CN106497389B - A kind of graphene bilayer optical fiber coatings and its preparation method and application - Google Patents

A kind of graphene bilayer optical fiber coatings and its preparation method and application Download PDF

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CN106497389B
CN106497389B CN201610942695.4A CN201610942695A CN106497389B CN 106497389 B CN106497389 B CN 106497389B CN 201610942695 A CN201610942695 A CN 201610942695A CN 106497389 B CN106497389 B CN 106497389B
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optical fiber
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graphene
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layer coating
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CN106497389A (en
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陶宇
翁亚楠
杨超
仲崇盟
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Jiangsu Teliliang New Material Technology Co ltd
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Changchang Tanrun New Material Co Ltd
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    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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    • C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
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    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
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    • C08L2205/00—Polymer mixtures characterised by other features
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    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention belongs to optical fiber coatings field, more particularly to a kind of graphene bilayer optical fiber coatings and its preparation method and application.Unsaturated polyester (UP), urethane acrylate, toughener, photoinitiator, curing agent, modified graphene are mixed as interlayer coatings, and fluorinated acrylate, polyester acrylate, photoinitiator, rare-earth salts, modified graphene are mixed as outer layer coating, after being coated using interlayer coatings to optical fiber, then coat outer layer coating and cure.

Description

A kind of graphene bilayer optical fiber coatings and its preparation method and application
Technical field
The invention belongs to optical fiber coatings field, more particularly to a kind of graphene bilayer optical fiber coatings and preparation method thereof and should With.
Background technology
Optical fiber is mainly constrained light in using the total reflection principle of light in optical fiber, and guiding light wave is propagated in the axial direction, There is the low, bandwidth of loss, small, light-weight, efficient, be applied in many fields.
Currently there are optical fiber mainly using quartz glass optical fiber, there are the shortcomings of thin and crisp, frangibility, Under the influence of external environment, easily occur oxidation, absorption dust and moisture, it is micro-bend the shortcomings of, influence the signal transmission quality of optical fiber. Therefore one layer must be coated in optical fiber surface or multilayer fibers coating is protected.And this coating will complete squeeze out and It is coated in several seconds stretched on optical fiber, possesses some specific physical properties, in very wide temperature use scope, still can Enough keep excellent physical property and mechanical performance.Mainly still there are hardening times for common optical fiber coatings currently on the market Long, the shortcomings of production cost is high, therefore develop that a kind of hardening time is short, long-time interior energy keep excellent physics and mechanicalness Energy, optical fiber coatings at low cost are determined to win.
The content of the invention
The present invention provides a kind of graphene bilayer optical fiber coatings and its preparation method and application, using double-layer structure, assign The performance that ectonexine is different is given, meets respective use condition, widens the scope of application of optical fiber；Using dual cure means, make It obtains coating fast shaping or reaches " surface drying ", further such that fully curing inside coating, can effectively shorten hardening time, Production cost is reduced, assigns the better mechanical property of coating, cured film refractive index is more than 1.48, meets the requirement of 25 years.
Double-deck optical fiber coatings are divided into interlayer coatings and outer layer coating,
Interlayer coatings include following component in parts by weight：
Wherein, the line polymer that unsaturated polyester (UP) forms for binary acid and dihydric alcohol polycondensation, and by cross-linking monomer or Active solvent dilutes the resin solution with certain viscosity to be formed, main to include adjacent benzene-type unsaturated polyester (UP), metaphenylene insatiable hunger With polyester, bisphenol A-type unsaturated polyester (UP), vinylite etc., such as TM-v820,802, HN-191, DC191, HN-196,
Urethane acrylate is RJ4236, YWU2620,2203A, U-600, RJ821 etc., these resin viscosities are relatively low, It is good with the compatibility of unsaturated polyester (UP), the curing rate of interlayer coatings can be improved and effectively reduce the intensity and modulus of internal layer, It is smaller to the damage of optical fiber,
Toughener is mainly polysulfide rubber, the advance polymers of carbamate, modified polyether etc., it is common for CYH-227, DY-040, JHJD-301, CMP-410, FD-400 etc., these toughener can be with above-mentioned unsaturated polyester (UP)s and polyurethane propylene Acid esters one or two kinds of reaction therein forms block so as to achieve the purpose that toughening, and the toughener added does not influence Other performances of optical fiber coatings,
Photoinitiator is that can absorb certain wavelength in ultraviolet region (250~420nm) or visible region (400~800nm) Energy and generate free radicals, cation etc., so as to trigger the compound of monomer polymerization crosslinking curing, such as dialkoxy benzene second Ketone, alpha-hydroxyalkyl benzophenone, α-amine alkyl phenones, acylphosphanes hydride, aryl peroxide ester compounds, halogenated methyl arone etc., often See to be 819,1173, tpo, KIP 150,184 etc.,
Curing agent requirement solidification temperature is relatively low, curing rate is very fast, such as cyclohexanone peroxide, benzoyl peroxide, cycloalkanes Sour cobalt, hyperis, benzoyl peroxide etc.,
The above-mentioned specific preparation process of modified graphene is：By graphene (400~500g) be scattered in DMF (200~ In 400ml), triethylamine (0.5~1ml) and coupling agent (5~10g) are successively added under nitrogen protective condition simultaneously after supersound process 24~30h, filtering are reacted under the conditions of 110 DEG C, deionized water is washed to neutrality, vacuum drying,
Dispersiveness of the coupling agent added in modified technique mainly for improvement graphene in matrix resin, it is ensured that apply The uniformity and performance of material are stablized, and the present invention mainly uses fluorine-containing silane coupling agent (such as poly- silicon of trifluoro propyl methyl ethylene Oxygen alkane, 17 fluorine decyl triethoxysilane silicon fluorides etc.), it on the one hand can improve the dispersiveness of graphene in the base, in addition The relatively other kinds of coupling agent performance of fluorine-containing coupling agent is more stablized on one side, and can improve the corrosion resistant of interlayer coatings Corrosion energy；
Outer layer coating includes following component in parts by weight：
Wherein, fluorinated acrylate is dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, acrylic acid hexafluoro fourth Ester, Hexafluorobutyl mathacrylate, methacrylic acid 2,2, the homopolymer or bipolymer of 2- trifluoro ethyl esters, fluorine-containing propene Acid esters can effectively improve the Corrosion Protection of outer layer coating, and that widens optical fiber uses field,
Polyester acrylate is BC-2210, RJ513,4026,604 etc., these resin viscosities are relatively low, with fluorine-containing The compatibility of ester is good, can improve the viscosity of fluorinated acrylate after compounding, increases the flexibility of coating itself,
In outer layer coating, the situation of photoinitiator and modified graphene is consistent with interlayer coatings,
The present invention can realize rapid curing, rare earth element therein using curing agent of the rare-earth salts as outer layer coating The mechanical performance and weather resistance of outer layer coating can also be improved, reduce interference of the ambient to inside of optical fibre signal, rare earth Salt is specially RE phosphate, sulfate (rare earth element：La, Ce, Pr, Nd, Sm etc.), it is common such as Ce2(SO4)3、CePO4、 LaPO4、PrPO4Deng.
The present invention also provides a kind of preparation methods of above-mentioned graphene bilayer optical fiber coatings, are specially：
(1) preparation of interlayer coatings
By the parts by weight of each component, will be stirred evenly under unsaturated polyester (UP) and urethane acrylate room temperature, Ran Houyi Secondary addition toughener, photoinitiator, curing agent, modified graphene simultaneously are again stirring for uniformly obtaining interlayer coatings, stand, for use；
(2) preparation of outer layer coating
By the parts by weight of each component, will be stirred evenly under fluorinated acrylate and polyester acrylate room temperature, Ran Houyi Secondary addition photoinitiator, rare-earth salts, modified graphene simultaneously are again stirring for uniformly obtaining outer layer coating, stand, for use.
The present invention also provides a kind of applications of above-mentioned double-deck optical fiber coatings, and optical fiber is carried out using for use interlayer coatings Solidify afterwards are coated, then coats outer layer coating and cures, the curing rate of the two will match, and curing rate is controlled in 200m/min Or faster, paint viscosity control is moderate,
Internal layer and outer layer avoid individually shortcoming caused by certain curing using dual cure means, wherein, first Carry out photocuring so that coating fast shaping reaches " surface drying "；Heat cure is carried out again so that is fully cured inside coating and is assigned The better mechanical property of coating is given,
Double-coating is realized to optical fiber after curing, wherein, internal layer meets stretch modulus in 0.1~2Mpa, extension at break Rate is more than 110%, while the glass transition temperature of internal layer should be less than -70 DEG C, and stress is relatively low under cryogenic, to optical fiber Damage is smaller；
And outer layer meets cured film refractive index more than 1.48, reduces interference of the ambient to inside of optical fibre signal, outside Layer glass transition temperature still has preferable mechanical strength at high temperature higher than 80 DEG C.
The beneficial effects of the present invention are：
(1) optical fiber coatings of the present invention are double-layer structure, assign different performance indicators respectively, meet optical fiber Requirement widens it and uses field；
(2) internal layer and outer layer avoid individually shortcoming caused by certain curing using dual cure means, wherein Photocuring causes coating fast shaping or reaches " surface drying " that heat cure fully to cure inside coating, and it is more preferable to assign coating Mechanical property；
(3) optical fiber surface is coated into matcoveredn, plays the role of completely cutting off water and steam, and internal layer and outer layer coating add Enter graphene, graphene itself is based on special two-dimensional layered structure and abundant surface functional group and with higher bendable Folding ability optimizes the dynamic fatigue resistance energy of coating material, even more improves the buckle resistance energy of institute's clad optical fiber, this It is one of main purpose of the application；
(4) fluorinated acrylate used by outer layer coating can effectively improve the Corrosion Protection of outer layer coating, widen Optical fiber uses field；RE phosphate can as the curing agent of outer layer coating, can rapid curing, rare earth element therein The mechanical performance and weather resistance of outer layer coating can also be improved, reduce interference of the ambient to inside of optical fibre signal.
Description of the drawings
Fig. 1 is the schematic diagram of the graphene bilayer optical fiber coatings coated fiber of the present invention.
Specific embodiment
Respectively according to the formula (in terms of each component parts by weight) listed by Tables 1 and 2, by resin, initiator, toughener, The components such as curing agent, modified graphene stir evenly at room temperature, dip one end that appropriate coating is placed in glass plate with glass bar, make Certain thickness is coated into silk rod coating device, glass plate is put into during ultraviolet light cures after levelling and is cured, condition of cure： Uv light irradiation intensity 1000W；It is complete after heat cure at 100 DEG C to reach " surface drying " by irradiation distance 40cm.It tests respectively in it The properties of outer layer, it is specific as shown in table 3；
Optical fiber is coated successively using the inside and outside coating in table 1, table 2, coating processes：A diameter of 80mm's is prefabricated Stick under the 2000 DEG C of high temperature actions of heating furnace that reel off raw silk from cocoons, melt to can free fall state, being reeled off raw silk from cocoons by 150g tractive force becomes The bare fibre of 125um；Bare fibre passes through the cooling of cooling cylinder, and temperature drops to 85 ± 5 DEG C, by the painting of internal layer application system It covers, UV lamp cures, heat ageing, cooling；The coating of outer layer application system is carried out again, and UV lamp cures, heat ageing, and cooling takes drawing It under the action of wheel, is wrapped on take-up reel, completes optical fiber coating process.The buckle resistance of optical fiber can be as shown in table 4 after coating.
Wherein, the preparation process of modified graphene is in each embodiment：
Graphene 450g is scattered in DMF400ml, triethylamine is successively added under nitrogen protective condition after supersound process 0.75ml and trifluoro propyl methylvinyl-polysiloxane 8g simultaneously reacts 25h under the conditions of 110 DEG C, filtering, deionized water washing To neutrality, vacuum drying.
Viscosity is tested：
According to the regulation of GB/T 1723-93, the NDJ-8S type viscosities of Shanghai Precision Scientific Apparatus Co., Ltd are used Meter is measured.First by paint heating to be measured to 25 DEG C, constant temperature is kept.Corresponding rotor is selected according to the size of paint viscosity And rotating speed, rotor is then started, treats that reading is constant, records the data, measures three times, if data are as differed smaller, is averaged It is as larger in differed as paint viscosity, it needs to redeterminate.
Refractive index：
It is measured using the WAY type abbe's refractometers of Shanghai Precision Scientific Apparatus Co., Ltd.Liquid before curing applies Material is directly measured using abbe's refractometer, and the assay method of coating refractive index is after curing：It will apply that gob is several to drip to load glass It is carefully removed after on piece, ultra-violet curing and heat cure, 1~2 drop naphthalene bromide is added dropwise on the loading lens of abbe's refractometer, it will be solid The shiny surface of coating is placed on it after change, and observed reading is the refractive index of coating after curing.
Tensile property：
According to the regulation of GB/T1040-92, measured on universal testing machine.Assay method：Pour coating into horseshoe In the standard tensile mold of shape, cured, tensile bars are taken out after curing, be placed at room temperature for for 24 hours, on universal testing machine Measure tensile strength, elongation at break and the stretch modulus of coating, rate of extension 50mm/min.
Glass transition temperature：It is measured using differential scanning calorimetric analysis instrument, atmosphere is high pure nitrogen, flow velocity 50ml/ Min, Range of measuring temp：Internal layer is -100~20 DEG C, and outer layer is 20~150 DEG C, and heating rate is 10 DEG C/min.
1 interlayer coatings of table
2 outer layer coating of table
Performance test data after ectonexine paint solidification film forming prepared by 3 specific embodiment 1~4 of table
The performance test data of the optical fiber after inside and outside coating cladding prepared by specific embodiment 1~4 of table 4
Test event Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Static fatigue parameter/Nd 30.1 31.3 32.2 33.0
Comparative example 1
Modified graphene is not added in interlayer coatings and outer layer coating, remaining component is with embodiment 4, in optical fiber External sheath technique, detection means are also completely the same as embodiment 4.
The static fatigue parameter of optical fiber is only 17.6Nd after the inside and outside coating cladding prepared through this comparative example.
Comparative example 2
" modified graphite " of corresponding weight is replaced to " modified graphene " in interlayer coatings and outer layer coating respectively, remaining Component is with embodiment 4, and ectonexine cladding process, detection means to optical fiber are also completely the same as embodiment 4.
The modified of graphite is operated with embodiment 4 in this comparative example：Graphite 450g is scattered in DMF400ml, is surpassed After sonication triethylamine 0.75ml and trifluoro propyl methylvinyl-polysiloxane 8g are successively added under nitrogen protective condition simultaneously 25h is reacted under the conditions of 110 DEG C, is filtered, deionized water is washed to neutrality, vacuum drying.
The static fatigue parameter of optical fiber is only 22.7Nd after the inside and outside coating cladding prepared through this comparative example.
Contrast experiment 3
Rare-earth salts component in outer layer coating is left out, remaining each component and dosage are the same as embodiment 4：By fluorinated acrylate It is stirred evenly under polyester acrylate room temperature, then sequentially add photoinitiator, modified graphene and is again stirring for uniform obtain To outer layer coating, stand；
One end that appropriate above-mentioned outer layer coating is placed in glass plate is dipped with glass bar, is coated into using silk rod coating device With the thickness of embodiment 4, glass plate received under uv light irradiation intensity 1000W, irradiation distance 40cm after levelling ultraviolet The illumination time same as Example 4, the time same as Example 4 is placed at 100 DEG C, have no that the outer layer coating is consolidated Change.

Claims (10)

1. a kind of graphene bilayer optical fiber coatings, it is characterised in that：The double-deck optical fiber coatings are divided into interlayer coatings and outer layer Coating,
The interlayer coatings include following component in parts by weight,
10 ~ 30 parts of unsaturated polyester (UP)s
50 ~ 80 parts of urethane acrylates
1 ~ 5 part of toughener
0.1 ~ 2 part of photoinitiator
0.1 ~ 2 part of curing agent
1 ~ 5 part of modified graphene；
The outer layer coating includes following component in parts by weight,
10 ~ 30 parts of fluorinated acrylates
40 ~ 60 parts of polyester acrylates
0.1 ~ 2 part of photoinitiator
1 ~ 5 part of modified graphene
1 ~ 5 part of rare-earth salts.
2. graphene bilayer optical fiber coatings as described in claim 1, it is characterised in that：Unsaturation described in interlayer coatings is gathered Ester is TM-v820, HN-191, DC191 or HN-196.
3. graphene bilayer optical fiber coatings as described in claim 1, it is characterised in that：Polyurethane third described in interlayer coatings Olefin(e) acid ester is RJ4236, YWU2620 or RJ821.
4. graphene bilayer optical fiber coatings as described in claim 1, it is characterised in that：Toughener described in interlayer coatings is CYH-227, DY-040, JHJD-301, CMP-410 or FD-400.
5. graphene bilayer optical fiber coatings as described in claim 1, it is characterised in that：Fluorine-containing propene described in outer layer coating Acid esters is dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, hexafluorobutyl acrylate or methacrylic acid hexafluoro fourth Ester.
6. graphene bilayer optical fiber coatings as described in claim 1, it is characterised in that：Polyester described in outer layer coating Acid esters is BC-2210, RJ513,4026 or 604.
7. graphene bilayer optical fiber coatings as described in claim 1, it is characterised in that：Described in outer layer coating or interlayer coatings Photoinitiator for 819,1173, tpo, KIP 150 or 184.
8. graphene bilayer optical fiber coatings as described in claim 1, it is characterised in that：Described in outer layer coating or interlayer coatings The preparation process of modified graphene be to disperse graphene in DMF, after supersound process under nitrogen protective condition successively plus Entering triethylamine and fluorine-containing silane coupling agent and 24 ~ 30h, filtering are reacted under the conditions of 110 DEG C, deionized water is washed to neutrality, Vacuum drying.
It is 9. a kind of such as the preparation method of claim 1 to 8 any one of them graphene bilayer optical fiber coatings, it is characterised in that： The preparation method is,
（1）The preparation of interlayer coatings
It by the parts by weight of each component, will stir evenly under unsaturated polyester (UP) and urethane acrylate room temperature, then add successively Enter toughener, photoinitiator, curing agent, modified graphene and be again stirring for uniformly obtaining interlayer coatings, stand, for use；
（2）The preparation of outer layer coating
It by the parts by weight of each component, will stir evenly under fluorinated acrylate and polyester acrylate room temperature, then add successively Enter photoinitiator, rare-earth salts, modified graphene and be again stirring for uniformly obtaining outer layer coating, stand, for use.
It is 10. a kind of such as the application of claim 1 to 8 any one of them graphene bilayer optical fiber coatings, it is characterised in that：It is described Application be that cladding solidify afterwards are carried out to optical fiber using interlayer coatings, then coats outer layer coating and cures.
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