKA-4673 of BASF AG; Rub can the 3060 of chemical industry, 2026,3027 and other companies provide go for UV system wetting dispersing agent.
Specifically, defoamer described in mill base is one or more mixture in any proportion in the non-silicon defoaming agent of polyacrylate or organic silicon defoamer. BKY-054, BYK-088, BYK-1790 of commercially available BKY company, EFKA-2020, EFKA-2022, EFKA-2008 of BASF AG can be selected from, Defom3100 that this moral of hamming is modest and the defoamer going for UV system that other companies provide.
By such scheme, described auxiliary agent includes levelling agent, defoamer, antioxidant, antistatic additive, and by weight percentage, its each constituent content is the antistatic additive of the levelling agent of 10-30%, the defoamer of 10-20%, the antioxidant of 5-15%, 35-60%.
Specifically, levelling agent described in auxiliary agent can be organic silicon modified by polyether, polyester resin change properties of organic silicon and one or more mixture in any proportion of Organic fluoride modification acrylate apoplexy due to endogenous wind, the levelling agent that can increase slippery that the DC-57 of commercially available Dow Corning Corporation, BYK-307, BYK-373, BYK-333 of EFKA-3288, EFKA-3299, BYK company of BASF AG and other companies provide can be selected from.
Specifically, defoamer described in auxiliary agent is one or more mixture in any proportion in the non-silicon defoaming agent of polyacrylate or organic silicon defoamer. BKY-054, BYK-088, BYK-1790 of commercially available BKY company, EFKA-2020, EFKA-2022, EFKA-2008 of BASF AG can be selected from, Defom3100 that this moral of hamming is modest and the defoamer going for UV system that other companies provide.
Specifically, the effect of antioxidant described in auxiliary agent is the ageing-resistant performance improving ink, the mixture of one or more arbitrary proportions of hydroquinone, benzoquinone, tert-butylhydroquinone, t-butyl catechol, methyl hydroquinone, 2,6-di-tert-butyl-4-methy phenols (BHT), p methoxy phenol (MEHQ), IRGANOX1010, IRGANOX1035, IRGANOX1076, IRGANOX1222 can be selected from.
Specifically, antistatic additive described in auxiliary agent be used to eliminate high speed fibre painted time produce electrostatic, coating surface resistance can be effectively reduced and better with Miscibility, it can be cationic antistatic agent, anionic antistatic agent and non-ionic antistatic agent, preferably non-ionic antistatic agent good with Miscibility, cationic antistatic agent, suitable antistatic additive can be selected from the antistatic additive SN that commercially available Jiangsu Hai'an Petrochemical Plant produces, SANYO GS chemical conversion antistatic agent C HEMISTAT3500, Clariant sas93 and other suitable antistatic additive.
By such scheme, described UV resin is one or more mixture in any proportion of urethane acrylate, epoxy acrylate, polyester acrylate, amino acrylates, by weight percentage, its each constituent content is the amino acrylates of the urethane acrylate of 0-100%, the epoxy acrylate of 0-60%, 0-30% polyester acrylate, 0-60%.
Specifically, the vitrification point of described epoxy acrylate is more than 60 DEG C, vitrification point preferably is more than 80 DEG C, it is possible to any one in the EBECRYL-600 of CN2204, Qing Te company and other satisfactory epoxy acrylates of commercially available Sartomer. Introduce epoxy acrylate and can improve vitrification point and the modulus of described ink.
Specifically, pigment is had good wettability by described polyester acrylate, can effectively improve the stability of ink, mobility, it is possible to any one in UV7060, UV7041 of CN2203, CN8200, Zhong Shanqianyou chemical material company limited and other satisfactory polyester acrylates of commercially available Sartomer.
Specifically, described amino acrylates is prepared from by the melmac of methyl-etherified or butyl ether, and degree of functionality is 2.5��6 officials, it is possible to selected from the DR-M541 of UN003, UN111-6 of commercially available Zhong Shanqianyou chemical material company limited and Changxing group. The advantage such as amino acrylates has splendid base material adhesive force, curing rate is fast, heat resistance good, solvent resistance is good, volume contraction is little, the introducing of amino acrylates can improve curing rate and the solvent resistance of ink.
By such scheme, UV resin all includes polyether urethane and polyester-polyurethane acrylate with urethane acrylate described in mill base. The elastic modelling quantity of described polyester-polyurethane acrylate should be not less than 600MPa, and elongation at break is not less than 5%, and the elastic modelling quantity of described polyether urethane should be not more than 100MPA, and elongation at break should be not less than 50%. Polyester-polyurethane acrylate provides rigidity for ink; Polyether urethane provides flexibility for ink, can obtain, by regulating the ratio of two kinds of polyurethane, the material coupled hardness with softness, and concrete preparation method is as follows:
After (methyl) crylic acid hydroxy ester of 1mol is mixed homogeneously with the diisocyanate of 1mol, add the millesimal catalyst of gross mass and millesimal polymerization inhibitor, after maintaining 40-45 DEG C of reaction 3-4 hour, the polyether polyol or the PEPA that add 0.5mol are warming up to 70-80 DEG C and continue reaction 4-5 hour, NCO content to be detected lower than 0.1% after discharging, namely obtain polyether urethane or polyester-polyurethane acrylate.
Specifically, described PEPA, pigment wetting is good, include but are not limited to poly-adipic acid hexanediol ester dihydroxylic alcohols, poly adipate succinic acid ester dihydroxylic alcohols, polyneopentyl glycol adipate dihydroxylic alcohols, poly-SA certain herbaceous plants with big flowers diol ester dihydroxylic alcohols, poly-SA hexanediol ester dihydroxylic alcohols, poly-SA butanediol ester dihydroxylic alcohols, polycaprolactone diols, PCDL, polyethylene glycol phthalate dihydroxylic alcohols, polyethylene terephthalate dihydroxylic alcohols. In these PEPAs, it is preferred that one or more mixture in any proportion in poly-adipic acid hexanediol ester dihydroxylic alcohols, poly-SA certain herbaceous plants with big flowers diol ester dihydroxylic alcohols, PCDL.
Specifically, described polyether polyol can be homopolymer or the copolymer of the alkylene oxide of C2��C5, wherein the alkylene oxide of C2��C5 in oxirane, expoxy propane, epoxy butane, oxolane and 3-methyltetrahydrofuran one or more. Specifically, described polyether polyol can select PPG-1000, PPG-600, PEG-600, PTMG650, PTMG1000, PTMG2000 etc.
Specifically, described diisocyanate includes but are not limited to toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI), naphthalene diisocyanate (NDI), to phenyl diisocyanate (PPDI), dimethylenebenzene diisocyanate (XDI), isophorone diisocyanate (IPDI), dicyclohexyl methyl hydride diisocyanate (HMDI), lysinediisocyanate (LDI), dicyclohexyl methyl hydride diisocyanate (HMDI), hexamethylene diisocyanate (HDI), trimethyl hexamethylene diisocyanate (TMDI). preferably, described diisocyanate is selected in toluene di-isocyanate(TDI) (TDI), isophorone diisocyanate (IPDI), dicyclohexyl methyl hydride diisocyanate (HMDI) a kind of.
In such scheme, described light trigger and aided initiating, its each constituent content is by weight percentage: the light trigger of 70-90%, 10-30% aided initiating.
Specifically, described light trigger is the key causing ink solidification, selected from benzophenone (BP), 4-phenyl benzophenone (PBZ), 4-methyl benzophenone (MBZ), 4-benzoyl-4 '-methyl-diphenyl sulfide (BMS), methyl benzoylformate (MBF), benzoin dimethylether (651), 2,4,6-trimethylbenzoyl diphenyl phosphate oxidations (TPO), 2,4,6-trimethylbenzoyl phosphinic acid ethyl esters (TPO-L), double, two (2,4,6-trimethylbenzene methylacyl) phenylphosphine oxide (819), 2-methyl isophthalic acid-(4-first mercaptophenyl)-2-morpholine-1-acetone (907), 1-hydroxy cyclohexyl phenylketone (184), 2-hydroxy-2-methyl-1-phenylacetone (1173), a, a-diethoxy acetophenone (DEAP), 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone (369), 2-isopropyl thioxanthone (ITX), 2,4-diethyl thioxanthones (DETX), 2-chlorothiaxanthenone (CTX), 1-chloro-4-propoxyl group thioxanthone (CPTX), o-benzoyl yl benzoic acid methyl ester (OMBB), one or more in light trigger 754 mixture in any proportion.
Specifically, described aided initiating includes but not limited to one or more mixture in any proportion in the CN371 of 4 (N, N dimethylamino) ethyl benzoate (EDAB), the different monooctyl ester of 4 dimethylaminobenzoic acid (EHA), tertiary amine groups acrylate (P113, P115, P116, P117), Sartomer.
The viscosity of the optical fiber coloring ink of radiation-hardenable of the present invention is 1200-4000mpa.s (25 DEG C), it is therefore preferable to 1600-2700mpa.s (25 DEG C), is more preferably 1900-2500mpa.s (25 DEG C). The viscosity of ink of the present invention can affect its paintability on optical fiber, causes dyed layer blocked up if viscosity crosses conference and produces decay, is not easily distinguishable if the too small meeting of viscosity causes dyed layer to cross thin color.
The elongation at break of the optical fiber coloring ink of radiation-hardenable of the present invention is 2-10%, and specific modulus (2.5% elongation) is 600-1400MPa, and tensile strength is 15-50MPa; Preferably, elongation at break is 3-8%, and specific modulus is 800-1200MPa, and tensile strength is 20-40MPa.
Compared with prior art, the invention has the beneficial effects as follows:
First, the curing rate of the optical fiber coloring ink of radiation-hardenable of the present invention is fast, and solidification effect is good, use its painted rear optical fiber bright not fade, smooth surface sense of touch good, can also effectively make a distinction under dark light.
Second, use the optical fiber surface slippery of this ink colorant good and not easily play electrostatic, follow-up prepare optical cable time can effectively prevent because electrostatic causes disconnected fine situation.
3rd, use the smooth zero defect of optical fiber surface of this ink colorant, when preparing fibre ribbon with matrix material coupling, stripping performance is splendid, makes the flatness of fibre ribbon be better than common ink owing to being not likely to produce electrostatic when preparing fibre ribbon containing antistatic additive.
The present invention is directed to the special process performance of optical fiber coloring ink, and the technical specification performance requirement of regulation and the photocuring optical fiber ink of multiple different colours (blue, orange, green, brown, Lycoperdon polymorphum Vitt, white, redness, black, yellow, purple, pink, dark green) researched and developed, its ink complies fully with the demand of optical fiber coloring ink, use its painted rear optical fiber bright not fade, smooth surface sense of touch good, the highest colouring speeds can reach 2400m/min.
Detailed description of the invention
Following example provide as the specific embodiment of the present invention, and are used for the embodiment and advantages of the present invention are described. It is to be understood that these embodiments are merely illustrative, and has no intention any mode and this specification or claims are limited.
The urethane acrylate adopted in the present invention relates to polyether urethane, polyester-polyurethane acrylate, and concrete preparation method is as follows:
1, the synthesis of polyether urethane:
116.12g 2-(Acryloyloxy)ethanol and 174.16g toluene di-isocyanate(TDI) are added in flask, are stirring evenly and then adding into 1.34g catalyst dibutyltin dilaurylate and 1.34g hydroquinone of polymerization retarder (HQ), the polyether polyol (PPG1000) adding 1000g after maintaining 50 DEG C of reactions 3 hours is warming up to 80 DEG C of continuation reactions 5 hours, NCO content to be detected lower than 0.1% after, vacuum defoamation, filter discharging, obtain resin UV1000.
Viscosity is 15256mpa.s (25 DEG C) after measured, and stretch modulus is 5.5MPa, percentage elongation is 189%, tensile strength 3.5MPa.
2, the synthesis of polyester-polyurethane acrylate:
116.12g 2-(Acryloyloxy)ethanol and 262.35g dicyclohexyl methyl hydride diisocyanate are added in flask, are stirring evenly and then adding into 0.88g catalyst dibutyltin dilaurylate and 0.88g polymerization inhibitor MEHQ (MEHQ), the 500gPOL-5122 (poly-adipic acid hexanediol ester dihydroxylic alcohols) adding set amount after maintaining 40 DEG C of reactions 4 hours is warming up to 70 DEG C of continuation reactions 4 hours, NCO content to be detected lower than 0.1% after, vacuum defoamation, filter discharging, obtain resin M-512.
Viscosity is 8221mpa.s (40 DEG C) after measured, and stretch modulus is 1120MPa, percentage elongation is 18%, tensile strength 38MPa.
Embodiment 1
The white optical fiber coloring printing ink of a kind of radiation-hardenable, by weight percentage, the content of its each component is: white colorant 15%, reactive diluent 27.4%, UV resin 45%, auxiliary agent 3.6%, light trigger and aided initiating 9%.
Wherein, white colorant is as follows by weight ratio: 50% titanium dioxide white, 3%BYK-111,1%BYK-1790,10% resin M-512,36% trimethylolpropane trimethacrylate, amount to 100%, concrete compound method is as follows: (1), by trimethylolpropane trimethacrylate, BYK-111 and BYK-1790,10% resin M-512 Homogeneous phase mixing, obtains mixing liquid component; Then under the stirring of 500r/min, pigmentary titanium dioxide is added in vain in described mixing liquid component, after pigment adds, raise rotating speed and stir 1.0 hours to 1000r/min, the rough color slurry of UV obtained; (2) rough for described UV mill base is ground 25min and uses laser particle analyzer to measure fineness, it is respectively less than 1 micron when measuring all granules of pigments, namely the UV white colorant that can be used for optical fiber coloring ink is prepared, initial fineness D90163.284 micron, final fineness D900.205 micron after grinding 25min.
Described reactive diluent, its composition is by weight percentage: 20% (2) third oxidation neopentylglycol diacrylate, 20% tripropylene glycol diacrylate, 10% double pentaerythritol methacrylate, 10% 2-trimethylolpropane tetra-acrylate, 30% glycol phthalate, 10% hexa-methylene diacrylate; Described UV resin, its composition is by weight percentage: 30% self-control polyether urethane UV1000,20% self-control polyester-polyurethane acrylate M-512,30% amino acrylates UN003,20% epoxy acrylate EBECRYL-600; Described auxiliary agent, its composition is by weight percentage: 22% levelling agent DC-57,14% defoamer BYK-1790,8% antioxidant 1035,56% antistatic additive SN; Described light trigger and aided initiating, its composition is by weight percentage: 22% light trigger TPO, 44% light trigger 754,17% light trigger 184,6% light trigger 907,11% aided initiating P115.
The preparation method of the optical fiber coloring ink of above-mentioned radiation-hardenable is: by said ratio, weigh each raw material components, dispersion machine is used to stir 60 minutes at about 40 DEG C with the rotating speed of 1000 revs/min, after light trigger and aided initiating are completely dissolved, use 1500 order filters to filter, be placed in 40 DEG C of baking ovens deaeration and get product after 1 day optical fiber coloring ink.
The viscosity of the optical fiber coloring ink prepared by the present embodiment is 2410mpa.s (25 DEG C), and elongation at break is 3.5%, and specific modulus (2.5% elongation) is 960MPa, and tensile strength is 30MPa.
Embodiment 2
The black optical fiber coloring printing ink of a kind of radiation-hardenable, by weight percentage, the content of its each component is: black color paste 10%, reactive diluent 24.4%, UV resin 53%, auxiliary agent 3.6%, light trigger and aided initiating 9%.
Wherein, black color paste is as follows by weight ratio: 20% white carbon black, 18%BYK-163,1%BYK-1790,20% resin M-512,41% trimethylolpropane trimethacrylate, amount to 100%, initial fineness D9014.292 micron, after grinding 15min, final fineness D900.131 micron, prepares according to the compound method of embodiment 1;
Wherein, described reactive diluent, its composition is by weight percentage: 20% (2) third oxidation neopentylglycol diacrylate, 20% tripropylene glycol diacrylate, 10% double pentaerythritol methacrylate, 10% 2-trimethylolpropane tetra-acrylate, 25% glycol phthalate, 15% propylene glycol diacrylate; Described UV resin, its composition is by weight percentage: 30% self-control polyether urethane UV1000,20% self-control polyester-polyurethane acrylate M-512,30% amino acrylates UN003,20% epoxy acrylate EBECRYL-600; Described auxiliary agent, its composition is by weight percentage: 22% levelling agent BYK-373,14% defoamer EFKA-2022,8% antioxidant 1035,56% antistatic additive SN; Described light trigger, its composition is by weight percentage: 30% light trigger 369,20% light trigger 907,10% light trigger ITX, 20% light trigger 819,2% aided initiating EDAB.
The preparation method of the optical fiber coloring ink of above-mentioned radiation-hardenable is: by said ratio, weigh each raw material components, dispersion machine is used to stir 60 minutes at about 40 DEG C with the rotating speed of 1000 revs/min, after light trigger and aided initiating are completely dissolved, use 1500 order filters to filter, be placed in 40 DEG C of baking ovens deaeration and get product after 1 day optical fiber coloring ink.
The viscosity of the optical fiber coloring ink prepared by the present embodiment is 1960mpa.s (25 DEG C), and elongation at break is 6.3%, and specific modulus (2.5% elongation) is 852MPa, and tensile strength is 26MPa.
Embodiment 3
The red optical fiber coloring printing ink of a kind of radiation-hardenable, by weight percentage, the content of its each component is: white colorant 4%, red mill base 10%, reactive diluent 25.4%, UV resin 50%, auxiliary agent 3.6%, light trigger and aided initiating 7%.
Wherein, red mill base is as follows by weight ratio: 20% quinacridone is red, 8%BYK-163,1%BYK-1790,10% resin M-512,61% tripropylene glycol diacrylate, amount to 100%, initial fineness D9086.654 micron, final fineness D900.215 micron after grinding 10min; White colorant is prepared according to the compound method of embodiment 1;
Wherein, described reactive diluent, its composition is by weight percentage: 20% (2) third oxidation neopentylglycol diacrylate, 20% tripropylene glycol diacrylate, 10% double pentaerythritol methacrylate, 10% 2-trimethylolpropane tetra-acrylate, 32% (3) third oxidation trimethylolpropane trimethacrylate, 8% hexa-methylene diacrylate; Described UV resin, its composition is by weight percentage: 30% self-control polyether urethane UV1000,20% polyester acrylate UV7041,30% amino acrylates UN003,20% epoxy acrylate EBECRYL-600; Described auxiliary agent, its composition is by weight percentage: 22% levelling agent EFKA-3288,14% defoamer BYK-1790,8% antioxidant 1035,56% antistatic additive SN; Light trigger and aided initiating, its composition is by weight percentage: 14% light trigger TPO, 14% light trigger 369,15% light trigger 907,29% light trigger 651,7% light trigger 819,7% light trigger DETX, 14% aided initiating P113.
The preparation method of the optical fiber coloring ink of above-mentioned radiation-hardenable is: by said ratio, weigh each raw material components, dispersion machine is used to stir 60 minutes at about 40 DEG C with the rotating speed of 1000 revs/min, after light trigger and aided initiating are completely dissolved, use 1500 order filters to filter, be placed in 40 DEG C of baking ovens deaeration and get product after 1 day optical fiber coloring ink.
The viscosity of the optical fiber coloring ink prepared by the present embodiment is 2145mpa.s (25 DEG C), and elongation at break is 3.2%, and specific modulus (2.5% elongation) is 1125MPa, and tensile strength is 28MPa.
Embodiment 4
A kind of blue optical fiber coloring printing ink of radiation-hardenable, by weight percentage, the content of its each component is: white colorant 4%, blue mill base 7.5%, red mill base 0.5%, reactive diluent 25.4%, UV resin 50%, auxiliary agent 3.6%, light trigger and aided initiating 9%.
Wherein, blue mill base is as follows by weight ratio: 25% Phthalocyanine Blue BGS, 7.5%BYK-163,1%BYK-1790,13% resin M-512,53.5% tripropylene glycol diacrylate, amount to 100%, initial fineness D9025.207 micron, final fineness D900.207 micron after grinding 25min, white colorant and red mill base are prepared according to the compound method of embodiment 1 and 3 respectively;
Wherein, described reactive diluent, its composition is by weight percentage: (2) third oxidation neopentylglycol diacrylate 20%, tripropylene glycol diacrylate 20%, double pentaerythritol methacrylate 10%, two-trimethylolpropane tetra-acrylate 10%, glycol phthalate 20%, hexa-methylene diacrylates 20%; Described UV resin, its composition is by weight percentage: 10% self-control polyether urethane UV1000,20% self-control polyester-polyurethane acrylate M-512,20% polyester acrylate UV7041,30% amino acrylates UN003,20% epoxy acrylate EBECRYL-600; Described auxiliary agent, its composition is by weight percentage: 22% levelling agent DC-57,14% defoamer BYK-1790,8% antioxidant 1035,56% antistatic additive SN; Light trigger and aided initiating, its composition is by weight percentage: 10% light trigger 369,50% light trigger 907,10% light trigger 819,20% light trigger ITX, aided initiating EDAB10%.
The preparation method of the optical fiber coloring ink of above-mentioned radiation-hardenable is: by said ratio, weigh each raw material components, dispersion machine is used to stir 60 minutes at about 40 DEG C with the rotating speed of 1000 revs/min, after light trigger and aided initiating are completely dissolved, use 1500 order filters to filter, be placed in 40 DEG C of baking ovens deaeration and get product after 1 day optical fiber coloring ink.
The viscosity of the optical fiber coloring ink prepared by the present embodiment is 1901mpa.s (25 DEG C), and elongation at break is 5.1%, and specific modulus (2.5% elongation) is 1012MPa, and tensile strength is 31MPa.
The coating test of optical fiber coloring ink:
Decay refers to the phenomenon that in fiber middle light signal transmitting procedure, signal intensity dies down, and the decay of optical fiber is to measure by the decay testing method provided in GB GB/T15972 " Fiber Optic Test method specification ". The solvent resistance of optical fiber coloring ink of radiation-hardenable described in embodiment 1-4, the compatibility are all tested according to GJB6792-2009 optical fiber coloring ink specification, being respectively adopted domestically produced machine and import M-S machine carries out painted experiment, result is respectively in Table 1 and table 2.
Table 1-domestically produced machine colouring results
Table 2-import M-S machine colouring results
No matter the optical fiber coloring ink prepared through above-mentioned formula is the extraordinary effect that all played on domestically produced machine or import machine, and painted front and back optical fiber attenuation is almost constant, and solvent resistance, the compatibility simultaneously is all better.
The above is only the preferred embodiment of the present invention, it is noted that for the person of ordinary skill of the art, without departing from the concept of the premise of the invention, it is also possible to making some improvement and conversion, these broadly fall into protection scope of the present invention.

Claims (7)

1. the optical fiber coloring ink of a radiation-hardenable, it is characterised in that by weight percentage, the content of its each component is: mill base 1-20%, reactive diluent 20-40%, auxiliary agent 0.5-4%, UV resin 40-60%, light trigger and aided initiating 3-10%, each component sum meets 100%;
By weight percentage, its each constituent content is described mill base: pigment 10-50%, reactive diluent 30-70%, urethane acrylate 3-20%, defoamer 1-2%, wetting dispersing agent 3-10%, and each component sum meets 100%;
Described reactive diluent is 4-tert-butylcyclohexyl acrylate, isodecyl acrylate, ethoxyethoxyethyl acrylate, 2-phenoxy group acrylate, ring trimethylolpropane dimethoxym ethane acrylate, trimethylolpropane trimethacrylate, two-trimethylolpropane tetra-acrylate, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, double pentaerythritol methacrylate, propylene glycol diacrylate, tripropylene glycol diacrylate, 1, 6-hexanediyl ester, neopentylglycol diacrylate, (2) third oxidation neopentylglycol diacrylates, (3) third oxidation trimethylolpropane trimethacrylates, (3) ethoxyquin trimethylolpropane trimethacrylate, glycerol propoxylate triacrylate, isobornyl acrylate, one or more in glycol phthalate mixture in any proportion,
Described UV resin is one or more mixture in any proportion of urethane acrylate, epoxy acrylate, polyester acrylate, amino acrylates, by weight percentage, its each constituent content is the amino acrylates of the urethane acrylate of 0-100%, the epoxy acrylate of 0-60%, 0-30% polyester acrylate, 0-60%.
2. the optical fiber coloring ink of a kind of radiation-hardenable according to claim 1, it is characterized in that described auxiliary agent includes levelling agent, defoamer, antioxidant, antistatic additive, by weight percentage, its each constituent content is the antistatic additive of the levelling agent of 10-30%, the defoamer of 10-20%, the antioxidant of 5-15%, 35-60%.
3. the optical fiber coloring ink of a kind of radiation-hardenable according to claim 2, it is characterised in that described levelling agent is organic silicon modified by polyether, polyester resin change properties of organic silicon and one or more mixture in any proportion of Organic fluoride modification acrylate apoplexy due to endogenous wind; Described defoamer is one or more mixture in any proportion in the non-silicon defoaming agent of polyacrylate or organic silicon defoamer; Described antioxidant is selected from the mixture of one or more arbitrary proportions of hydroquinone, benzoquinone, tert-butylhydroquinone, t-butyl catechol, methyl hydroquinone, 2,6-di-tert-butyl-4-methy phenols, p methoxy phenol, IRGANOX1010, IRGANOX1035, IRGANOX1076, IRGANOX1222; Described antistatic additive is cationic antistatic agent, anionic antistatic agent and non-ionic antistatic agent.
4. the optical fiber coloring ink of a kind of radiation-hardenable according to claim 1, it is characterised in that described urethane acrylate includes polyether urethane and polyester-polyurethane acrylate.
5. the optical fiber coloring ink of a kind of radiation-hardenable according to claim 1, it is characterised in that described light trigger and aided initiating, its each constituent content is by weight percentage: the light trigger of 70-90%, 10-30% aided initiating.
6. the optical fiber coloring ink of a kind of radiation-hardenable according to claim 1, it is characterized in that described light trigger is selected from benzophenone, 4-phenyl benzophenone, 4-methyl benzophenone, 4-benzoyl-4 '-methyl-diphenyl sulfide, methyl benzoylformate, benzoin dimethylether, 2, 4, 6-trimethylbenzoyl diphenyl phosphate oxidation, 2, 4, 6-trimethylbenzoyl phosphinic acid ethyl ester, double, two (2, 4, 6-trimethylbenzene methylacyl) phenylphosphine oxide, 2-methyl isophthalic acid-(4-first mercaptophenyl)-2-morpholine-1-acetone, 1-hydroxy cyclohexyl phenylketone, 2-hydroxy-2-methyl-1-phenylacetone, ��, ��-diethoxy acetophenone, 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone, 2-isopropyl thioxanthone, 2, 4-diethyl thioxanthone, 2-chlorothiaxanthenone, the chloro-4-propoxyl group thioxanthone of 1-, o-benzoyl yl benzoic acid methyl ester, one or more in light trigger 754 mixture in any proportion.
7. the optical fiber coloring ink of a kind of radiation-hardenable according to claim 1, it is characterized in that described aided initiating includes but not limited to one or more mixture in any proportion in the CN371 of 4 (N, N dimethylamino) ethyl benzoate, the 4 different monooctyl esters of dimethylaminobenzoic acid, tertiary amine groups acrylate, Sartomer.
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