CN102746787A - Optical fiber coating paint transmittable for deep ultraviolet light - Google Patents
Optical fiber coating paint transmittable for deep ultraviolet light Download PDFInfo
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- CN102746787A CN102746787A CN201210210347XA CN201210210347A CN102746787A CN 102746787 A CN102746787 A CN 102746787A CN 201210210347X A CN201210210347X A CN 201210210347XA CN 201210210347 A CN201210210347 A CN 201210210347A CN 102746787 A CN102746787 A CN 102746787A
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Abstract
The invention provides optical fiber coating paint transmittable for deep ultraviolet light, a preparation method and an application thereof. The optical fiber coating paint transmittable for deep ultraviolet light comprises 70-83% (by weight) of aliphatic polyurethane acrylate, 15-28% (by weight) of active diluents, 0.05-1% (by weight) of additives, and 1-3% (by weight) of photoinitiators. The optical fiber coating paint of the invention has excellent mechanical properties and tolerance, can be etched directly without stripping, and can improve grating intensity and reliability.
Description
Technical field
The present invention relates to a kind of optical-fibre coating coating, be specifically related to a kind of optical-fibre coating coating of DUV.
Background technology
Along with the widespread use of optical-fibre communications, optical attenuator, FIBER OPTIC SENSORS etc., fiber grating became one of fiber optic component of speed with fastest developing speed in recent years.Extensively adopt phase place light shield method directly to inscribe fiber grating at present, form the phase place light shield by certain cycle etching glass earlier, utilize the 248nmKBr laser light to see through this phase place light shield exposure optical fiber again and inscribe grating.
Because optical fiber need apply certain coating as impact plies when drawing moulding, protect optical fiber to avoid ectocine, keeps its physical strength and optical characteristics.And before inscribing fiber grating, need the peeling optical fibre coat; This not only can cause damage to optical fiber, reduce the intensity at grating position; And the later stage also to carry out complicacy cover and mould and handle or the metal covering protection, may make grating position discontinuity, influence the sensitivity of grating; Also increase the size and the quality of grating, influenced the making and the stability of optical fibre device.
Therefore, need provide a kind of DUV the optical-fibre coating coating and its production and use avoid the influence of above-mentioned unfavorable factor.
Summary of the invention
The object of the invention is that a kind of optical-fibre coating coating that can directly utilize the KBr laser light to inscribe and have the passed through DUV of excellent mechanical property and tolerance performance is provided.
For realizing foregoing invention purpose of the present invention, the present invention adopts following technical scheme:
A kind of optical-fibre coating coating of DUV comprises weight percentage: 70 ~ 83% aliphatic urethane acrylates, 15 ~ 28% reactive thinners, 0.05 ~ 1% auxiliary agent and 1 ~ 3% light trigger.
Aliphatic urethane acrylate among the present invention; Be polymerized by aliphatic diisocyanate, divalent alcohol and crylic acid hydroxy ester; Water white transparency; About 5500 ~ the 6000cp of viscosity, wherein the molar ratio of divalent alcohol and aliphatic diisocyanate is 0.9 ~ 1.0:1, the molar ratio of crylic acid hydroxy ester and aliphatic diisocyanate is between 1.05 ~ 1:1.
Aliphatic diisocyanate is a kind of in isophorone diisocyanate, dicyclohexyl methane diisocyanate, trimethylammonium hexamethylene diisocyanate, the six hydrogen methyl vulcabond.Divalent alcohol is 1, a kind of in 6-pinakon, glycol ether, polyether Glycols, polyester diol, the end hydroxyl silicone oil.Crylic acid hydroxy ester is a kind of in Rocryl 400, Rocryl 410, Hydroxyethyl acrylate, the Propylene glycol monoacrylate.
The present invention when synthetic fat family urethane acrylate, the preferred isophorone diisocyanate of aliphatic diisocyanate.Because coating is in exposure process, the 248nm laser light itself has stronger power, prolongs with irradiation time; The local certain high temperature that produces causes ammonia ester bond to decompose, and makes coating produce the xanthochromia phenomenon; And the isophorone diisocyanate ammonia ester bond is very stable, has splendid tolerance.
The present invention is when synthetic fat family urethane acrylate, and preferred divalent alcohol is end hydroxyl silicone oil or polyester diol.
The present invention is in preparation can pass through the optical-fibre coating coating of DUV the time, and preferred aliphatic urethane acrylate is for by hydroxypropyl silicone oil synthetic aliphatic urethane acrylate and the aliphatic urethane acrylate that formed with the mixed of weight ratio 0.6 ~ 1.3:1 by aliphatic polyester binary alcohol synthetic aliphatic urethane acrylate.The coating that makes with this scheme has splendid tensile strength, extension property and water-fast, medium-resistance.
Hydroxypropyl silicone oil has good kindliness and high and low temperature resistance, and preferred molar mass is 1200 ~ 2000g/mol, and hydroxy radical content is 1.7% ~ 2.8%.Aliphatic polyester binary alcohol is because the existence of ester bond; Make coating obtain excellent physical strength and medium-resistance; Preferred aliphatic polyester binary alcohol is formed by hexanodioic acid, glycol ether or TriMethylolPropane(TMP) condensation, and its molecular weight is about 500 ~ 1500, hydroxy radical content 1.3% ~ 5.0%.
The present invention considers that the preferred crylic acid hydroxy ester of coating yellowing resistance and reactive behavior is a Hydroxyethyl acrylate when synthetic fat family urethane acrylate.
Reactive thinner of the present invention is contract in propylene glycol diacrylate, tripropylene glycol diacrylate, the Viscoat 295 one or more of Bing Xisuandingzhi, ethyl acrylate, IBOA, methoxy polyethylene glycol methacrylate-styrene polymer, 1,6 hexanediol diacrylate, two.
Auxiliary agent of the present invention comprises photostabilizer, skimmer, flow agent etc.
Light trigger of the present invention is made up of the mixed light initiator more than three kinds or three kinds at least, comprises 2-hydroxy-2-methyl-1-phenyl-1-acetone (Darocur 1173D), 2-methyl isophthalic acid-(4-first sulfydryl phenyl)-2-morpholine-1-acetone (Irgacure 907), 1-hydroxyl-cyclohexyl benzophenone (Irgacure 184), UVNUL MS-40 (BP) etc.
The dope viscosity of the present invention's preparation is about 2000cp ~ 4000cp.Above-mentioned coating is coated on optical fiber surface through drawing process; And form through ultraviolet light polymerization and can pass through DUV optical-fibre coating coating, the transmitance of its 248nm DUV is greater than 60%, tensile strength >=20MPa; Elongation >=40% can use in-45 ℃ ~ 80 ℃ TRs.
The present invention also provides a kind of method for preparing the optical-fibre coating coating of above-mentioned passed through DUV, and this method comprises:
(1) synthetic fat family urethane acrylate: in having the reaction flask of agitating heater, at first add divalent alcohol, start and stir and the slow nitrogen that feeds, be warming up to 60 ℃ ~ 65 ℃ insulations 30 minutes; Be cooled to 45 ℃ ~ 55 ℃ subsequently, add aliphatic diisocyanate and catalyzer, the molar ratio of said divalent alcohol and said aliphatic diisocyanate is 0.9 ~ 1.0; Said catalyzer accounts for 0.05% ~ 0.2% of the gross weight that feeds intake; Insulation reaction 2 hours continues heating, treats to be incubated 1 hour when temperature rises to 50 ℃ ~ 60 ℃; The end that forms-NCO prepolymer is adopted Di-n-Butyl Amine titration measuring NCO content; In 40 ℃ ~ 60 ℃ adding crylic acid hydroxy esters and stopper, the molar ratio of said crylic acid hydroxy ester and said aliphatic diisocyanate is between 1.05 ~ 1 then, and said stopper accounts for 0.005% ~ 0.02% of said crylic acid hydroxy ester weight; Insulation reaction to NCO group complete reaction, it is subsequent use to lower the temperature;
(2) preparation: the light trigger of the auxiliary agent and 1 ~ 3% (weight) of the reactive thinner, 0.05 ~ 1% (weight) of 15 ~ 28% (weight) is joined in the aliphatic urethane acrylate of step (1) preparation of 70 ~ 83% (weight); Deaeration behind the dispersion homogeneous adopts ultra-violet lamp to be cured at last after in light tight container, mixing.
Wherein, said catalyzer is a dibutyl tin laurate, and said stopper is p methoxy phenol or Resorcinol.
The present invention also provides a kind of optical-fibre coating coating application on the supercoat outside preparation optical fiber of above-mentioned DUV.
The optical-fibre coating coating of DUV of the present invention has excellent mechanical property and tolerance performance, and this coating can directly be inscribed without just divesting, and has improved the intensity and the safety of grating.
Description of drawings
Fig. 1 is preparation technology's schema of the optical-fibre coating coating of DUV of the present invention.
Embodiment
Below, the present invention is further specified, but the present invention is not limited to these embodiment through exemplary embodiments.
The preparation method of the optical-fibre coating coating of DUV of the present invention is:
Synthetic fat family urethane acrylate at first: in having the reaction flask of agitating heater, at first add divalent alcohol; Start and stir and slowly feed nitrogen; Be warming up to 60 ℃ ~ 65 ℃ insulations 30 minutes, purpose is to remove the moisture that divalent alcohol forms in storage process.Be cooled to 45 ℃ ~ 55 ℃ subsequently; Add aliphatic diisocyanate and catalyzer dibutyl tin laurate (account for the gross weight that feeds intake 0.05% ~ 0.2%); Wherein the molar ratio of divalent alcohol and aliphatic diisocyanate is 0.9 ~ 1.0, and insulation reaction 2 hours continues heating; Treat to be incubated 1 hour when temperature rises to 50 ℃ ~ 60 ℃, the end that forms-NCO prepolymer is adopted Di-n-Butyl Amine titration measuring NCO content.Add crylic acid hydroxy esters and a small amount of stopper (account for crylic acid hydroxy ester weight 0.005% ~ 0.02%) in 40 ℃ ~ 60 ℃ then; The molar ratio of crylic acid hydroxy ester and aliphatic diisocyanate between 1.05 ~ 1, insulation reaction to NCO group complete reaction.It is subsequent use to lower the temperature.
Then, get above-mentioned aliphatic urethane acrylate, add reactive thinner, auxiliary agent and light trigger blending dispersion homogeneous, deaeration in proportion and make and to pass through DUV optical-fibre coating coating.Above-mentioned coating is added wire-drawer-tower, can solidify by 80 meters/minute wire drawing UV, prepare the optical-fibre coating coating that to pass through DUV.
The embodiment for preparing aliphatic urethane acrylate of the present invention is following:
Embodiment 1
In reaction flask, at first add hydroxypropyl silicone oil 778.2g (molecular weight 1730, hydroxy radical content 1.96%), start stirring; Logical nitrogen, and be warming up to 60 ℃ ~ 65 ℃ insulations 30 minutes, be cooled to 50 ℃ ~ 55 ℃; Drip the mixture of isophorone diisocyanate 200g and catalyzer dibutyl tin laurate 0.68g, dripped off in 1 hour, in 50 ℃ ~ 55 ℃ insulations 2 hours; Slowly be warming up to 55 ℃ ~ 60 ℃ insulations 1 hour subsequently, adopt the Di-n-Butyl Amine method to measure NCO content≤3.86%; Be cooled to 45 ℃ ~ 55 ℃, dropwise addition of acrylic acid hydroxyl ethyl ester 109.6g and stopper p methoxy phenol 0.01g, drip off half a hour the back in 45 ℃ ~ 55 ℃ insulation reaction to NCO content≤0.10%.The cooling of qualified back is subsequent use.
Embodiment 2
In reaction flask, at first add polyester diol (molecular weight 1308, hydroxy radical content 1.3%) 588.4g, start stirring; Logical nitrogen, and be warming up to 60 ℃ ~ 65 ℃ insulations 30 minutes, be cooled to 45 ℃ ~ 50 ℃; Drip isophorone diisocyanate 200g and dibutyl tin laurate 0.55g mixture, dripped off in 1 hour, in 45 ℃ ~ 50 ℃ insulations 2 hours; Slowly be warming up to 50 ℃ ~ 60 ℃ insulations 1 hour subsequently, adopt the Di-n-Butyl Amine method to measure NCO content≤2.77%; Be cooled to 40 ℃ ~ 50 ℃, dropwise addition of acrylic acid hydroxyl ethyl ester 109.6g and hydroquinone of polymerization retarder 0.01g drip off the back half a hour in 40 ℃ ~ 50 ℃ insulation reaction, react to NCO content≤0.10%.The cooling of qualified back is subsequent use.
Embodiment 3
In reaction flask, at first add polyether Glycols N210:450g, start stirring, logical nitrogen; And be warming up to 60 ℃ ~ 65 ℃ insulations 30 minutes, and be cooled to 45 ℃ ~ 50 ℃, drip six hydrogen methyl vulcabond 162g and dibutyl tin laurate 0.67g mixture; Dripped off in 1 hour; In 45 ℃ ~ 50 ℃ insulations 2 hours, slowly be warming up to 55 ℃ ~ 60 ℃ insulations 1 hour subsequently, adopt the Di-n-Butyl Amine method to measure NCO content≤5.77%; Be cooled to 50 ℃ ~ 60 ℃, dropwise addition of acrylic acid hydroxyl ethyl ester 104.4g and p methoxy phenol 0.01g drip off the back half a hour in 55 ℃ ~ 60 ℃ insulation reaction, react to NCO content≤0.10%.The cooling of qualified back is subsequent use.
The embodiment of the optical-fibre coating coating of preparation DUV of the present invention is following:
Embodiment 4
Get the aliphatic urethane acrylate 310g of embodiment 1 preparation; Add Viscoat 295 80g; The two propylene glycol diacrylate 30g that contract; Light trigger Darocur1173D:5.4g, BP:2.7g, Irgacure 907:2.7g, flow agent BYK-UV3530 0.21g, photostabilizer diethylamine: 0.2g.Deaeration behind the dispersion homogeneous after in light tight container, mixing.This coating water white transparency, viscosity 4000cp adopts U.S. Fusion UV 3KW ultra-violet lamp that above-mentioned coating is cured, thickness 60 μ m, curing speed is less than 0.5s.
Testing coating performance: tensile strength 12.72MPa; Elongation 56.61%; 248nm DUV transmitance 67%.
Embodiment 5
Get the aliphatic urethane acrylate 310g of embodiment 2 preparations, add tripropylene glycol diacrylate 40g, 1; 6-hexanediyl ester 18g, Darocur 1173D:4.7g, BP:2.3g; Irgacure184:2.3g, BYK-UV3530:0.19g, diethylamine: 0.18g.Deaeration behind the dispersion homogeneous after in light tight container, mixing.This coating water white transparency, viscosity 3600cp adopts U.S. Fusion UV 3KW ultra-violet lamp that above-mentioned coating is cured, thickness 60 μ m, curing speed is less than 0.5s.
Testing coating performance: tensile strength 16.72MPa; Elongation 46.91 %; 248nm DUV transmitance 64%.
Embodiment 6
Get the aliphatic urethane acrylate 125g of embodiment 1 preparation, the aliphatic urethane acrylate 185g of embodiment 2 preparations adds Viscoat 295 35g; The two propylene glycol diacrylate 40g that contract, methoxy polyethylene glycol methacrylate-styrene polymer (CD550) 15g, Darocur1173D:5.0g; BP:2.5g; Irgacure 184:2.5g, BYK-UV3530 0.2g, diethylamine: 0.19g.Deaeration behind the dispersion homogeneous after in light tight container, mixing.This coating water white transparency, viscosity 4000cp adopts U.S. Fusion UV 3KW ultra-violet lamp that above-mentioned coating is cured, thickness 60 μ m, curing speed is less than 0.5s.
Testing coating performance: tensile strength 20.09MPa; Elongation 42.23%; 248nm DUV transmitance 66%, 80 ℃ of 200h coatings of heatproof are no abnormal, and coating lucifuge sealing stores that viscosity does not increase after 6 months.
DUV optical-fibre coating coating of the present invention, through ultraviolet light polymerization, the transmitance of its 248nm DUV is greater than 60%, has excellent mechanical property and tolerance performance, can be outside high-speed wire-drawing prepared optical fiber supercoat.This coating is mainly used in the inscription fiber grating, and coating can directly be inscribed (can directly utilize the KBr laser light to inscribe the preparation fiber grating) without just divesting, and has improved the intensity and the safety of grating.Applicable field comprises aspects such as aircraft health monitoring systems, fibre optic hydrophone, transmitter detection and supervisory system, civil defence earthquake monitoring, bridge tunnel monitoring, the monitoring of safe antitheft sensing.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any professional and technical personnel of being familiar with possibly utilize the technology contents of above-mentioned announcement to change or be modified as the equivalent embodiment of equivalent variations.But everyly do not break away from technical scheme content of the present invention, to any simple modification, equivalent variations and remodeling that above embodiment did, still belong to the protection domain of technical scheme of the present invention according to technical spirit of the present invention.
Claims (10)
1. optical-fibre coating coating that can pass through DUV comprises weight percentage: 70 ~ 83% aliphatic urethane acrylate, 15 ~ 28% reactive thinner, 0.05 ~ 1% auxiliary agent and 1 ~ 3% light trigger.
2. optical-fibre coating coating as claimed in claim 1; It is characterized in that; Said aliphatic urethane acrylate is polymerized by aliphatic diisocyanate, divalent alcohol and crylic acid hydroxy ester; Viscosity is 5500 ~ 6000cp, and the mol ratio of wherein said divalent alcohol and said aliphatic diisocyanate is 0.9 ~ 1.0:1, and the mol ratio of said crylic acid hydroxy ester and said aliphatic diisocyanate is 1.05 ~ 1:1.
3. optical-fibre coating coating as claimed in claim 2 is characterized in that, said aliphatic diisocyanate is a kind of in isophorone diisocyanate, dicyclohexyl methane diisocyanate, trimethylammonium hexamethylene diisocyanate, the six hydrogen methyl vulcabond.
4. optical-fibre coating coating as claimed in claim 2; It is characterized in that; Said divalent alcohol is 1; A kind of in 6-pinakon, glycol ether, polyether Glycols, polyester diol, the end hydroxyl silicone oil, being preferably molar mass is that 1200 ~ 2000g/mol, hydroxy radical content are 1.7% ~ 2.8% hydroxypropyl silicone oil or are formed by hexanodioic acid, glycol ether or TriMethylolPropane(TMP) condensation, molecular weight is 500 ~ 1500, hydroxy radical content is 1.3% ~ 5.0% aliphatic polyester binary alcohol.
5. like the described optical-fibre coating coating of claim 2-4, wherein said aliphatic urethane acrylate is for by said hydroxypropyl silicone oil synthetic aliphatic urethane acrylate and the aliphatic urethane acrylate that formed with the mixed of weight ratio 0.6 ~ 1.3:1 by said aliphatic polyester binary alcohol synthetic aliphatic urethane acrylate.
6. optical-fibre coating coating as claimed in claim 2 is characterized in that, said crylic acid hydroxy ester is a kind of in Rocryl 400, Rocryl 410, Hydroxyethyl acrylate, the Propylene glycol monoacrylate.
7. optical-fibre coating coating as claimed in claim 1; It is characterized in that; Said reactive thinner is contract in propylene glycol diacrylate, tripropylene glycol diacrylate, the Viscoat 295 one or more of Bing Xisuandingzhi, ethyl acrylate, IBOA, methoxy polyethylene glycol methacrylate-styrene polymer, 1,6 hexanediol diacrylate, two; Said auxiliary agent is one or more in photostabilizer, skimmer, the flow agent; Said light trigger is made up of the light trigger that is selected from 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-methyl isophthalic acid-(4-first sulfydryl phenyl)-2-morpholine-1-acetone, 1-hydroxyl-cyclohexyl benzophenone, UVNUL MS-40 more than three kinds or three kinds at least.
8. method for preparing the optical-fibre coating coating of DUV as claimed in claim 1 comprises:
(1) synthetic fat family urethane acrylate: in having the reaction flask of agitating heater, at first add divalent alcohol, start and stir and the slow nitrogen that feeds, be warming up to 60 ℃ ~ 65 ℃ insulations 30 minutes; Be cooled to 45 ℃ ~ 55 ℃ subsequently, add aliphatic diisocyanate and catalyzer, the molar ratio of said divalent alcohol and said aliphatic diisocyanate is 0.9 ~ 1.0:1; Said catalyzer accounts for 0.05% ~ 0.2% of the gross weight that feeds intake; Insulation reaction 2 hours continues heating, treats to be incubated 1 hour when temperature rises to 50 ℃ ~ 60 ℃; The end that forms-NCO prepolymer is adopted Di-n-Butyl Amine titration measuring NCO content; In 40 ℃ ~ 60 ℃ adding crylic acid hydroxy esters and stopper, the molar ratio of said crylic acid hydroxy ester and said aliphatic diisocyanate is 1.05 ~ 1:1 then, and said stopper accounts for 0.005% ~ 0.02% of said crylic acid hydroxy ester weight; Insulation reaction to NCO group complete reaction, it is subsequent use to lower the temperature;
(2) preparation: the reactive thinner of 15 ~ 28% weight percentage, the auxiliary agent of 0.05 ~ 1% weight percentage and the light trigger of 1 ~ 3% weight percentage are joined in the aliphatic urethane acrylate like step (1) preparation of 70 ~ 83% (weight percentage); Deaeration behind the dispersion homogeneous adopts ultra-violet lamp to be cured at last after in light tight container, mixing.
9. method as claimed in claim 8, wherein said catalyzer are dibutyl tin laurate; Said stopper is p methoxy phenol or Resorcinol.
10. the optical-fibre coating coating of a DUV as claimed in claim 1 application on the supercoat outside preparation optical fiber.
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| CN103030768A (en) * | 2013-01-06 | 2013-04-10 | 久盛地板有限公司 | Polyurethane acrylate prepolymer and preparation method thereof as well as paint prepared by same |
| CN103396518A (en) * | 2013-08-26 | 2013-11-20 | 张家港康得新光电材料有限公司 | Organic silicon modified water-based acrylate resin and preparation method thereof |
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| CN103774448A (en) * | 2013-05-03 | 2014-05-07 | 江南大学 | Method for flame-proof treatment of textiles based on light curing method |
| CN103396518A (en) * | 2013-08-26 | 2013-11-20 | 张家港康得新光电材料有限公司 | Organic silicon modified water-based acrylate resin and preparation method thereof |
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