CN110698080B - Coating resin for optical fiber and preparation method and application thereof - Google Patents

Coating resin for optical fiber and preparation method and application thereof Download PDF

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CN110698080B
CN110698080B CN201911003549.5A CN201911003549A CN110698080B CN 110698080 B CN110698080 B CN 110698080B CN 201911003549 A CN201911003549 A CN 201911003549A CN 110698080 B CN110698080 B CN 110698080B
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coating resin
optical fiber
photoinitiator
graphene
coating
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CN110698080A (en
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吴海港
胡涛涛
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Hangzhou Futong Communication Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/48Coating with two or more coatings having different compositions
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/44Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/26Esters containing oxygen in addition to the carboxy oxygen
    • C08F220/30Esters containing oxygen in addition to the carboxy oxygen containing aromatic rings in the alcohol moiety
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F265/00Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
    • C08F265/04Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
    • C08F265/06Polymerisation of acrylate or methacrylate esters on to polymers thereof

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  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
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  • Paints Or Removers (AREA)

Abstract

The invention relates to the technical field of optical fiber manufacturing, and provides a coating resin for an optical fiber, a preparation method and application thereof, aiming at solving the problems that the oil accumulation of a quartz lamp tube is easy to cause the optical fiber to become brittle and the optical fiber is broken in the light curing process of the existing coating resin for the optical fiber, wherein the coating resin for the optical fiber comprises a first coating resin and a second coating resin, the first coating resin is prepared from acrylic acid-2-phenoxyethyl ester, vinyl hexahydro-2H-azepin-2-copper, a first photoinitiator, 3-trimethoxysilylpropane-1-thiol, trimethylolpropane triacrylate, trimethylene glycol diacrylate, 2-ethyl-2- [ 3-carboxy-1-oxopropoxy ] methyl ] propane-1, 3-diylbis [ 3-mercaptopropionic acid ], graphene and the balance of a first auxiliary agent. The resin system can realize rapid curing of the LED, the coating curing rate is high, volatile substances which are not removed in a photocatalytic degradation system are not removed, and the quartz lamp tube has no accumulated oil.

Description

Coating resin for optical fiber and preparation method and application thereof
Technical Field
The invention relates to the technical field of optical fiber manufacturing, in particular to coating resin for an optical fiber and a preparation method thereof.
Background
In the existing wire drawing coating curing process, the LED curing optical fiber is used for coating resin, so that the LED lamp with low energy consumption replaces UV curing, but the temperature of a curing system of the LED lamp is low, part of volatile substances are not easy to discharge, oil is easy to accumulate in a quartz lamp tube, the optical fiber curing effect is influenced, and the optical fiber is fragile and broken when the optical fiber is serious.
In order to avoid oil accumulation, the conventional method is to install an air draft mechanism in the curing device, and inert gas (such as nitrogen) is introduced to take away volatile substances in the curing process, but the method may cause the optical fiber to shake, may damage the required oxygen content in the curing environment, and may even introduce impurities, which brings new uncontrollable factors.
Chinese patent literature discloses a method and equipment for manufacturing optical fibers with UV LED curing coating layers, the publication number of the method is CN 106277842A. Because the light-emitting spectrum of the UV LED can be completely used for curing the optical fiber coating, the UV LED system can save a large amount of energy consumption under the condition of achieving the same curing effect. However, the invention also has the problems that the temperature of the curing system of the LED lamp is low, and partial volatile substances are not easy to discharge.
Disclosure of Invention
The invention provides a coating resin for optical fibers, which is coated twice and cured by photocatalysis simultaneously, in order to solve the problems that the system temperature of the existing coating resin for optical fibers is low in the LED photocuring process, part of volatile substances are not easy to discharge, oil is easy to accumulate in a quartz lamp tube, the optical fiber curing effect is influenced, and the optical fibers become brittle and are broken.
The invention also provides a preparation method of the coating resin for the optical fiber, which has simple steps, has no special requirements on equipment and is easy for industrial production.
The invention also provides application of the coating resin for the optical fiber in preparing an optical fiber coating by using an LED photocuring technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
the coating resin for the optical fiber comprises a first coating resin and a second coating resin, wherein the first coating resin comprises the following components in percentage by mass: 5-15% of 2-phenoxyethyl acrylate, 1-5% of vinylhexahydro-2H-azepine-2-copper, 2-6% of a first photoinitiator, 0-1% of 3-trimethoxysilylpropane-1-thiol, 0-1% of trimethylolpropane triacrylate, 0-1% of tripropylene glycol diacrylate, 0-1% of 2-ethyl-2- [ 3-carboxy-1-oxopropoxy) methyl ] propane-1, 3-diylbis [ 3-mercaptopropionic acid ], 0.005-0.01% of graphene, and the balance of a first auxiliary agent; the graphene is prepared by hummers;
the second coating resin comprises the following components in percentage by mass: 25-50% of 4, 4' - (1-methylethylidene) diphenol, polymer of hydrogenmethyl oxirane and 2-acrylate, 10-25% of tripropylene glycol diacrylate, 1-5% of dioxy (methyl-2, 1-ethanediyl) diacrylate, 1-5% of 2-phenoxyethyl acrylate, 0-1% of hydroquinone monomethyl ether, 1-5% of second photoinitiator and nano g-C3N4 0.05~0.1%,The balance of the second auxiliary agent;
the absorption wavelength of the first photoinitiator and the absorption wavelength of the second photoinitiator are 385-405 nm.
The coating resin for the optical fiber comprises a first coating resin and a second coating resin, wherein in the process of coating the optical fiber, the first coating resin is coated firstly, then the second coating resin is coated, the absorption wavelengths of a first photoinitiator and a second photoinitiator are limited to visible light, the two-time coating and the simultaneous curing of an LED light source are realized, the operation is simple and efficient, and the problem that UV curing is easy to generate heat is solved.
In order to solve the problems that the temperature of an LED lamp curing system is low, part of volatile substances are not easy to discharge, oil is easy to accumulate in a quartz lamp tube, the curing effect of an optical fiber is influenced, and the optical fiber is embrittled and broken when the curing effect is serious, the graphene material is doped into a first coating resin and the nano g-C material is doped into a second coating resin respectively3N4Visible light catalyst (forbidden band width 3.24eV), based on graphene material and nano g-C when the second coating resin is coated on the outer surface of the first coating resin3N4The two-dimensional network structure can be quickly crosslinked and mixed to jointly exert a synergistic effect, and can construct a high-efficiency conductive network at the junction of the first coating resin and the second coating resin, so that the two-dimensional network structure can be in contact with an acrylic monomer to the maximum extent, and the nano g-C can be greatly improved3N4Thereby enabling the coating resin for optical fiber to be rapidly photo-cured.
In an LED light curing system, under the irradiation of visible light, graphene/nano g-C in the system3N4The first photoinitiator and the second photoinitiator are quickly cured through photocatalysis, and the graphene material can improve the separation efficiency of photon-generated carriers in the photocatalysis process and broaden the range of nano g-C3N4The forbidden band width of the visible light catalyst further improves the photocatalytic curing efficiency, and meanwhile, because of low temperature, the forbidden band width is not excluded from the systemVolatile substances, also by graphene/nanog-C3N4Photocatalytic degradation avoids the situation that inert gas (such as nitrogen) is introduced in the curing process to cause optical fiber shaking, ensures that a system has stable oxygen content, avoids the risk of introducing impurities, reduces uncontrollable factors, avoids oil accumulation on a quartz lamp tube, and ensures the curing effect of the optical fiber.
Preferably, the number of graphene layers is less than 10, and the specific surface area is more than 500m2/g。
Preferably, the nano g-C3N4Is g-C3N4Nanotubes of said g-C3N4The length-diameter ratio of the nanotube is 7500-10000. The nanotube structure can improve g-C3N4The crosslinking rate with the polymer and the high length-diameter ratio can improve the transmission of photon-generated carriers generated by the photocatalytic reaction, and further improve the photocatalytic curing efficiency and the degradation rate of volatile matters. g-C3N4The nano tube is prepared by directly calcining melamine without adding a template agent, and the cost is low.
Preferably, the first photoinitiator is phenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide; the second photoinitiator is biphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide.
Preferably, the first auxiliary agent and the second auxiliary agent are at least one of a defoaming agent, a leveling agent and a dispersing agent.
The defoaming agent is a polydimethylsiloxane defoaming agent;
a method for preparing a coating resin for an optical fiber, comprising the steps of:
(1) preparing a first coating resin:
(a) according to the proportion, uniformly mixing a first initiator and graphene, and dissolving the first initiator and the graphene into a mixture of acrylic acid-2-phenoxyethyl ester tripropylene glycol diacrylate and trimethylolpropane triacrylate to obtain a photoinitiator-graphene-acrylic monomer premix;
(b) uniformly mixing the photoinitiator-graphene-acrylic monomer premix obtained in the step (1), vinyl hexahydro-2H-azepine-2-copper, 3-trimethoxysilylpropane-1-thiol, 2-ethyl-2- [ 3-carboxyl-1-oxopropoxy) methyl ] propane-1, 3-diylbis [ 3-mercaptopropionic acid ] and a first auxiliary agent, reacting for 1-2H at 45-60 ℃, and filtering to obtain a first coating resin.
(2) Preparing a second coating resin:
(a) according to the proportion, the second initiator and the nano g-C3N4Uniformly mixing, dissolving in the mixture of 4, 4' - (1-methylethylidene) diphenol, polymer of hydrogenmethyloxirane and 2-acrylate, tripropylene glycol diacrylate, dioxy (methyl-2, 1-ethanediyl) diacrylate and 2-phenoxyethyl acrylate to obtain photoinitiator-g-C3N4-an acrylic monomer premix;
(b) the photoinitiator-g-C obtained in the step (1)3N4Uniformly mixing the acrylic monomer premix with hydroquinone monomethyl ether, hydroquinone monomethyl ether and a second auxiliary agent, reacting for 0.5-1 h at 30-40 ℃ under the irradiation of visible light, and filtering to obtain a second coating resin; the step reduces the reaction temperature of a preparation system by visible light assisted catalysis, and increases g-C3N4Bondability to other materials.
An application of coating resin for optical fibers in preparing optical fiber coatings by using an LED photocuring technology.
Preferably, the surface of the bare fiber is coated with a first coating resin, then coated with a second coating resin, and then subjected to simultaneous photocuring under a 385-405 nm wavelength LED light source.
Preferably, the oxygen content is controlled to be less than 1000ppm during the photocuring process, and the photocuring temperature of the first coating resin and the second coating resin is 45-55 ℃. The oxygen content affects the amount of free radical generation and the quality of the optical fiber.
Preferably, the wire drawing speed is controlled to be 3000-5000 m/min in the photocuring process.
Therefore, the invention has the following beneficial effects:
(1) graphene/nanog-C in coating resin system for optical fiber of the present invention3N4The first photoinitiator and the second photoinitiator are quickly cured through photocatalysis, the graphene material can improve the separation efficiency of photo-generated carriers in the photocatalysis process, the photocatalysis curing efficiency is further improved, the coating curing rate is high, volatile substances which are not removed in a photocatalysis degradation system are simultaneously degraded, oil accumulation in a quartz lamp tube is avoided, and the optical fiber curing effect is ensured;
(2) the preparation method has simple steps, has no special requirements on equipment and is easy for industrial production;
(3) the coating resin for the optical fiber can be applied to LED photocuring to prepare an optical fiber coating, the radiation energy can be controlled, the heat is less, the curing temperature is low, the wire drawing speed is high, the surface temperature of a product cannot exceed 55 ℃, and the problem that the product is not defective due to displacement caused by positioning of the product can be avoided.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
(1) Preparation of a first coating resin (sum of components 100 wt%):
(a) 2 wt% of phenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide (absorption wavelength 385-405 nm) and 0.005 wt% of layers with the specific surface area of 548m, wherein the layers are less than 102Uniformly mixing the graphene per gram, and dissolving the graphene in a mixture of 15 wt% of acrylic acid-2-phenoxyethyl ester and 1 wt% of tripropylene glycol diacrylate to obtain a photoinitiator-graphene-acrylic monomer premix;
(b) uniformly mixing the photoinitiator-graphene-acrylic monomer premix obtained in the step (1) with 5 wt% of vinyl hexahydro-2H-azepine-2-copper, 1 wt% of 3-trimethoxysilylpropane-1-thiol and the balance of polydimethylsiloxane defoamer, reacting for 2H at 45 ℃, and filtering to obtain the first coating resin.
(2) Preparation of a second coating resin (sum of components 100 wt%):
(a) 5 wt% of biphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide (absorption wavelength 385-405 nm) and 0.05 wt% of g-C with aspect ratio of 75003N4The nano-tubes are uniformly mixed and dissolved in a mixture of 25 wt% of 4, 4' - (1-methylethylidene) diphenol, a polymer of hydrogenmethyloxirane and 2-acrylate, 25 wt% of tripropylene glycol diacrylate, 1 wt% of dioxy (methyl-2, 1-ethanediyl) diacrylate and 1 wt% of 2-phenoxyethyl acrylate to obtain the photoinitiator-g-C3N4-an acrylic monomer premix;
(b) the photoinitiator-g-C obtained in the step (1)3N4And (3) uniformly mixing the acrylic monomer premix, 1 wt% of hydroquinone monomethyl ether and the balance of a flatting agent, reacting for 1h at 30 ℃ under the condition of visible light irradiation, and filtering to obtain a second coating resin.
(3) The above-mentioned first coating resin and second coating resin of the coating resin for an optical fiber perform two times of coating of the optical fiber through one die and then simultaneously cure:
coating a first coating resin on the surface of a bare fiber, then coating a second coating resin, and then carrying out simultaneous photocuring under a 385nm wavelength LED light source, wherein the oxygen content is controlled to be 858ppm in the photocuring process, the photocuring temperature of the first coating resin and the second coating resin is 45 ℃, and the wire drawing speed is controlled to be 3000m/min in the photocuring process.
Example 2
(1) Preparation of a first coating resin (sum of components 100 wt%):
(a) 6 wt% of phenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide (absorption wavelength 385-405 nm) and 0.01 wt% of layer number less than 10, the specific surface area 608m2Uniformly mixing the graphene per gram, and dissolving the graphene in a mixture of 5 wt% of acrylic acid-2-phenoxyethyl ester and 1 wt% of trimethylolpropane triacrylate to obtain a photoinitiator-graphene-acrylic monomer premix;
(b) uniformly mixing the photoinitiator-graphene-acrylic monomer premix obtained in the step (1), 1 wt% of vinyl hexahydro-2H-azepine-2-copper, 1 wt% of 2-ethyl-2- [ 3-carboxyl-1-oxopropoxy) methyl ] propane-1, 3-diylbis [ 3-mercaptopropionic acid ] and the balance of a dispersant, reacting for 1H at 60 ℃, and filtering to obtain a first coating resin.
(2) Preparation of a second coating resin (sum of components 100 wt%):
(a) 1 wt% of biphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide (absorption wavelength 385-405 nm) and 0.1 wt% of g-C with aspect ratio of 100003N4The nano-tubes are uniformly mixed and dissolved in a mixture of 50 wt% of 4, 4' - (1-methylethylidene) diphenol, polymer of hydrogenmethyl ethylene oxide and 2-acrylate, 10 wt% of tripropylene glycol diacrylate, 5 wt% of dioxy (methyl-2, 1-ethanediyl) diacrylate and 5 wt% of 2-phenoxyethyl acrylate to obtain the photoinitiator-g-C3N4-an acrylic monomer premix;
(b) the photoinitiator-g-C obtained in the step (1)3N4And (3) uniformly mixing the acrylic monomer premix, the polydimethylsiloxane defoamer and the dispersant in balance, reacting for 0.5h at 40 ℃ under the condition of visible light irradiation, and filtering to obtain second coating resin.
(3) The above-mentioned first coating resin and second coating resin of the coating resin for an optical fiber perform two times of coating of the optical fiber through one die and then simultaneously cure:
coating first coating resin on the surface of a bare fiber, then coating second coating resin, and then carrying out simultaneous photocuring under an LED light source with the wavelength of 405nm, wherein the oxygen content is controlled to be 781ppm in the photocuring process, the photocuring temperature of the first coating resin and the second coating resin is controlled to be 45 ℃, and the wire drawing speed is controlled to be 5000m/min in the photocuring process.
Example 3
(1) Preparation of a first coating resin (sum of components 100 wt%):
(a) 3 wt% of phenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide (absorption wavelength 385-405 nm) and 0.008 wt% of layers with the specific surface area 658m2The graphene is uniformly mixed and dissolved in a mixture of 10 wt% of acrylic acid-2-phenoxyethyl ester, 0.5 wt% of tripropylene glycol diacrylate and 0.6 wt% of trimethylolpropane triacrylate to obtain the photoinitiator-graphene-acrylic acidA monomer premix;
(b) uniformly mixing the photoinitiator-graphene-acrylic monomer premix obtained in the step (1) with 4 wt% of vinyl hexahydro-2H-azepine-2-copper, 0.5 wt% of 3-trimethoxysilylpropane-1-thiol, 0.3 wt% of 2-ethyl-2- [ 3-carboxy-1-oxopropoxy) methyl ] propane-1, 3-diylbis [ 3-mercaptopropionic acid ] and the balance of a dispersant, reacting for 1.5H at 50 ℃, and filtering to obtain a first coating resin.
(2) Preparation of a second coating resin (sum of components 100 wt%):
(a) 4 wt% of biphenyl (2, 4, 6-trimethyl benzoyl) phosphine oxide (absorption wavelength is 385-405 nm) and 0.08 wt% of g-C with length-diameter ratio of 80003N4The nano-tubes are uniformly mixed and dissolved in a mixture of 45 wt% of 4, 4' - (1-methylethylidene) diphenol, a polymer of hydrogenmethyloxirane and 2-acrylate, 15 wt% of tripropylene glycol diacrylate, 4 wt% of dioxy (methyl-2, 1-ethanediyl) diacrylate and 3 wt% of 2-phenoxyethyl acrylate to obtain the photoinitiator-g-C3N4-an acrylic monomer premix;
(b) the photoinitiator-g-C obtained in the step (1)3N4Uniformly mixing the acrylic monomer premix with 0.5 wt% of hydroquinone monomethyl ether and the balance of polydimethylsiloxane defoamer (flatting agent and dispersing agent), reacting for 50min at 35 ℃ under the condition of visible light irradiation, and filtering to obtain second coating resin.
(3) The above-mentioned first coating resin and second coating resin of the coating resin for an optical fiber perform two times of coating of the optical fiber through one die and then simultaneously cure:
the method comprises the steps of coating first coating resin on the surface of a bare fiber, then coating second coating resin, and then carrying out simultaneous photocuring under a 390nm wavelength LED light source, wherein the oxygen content is controlled to be 989ppm in the photocuring process, the photocuring temperature of the first coating resin and the second coating resin is controlled to be 50 ℃, and the wire drawing speed is controlled to be 4000m/min in the photocuring process.
Comparative example 1
Comparative example 1 is different from example 1 in that graphene is not added to the first coating resin, and the second coatingThe resin is not added with g-C3N4The nano tube is prepared by controlling the wire drawing speed to be 2500m/min in the photocuring process, and the rest processes are completely the same.
Comparative example 2
The comparative example 1 is different from the example 1 in that graphene is not added to the first coating resin, the drawing speed is controlled to 2800m/min during photocuring, and the rest of the processes are completely the same.
Comparative example 3
Comparative example 1 differs from example 1 in that g-C was not added to the second coating resin3N4The drawing speed of the nanotube is controlled to be 2600m/min in the photocuring process, and other processes are completely the same.
Comparative example 4
Comparative example 1 differs from example 1 in that g-C was added to the first coating resin3N4The nano tube and the second coating resin are added with graphene, the wire drawing speed is controlled to be 3000m/min in the photocuring process, and the other processes are completely the same.
The optical fibers obtained by using the coating resins for optical fibers of examples 1 to 3 and comparative examples 1 to 3 were examined for their performance parameters, and the results are shown in Table 1:
TABLE 1 test results
Figure BDA0002242054480000071
Figure BDA0002242054480000081
As can be seen from Table 1, only when the coating resin for optical fiber is doped with the graphene material in the first coating resin and the nanog-C is doped in the second coating resin3N4The visible light catalyst can be used for improving the coating curing degree in a synergistic manner, improving the strength of the optical fiber and further improving the wire drawing speed; neither addition (comparative example 1), addition of either component alone (comparative examples 2 and 3) or adjustment of the addition position (comparative example 4) resulted in a decrease in the performance parameters of the optical fiber. Of these, comparative example 13, no photocatalyst is added, so that the deposition of lamp tube volatile matters is caused, the curing effect of the optical fiber is influenced, the optical fiber is embrittled and the fiber breakage phenomenon is caused in severe cases, and the graphene is not added in the comparative example 2, so that the photocatalytic efficiency is low, and the curing rate of the coating is low; comparative example 4 graphene and nanog g-C were adjusted3N4After the visible light catalyst is added to the coating position, although the optical fiber strength can be improved, the wire drawing speed is improved, and no volatile matter is deposited on the lamp tube, the nano g-C3N4The visible light catalyst is less in contact with visible light in the inner layer first coating resin, and the light utilization rate is low, resulting in a decrease in the light curing rate.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.

Claims (7)

1. The application of the coating resin for the optical fiber in preparing the optical fiber coating by using the LED light curing technology is characterized in that the coating resin for the optical fiber comprises a first coating resin and a second coating resin, wherein the first coating resin is coated on the surface of a bare fiber, then the second coating resin is coated, and then the simultaneous light curing is carried out under an LED light source with the wavelength of 385-405 nm; the photocuring temperature of the first coating resin and the second coating resin is 45-55 ℃; controlling the wire drawing speed to be 3000-5000 m/min in the photocuring process;
the first coating resin comprises the following components in percentage by mass: 5-15% of acrylic acid-2-phenoxyethyl ester, 1-ethylhexahydro-2H-azepine-2-one, 2-6% of a first photoinitiator, 0-1% of 3- (trimethoxysilyl) -1-propanethiol, 0-1% of trimethylolpropane triacrylate, 0-1% of tripropylene glycol diacrylate, 0-1% of 2-ethyl-2- [ 3-carboxy-1-oxopropoxy) methyl ] propane-1, 3-diylbis [ 3-mercaptopropionic acid ], 0.005-0.01% of graphene and the balance of a first auxiliary agent;
the second coating resin comprises the following components in percentage by mass: polymerization of 4, 4' - (1-methylethylidene) diphenol with hydromethyloxirane and 2-acrylate25-50% of a material, 10-25% of tripropylene glycol diacrylate, 1-5% of bis (methyl-2, 1-ethanediyl) diacrylate, 1-5% of 2-phenoxyethyl acrylate, 0-1% of hydroquinone monomethyl ether, 1-5% of a second photoinitiator, and nano g-C3N40.05-0.1% of a second auxiliary agent, and the balance of the second auxiliary agent;
the absorption wavelength of the first photoinitiator and the absorption wavelength of the second photoinitiator are 385-405 nm.
2. The use according to claim 1, wherein the number of graphene layers is less than 10 and the specific surface area is greater than 500m2/g。
3. Use according to claim 1, wherein the nanog-C is3N4Is g-C3N4Nanotubes of said g-C3N4The length-diameter ratio of the nanotube is 7500-10000.
4. Use according to claim 1, wherein the first photoinitiator is phenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide; the second photoinitiator is biphenyl (2, 4, 6-trimethylbenzoyl) phosphine oxide.
5. The use according to claim 1, wherein the first and second auxiliary agents are at least one of antifoaming agents, leveling agents, and dispersing agents.
6. Use according to any one of claims 1 to 3, wherein the first coating resin is obtained by a process comprising the steps of:
(a) uniformly mixing a first initiator and graphene according to the proportion, and dissolving the mixture into a mixture of acrylic acid-2-phenoxyethyl ester, tripropylene glycol diacrylate and trimethylolpropane triacrylate to obtain a photoinitiator-graphene-acrylic acid monomer premix;
(b) uniformly mixing the photoinitiator-graphene-acrylic monomer premix obtained in the step (1), 1-ethylhexahydro-2H-azepine-2-one, 3- (trimethoxysilyl) -1-propanethiol, 2-ethyl-2- [ 3-carboxyl-1-oxopropoxy) methyl ] propane-1, 3-diyl bis [ 3-mercaptopropionic acid ] and a first auxiliary agent, reacting at 45-60 ℃, and filtering to obtain a first coating resin;
the second coating resin is prepared by a method comprising the following steps:
(a) according to the proportion, the second initiator and the nano g-C3N4Uniformly mixing, dissolving in the mixture of 4, 4' - (1-methylethylidene) diphenol, polymer of hydrogenmethyloxirane and 2-acrylate, tripropylene glycol diacrylate, dioxy (methyl-2, 1-ethanediyl) diacrylate and 2-phenoxyethyl acrylate to obtain photoinitiator-g-C3N4-an acrylic monomer premix;
(b) the photoinitiator-g-C obtained in the step (1)3N4And (3) uniformly mixing the acrylic monomer premix, hydroquinone monomethyl ether and a second auxiliary agent, reacting at 30-40 ℃ under the irradiation of visible light, and filtering to obtain a second coating resin.
7. Use according to claim 1, wherein the oxygen content is controlled to be less than 1000ppm during photocuring.
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CN107474605A (en) * 2017-08-18 2017-12-15 华南师范大学 A kind of optical fiber doping coating layer material and preparation method thereof

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CN106010144A (en) * 2016-06-20 2016-10-12 上海飞凯光电材料股份有限公司 UV-LED-curing optical fiber coating resin and preparing method and application thereof
CN106189418A (en) * 2016-07-22 2016-12-07 长飞光纤光缆股份有限公司 A kind of photocureable coating based on Graphene and preparation method thereof
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