CN100408318C - Preparation method of gradient polymer optical fiber premade rod - Google Patents
Preparation method of gradient polymer optical fiber premade rod Download PDFInfo
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- CN100408318C CN100408318C CNB2005101245859A CN200510124585A CN100408318C CN 100408318 C CN100408318 C CN 100408318C CN B2005101245859 A CNB2005101245859 A CN B2005101245859A CN 200510124585 A CN200510124585 A CN 200510124585A CN 100408318 C CN100408318 C CN 100408318C
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Abstract
The present invention discloses a preparation method of gradient polymer optical fiber premade rods, which has the steps that firstly initiator and chain transfer agent are added into a certain amount of monomer high-purity methyl methacrylate; under the temperature of 70 to 95DEG. C, when the prepoly degrees reaches to a conversion rate of 8 to 20%, the prepolymer is added into a stainless steel container or a glass tube with one end closed, and then the methyl methacrylate is tightly clung to the inner wall of the container for polymerization to form a polymethyl methacrylate layer with certain thickness for polymer optical fiber by the centrifugal rotation at the rotary speed of 500 rpm to 3000 rpm for 12h to 36h; then, initiator, chain transfer agent and doping agent are added into another high-purity methyl methacrylate, and the preparation process is repeated continuously to easily prepare a polymer optical fiber premade rod with large size and no defects. The distribution curve of refractive index in the radial direction of the premade rod can be controlled precisely, so that polymer optical fiber drawn by the premade rod certainly has favorable bandwidth performance.
Description
Technical field
The invention belongs to broadband access and information communication field and field of photovoltaic materials in the high speed optical communication network, be specifically related to a kind of preparation method of gradient polymer optical fiber premade rod.
Background technology
Compare with silica fibre, polymer optical fiber (Polymer Optical Fibers, POF) have advantages such as pliability is good, fibre diameter is big, the easy adjusting of numerical aperture, have lower comprehensive use cost, be considered to the perfect medium in the short distance distributed network.POF is divided into directly indeclinable step change type optical fiber of refractive index (SI-POF) and footpath gradient fiber (GI-POF) two major types that refractive index gradually changes that make progress upwards of optical fiber.Compare with the former, the latter has less modal dispersion, thereby bandwidth is big far beyond the former, and along with the development of digital video signal etc. is more and more higher to network bandwidth performance demands, GI-POF more and more causes people's attention.
The main flow preparation method of GI-POF has three kinds at present: interface-gel copolymerization method, multi-layer co-extruded method and centrifugal polymerization method.First method is the Koike Kangbo professor of Japanese keio university and partner's invention thereof, and its appearance has changed the history that polymeric material can not prepare gradient fiber.Its principle is the gel effect that has adopted in the high molecular weight reactive process.At first in high-purity lucite tube of one one end closure, pour into the mixed solution of methyl methacrylate (MMA) monomer, adulterant, initator, chain-transferring agent, monomer is with the tube wall swelling under the uniform temperature, form gel layer, because gel effect, the MMA polymerization is very fast in this layer, with the radially inwardly propelling of adulterant, make adulterant (refractive index) form the gradient distribution that the footpath makes progress along gel layer.This method is present the most ripe a kind of method, but is not easy to regulate the upwards distribution of refractive index of footpath (Refractive Index Distribution, RID) curve, and RID directly has influence on obtained bandwidth of an optical fiber performance in the future.
Multi-layer co-extruded method is that the transparent polymer material of two or more different refractivities (as the pmma material of the different amount adulterants that mixed) is extruded simultaneously by the mould of a particular design, make the higher material of refractive index occupy the center, the material that refractive index is low slightly is centered around around it, the index distribution that initial gained optical fiber directly makes progress is actual to be stair-stepping, through Overheating Treatment, obtain the smoothed curve (gradient type) of index distribution then.The main shortcoming of this method be equipment is required very high, also very immature at present.
The centrifugal polymerization method mainly is that the centrifugal force that relies on different refractivity, different densities material to receive in centrifugal field is different and form refractive index gradient, and its detailed principle and process are in the Chinese patent (patent No.: detailed introduction is arranged ZL01100428.2).The shortcoming of this method equally also is accurately to control the directly distribution curve of refractive index upwards of optical fiber, thereby gained bandwidth of an optical fiber performance is also usually undesirable.
Summary of the invention
As mentioned above, although the several different methods of preparation GI-POF has been arranged now, these methods all exist certain defective and deficiency, and directly upwards the ability of regulation and control of the distribution curve of refractive index is limited to optical fiber for existing method in outstanding behaviours.Purpose of the present invention overcomes this defective just, and a kind of preparation method of gradient polymer optical fiber premade rod is provided, and this method makes and the regulation and control that the index distribution of prepared fiber products can be more freely do not rely on simultaneously very complex apparatus again.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of preparation method of gradient polymer optical fiber premade rod is characterized in that, comprises the following steps:
The first step: at first in a certain amount of monomer high purity methacrylic acid methyl esters, add the initator of 0.1wt%～1wt% and the chain-transferring agent of 0.1wt%～0.5wt%, under 70 ℃～95 ℃ temperature, when pre-polymerization when conversion ratio is 8%～20%, reduce temperature of charge to room temperature, join then in the rustless steel container or glass tube of one one end sealing, and should become rusty steel container or glass tube under 35 ℃～60 ℃ temperature, with the 500rpm～centrifugal rotation of 3000rpm rotating speed 12h～36h, make methyl methacrylate be close to container inner wall and be polymerized to conversion ratio 60%～80% and form and to have certain thickness polymethyl methacrylate (PMMA) layer;
Second step: the initator that in other a certain amount of monomer high purity methacrylic acid methyl esters, adds 0.1wt%～1wt% then, the chain-transferring agent of 0.1wt%～0.5wt% and the adulterant of 5wt%～30wt%, perhaps have two keys and differ bigger monomer with high purity methacrylic acid methyl esters refractive index, when pre-polymerization when conversion ratio is 8%～20%, reduce temperature of charge to room temperature, stop to stir, join in polymethyl methacrylate (PMMA) pipe of front polymerization, under 35 ℃～60 ℃ temperature, with 500rpm～3000rpm rotating speed centrifugal polymerization to conversion ratio is 60%～80%, the PMMA layer that makes it form the tool certain thickness once more and added adulterant on the inwall of the established PMMA layer of first step;
The 3rd step: the process that repeated for second step, on the PMMA layer inwall of preparation, form the polymer that one deck is made of initator, chain-transferring agent and adulterant again, so continuous repetition, make polymeric layer more and more thicker, and one layer of polymeric contained adulterant in back is more than preceding one deck, the final solid gradient polymer optical fiber premade rod that does not have hole that forms.
By method of the present invention, can be relatively easy to prepare and have large-size, flawless polymer optical fiber prefabricated stick; And can control accurately along prefabricated rods refractive index distribution curve radially in the gained prefabricated rods, thereby must have bandwidth performance preferably by the polymer optical fiber that this prefabricated rods draws out.
Description of drawings
Fig. 1 prepares the principle schematic of gradient polymer optical fiber premade rod for existing with interface-gel copolymerization method.
Fig. 2 is the principle schematic of preparation gradient polymer optical fiber premade rod of the present invention.
Fig. 3 is the distribution curve with refractive index in the prepared prefabricated rods of embodiment one.
Fig. 4 is the distribution curve with refractive index in the prepared prefabricated rods of embodiment two.
Fig. 5 is the distribution curve with refractive index in the prepared prefabricated rods of embodiment three.
The present invention is described in further detail below in conjunction with embodiment that accompanying drawing and inventor provide.
The specific embodiment
Gradient polymer optical fiber premade rod according to method preparation of the present invention comprises the following steps:
The initator that at first in a certain amount of monomer high purity methacrylic acid methyl esters MMA, adds 0.1wt%～1wt%, the chain-transferring agent of 0.1wt%～0.5wt%, at 70 ℃～95 ℃ following pre-polymerization to conversion ratios is 8%～20%, reduce temperature of charge to room temperature, join in the stainless steel or glass tube of one one end sealing, make this container under 35 ℃～60 ℃ temperature with the 500rpm～centrifugal rotation of 3000rpm rotating speed 12h～36h, make MMA be close to container inner wall and be polymerized to conversion ratio 60%～80% and form the have certain thickness PMMA layer of (occurrence of thickness is by the amount decision of the MMA that is added);
In the high-purity MMA of other a certain amount of monomer, add the initator of 0.1wt%～1wt%, the chain-transferring agent of 0.1wt%～0.5wt%, the adulterant (perhaps have two keys and differ bigger monomer) of 5wt%～30wt% then with the MMA refractive index, 500rpm under 35 ℃～60 ℃ temperature～3000rpm rotating speed centrifugal polymerization to conversion ratio is 60%～80%, makes it form the certain thickness PMMA layer that has added adulterant of tool again at established PMMA layer inwall;
The 3rd step, repeat the process in second step, form one layer of polymeric again in preceding one deck PMMA layer inside, so continuous repetition, polymeric layer more and more thicker (and one layer of polymeric contained adulterant in back is more than preceding one deck), the final solid gradient polymer optical fiber premade rod that does not have hole that forms.Whole process as shown in Figure 2.
Below be the embodiment that the inventor provides, need to prove, the invention is not restricted to these embodiment.
Embodiment 1:
At first in the high-purity MMA monomer of 600g, add the high-purity azodiisobutyronitrile of 1.8g (AIBN), 2ml lauryl mercaptan, stirring, pre-polymerization to conversion ratio are 15% down at 85 ℃, lower the temperature, stop to stir, join inwall through in stainless steel tube polishing, end sealing, this pipe diameter is 32mm, and length is 1000mm., seal with the oxygen in the eliminating system at the Guan Zhongtong high pure nitrogen.Stainless steel tube is fixed on centrifugal device, open centrifugally, rotating speed is 1000rpm, and design temperature is 45 ℃, centrifugal rotation 6h, and making the MMA that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer about 6mm.
Second step, in the high-purity MMA monomer of 300g, add the high-purity azodiisobutyronitrile of 1.2g (AIBN), 1ml lauryl mercaptan, 14ml bromobenzene, stirring, pre-polymerization to conversion ratio are 15% under 85 ℃, lower the temperature, stop to stir, and join in the PMMA pipe of front polymerization, it is fixed on centrifugal device, open centrifugally, rotating speed is 1500rpm, and design temperature is 45 ℃, centrifugal rotation 12h, making the material that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer about 4mm.
The 3rd step, in the high-purity MMA monomer of 150g, add the high-purity azodiisobutyronitrile of 0.75g (AIBN), 0.5ml lauryl mercaptan, 15ml bromobenzene, stirring, pre-polymerization to conversion ratio are 15% down at 85 ℃, lower the temperature, stop to stir, join in the PMMA pipe of front polymerization, it is fixed on centrifugal device, open centrifugal, rotating speed is 2000rpm, design temperature is 45 ℃, centrifugal rotation 24h, making the material that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer (residue aperture 1mm) about 5.5mm.Constantly add the mixture of MMA, AIBN, lauryl mercaptan etc. then in this hole, 45 ℃ of following polymerizations, and be warmed up to 115 ℃ gradually, final cooling, the demoulding, to obtain length be 1m, and diameter is the polymer optical fiber prefabricated stick of 32mm.
Embodiment 2:
At first in the high-purity MMA monomer of 600g, add the high-purity azodiisobutyronitrile of 2.4g (AIBN), 2ml lauryl mercaptan, stirring, pre-polymerization to conversion ratio are 15% down at 85 ℃, lower the temperature, stop to stir, join inwall through in stainless steel tube polishing, end sealing, this pipe diameter is 32mm, and length is 1000mm., seal with the oxygen in the eliminating system at the Guan Zhongtong high pure nitrogen.Stainless steel tube is fixed on centrifugal device, open centrifugally, rotating speed is 1000rpm, and design temperature is 50 ℃, centrifugal rotation 3h, and making the MMA that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer about 6mm.
Second step, in the high-purity MMA monomer of 300g, add the high-purity azodiisobutyronitrile of 1.5g (AIBN), 1ml lauryl mercaptan, 14ml bromobenzene, stirring, pre-polymerization to conversion ratio are 15% under 85 ℃, lower the temperature, stop to stir, and join in the PMMA pipe of front polymerization, it is fixed on centrifugal device, open centrifugally, rotating speed is 1500rpm, and design temperature is 50 ℃, centrifugal rotation 8h, making the material that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer about 4mm.
The 3rd step added the high-purity azodiisobutyronitrile of 1.05g (AIBN), 0.5ml lauryl mercaptan, 15ml bromobenzene in the high-purity MMA monomer of 150g, stirring, pre-polymerization to conversion ratio are 15% down at 85 ℃, lower the temperature, stop to stir, join in the PMMA pipe of front polymerization, it is fixed on centrifugal device, open centrifugal, rotating speed is 2000rpm, design temperature is 50 ℃, centrifugal rotation 18h, making the material that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer (residue aperture 1mm) about 5.5mm.Constantly add the mixture of MMA, AIBN, lauryl mercaptan etc. then in this hole, 50 ℃ of following polymerizations, and be warmed up to 115 ℃ gradually, final cooling, the demoulding, to obtain length be 1m, and diameter is the polymer optical fiber prefabricated stick of 32mm.
Embodiment 3:
At first in the high-purity MMA monomer of 600g, add the high-purity azodiisobutyronitrile of 1.8g (AIBN), 2ml lauryl mercaptan, stirring, pre-polymerization to conversion ratio are 15% down at 85 ℃, lower the temperature, stop to stir, join inwall through in stainless steel tube polishing, end sealing, this pipe diameter is 32mm, and length is 1000mm., seal with the oxygen in the eliminating system at the Guan Zhongtong high pure nitrogen.Stainless steel tube is fixed on centrifugal device, open centrifugally, rotating speed is 1000rpm, and design temperature is 45 ℃, centrifugal rotation 6h, and making the MMA that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer about 6mm.
Second step, in the high-purity MMA monomer of 300g, add the high-purity azodiisobutyronitrile of 1.2g (AIBN), 1ml lauryl mercaptan, 21ml bromobenzene, stirring, pre-polymerization to conversion ratio are 15% under 85 ℃, lower the temperature, stop to stir, and join in the PMMA pipe of front polymerization, it is fixed on centrifugal device, open centrifugally, rotating speed is 1500rpm, and design temperature is 45 ℃, centrifugal rotation 12h, making the material that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer about 4mm.
The 3rd step added the high-purity azodiisobutyronitrile of 0.75g (AIBN), 0.5ml lauryl mercaptan, 22.5ml bromobenzene in the high-purity MMA monomer of 150g, stirring, pre-polymerization to conversion ratio are 15% down at 85 ℃, lower the temperature, stop to stir, join in the PMMA pipe of front polymerization, it is fixed on centrifugal device, open centrifugal, rotating speed is 2000rpm, design temperature is 45 ℃, centrifugal rotation 24h, making the material that is added be close to the stainless steel inside pipe wall polymerization, to form thickness be PMMA layer (residue aperture 1mm) about 5.5mm.Constantly add the mixture of MMA, AIBN, lauryl mercaptan etc. then in this hole, 45 ℃ of following polymerizations, and be warmed up to 115 ℃ gradually, final cooling, the demoulding, to obtain length be 1m, and diameter is the polymer optical fiber prefabricated stick of 32mm.
The foregoing description can also be enumerated many, and as space is limited, the applicant does not enumerate one by one, can select a kind of in following as initator:
Azodiisobutyronitrile, di-isopropyl peroxydicarbonate, dibenzoyl peroxide etc.;
Chain-transferring agent is selected n-butyl mercaptan, lauryl mercaptan or other thio-alcohol materials;
Adulterant is selected one of them in bromobenzene, biphenyl, Ergol, diphenyl phthalate, diphenyl sulfide, the triphenyl phosphate;
Have two keys and select benzyl methacrylate, phenyl methacrylate, methyl methacrylate cyclohexyl, cyclohexyl methacrylate, methacrylic acid benzyl chloride ester, methacrylic acid phenethyl ester, 1 with the monomer that high purity methacrylic acid methyl esters refractive index differs bigger, 2-diphenyl-ethyl methacrylate, methacrylic acid diphenyl methyl esters, trifluoroethyl methacrylate, methacrylic acid five fluorine propyl ester, methacrylic acid hexafluoro isopropyl ester, methacrylic acid seven fluorine butyl esters one of them.
With the initator of above-mentioned selection, chain-transferring agent, adulterant or or have two keys and with high purity methacrylic acid methyl esters refractive index differ bigger monomer, be prepared according to the solution of the present invention, all can realize preparing gradient polymer optical fiber premade rod.
Claims (2)
1. the preparation method of a gradient polymer optical fiber premade rod is characterized in that, comprises the following steps:
The first step: at first in a certain amount of monomer high purity methacrylic acid methyl esters, add the initator of 0.1wt%～1wt% and the chain-transferring agent of 0.1wt%～0.5wt%, under 70 ℃～95 ℃ temperature, when pre-polymerization when conversion ratio is 8%～20%, reduce temperature of charge to room temperature, join then in the rustless steel container or glass tube of one one end sealing, and should become rusty steel container or glass tube under 35 ℃～60 ℃ temperature, with the 500rpm～centrifugal rotation of 3000rpm rotating speed 12h～36h, make methyl methacrylate be close to container inner wall and be polymerized to conversion ratio 60%～80% and form and to have certain thickness polymethyl methacrylate layers;
Second step: the initator that in other a certain amount of monomer high purity methacrylic acid methyl esters, adds 0.1wt%～1wt% then, the chain-transferring agent of 0.1wt%～0.5wt% and the adulterant of 5wt%～30wt%, when pre-polymerization when conversion ratio is 8%～20%, reduce temperature of charge to room temperature, stop to stir, join in the polymethyl methacrylate pipe of first step polymerization, under 35 ℃～60 ℃ temperature, with 500rpm～3000rpm rotating speed centrifugal polymerization to conversion ratio is 60%～80%, makes its inwall in the established polymethyl methacrylate layers of the first step form the certain thickness polymethyl methacrylate layers of adding adulterant of tool again;
The 3rd step: the process that repeated for second step, on the polymethyl methacrylate layers inwall of preparation, form the polymer that one deck is made of initator, chain-transferring agent and adulterant again, so continuous repetition, make polymeric layer more and more thicker, and one layer of polymeric contained adulterant in back is more than preceding one deck, the final solid gradient polymer optical fiber premade rod that does not have hole that forms.
2. the method for claim 1 is characterized in that, described initator is wherein a kind of of azodiisobutyronitrile, di-isopropyl peroxydicarbonate, dibenzoyl peroxide;
Described chain-transferring agent is n-butyl mercaptan or lauryl mercaptan or other thio-alcohol material;
Described adulterant be bromobenzene, biphenyl, Ergol, diphenyl phthalate, diphenyl sulfide, triphenyl phosphate one of them;
Described adulterant or to have two keys and to substitute with monomer that high purity methacrylic acid methyl esters refractive index differs bigger, describedly have two keys and comprise benzyl methacrylate with monomer that high purity methacrylic acid methyl esters refractive index differs bigger, phenyl methacrylate, the methyl methacrylate cyclohexyl, cyclohexyl methacrylate, methacrylic acid benzyl chloride ester, the methacrylic acid phenethyl ester, 1,2-diphenyl-ethyl methacrylate, methacrylic acid diphenyl methyl esters, trifluoroethyl methacrylate, methacrylic acid five fluorine propyl ester, methacrylic acid hexafluoro isopropyl ester, methacrylic acid seven fluorine butyl esters one of them.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60119510A (en) * | 1983-12-02 | 1985-06-27 | Sumitomo Electric Ind Ltd | Manufacture of preform for plastic optical fiber |
| CN1267643A (en) * | 1999-03-22 | 2000-09-27 | 中国科学院感光化学研究所 | Preparation of prefabricated graded plastic fiber bar with radial graded index |
| US6136234A (en) * | 1998-11-30 | 2000-10-24 | National Science Council | Process for fabricating a gradient refractive-index plastic rod using centrifugal diffusing polymerization method |
| WO2003098289A1 (en) * | 2002-05-22 | 2003-11-27 | Sscp Co., Ltd. | Method for preparing plastic optical fiber preform |
| CN1594377A (en) * | 2004-06-24 | 2005-03-16 | 西安交通大学 | Process for rapid polymerization preparation of polymethyl methacrylate used for polymer fiber |
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2005
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60119510A (en) * | 1983-12-02 | 1985-06-27 | Sumitomo Electric Ind Ltd | Manufacture of preform for plastic optical fiber |
| US6136234A (en) * | 1998-11-30 | 2000-10-24 | National Science Council | Process for fabricating a gradient refractive-index plastic rod using centrifugal diffusing polymerization method |
| CN1267643A (en) * | 1999-03-22 | 2000-09-27 | 中国科学院感光化学研究所 | Preparation of prefabricated graded plastic fiber bar with radial graded index |
| WO2003098289A1 (en) * | 2002-05-22 | 2003-11-27 | Sscp Co., Ltd. | Method for preparing plastic optical fiber preform |
| CN1594377A (en) * | 2004-06-24 | 2005-03-16 | 西安交通大学 | Process for rapid polymerization preparation of polymethyl methacrylate used for polymer fiber |
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