CN110007391A - A kind of low temperature preparation method of polyimide coating optical fiber - Google Patents
A kind of low temperature preparation method of polyimide coating optical fiber Download PDFInfo
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- CN110007391A CN110007391A CN201910292805.0A CN201910292805A CN110007391A CN 110007391 A CN110007391 A CN 110007391A CN 201910292805 A CN201910292805 A CN 201910292805A CN 110007391 A CN110007391 A CN 110007391A
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/02395—Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture
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Abstract
The present invention relates to polyimide coating optical fiber preparation technical fields, and disclose a kind of low temperature preparation method of polyimide coating optical fiber, the following steps are included: using pyromellitic acid anhydride and phenylenediamine as raw material, in N, synthesizing polyamides acid in dinethylformamide solvent, maleic anhydride trigger for optical solidification is added into polyamic acid, and with PDADMAC binder jointly under ultraviolet light, make the polyamic acid slurry sticked on optical fiber, at 80 DEG C of temperature, under the ultraviolet lamp of wavelength 365nm, ultraviolet light curing reaction occurs and generates polyimide coating, polyimide coating optical fiber is prepared.The present invention solves the preparation method of polyimide coating optical fiber in the prior art, during preparation, the relatively high technical problem of existing curing reaction temperature.
Description
Technical field
The present invention relates to polyimide coating optical fiber preparation technical field, specially a kind of polyimide coating optical fiber it is low
Warm preparation method.
Background technique
Optical fiber primary structure includes sandwich layer, covering and coat.The application stability and service life of optical fiber and painting
Layer has close relationship.Ordinary optic fibre uses ultra-violet curing acrylic resin coating, the use of temperature is -60C~85 DEG C.If
It works in the environment of being higher than 85 DEG C for a long time, heat ageing can occur for general ultraviolet solidify coating, especially have O2It is existing
Thermo-oxidative ageing can occur under environment, accelerate the fracture process of coating macromolecular chain, so that coating is made to lose the effect for protecting optical fiber,
It can not prevent hydrone from invading optical fiber, accelerate the fatigue process of optical fiber, cause optical fiber surface micro-crack to expand, and eventually lead to
Optical fiber failure.With the extension of fiber optic applications environment, common acrylate coated optical fiber can no longer meet answering for particular surroundings
With requiring.It needs to carry out high-temperature resistant optical fiber research and development thus, using different high-temperaure coatings, improves the heat resistance and machinery of optical fiber
Performance allows to use under the adverse circumstances such as high temperature, high humidity.
In existing high molecular material, polyimides (PI) is a kind of high molecular material for integrating numerous performances,
Main performance include: 1. heat resistance it is good, glass transition temperature be 350 DEG C~400 DEG C, decomposition starting temperature be greater than 500 DEG C；
2. resistance to low temperature is good, it is not broken at -200 DEG C or less；3. comparing other high molecular materials, thermal expansion coefficient is lower, can
Reach 10-6℃；4. having excellent mechanical performance, tensile strength is greater than 100MPa；5. having biological friendly, it can be used for medicine
Field.
The patent of invention that Authorization Notice No. is CN101726792B discloses a kind of high-temperature resistant optical fiber and its manufacturing method, should
High temperature optical fiber includes optical fiber and the coating for being coated on fiber outer surface, and coating is polyimide coating, and polyimide coating is by light
Polyimide solution is heated on fine surface dip-coating solidifies, including precoating, precuring and secondary coating；Wherein, pre- solid
The high temperature of change divides into two regions, and one is solvent volatilization area, and temperature range is 100 DEG C~240 DEG C, the other is molecule closes
At area, temperature is 240 DEG C~460 DEG C；Secondary coating and cured high temperature divide into two regions, and one is solvent volatilization area,
The temperature range in the area is 120 DEG C~300 DEG C, completes the volatilization process of solvent, the other is molecule synthesis area, the temperature in the area
It is 300 DEG C~500 DEG C, completes the polymerization process of solute small molecule, secondary coating carries out 1 to 6 time.
Although foregoing invention can be used for high temperature and harsh environments, long-term use temperature can be up to 300 DEG C, and
Using stability of characteristics, it is able to maintain good persistence, still, above-mentioned preparation method is needed by repeatedly coating solidification process ability
Coating is completed to make, and more importantly, curing reaction temperature is relatively high.
The present invention provides a kind of low temperature preparation method of polyimide coating optical fiber, it is intended to solve polyamides in the prior art
The preparation method of imines coated optical fiber, during preparation, the relatively high technical problem of existing curing reaction temperature.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of low temperature preparation method of polyimide coating optical fiber, solutions
It has determined the preparation method of polyimide coating optical fiber in the prior art, during preparation, existing curing reaction temperature
Relatively high technical problem.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of low temperature preparation method of polyimide coating optical fiber, comprising the following steps:
S101. 50mLN is added into the reactor equipped with blender, condenser pipe, in dinethylformamide, be passed through N2It protects
Shield is warming up to 40~65 DEG C, and 10.8g phenylenediamine is added into reactor, and stirring is to being completely dissolved, in temperature 50 C, stirring speed
Under rate 120r/min, be slowly added to 21.8g pyromellitic acid anhydride into reactor, after addition, 40~65 DEG C of temperature,
1h is reacted under stirring rate 120r/min, polyamic acid is prepared；
S102. 20g maleic anhydride monomer is added in the reactor in step S101, in 80 DEG C of temperature, stirring rate
1h is reacted under 120r/min, later, reacts 3h at 180 DEG C of temperature, stirring rate 120r/min, thick liquid is prepared；
S103. using the thick liquid in dehydrated alcohol repeatedly washing step S102, organic solvent N, N- dimethyl are removed
Formamide；
S104. the thick liquid in step S103 is added in 15~30mLPDADMAC, is stirred evenly, is prepared
Polyamic acid slurry；
S105. radial diameter≤220um optical fiber is immersed in the polyamic acid slurry in step S104, is submerged
Taken out after 30min, by stick the optical fiber for having polyamic acid slurry be placed in 60~80 DEG C of temperature, wavelength 365nm ultraviolet lamp under spoke
6~10h is penetrated, polyamic acid slurry is solidified into polyimide coating in optical fiber surface, and polyimide coating optical fiber is prepared.
Preferably, in the step S101, after pyromellitic acid anhydride adds, in temperature 50 C, stirring rate
1h is reacted under 120r/min.
Preferably, in the step S104, thick liquid is added in 20mLPDADMAC.
Preferably, in the step S105, the optical fiber for having polyamic acid slurry will be sticked and be placed in temperature 60 C, wavelength
10h is radiated under the ultraviolet lamp of 365nm.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
The present invention synthesizes polyamides in n,N-Dimethylformamide solvent using pyromellitic acid anhydride and phenylenediamine as raw material
Amino acid adds maleic anhydride trigger for optical solidification into polyamic acid, and with PDADMAC binder jointly in ultraviolet light
Under, make the polyamic acid slurry sticked on optical fiber, 80 DEG C of temperature, wavelength 365nm ultraviolet lamp under, it is anti-that ultraviolet light solidification occurs
Polyimide coating should be generated, polyimide coating optical fiber is prepared；80 DEG C of curing reaction temperature of the invention and existing skill
300 DEG C~500 DEG C of solidification temperature in art are compared, and realize the technology effect for significantly reducing polyimide coating curing reaction temperature
Fruit.
Specific embodiment
Embodiment one:
S101. 50mLN is added into the reactor equipped with blender, condenser pipe, in dinethylformamide, be passed through N2It protects
Shield is warming up to 40 DEG C, and 10.8g phenylenediamine is added into reactor, stirs to being completely dissolved, in temperature 50 C, stirring rate
Under 120r/min, 21.8g pyromellitic acid anhydride is slowly added into reactor, after addition, in 40 DEG C of temperature, stirring speed
1h is reacted under rate 120r/min, polyamic acid is prepared；
S102. 20g maleic anhydride monomer is added in the reactor in step S101, in 80 DEG C of temperature, stirring rate
1h is reacted under 120r/min, later, reacts 3h at 180 DEG C of temperature, stirring rate 120r/min, thick liquid is prepared；
S103. using the thick liquid in dehydrated alcohol repeatedly washing step S102, organic solvent N, N- dimethyl are removed
Formamide；
S104. the thick liquid in step S103 is added in 15mLPDADMAC, is stirred evenly, polyamides is prepared
Amino acid slurry；
S105. radial diameter≤220um optical fiber is immersed in the polyamic acid slurry in step S104, is submerged
It is taken out after 30min, the optical fiber for having polyamic acid slurry will be sticked and be placed under the ultraviolet lamp of temperature 60 C, wavelength 365nm and radiate 6h,
Polyamic acid slurry is solidified into polyimide coating in optical fiber surface, and polyimide coating optical fiber is prepared；
S106. the performance of the polyimide coating of polyimide coating optical fiber in step S105 is tested, as a result are as follows:
The adhesive force of polyimide coating is 1 grade, and the surface of polyimide coating is in even compact state.
Embodiment two:
S101. 50mLN is added into the reactor equipped with blender, condenser pipe, in dinethylformamide, be passed through N2It protects
Shield is warming up to 65 DEG C, and 10.8g phenylenediamine is added into reactor, stirs to being completely dissolved, in temperature 50 C, stirring rate
Under 120r/min, 21.8g pyromellitic acid anhydride is slowly added into reactor, after addition, in 65 DEG C of temperature, stirring speed
1h is reacted under rate 120r/min, polyamic acid is prepared；
S102. 20g maleic anhydride monomer is added in the reactor in step S101, in 80 DEG C of temperature, stirring rate
1h is reacted under 120r/min, later, reacts 3h at 180 DEG C of temperature, stirring rate 120r/min, thick liquid is prepared；
S103. using the thick liquid in dehydrated alcohol repeatedly washing step S102, organic solvent N, N- dimethyl are removed
Formamide；
S104. the thick liquid in step S103 is added in 30mLPDADMAC, is stirred evenly, polyamides is prepared
Amino acid slurry；
S105. radial diameter≤220um optical fiber is immersed in the polyamic acid slurry in step S104, is submerged
Taken out after 30min, by stick the optical fiber for having polyamic acid slurry be placed in 80 DEG C of temperature, wavelength 365nm ultraviolet lamp under radiate
10h, polyamic acid slurry are solidified into polyimide coating in optical fiber surface, and polyimide coating optical fiber is prepared；
S106. the performance of the polyimide coating of polyimide coating optical fiber in step S105 is tested, as a result are as follows:
The adhesive force of polyimide coating is 1 grade, and the surface of polyimide coating is in even compact state.
Embodiment three:
S101. 50mLN is added into the reactor equipped with blender, condenser pipe, in dinethylformamide, be passed through N2It protects
Shield is warming up to 50 DEG C, and 10.8g phenylenediamine is added into reactor, stirs to being completely dissolved, in temperature 50 C, stirring rate
Under 120r/min, 21.8g pyromellitic acid anhydride is slowly added into reactor, after addition, in temperature 50 C, stirring speed
1h is reacted under rate 120r/min, polyamic acid is prepared；
S102. 20g maleic anhydride monomer is added in the reactor in step S101, in 80 DEG C of temperature, stirring rate
1h is reacted under 120r/min, later, reacts 3h at 180 DEG C of temperature, stirring rate 120r/min, thick liquid is prepared；
S103. using the thick liquid in dehydrated alcohol repeatedly washing step S102, organic solvent N, N- dimethyl are removed
Formamide；
S104. the thick liquid in step S103 is added in 20mLPDADMAC, is stirred evenly, polyamides is prepared
Amino acid slurry；
S105. radial diameter≤220um optical fiber is immersed in the polyamic acid slurry in step S104, is submerged
It is taken out after 30min, the optical fiber for having polyamic acid slurry will be sticked and be placed under the ultraviolet lamp of temperature 60 C, wavelength 365nm and radiate
10h, polyamic acid slurry are solidified into polyimide coating in optical fiber surface, and polyimide coating optical fiber is prepared；
S106. the performance of the polyimide coating of polyimide coating optical fiber in step S105 is tested, as a result are as follows:
The adhesive force of polyimide coating is 1 grade, and the surface of polyimide coating is in even compact state.
Claims (4)
1. a kind of low temperature preparation method of polyimide coating optical fiber, which comprises the following steps:
S101. 50mLN is added into the reactor equipped with blender, condenser pipe, in dinethylformamide, be passed through N2Protection rises
Temperature is added 10.8g phenylenediamine into reactor, stirs to being completely dissolved, in temperature 50 C, stirring rate to 40~65 DEG C
Under 120r/min, 21.8g pyromellitic acid anhydride is slowly added into reactor, after addition, in 40~65 DEG C of temperature, is stirred
It mixes and reacts 1h under rate 120r/min, polyamic acid is prepared；
S102. 20g maleic anhydride monomer is added in the reactor in step S101, in 80 DEG C of temperature, stirring rate 120r/
1h is reacted under min, later, reacts 3h at 180 DEG C of temperature, stirring rate 120r/min, thick liquid is prepared；
S103. using the thick liquid in dehydrated alcohol repeatedly washing step S102, organic solvent N, N- dimethyl formyl are removed
Amine；
S104. the thick liquid in step S103 is added in 15~30mLPDADMAC, is stirred evenly, polyamides is prepared
Amino acid slurry；
S105. radial diameter≤220um optical fiber is immersed in the polyamic acid slurry in step S104, after submerging 30min
Take out, by stick the optical fiber for having polyamic acid slurry be placed in 60~80 DEG C of temperature, wavelength 365nm ultraviolet lamp under radiation 6~
10h, polyamic acid slurry are solidified into polyimide coating in optical fiber surface, and polyimide coating optical fiber is prepared.
2. low temperature preparation method according to claim 1, which is characterized in that in the step S101, Pyromellitic Acid two
After acid anhydride adds, 1h is reacted at temperature 50 C, stirring rate 120r/min.
3. low temperature preparation method according to claim 1, which is characterized in that in the step S104, by thick liquid plus
Enter into 20mLPDADMAC.
4. low temperature preparation method according to claim 1, which is characterized in that in the step S105, have polyamides for sticking
The optical fiber of amino acid slurry is placed under the ultraviolet lamp of temperature 60 C, wavelength 365nm and radiates 10h.
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| US5567219A (en) * | 1994-07-20 | 1996-10-22 | Galileo Electro-Optics Corporation | Polyimide coated heavy metal fluoride glass fiber and method of manufacture |
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| CN104193993A (en) * | 2014-08-13 | 2014-12-10 | 南京理工大学 | Polyamide acid copolymer and polyimide film prepared from polyamide acid copolymer |
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|---|---|---|---|---|
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| CN107936531A (en) * | 2016-05-31 | 2018-04-20 | 王翔 | A kind of preparation method of glass fiber reinforced polyester urethane |
| CN106098145A (en) * | 2016-07-06 | 2016-11-09 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of low-temperature cured conductive paste based on flexible parent metal and preparation method thereof |
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| CN109181622A (en) * | 2018-09-03 | 2019-01-11 | 浙江福斯特新材料研究院有限公司 | A kind of highly heat-resistant polyimide insulating materials of low-temperature setting |
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Application publication date: 20190712 |