CN111187568B - Low-refractive-index optical fiber inner layer coating and preparation method thereof - Google Patents
Low-refractive-index optical fiber inner layer coating and preparation method thereof Download PDFInfo
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- CN111187568B CN111187568B CN202010121219.2A CN202010121219A CN111187568B CN 111187568 B CN111187568 B CN 111187568B CN 202010121219 A CN202010121219 A CN 202010121219A CN 111187568 B CN111187568 B CN 111187568B
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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
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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
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5003—Polyethers having heteroatoms other than oxygen having halogens
- C08G18/5015—Polyethers having heteroatoms other than oxygen having halogens having fluorine atoms
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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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- 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
- 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
- C09D7/63—Additives non-macromolecular organic
Abstract
The invention discloses a low-refractive index optical fiber inner layer coating and a preparation method thereof; the low-refractive-index optical fiber inner layer coating comprises the following components in percentage by weight: 50-70% of fluorinated urethane acrylate oligomer, 10-30% of fluorinated monofunctional monomer, 10-30% of fluorinated difunctional monomer, 1-5% of initiator, 0.2-2% of silane coupling agent and 0.3-2% of flatting agent. The coating has the characteristics of low refractive index, large modulus and excellent bare optical fiber adhesive force, and can effectively improve the numerical aperture of optical signal transmission while ensuring the mechanical property of the optical fiber.
Description
Technical Field
The invention relates to the field of photocuring, in particular to a low-refractive-index optical fiber inner layer coating and a preparation method thereof.
Background
The optical fiber mainly comprises a core layer, a cladding layer, an inner coating and an outer coating. In general, the inner coating is soft and elastic, and is coated on the surface of the cladding to play a role in buffering external impact; the outer coating has high rigidity and strength, can improve the mechanical strength of the optical fiber, resists external force impact and protects the optical fiber from being influenced by external environment. The refractive index of the conventional optical fiber internal coating is 1.46-1.48, however, some special optical fibers need to use an internal coating with low refractive index, high mechanical strength and excellent adhesion to realize larger numerical aperture and smaller optical signal attenuation.
At present, the low-refractive-index optical fiber inner layer coating on the market is generally formed by combining fluorine-containing polyurethane acrylate oligomer, a monofunctional fluorine-containing acrylate monomer and an initiator, and the refractive index can be as low as 1.37, so that the aim of high numerical aperture can be fulfilled. However, the low-refractive-index coating in China at present generally has low mechanical strength and poor adhesion with glass, and is easily applied to special optical fibers to cause the problems of poor production stability, easy damage of finished products and the like.
Disclosure of Invention
Aiming at the defects of the existing low-refractive index coating, the invention provides a low-refractive index optical fiber inner layer coating with low refractive index, high mechanical strength and high adhesive force and a preparation method thereof, which are used for improving the numerical aperture and the mechanical strength of an optical fiber. According to the invention, the fluorine-containing polyurethane acrylate oligomer, the difunctional fluorine-containing acrylate monomer, the long-chain monofunctional fluorine-containing acrylate monomer, the initiator, the leveling agent and the silane coupling agent are matched, so that the low refractive index of the coating is ensured, and meanwhile, higher mechanical strength and excellent glass adhesion are maintained. Wherein the difunctional fluorine-containing acrylate monomer can obviously improve the film forming modulus of the formula.
The above object of the present invention is achieved by the following technical solutions:
the invention provides a low-refractive-index optical fiber inner layer coating, which comprises the following components in percentage by weight: 50-70% of fluorinated urethane acrylate oligomer, 10-30% of fluorinated monofunctional monomer, 10-30% of fluorinated difunctional monomer, 1-5% of initiator, 0.2-2% of silane coupling agent and 0.3-2% of flatting agent.
Further, the fluorinated urethane acrylate oligomer is synthesized from (i) a fluorinated polyether polyol, (ii) a polyisocyanate, (iii) a hydroxyl acrylate, (iv) a polycondensation catalyst, and (v) a polymerization inhibitor.
Further, 3, a low refractive index optical fiber inner layer coating according to claim 2, wherein the fluorinated urethane acrylate oligomer is synthesized by the steps of: adding fluorinated polyether polyol, diisocyanate and a polycondensation catalyst at room temperature, heating and stirring, reacting until the NCO% reaches the theoretical midpoint, and stopping the reaction to obtain an intermediate mixture; then adding hydroxyl acrylate, a polycondensation catalyst and a polymerization inhibitor, heating and stirring, reacting until NCO% is less than or equal to 0.15%, and stopping the reaction to obtain the fluorinated urethane acrylate oligomer; wherein the feeding molar ratio of the fluorinated polyether polyol to the diisocyanate to the hydroxy acrylate is (1.0-5.0): (2.0-8.0): (2.0-8.0), the amount of the polycondensation catalyst used for two times is 0.01-0.1% of the total mass of the prepolymer, and the amount of the polymerization inhibitor used for two times is 0.5-1% of the total mass of the prepolymer.
Further, the fluorinated polyether polyol is a polyether polyol having a molecular weight of 50 to 5000 containing-CF as a repeating unit2CF2-or-CF2CF2An O-fluorinated polyether polyol.
Further, the polyisocyanate is selected from at least one of aliphatic diisocyanate and aromatic diisocyanate. Specifically, the diisocyanate is selected from one or more of 1, 6-hexane diisocyanate, isophorone diisocyanate, methylene bis (4-cyclohexyl isocyanate), 2, 4-trimethyl hexamethylene diisocyanate, 2, 5-bis (isocyanatomethyl) -bicyclo [2.2.1] heptane, 2, 6-bis (isocyanatomethyl) -bicyclo [2.2.1] heptane, m-phenylene diisocyanate, p-phenylene diisocyanate, 3 '-dimethyl-4, 4' -diphenylmethane diisocyanate, 3 '-dimethylphenylene diisocyanate and 4, 4' -biphenyl diisocyanate. More preferably, the diisocyanate is isophorone diisocyanate.
Further, the acrylic acid hydroxy ester is selected from 2-hydroxy ethyl (meth) acrylate, 2-hydroxy propyl (meth) acrylate, 2-hydroxy butyl (meth) acrylate, neopentyl glycol mono (meth) acrylate.
Further, the polycondensation catalyst is dibutyltin dilaurate, N-dimethylbenzylamine, N-dimethylcyclohexylamine, N' -dimethylpyridine or tetraisooctyl titanate.
Further, the polymerization inhibitor is tert-butyl hydroquinone, p-hydroxyanisole, hydroquinone or o-methyl hydroquinone.
Further, the fluorinated monofunctional monomer includes one or more of hexafluorobutyl (meth) acrylate, octafluoropentyl (meth) acrylate, tridecyl octyl (meth) acrylate, dodecafluoroheptyl (meth) acrylate, 1,2, 2-tetrahydroheptadecafluorodecyl methacrylate, icosane methacrylate, or 1,1,2, 2-tetrahydropentacosafluorotetradecyl methacrylate.
Further, the fluorinated bifunctional monomer is synthesized from (i) a fluorinated diol having a molecular weight of 50 to 600, (ii) acrylic acid, (iii) a catalyst and (iv) a polymerization inhibitor.
Further, the fluorinated bifunctional monomer is synthesized by the following steps: heating and stirring the fluorinated dihydric alcohol, the acrylic acid, the catalyst and the polymerization inhibitor at the temperature of 80-100 ℃ to perform esterification reaction; discharging water generated by the reaction by a water-carrying agent cyclohexane; then washing the mixture to be neutral by sodium bicarbonate solution, saturated sodium chloride solution and distilled water, and finally removing the solvent by decompression to obtain the fluorinated bifunctional monomer; wherein the fluorinated dihydric alcohol, the acrylic acid, the catalyst and the polymerization inhibitor are respectively 45-78%, 18-50%, 1.5-3.5% and 0.5-1.5%.
Further, the fluorinated diol having a molecular weight of 200-.
Further, the catalyst is p-toluenesulfonic acid.
Furthermore, the polymerization inhibitor is hydroquinone.
Further, the initiator comprises one or more of 2,4, 6-trimethylbenzoyldiphenylphosphine oxide, phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide, 1-hydroxycyclohexylphenylketone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinylbenzyl) butanone, 2-methyl-1- [4- (methylthio) phenyl ] -2- (4-morpholinyl) -1-propanone and benzoin dimethyl ether.
Further, the silane coupling agent is one or more of gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane and gamma-mercaptopropyltrimethoxysilane.
Further, the leveling agent comprises one or two of a polyether modified organic silicon leveling agent and an acrylic acid modified organic silicon leveling agent.
Compared with the prior art, the invention uses the fluorine-containing polyurethane acrylate oligomer, the difunctional fluorine-containing acrylate monomer, the long-chain monofunctional fluorine-containing acrylate monomer, the initiator, the leveling agent and the silane coupling agent, and keeps higher mechanical strength and excellent glass adhesion while ensuring the low refractive index of the coating.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
The fluorinated urethane acrylate oligomer and the fluorinated bifunctional monomer adopted by the invention are synthesized by the following modes:
(1) synthesis of fluorinated urethane acrylate oligomer a:
respectively adding 0.12mol of isophorone diisocyanate and 0.040g of dibutyltin dilaurate into a 250ml reaction bottle, dropwise adding 0.06mol of fluoropolyether diol fluoroolink AD1700 under a stirring state, heating in an oil bath to maintain the reaction system at 40-50 ℃ until the NCO content in the system is close to a theoretical terminal point, adding 0.12mol of hydroxyethyl acrylate, 0.803g of p-hydroxyanisole and 0.040g of dibutyltin dilaurate, simultaneously adjusting the temperature of the reaction system to 70-90 ℃, and finishing the reaction when the NCO content is less than 0.15%.
The resulting fluorinated urethane acrylate oligomer A was measured for viscosity 15000cps (25 ℃ C.), and refractive index 1.387(25 ℃ C.).
(2) Synthesis of fluorinated difunctional monomer A:
1H,1H,9H, 9H-perfluoro-1, 9-nonanediol with the mass fraction of 71.5%, 25% of acrylic acid, 2.5% of p-toluenesulfonic acid and 1% of hydroquinone are heated and stirred at the temperature of 80-100 ℃ for esterification reaction. The water produced by the reaction is discharged by cyclohexane as a water-carrying agent. Then washing the mixture to be neutral by sodium bicarbonate solution, saturated sodium chloride solution and distilled water, and finally removing the solvent by decompression to obtain the fluorinated bifunctional monomer A.
The resulting fluorinated difunctional monomer A was determined to have a viscosity of 50cps (25 ℃ C.), a refractive index of 1.353(25 ℃ C.).
Example 1
This example provides a low index inner coating for optical fibers having a formulation as shown in Table 1
TABLE 1
The preparation method of the low-refractive-index inner layer coating comprises the steps of accurately weighing all the components, stirring for 2 hours at 500rpm and 50 ℃, and discharging through 2-level filtration to obtain a finished product.
Example 2
This example provides a low index inner coating for optical fibers having a formulation as shown in Table 2
TABLE 2
The preparation method of the low-refractive-index inner layer coating comprises the steps of accurately weighing all the components, stirring for 2 hours at 500rpm and 50 ℃, and discharging through 2-level filtration to obtain a finished product.
Example 3
This example provides a low index inner coating for optical fibers having a formulation as shown in Table 3
TABLE 3
The preparation method of the low-refractive-index inner layer coating comprises the steps of accurately weighing all the components, stirring for 2 hours at 500rpm and 50 ℃, and discharging through 2-level filtration to obtain a finished product.
Example 4
This example provides a low refractive index inner coating for optical fibers having a formulation as shown in Table 4
TABLE 4
The preparation method of the low-refractive-index inner layer coating comprises the steps of accurately weighing all the components, stirring for 2 hours at 500rpm and 50 ℃, and discharging through 2-level filtration to obtain a finished product.
Comparative example 1
This comparative example provides a low refractive index inner coating material for optical fiber, whose formulation is shown in Table 5
TABLE 5
The preparation method of the low-refractive-index inner layer coating comprises the steps of accurately weighing all the components, stirring for 2 hours at 500rpm and 50 ℃, and discharging through 2-level filtration to obtain a finished product.
The coatings of examples 1 to 4 and comparative example 1 were tested for their properties, and the results and methods are shown in Table 6.
TABLE 6
From the above, the low-refractive-index inner layer coating for the optical fiber provided by the invention has the characteristics of high modulus, good glass adhesion and low refractive index, and can meet the requirements of high numerical aperture, low loss and high mechanical strength of special optical fibers.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (4)
1. The low-refractive-index optical fiber inner layer coating is characterized by comprising the following components in percentage by weight: 50-70% of fluorinated urethane acrylate oligomer, 10-30% of fluorinated monofunctional monomer, 10-30% of fluorinated difunctional monomer, 1-5% of initiator, 0.2-2% of silane coupling agent and 0.3-2% of flatting agent;
the fluorinated urethane acrylate oligomer is synthesized by the following steps: respectively adding 0.12mol of isophorone diisocyanate and 0.040g of dibutyltin dilaurate, dropwise adding 0.06mol of fluoropolyether diol fluorolanink AD1700 under a stirring state, heating in an oil bath to maintain the reaction system at 40-50 ℃, adding 0.12mol of hydroxyethyl acrylate, 0.803g of p-hydroxyanisole and 0.040g of dibutyltin dilaurate until the NCO content in the system is close to a theoretical terminal point, simultaneously adjusting the temperature of the reaction system to 70-90 ℃, and finishing the reaction when the NCO content is less than 0.15%; the obtained fluorinated urethane acrylate oligomer has the viscosity of 15000cps and the refractive index of 1.387 at the temperature of 25 ℃;
the fluorinated bifunctional monomer is synthesized by: heating and stirring 1H,1H,9H, 9H-perfluoro-1, 9-nonanediol with the mass fraction of 71.5%, 25% of acrylic acid, 2.5% of p-toluenesulfonic acid and 1% of hydroquinone at the temperature of 80-100 ℃ to perform esterification reaction, discharging water generated by the reaction from cyclohexane as a water-carrying agent, washing the water to be neutral through a sodium bicarbonate solution, a saturated sodium chloride solution and distilled water, and finally removing the solvent under reduced pressure to obtain the fluorinated bifunctional monomer; the obtained fluorinated bifunctional monomer has a viscosity of 50cps and a refractive index of 1.353 at 25 ℃;
the initiator is one or more of 2,4, 6-trimethylbenzoyl diphenyl phosphine oxide, phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-benzyl-2-dimethylamine-1- (4-morpholine benzyl phenyl) butanone, 2-methyl-1- [4- (methylthio) phenyl ] -2- (4-morpholinyl) -1-acetone and benzoin dimethyl ether.
2. The low refractive index optical fiber inner layer coating of claim 1, wherein the fluorinated monofunctional monomer comprises one or more of hexafluorobutyl (meth) acrylate, octafluoropentyl (meth) acrylate, tridecyl (meth) acrylate, dodecafluoroheptyl (meth) acrylate, 1,2, 2-tetrahydroheptadecafluorodecyl methacrylate, eicosafluoroundecanoacrylate, 1,2, 2-tetrahydropentacosafluorotetradecyl methacrylate.
3. The low refractive index optical fiber inner layer coating material according to claim 1, wherein the silane coupling agent comprises one or more of gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, 3-mercaptopropyltriethoxysilane, and gamma-mercaptopropyltrimethoxysilane.
4. The low refractive index optical fiber inner layer coating material according to claim 1, wherein the leveling agent comprises one or two of a polyether modified silicone leveling agent and an acrylic modified silicone leveling agent.
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| CN112759961B (en) * | 2021-02-09 | 2022-01-04 | 上海先权光纤科技有限公司 | Low-refractive-index optical fiber coating and preparation method thereof |
| CN113355017B (en) * | 2021-05-06 | 2022-04-29 | 武汉长盈鑫科技有限公司 | Low-refractive-index optical fiber coating resin with high glass transition temperature |
| CN114773985B (en) * | 2022-05-06 | 2022-11-04 | 长飞光纤光缆股份有限公司 | Low-refractive-index optical fiber coating |
| CN115466593A (en) * | 2022-09-02 | 2022-12-13 | 深圳市浩力新材料技术有限公司 | Ultraviolet light curing adhesive |
| CN115403716A (en) * | 2022-09-14 | 2022-11-29 | 武汉镱得飞光电技术有限公司 | Ultraviolet-curing acrylic resin composition and preparation and application thereof |
| CN116042083A (en) * | 2022-12-21 | 2023-05-02 | 长飞光纤光缆股份有限公司 | Silane modified low-refractive-index optical fiber coating |
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