CN107418423A - It is a kind of to be used to protect the UV LED of telecommunication optical fiber coating material solidified - Google Patents
It is a kind of to be used to protect the UV LED of telecommunication optical fiber coating material solidified Download PDFInfo
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- CN107418423A CN107418423A CN201710598773.8A CN201710598773A CN107418423A CN 107418423 A CN107418423 A CN 107418423A CN 201710598773 A CN201710598773 A CN 201710598773A CN 107418423 A CN107418423 A CN 107418423A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Surface Treatment Of Glass Fibres Or Filaments (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
Abstract
It is used to protect the UV LED of telecommunication optical fiber coating material solidified the invention discloses a kind of, belongs to fine painting product scope.The invention includes fiber inner layer coating and fiber outer layer coating, fiber inner layer coating directly contact with optical fiber surface, and fiber outer layer coating is coated in interlayer coatings surface, and fiber inner layer coating includes the raw material of following mass numbers：Interlayer coatings oligomer 60% 80%, interlayer coatings reactive diluent 15% 35%, interlayer coatings light trigger 4.0% 6.0%, interlayer coatings function additive 0.6% 6.5%, fiber outer layer coating includes the raw material of following mass numbers：Outer layer coating oligomer 20% 35%, epoxy acrylate 30% 45%, outer layer coating reactive diluent 15% 35%, outer layer coating light trigger 6.0% 8.0%, outer layer coating function additive 0.6% 6.5%.Inventive formulation composition is reasonable, prepares that the structural regularity of oligomer is good, and coated fiber has enough mechanical strengths and excellent optical property, is effectively improved optic communication quality and optical fiber service life, meets the needs used.
Description
Technical field
The present invention relates to a kind of coating, more particularly to it is a kind of be used to protect the UV-LED of telecommunication optical fiber coating material solidified, belong to
Fine painting product scope.
Background technology
Optical fiber abbreviation optical fiber (optical fiber), it is one kind fine-fibrous made of quartz glass is doped
Material, when light by when can form total reflection and carry out signal transmission.Therefore have and low, small volume, bandwidth is lost, resists and does
Disturb, be in light weight, efficiency high many advantages, such as, be used as the transmission medium of bulk information, the popularization and application of optical fiber is modern logical
Letter is laid a good foundation.
Optical fiber coatings be used for protect optical glass fibre to exempt to be affected by the external environment, keep its enough mechanical strength and
The coating of excellent optical property.Optical fiber coats one layer of soft cushion and applied as optical fiber internal layer first in wire-drawing shape
Material, one layer of fiber outer layer coating tough and tensile, wear-resisting, chemical resistance and ageing properties are excellent is then coated with, is thus combined into light
Fine protection system.High-performance optical fiber coating can effectively improve optic communication quality and optical fiber service life, so as to reduce light net into
This, improves the stability of wide-band-message network.Optical fiber coatings are generally made up of fiber inner layer coating and fiber outer layer coating,
Inside and outside coating is respectively by two coating cups during drawing optical fibers, the one-shot forming after ultraviolet lighting solidifies.Optical fiber inside and outside coating point
Do not formed by prepolymer, reactive diluent, light trigger and function additive according to the combination allotment of specific ratio.The performance of optical fiber
The structure of prepolymer is depended primarily on, when the molecular structure of prepolymer is controllable, molecular weight and molecular weight distribution for the moment, are referred to as neat
Polymers, otherwise referred to as oligomer.Acrylic carbamate is a kind of prepolymer containing more block structures, more by macromolecular
Acrylate reactions of first alcohol with diisocyanate and containing hydroxyl generate.When macromolecular polyol flocks together, formed
The glass transition temperature (Tg) of segment microcell is less than room temperature, referred to as rubber phase.And carbamate association together when, shape
Glass transition temperature (Tg) into segment microcell is higher than room temperature, at normal temperatures in glassy state, crystallite or paracrystalline state, therefore also
They are referred to as plastics phase.Due to existing incompatibility between hard and soft chain segment microcell, cause micro phase separation structure occur.Acrylic acid
Aminocarbamic acid ester can be fitted in building-up process by changing in molecular structure the content of hard and soft chain segment, species and molecular weight
Answer the requirement in the fields such as optical fiber coatings, damping material, functional material.Polymerization methodses also can be a variety of, such as initiator, electron beam, spoke
According to and ultraviolet light Deng , And can be copolymerized with various vinyl monomers, obtained in the preparation of optical fiber coatings extensive
Using.
Optical fiber is often synthesized with acrylic carbamate prepolymer with the method for fractional steps：One method is first acrylic acid synthesizing base Dan Yi
Cyanate, then add macromolecular diol chain extension.Another method is first to be reacted by excess diisocyanate and macromolecular diol, then
Add 2- hydroxyalkyl acrylates end-blocking.Patent document CN1651533A discloses one kind and uses toluene di-isocyanate(TDI) (TDI)
Reacted with the mixture of IPDI (IPDI) with PPG, prepare the acrylic acid available for optical fiber coatings
The urethane oligomer of esterification, can reduce coating material solidified crystallinity, but the aromatic structure and IPDI due to TDI
Existing-NCO reactivity differences between alicyclic structure, it can finally cause the structure of synthetic product more chaotic.
CN1456622, which proposes to mix the propenoic methyl carbamate of HMW and the propenoic methyl carbamate of low molecule amount, to be made
With the number-average molecular weight for controlling the oligomer of free redical polymerization is 800-10000, and is adjusted in optical fiber coatings resin combination
Urethanes connection concentration be 1.85-3.00mol/kg, cured resin coating has preferable toughness and tear-proof strong
Degree, due to the variation of manufacturing process, trouble is with the addition of to production and application.Based on above-mentioned background, patent utilization propylene of the present invention
More block structure characteristics of sour carbamate, reasonably adjust the structure and content of hard and soft chain segment so that manufactured coating applies
After overlaying on optical fiber surface, it can keep optical fiber that there is enough mechanical strengths and excellent optical property, thus form this hair
Bright substance.
The content of the invention
It is used to protect that the UV-LED of telecommunication optical fiber is coating material solidified, and UV-LED is coating material solidified it is an object of the invention to provide a kind of
With preferable toughness and tear resistance, and after this is coating material solidified coated in optical fiber surface, optical fiber can be kept to have
Enough mechanical strengths and excellent chemical fibre performance, improve optic communication quality and optical fiber service life.
The technical solution adopted for the present invention to solve the technical problems is：
It is a kind of to be used to protect the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：It is described to be used to protect telecommunication optical fiber
UV-LED coating material solidified directly connect including fiber inner layer coating and fiber outer layer coating, fiber inner layer coating with optical fiber surface
Touch, fiber outer layer coating is coated in interlayer coatings surface, and the fiber inner layer coating includes the raw material of following mass numbers：Internal layer applies
Material uses oligomer 60%-80%, interlayer coatings reactive diluent 15%-35%, interlayer coatings light trigger 4.0%-
6.0%, interlayer coatings functional agent 0.6%-6.5%, the fiber outer layer coating includes the raw material of following mass numbers：Outer layer applies
Material uses oligomer 20%-35%, epoxy acrylate 30%-45%, outer layer coating reactive diluent 15%-35%, outer layer
Coating light trigger 6.0%-8.0%, outer layer coating function additive 0.6%-6.5%.
Further, the physical parameter of the fiber inner layer coating is：
Before solidification (liquid coating)
Viscosity (mPas/25 DEG C) 5000-7500
Refractive index (25 DEG C) 1.4750-1.5000
Density (kg/m3, 25 DEG C) and 1.03-1.07
After solidification (solid-state coating)
Specific modulus (2.5% bullet becomes, mPa) 1.2-1.5
Elongation (%)>100
Tensile strength (mPa)>0.8
Cure shrinkage (%)<2.5
Glassy bond power (N)>0.7
The physical parameter of the fiber outer layer coating is：
Before solidification (liquid coating)
Viscosity (mPas/25 DEG C) 5000-7500
Refractive index (25 DEG C) 1.500-1.545
Density (kg/m3, 25 DEG C) and 1.10-1.13
After solidification (solid-state coating)
Specific modulus (2.5% bullet becomes, mPa) 600-950
Elongation (%)>10
Tensile strength (mPa)>30
Cure shrinkage (%)<7.0
Further, the interlayer coatings that the fiber inner layer coating includes are interlayer coatings acrylic ammonia with oligomer
Carbamate oligomer, the interlayer coatings reactive diluent is by acrylate, caprolactam, 3 third
Diol acrylate, Nonyl Phenol ethoxylated acrylate and one kind in 2 (2- ethoxy-ethoxies) ethyl propylene acid esters or
It is a variety of to be combined, the interlayer coatings light trigger by 2,4,6- trimethylbenzoy-dipheny phosphorous oxides, it is double (2,
4,6- trimethylbenzoyls) phenylphosphine oxide, 2- benzyls -2- (dimethylamino) -1- (4- (4- morpholinoes) phenyl) -1-
One or more in butanone and 4- benzoyl -4- dimethyl diphenyl sulfides are combined.
Further, the interlayer coatings synthesize system with acrylic carbamic acid ester oligomer by following ingredients reaction
：
(a) propylene oxide polyether polyalcohol and oxirane and propylene oxide copolyethers two of the molecular weight from 2000-6000
At least one of alcohol；
(b) at least one of aromatic diisocyanate and aliphatic diisocyanate；
(c) at least one of hydroxy-end capped acrylate and methacrylate.
Further, the interlayer coatings acrylic carbamic acid ester oligomer is prepared by diisocyanate mistake
The effects of hunger principle that amount and low temperature are added dropwise, target product is generated using step synthesis, reaction temperature is controlled at 40 DEG C -80
℃。
Further, the outer layer coating that the fiber outer layer coating includes is outer layer coating acrylic ammonia with oligomer
Carbamate oligomer, the outer layer coating reactive diluent is by isobornyl acrylate, acrylate, 1,6-
One or more in hexylene glycol double methacrylate and tri-propanediol diacrylate are combined, and the outer layer coating, which is used up, to be drawn
Agent is sent out by 2,4,6- trimethylbenzoy-diphenies phosphorous oxide, double (2,4,6- trimethylbenzoyls) phenylphosphine oxides, double
One or more in 2,6- bis- fluoro- 3- pyrroles's phenyl titanocenes and 4- benzoyl -4- dimethyl diphenyl sulfides are combined.
Further, the outer layer coating synthesizes system with acrylic carbamic acid ester oligomer by following ingredients reaction
：
(a) molecular weight is from least one of 400-2000 propylene oxide polyether polyalcohol；
(b) at least one of aromatic diisocyanate and aliphatic diisocyanate；
(c) at least one of hydroxy-end capped acrylate and methacrylate.
Further, the outer layer coating acrylic carbamic acid ester oligomer be prepared by PPG with
The long-chain midbody product of excessive di-isocyanate reaction generation isocyanate group end-blocking, then by midbody product and carry hydroxyl
(methyl) acrylate reactions generation target product, reaction temperature control at 50 DEG C -110 DEG C.
Interlayer coatings the acrylic carbamic acid ester oligomer and outer layer coating acrylic amino first of the present invention
Acid esters oligomer is respectively provided with following structure：
In formula：R1 is the propylene oxide polyether polyalcohol that number-average molecular weight is 400-6000 or oxirane and epoxy third
Alkane copolyether
Glycol
R2 is one kind in formula
R3 is including at least more than one methylene
R4 is hydrogen atom or methyl
Interlayer coatings the acrylic carbamic acid ester oligomer and outer layer coating acrylic amino first of the present invention
In the building-up process of acid esters oligomer, the diisocyanate of propylene acid blocked can be produced, the carbamate of propylene acid blocked is big
The product of the various structures such as molecular polylol.In order to obtain, molecular weight is homogeneous, double bond is evenly distributed, viscosity is low, storage stability
Good, the internal layer acrylic carbamic acid ester oligomer of structure-controllable, the present invention are preparing interlayer coatings acrylic amino
When formic acid ester oligomer and outer layer coating are with acrylic carbamic acid ester oligomer, the effects of hunger being added dropwise using low temperature is former
Reason, it is the effective way for realizing above-mentioned target to take step synthesis.
Interlayer coatings the acrylic carbamic acid ester oligomer and outer layer coating acrylic amino first of the present invention
Acid esters oligomer during using method of fractional steps synthesis, by equimolar than toluene di-isocyanate(TDI) and 2- hydroxy acrylic acid second
Ester reaction generation acrylic monoisocyanates, handles synthetic reaction dynamics data with linear fitting, obtains following result：
The condensation of toluene di-isocyanate(TDI) and 2- hydroxyl ethyl acrylates is second order reaction, reaction activity 64.9KJ/MOL, and such as
Fruit is first reacted by the toluene di-isocyanate(TDI) and PTMEG of excess, and reaction dynamics data is handled with above-mentioned identical method,
Obtained reaction activity is 36.2KJ/MOL.Toluene di-isocyanate(TDI) is more than toluene with PTMEG reactivity as can be seen here
The reactivity of diisocyanate and 2- hydroxyl ethyl acrylates, because vinyl existing for 2- hydroxyl ethyl acrylates is total to
Caused by yoke effect.In addition, the structural regularity of toluene di-isocyanate(TDI) is poor, and Existential Space steric effect, contraposition and ortho position-
NCO activity differences are larger, and existing active difference is raised and reduced with reaction temperature between this reactive group, improve
Reaction temperature is more beneficial for improving the reaction of the slower group of reaction speed.Therefore, reduce between differential responses active group
Gap.Test result indicates that：Acrylic carbamic acid ester oligomer active group can be improved using relatively low reaction temperature
Reaction selectivity between group, as a result it is beneficial to control the molecular structure of synthetic product, is taken off so as to be advantageously implemented the present invention
The target product that the molecular weight that shows is homogeneous, double bond is evenly distributed, segmented structure is controllable.
Preferably expoxy propane gathers in the building-up process of the interlayer coatings acrylic carbamic acid ester oligomer of the present invention
Ethoxylated polyhydric alcohol, its glass transition temperature are less than room temperature, commonly referred to as soft chain segment.Propylene oxide polyether polyalcohol stability to hydrolysis resistance
Good, structural regularity is poor, and strand is submissive, is not easy to crystallize.Particularly number-average molecular weight is more more than 2000 propylene oxide polyether
The acrylic carbamic acid ester oligomer of first alcohol synthesis, cryogenic property and excellent stability due to its protrusion are especially suitable
Together in fiber inner layer coating of the preparation with relatively low modulus.The acrylic synthesized by macromolecule propylene oxide polyether polyalcohol
Shortcoming existing for carbamic acid ester oligomer is exactly that refractive index is relatively low, it usually needs introduces the diisocyanate with benzene ring structure
To improve refractive index, but in order to avoid crystallite behavior caused by the rigid structure of phenyl ring, the carbamate that it is formed is existed
Concentration and its distribution in strand must be controlled strictly, thus further illustrate the internal layer acrylic amino first of the present invention
Importance of the structural regularity of acid esters oligomer in high-performance optical fiber coating is prepared.
The architectural feature of the interlayer coatings that the present invention synthesizes acrylic carbamic acid ester oligomer：At least containing one kind
Number-average molecular weight is 2000-6000 PPG, and PPG is gathered from oxirane PPG, expoxy propane
One or more in ethoxylated polyhydric alcohol, tetrahydrofuran polyether polyalcohol and copolymerization ethoxylated polyhydric alcohol, PPG of the invention are excellent
Ring selection Ethylene Oxide PPG, the copolymerization ethoxylated polyhydric alcohol particularly preferably synthesized by oxirane with expoxy propane.Two isocyanic acids
Ester is selected from least one of aromatic diisocyanate and aliphatic diisocyanate, and diisocyanate of the invention is preferably fragrant
Fragrant (cyclo) aliphatic diisocyanates, the refractive index of optical fiber coatings, particularly preferred 2,4- toluene diisocynates can be improved by introducing benzene ring structure
Ester, its ortho position and two isocyanate groups of contraposition cause the difference for reactivity occur due to being influenceed by methyl steric effect, have
Beneficial to the selectivity and structural regularity for improving synthetic product, product viscosity is reduced.Participate in the vinyl double bond of UV-LED solidifications
From the reactant of at least one hydroxy-end capped acrylate or methyl acrylate as initiation material.
The interlayer coatings of the present invention are synthesized with acrylic carbamic acid ester oligomer using the method for fractional steps, first by the first of excess
Phenylene diisocyanate reacts with macromolecular PPG, the polyether-polyurethane of generation isocyanate group end-blocking.In order to control synthesis
Single dimeric structure of product, toluene di-isocyanate(TDI) preferably 2,4- toluene di-isocyanate(TDI)s, the preferred ring of macromolecular PPG
Oxidative ethane and propylene oxide copolyethers dihydric alcohol, reaction temperature are controlled at 40-80 DEG C, preferably 45-60 DEG C.PPG is adopted
Method is fed with substep, keeps-NCO in reaction system to exist all the time in excessive state, the amount of-NCO and-OH material than control
3-5：1, residual monomer is removed by thin-film distillation technology after the completion of reaction, then adds the reaction of 2- hydroxyl ethyl acrylates
The acrylic carbamic acid ester oligomer that the present invention discloses is obtained after being wholly absent to-NCO.
When the interlayer coatings of the present invention prepare fiber inner layer coating with acrylic carbamic acid ester oligomer, interlayer coatings
Controlled with the number-average molecular weight of acrylic carbamic acid ester oligomer between 2000-8000, preferably 2500-5000 it
Between.The mass number of carbamate is 6%-15%, and glass transition temperature is existing micro- between hard and soft chain segment less than -50 DEG C
Phase separation structure is favorably improved the tearing toughness of optical fiber and has good joint stripping performance.
The interlayer coatings acrylic amino first of fiber inner layer coating prepared by the present invention by mass number for 60%-80%
Acid esters oligomer is formed, low in order to obtain glass transition temperature, and low temperature modulus is small, the good target product of tear resistance, excellent
Acrylic polyether-polyurethane is selected, it is poor particular with the propylene oxide polyether polyurethane of pending methyl group, hydrophily, it is not easy to tie
It is brilliant.It is submissive containing excellent low temperature can be provided with the ehter bond (- O-) of internal rotation in propylene oxide polyether polyurethane molecular main chain
Property and hydrolytic stability.The preferred 2600-4600 of number-average molecular weight of acrylic polyether-polyurethane.Molecular weight distributing index is less than
1.5, the molecular weight uniform of the small expression synthetic product of molecular weight distributing index is good, can reduce the viscosity of oligomer, be advantageous to
The optimization of coating property.
Fiber outer layer coating prepared by the present invention is 20%-35% outer layer coating acrylic carbamic acids by mass number
Ester oligomer and mass number are made up of 30%-45% epoxy acrylates, introduce epoxy acrylate except that can improve power
Refractive index can also be improved beyond performance by learning.Epoxy acrylate is by the polymerizable of epihydric alcohol ester compound and acrylic acid
What the carboxylic acid reaction of unsaturated group obtained, conventional has epoxy acrylic glycidol ether and propylene oxide acid glycidyl ester
Class.
The fiber outer layer coating of the present invention needs to have tough and tensile, wear-resisting, chemicals-resistant and ageing resistace, preferentially from low
The propylene oxide polyether polyalcohol synthesis outer layer acrylic carbamic acid ester oligomer of molecular weight.The outer layer of fiber outer layer coating
Coating is controlled between 400-2000 with the number-average molecular weight of acrylic carbamic acid ester oligomer, preferably 600-1600 it
Between, the carbamic acid ester oligomer synthesized using lower molecular weight PPG is advantageous to improve and acrylic acid epoxy resin
Compound compatibility.
In order to further improve the total reflectivity of optic communication, it is beneficial to introduce acrylic acid epoxy resin compounding.Acrylic acid
Epoxy resin has higher adhesion strength and refractive index, and solvent resistance is good.Propylene oxide polyether with low molecule amount is polynary
The outer layer acrylic carbamate of alcohol synthesis has extraordinary compatibility with acrylic acid epoxy resin.Pass through what is coated
The cushioning effect of flexible inner layer coating, the acrylic acid epoxy resin that can be effectively prevented from that there is high modulus volume in low temperature
Modulus change caused by contraction causes transmission loss caused by the microbend of optical fiber, this be also single layer optical fiber paint so far not yet
Wide variety of fundamental cause is obtained in long haul communication optical fiber.
Fiber inner layer coating and fiber outer layer coating prepared by the present invention includes the activity that mass number is 15%-35%
Diluent, reactive diluent is the monomer of the free redical polymerization containing mono-vinyl or more vinyl, in UV-LED photocurings
When directly participate in the reaction of internal layer acrylic carbamic acid ester oligomer and outer layer acrylic carbamic acid ester oligomer, draw
The purpose for entering reactive diluent is to be used to reduce viscosity, improves refractive index, And regulation physical property.As can be seen here, as preferable living
The features such as property diluent must have higher conversion ratio, and volume contraction is small, and viscosity is low, and refractive index is big, and smell is small.And as
The reactive diluent of fiber inner layer coating must also possess sufficiently low glass transition temperature in addition to above-mentioned condition to be met
Degree, crystallinity are small.Pass through the compounding of the various active diluent such as monofunctional vinyl monomer and polyfunctional group vinyl monomer
Use, can be with the viscosity of adjusting coating, refractive index and crosslink density.
The selectable monofunctional vinyl monomer of reactive diluent of the present invention has：2 (2- ethoxy-ethoxies) ethyls
Acrylate, dodecyl methyl acrylate, 0-phenyl phenoxyethyl acrylate, 2- benzene oxygen ethyl propylenes acid esters, (first
Base) isobornyl acrylate, Nonyl Phenol ethoxylated acrylate, NVP etc..Reactive diluent is selectable
Polyfunctional group vinyl monomer has：Ethylene glycol dimethacrylate, dimethacrylate, triethylene glycol diformazan
Base acrylate, tripropylene glycol diacrylate, 1,6- hexylene glycols two (methyl) acrylate, polyethyleneglycol diacrylate,
Ethoxylated bisphenol A diacrylates, ethoxyquin trimethylolpropane trimethacrylate etc..
The fiber inner layer coating and fiber outer layer coating of the present invention needs to use light trigger, and suitable light trigger has：
Acyl group phosphorous oxides, alkyl benzoylbenzoic acid ester, benzil and benzil derivative and benzoin alkylether.Conventional light gathers
Closing initiator has：1- hydroxy cyclohexyl phenylketones, 2,4,6- trimethylbenzoyl diphenyl phosphate oxidations, double (2,4,6- trimethyls
Benzoyl) phenylphosphine oxide, the fluoro- 3- pyrroles's phenyl titanocenes of double 2,6- bis-, 2- methyl isophthalic acids-(4- methyl mercaptos phenyl) -2-
Quinoline base -1- acetone, 2- benzyls -2- (dimethylamino) -1- (4- (4- morpholinoes) phenyl) -1- butanone, 4- benzoyls -4-
Dimethyl diphenyl sulfide etc..Although isopropyl thioxanthone also has higher efficiency of initiation in UV-LED photocurings, it holds
The characteristic for being easily caused xanthochromia limits its application in optical fiber coatings.Compounded using at least one above-mentioned Photoepolymerizationinitiater initiater
Use together, then can effectively improve the high speed curable performance of coating composition.
The interlayer coatings that fiber inner layer coating of the present invention uses are with light trigger：2,4,6- trimethylbenzoyls-two
Phenylphosphine oxide, double (2,4,6- trimethylbenzoyls) phenylphosphine oxides, 2- benzyls -2- (dimethylamino) -1- (4- (4-
Morpholino) phenyl) one or more in -1- butanone and 4- benzoyl -4- dimethyl diphenyl sulfides are combined.The present invention
The light trigger that fiber outer layer coating uses is：2,4,6- trimethylbenzoy-diphenies phosphorous oxide, double (2,4,6- front threes
Base benzoyl) phenylphosphine oxide, the fluoro- 3- pyrroles's phenyl titanocenes of double 2,6- bis- and 4- benzoyl -4- methyldiphenyl base sulphur
One or more in ether are combined.
Suitable function additive is added in the fiber inner layer coating and fiber outer layer coating of the present invention for improving optical fiber
Machinability and the conductibility of optical signal are also essential.The function additive that the present invention uses is adhesive force conditioning agent, stream
Flat agent and defoamer.The addition of adhesive force conditioning agent is advantageous to improve the interface interaction power of coating and glass, for example：Contain sulfydryl
Silane coupler may advantageously facilitate the profound curing performance of coating, the silane coupler containing chloropropyl, which is advantageous to improve, to be applied
The stability of layer, the silane coupler containing vinyl are advantageous to improve the caking property of coating, and it is one or more suitable to select
Coupling agent compounding use can also improve the stripping cleannes of interface.Currently preferred adhesive force conditioning agent has：Mercapto propyl group three
Methoxy silane, aminopropyl triethoxysilane, r-chloropropyl trimethoxyl silane, vinyltrimethoxy silane etc..The present invention
The mass number of adhesive force conditioning agent in fiber inner layer coating and fiber outer layer coating is 0.5-5.0%, the mass number of levelling agent
For 0.05-1.2%, the mass number of defoamer is 0.02-0.5%.
It is steady in order to improve the heat endurance after the coating material solidified storage stabilities of UV-LED of the present invention and solidification and oxidation
Qualitative, fiber inner layer coating of the invention and fiber outer layer coating can also include one or more light stabilizers or antioxidant.
Suitable light stabilizer has hindered amine, organic phosphite, hindered phenol and their mixture, particularly preferred light stabilizer
Have：Poly- [6- [(1,1,3,3- tetramethyl butyls) amino]] -1,3,5- triazines -2,4- [(2,2,6,6,-tetramethyl-piperidines
Base) imino group] -1,6- oneself two support [(2,2,6,6- tetramethyl -4- piperidyls) imino group], β-(3,5- di-t-butyl -4- hydroxyls
Base phenyl) propionic acid octadecanol ester, BHT, 4,4- thiobis (6- tertiary butyls metacresol) etc., this hair
Bright light stabilizer or the mass number of antioxidant are 0.5%-5%.
The present invention compared with prior art, has advantages below and effect：Inventive formulation composition is reasonable, prepares oligomer
Structural regularity it is good, can be with after manufactured fiber inner layer coating and fiber outer layer coating is uniformly sequentially coated at outer fiber
Protection optical fiber exempts to be affected by the external environment, and keeps enough mechanical strengths and excellent optical property, can effectively improve light and lead to
Believe quality and optical fiber service life, so as to reduce light net cost, improve the stability of wide-band-message network, fiber inner layer coating
Strand compliance is good, and refractive index is high, and has the anti-micro-bend effect of internal stress caused by sustained release variation of ambient temperature, fiber outer layer
Coating has good toughness, wear-resistant, solvent resistant and excellent ageing resistace.The UV- for being used to protect telecommunication optical fiber of the present invention
LED is coating material solidified, is concentrated very much to the absorption energy on 385 nano wavebands for 365 nanometers in wavelength, the deep layer for being advantageous to coating is consolidated
To change, solidify compared to medium pressure mercury lamp, energy consumption is low, and caloric value is low, and service life length, the solidification to fibre coating is more stable, Gu
Change speed and may be up to 1800 ms/min, meet the needs used.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment, and the embodiment can be made further to the present invention
Supplement and explanation, but the present invention is not limited to these embodiments.
Example 1
It is different with stirrer paddle, being heated to reflux adding 2,4- toluene two in the stainless steel reactor with nitrogen protection device
Cyanate 61kg, polymerization inhibitor 0.3kg, control temperature be less than 50 DEG C, be added portionwise number-average molecular weight be 4000 oxirane with
Propylene oxide copolyethers glycol 400kg, stirring reaction content of isocyano into system reach theoretical value and (utilize chemistry titration
Method determines), then removed using thin-film distillation technology after having neither part nor lot in the residual monomer of reaction, add 2- hydroxyl ethyl acrylates
23kg, continue the stirring reaction that heats up, be measured by sampling after being wholly absent by infrared spectrum confirmation-NCO absorptions and stop reaction, filtering
Cooling obtains optical fiber coatings acrylic carbamic acid ester oligomer (A1).It is 4580 to determine number-average molecular weight, molecular weight point
Cloth is 1.05, and primary structure is single aggressiveness of propenoic methyl carbamate.
Example 2
It is different with stirrer paddle, being heated to reflux adding 2,4- toluene two in the stainless steel reactor with nitrogen protection device
Cyanate 52kg, polymerization inhibitor 0.3kg, control temperature be less than 50 DEG C, be added portionwise number-average molecular weight be 2000 oxirane with
Propylene oxide copolyethers glycol 200kg, stirring reaction content of isocyano into system reach theoretical value.Then film is utilized
After distillation technique removing has neither part nor lot in the residual monomer of reaction, 2- hydroxyl ethyl acrylate 23kg are added, continue the stirring reaction that heats up.
It is measured by sampling after being wholly absent by infrared spectrum confirmation-NCO absorptions and stops reaction, filtering cooling obtains optical fiber coatings propylene
Acidic group carbamic acid ester oligomer (A2).It is 2596 to determine number-average molecular weight, and molecular weight distribution 1.09, primary structure is propylene
Single aggressiveness of sour carbamate.
Example 3
It is different with stirrer paddle, being heated to reflux adding 2,4- toluene two in the stainless steel reactor with nitrogen protection device
Cyanate 52kg, polymerization inhibitor 0.3kg, control temperature are less than 50 DEG C, and the expoxy propane that number-average molecular weight is 1000 is added portionwise and gathers
Ether glycol 100kg, stirring reaction content of isocyano into system reach theoretical value.Then removed using thin-film distillation technology
After having neither part nor lot in the residual monomer of reaction, 2- hydroxyl ethyl acrylate 23kg are added, continue the stirring reaction that heats up.Sampling and measuring passes through
Infrared spectrum confirmation-NCO absorptions stop reaction after being wholly absent, filtering cooling obtains optical fiber coatings acrylic carbamic acid
Ester oligomer (A3).It is 1680 to determine number-average molecular weight, and molecular weight distribution 1.12, primary structure is propenoic methyl carbamate
Single aggressiveness.
Example 4
It is different with stirrer paddle, being heated to reflux adding 2,4- toluene two in the stainless steel reactor with nitrogen protection device
Cyanate 45kg, polymerization inhibitor 0.3kg, control temperature are less than 50 DEG C, and the propylene oxide polyether that number-average molecular weight is 600 is added portionwise
Glycol 60kg, stirring reaction content of isocyano into system reach theoretical value.Then removed not using thin-film distillation technology
After the residual monomer for participating in reaction, 2- hydroxyl ethyl acrylate 23kg are added, continue the stirring reaction that heats up.It is measured by sampling by red
External spectrum confirmation-NCO absorptions stop reaction after being wholly absent, filtering cooling obtains optical fiber coatings acrylic carbamate
Oligomer (A4).It is 1276 to determine number-average molecular weight, molecular weight distribution 1.2, and primary structure is propenoic methyl carbamate
Single aggressiveness.
Comparison example 1
It is different with stirrer paddle, being heated to reflux adding 2,4- toluene two in the stainless steel reactor with nitrogen protection device
Cyanate 34.8kg, control temperature are less than 80 DEG C, and the propylene oxide polyether glycol that number-average molecular weight is 4000 is added portionwise
400kg, stirring reaction content of isocyano into system reach theoretical value, then add 2- hydroxyl ethyl acrylate 23kg,
Polymerization inhibitor 0.3kg, continues the stirring reaction that heats up, and gelation occurs in reaction later stage material.
Comparison example 2
With stirrer paddle, it is heated to reflux adding 2,4- toluene in the stainless steel reactor of device and nitrogen protection device
Diisocyanate 34.8kg, is added portionwise the propylene oxide polyether glycol 200kg that number-average molecular weight is 2000, and control temperature is less than
50 DEG C, stirring reaction content of isocyano into system reaches theoretical value, then adds 2- hydroxyl ethyl acrylate 25.5kg,
Polymerization inhibitor 0.3kg, continue the stirring reaction that heats up, it is anti-that stopping after being wholly absent by infrared spectrum confirmation-NCO absorptions is measured by sampling
Should, filtering cooling obtains optical fiber coatings acrylic carbamic acid ester oligomer (A5).It is 3285 to determine number-average molecular weight, point
Son amount is distributed as 2.1, and primary structure is the mixture of propenoic methyl carbamate.
Comparison example 3
With stirrer paddle, it is different to be heated to reflux addition isophorone two in the stainless steel reactor with nitrogen protection device
Cyanate 44.4Kg, control temperature are less than 80 DEG C, and the propylene oxide polyether glycol that number-average molecular weight is 1000 is added portionwise
100kg, stirring reaction content of isocyano into system reach theoretical value, then add 2- hydroxyl ethyl acrylates
25.5kg, polymerization inhibitor 0.3kg, continue the stirring reaction that heats up, be measured by sampling and be wholly absent by infrared spectrum confirmation-NCO absorptions
Stop reaction afterwards, filtering cooling obtains optical fiber coatings acrylic carbamic acid ester oligomer (A6).Determine number-average molecular weight
For 2950, molecular weight distribution 2.5, primary structure is the mixture of propenoic methyl carbamate.
Example 5
After being well mixed using acrylic carbamic acid ester oligomer (A1) with the component shown in table 1 by heating stirring
Liquid coating is made.Estimated viscosity：6500 (mPas/25 DEG C), density：1.03(kg/m3, 25 DEG C), refractive index： 1.4821
(25 DEG C), are suitable for preparing fiber inner layer coating.
The A1 formulation for coating material of table 1
| Component | Dosage (Wt.%) |
| Acrylic carbamate (A1) | 70 |
| Acrylate | 3.5 |
| Nonyl Phenol ethoxylated acrylate | 10 |
| Caprolactam | 7.5 |
| Internal layer light trigger | 5.5 |
| Silane coupler | 2.5 |
| Antioxidant | 1.5 |
| Levelling agent | 0.3 |
| Defoamer | 0.2 |
Example 6
After being well mixed using acrylic carbamic acid ester oligomer (A2) with the component shown in table 2 by heating stirring
Liquid coating is made.Estimated viscosity：5600 (mPas/25 DEG C), density：1.06(kg/m3, 25 DEG C), refractive index：1.4852
(25 DEG C), are suitable for preparing fiber inner layer coating.
The A2 formulation for coating material of table 2
| Component | Dosage (Wt.%) |
| Acrylic carbamate (A2) | 75 |
| 2 (2- ethoxy-ethoxies) ethyl propylene acid esters | 4.5 |
| Tri-propanediol diacrylate | 4.5 |
| Caprolactam | 5.0 |
| Internal layer light trigger | 6.0 |
| Silane coupler | 2.5 |
| Antioxidant | 1.5 |
| Defoamer | 0.2 |
| Antioxidant | 1.5 |
Example 7
Liquid is made after being well mixed using acrylic carbamate (A3) with the component shown in table 3 by heating stirring
State coating.Estimated viscosity：5500/ (mPas/25 DEG C), density：1.11(kg/m3, 25 DEG C), refractive index：1.5132 (25
DEG C), it is suitable for preparing fiber outer layer coating.
The A3 formulation for coating material of table 3
| Component | Dosage (Wt.%) |
| Acrylic carbamate (A3) | 28 |
| Epoxy acrylate | 37 |
| Isobornyl acrylate | 12 |
| 1,6- hexanediyl ester | 3.5 |
| Tri-propanediol diacrylate | 7 |
| Outer layer light trigger | 6.5 |
| Antioxidant | 1.5 |
| Light stabilizer | 2.5 |
| Modified polyorganosiloxane | 1.0 |
Example 8
After being well mixed using acrylic carbamic acid ester oligomer (A4) with the component shown in table 4 by heating stirring
Liquid coating is made.Estimated viscosity：6500/ (mPas/25 DEG C), density：1.12(kg/m3, 25 DEG C), refractive index： 1.5180
(25 DEG C), it is suitable for preparing fiber outer layer coating.
The A4 formulation for coating material of table 4
| Component | Dosage (Wt.%) |
| Acrylic carbamate (A4) | 30 |
| Epoxy acrylate | 44 |
| Tri-propanediol diacrylate | 8.5 |
| Acrylate | 3.5 |
| 1,6- hexanediyl ester | 2.5 |
| Outer layer light trigger | 6.5 |
| Antioxidant | 1.5 |
| Light stabilizer | 2.5 |
| Modified polyorganosiloxane | 1.0 |
Example 9
It is interlayer coatings from example 5, example 8 is outer layer coating, prefabricated rods G652D.On drawing optical fibers coating machine
Shaping, the burn-in test data of coated fiber are as shown in table 5.Test result has further been proved inside and outside the optical fiber of the invention prepared
The excellent properties of coating.
The burn-in test data of the coated fiber of table 5
Although the present invention is disclosed as above with embodiment, it is not limited to protection scope of the present invention, any ripe
The technical staff of this technology is known, in the change and retouching made without departing from the spirit and scope of the invention, this all should be belonged to
The protection domain of invention.
Claims (7)
1. a kind of be used to protect the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：It is described to be used to protect telecommunication optical fiber
UV-LED is coating material solidified directly to be contacted including fiber inner layer coating and fiber outer layer coating, fiber inner layer coating with optical fiber surface,
Fiber outer layer coating is coated in interlayer coatings surface, and the fiber inner layer coating includes the raw material of following mass numbers：Interlayer coatings
With oligomer 60%-80%, interlayer coatings reactive diluent 15%-35%, interlayer coatings light trigger 4.0%-6.0%, internal layer
Coating function additive 0.6%-6.5%, the fiber outer layer coating include the raw material of following mass numbers：Outer layer coating oligomer
20%-35%, epoxy acrylate 30%-45%, outer layer coating reactive diluent 15%-35%, outer layer coating light trigger
6.0%-8.0%, outer layer coating function additive 0.6%-6.5%.
It is 2. according to claim 1 a kind of for protecting the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：Institute
The physical parameter for stating fiber inner layer coating is：
Before solidification（Liquid coating）
Viscosity（mPa·s/25℃）5000-7500
Refractive index（25℃）1.4750-1.5000
Density（Kg/m3,25 DEG C）1.03-1.07
After solidification（Solid-state coating）
Specific modulus（2.5% bullet becomes, mPa）1.2-1.5
Elongation（%）>100
Tensile strength（mPa）>0.8
Cure shrinkage（%）<2.5
Glassy bond power（N）>0.7
The physical parameter of the fiber outer layer coating is：
Before solidification（Liquid coating）
Viscosity（ mPa·s/25℃）5000-7500
Refractive index（25℃）1.500-1.545
Density（Kg/m3,25 DEG C）1.10-1.13
After solidification（Solid-state coating）
Specific modulus（2.5% bullet becomes, mPa）600-950
Elongation（%）>10
Tensile strength（mPa）>30
Cure shrinkage（%）<7.0
It is according to claim 1 a kind of for protecting the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：The light
The interlayer coatings that fine interlayer coatings include are interlayer coatings acrylic carbamic acid ester oligomer with oligomer, the internal layer
Coating reactive diluent is by acrylate, caprolactam, tri-propanediol diacrylate, ethoxyquin nonyl
Base phenol acrylate and 2（2- ethoxy-ethoxies）One or more in ethyl propylene acid esters are combined, and the internal layer applies
Material light trigger is by 2,4,6- trimethylbenzoy-diphenies phosphorous oxide, double（2,4,6- trimethylbenzoyls）Phenyl
Phosphorous oxide, 2- benzyls -2-（Dimethylamino）-1-（4-（4- morpholinoes）Phenyl）- 1- butanone and 4- benzoyl -4- methyl two
One or more in aralkyl sulfid are combined.
It is 3. according to claim 3 a kind of for protecting the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：It is described
Interlayer coatings are synthesized by following ingredients reaction with acrylic carbamic acid ester oligomer and are made：
（a）Molecular weight is from 2000-6000 propylene oxide polyether polyalcohol and oxirane and propylene oxide copolyethers glycol
At least one；
（b）At least one of aromatic diisocyanate and aliphatic diisocyanate；
（c）At least one of hydroxy-end capped acrylate and methacrylate.
It is 4. according to claim 4 a kind of for protecting the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：It is described
Interlayer coatings acrylic carbamic acid ester oligomer is prepared by the excessive starvation being added dropwise with low temperature of diisocyanate instead
Principle is answered, generates target product using step synthesis, reaction temperature is controlled at 40 DEG C -80 DEG C.
It is 5. according to claim 1 a kind of for protecting the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：It is described
The outer layer coating that fiber outer layer coating includes is outer layer coating acrylic carbamic acid ester oligomer with oligomer, described outer
Coating reactive diluent is by isobornyl acrylate, acrylate, 1,6-HD double methacrylate and three
One or more in propane diols double methacrylate are combined, and the outer layer coating light trigger is by 2,4,6- trimethylbenzenes
It is formoxyl-diphenyl phosphate oxidation, double（2,4,6- trimethylbenzoyls）The fluoro- 3- pyrroles's phenyl of phenylphosphine oxide, double 2,6- bis-
One or more in titanocenes and 4- benzoyl -4- dimethyl diphenyl sulfides are combined.
It is 6. according to claim 6 a kind of for protecting the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：It is described
Outer layer coating is synthesized by following ingredients reaction with acrylic carbamic acid ester oligomer and is made：
（a）Molecular weight is from least one of 400-2000 propylene oxide polyether polyalcohol；
（b）At least one of aromatic diisocyanate and aliphatic diisocyanate；
（c）At least one of hydroxy-end capped acrylate and methacrylate.
It is 7. according to claim 7 a kind of for protecting the UV-LED of telecommunication optical fiber coating material solidified, it is characterised in that：It is described
Outer layer coating acrylic carbamic acid ester oligomer is prepared by PPG and excessive di-isocyanate reaction
The long-chain midbody product of isocyanate group end-blocking is generated, then by midbody product with carrying hydroxyl（Methyl）Acrylate reactions
Target product is generated, reaction temperature is controlled at 50 DEG C -110 DEG C.
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