CN1221374C - Continuous reaction and coextrusion process of preparing stepped plastic fiber - Google Patents
Continuous reaction and coextrusion process of preparing stepped plastic fiber Download PDFInfo
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- CN1221374C CN1221374C CN 03135641 CN03135641A CN1221374C CN 1221374 C CN1221374 C CN 1221374C CN 03135641 CN03135641 CN 03135641 CN 03135641 A CN03135641 A CN 03135641A CN 1221374 C CN1221374 C CN 1221374C
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Abstract
The present invention relates to a continuous reaction and coextrusion process of preparing a stepped plastic fiber, which comprises that: (1) polymerization monomer is purified, polymerization solution is prepared, and prepolymerization is carried out by heating or microwaves; then, prepolymer is pumped into a continuous reaction extrusion machine for carrying out reactive extrusion, non-reacted monomer and oligomer are discharged and recovered, and finally, transparent polymer molten masses or particulate matters by cooling and cutting are formed; (2) a transparent polymer core material is prepared by adopting the step (1) by using the continuous reaction extrusion machine, and a transparent leather material is extruded by another extrusion machine, or a transparent leather material is prepared by adopting the step (1) by using the continuous reaction extrusion machine; a transparent polymer core material is extruded by using another extrusion machine, or the transparent polymer core material and the leather material are respectively prepared by adopting the step (1) by using two continuous reaction extrusion machines. Melt combination, traction, stretch and cooling are carried out through a common extrusion mould to form a stepped plastic fiber.
Description
Technical field:
The invention belongs to optical information transferring material field, relevant with the production method that is equipped with phase step type plastics optical fibre by the continuous reaction coextrusion legal system.
Background technology:
Phase step type plastics optical fibre is that the high transparent polymer with high index of refraction is a core, is the novel biography light medium of covering with low-refraction, high transparent fluororesin.Have characteristics such as low-loss, good pliability and long service life because of it, be regarded as substituting the ideal material of existing decoration, lighting means, have remarkable advantages such as environmental protection, energy-conservation, safety, artistic effect be good; Can be used as short distance optical information transmission medium simultaneously, be used for fields such as LAN, Access Network, sensor, consumer electronics industry.
The preparation method of phase step type plastics optical fibre mainly contains:
(1) solution cladding process: the high transparent polymer of extruding high index of refraction by extruder is a core, and core makes its surface be stained with one deck solution by the solution of a low-refraction then, and heating makes its curing, cooling, forms phase step type plastics optical fibre.
(2) coextruding method: extrude the high transparent polymer core of high index of refraction and the covering polymer of low-refraction simultaneously by two extruders, through co-extrusion die head, traction, stretching, cooling form phase step type plastics optical fibre.
But said method production efficiency is low, can not produce the low-loss plastic optical fiber with special purpose.
Summary of the invention:
The objective of the invention is to produce the production method of utilizing continuous reaction coextrusion manufactured phase step type plastics optical fibre of low-loss plastic optical fiber for a kind of production efficiency height is provided.Another object of the present invention is the phase step type plastics optical fibre that adopts this method to produce in order to provide.
The object of the present invention is achieved like this:
The method that continuous reaction coextrusion legal system of the present invention is equipped with phase step type plastics optical fibre comprises the steps.
(1) polymerization single polymerization monomer is purified, the preparation polymeric solution, heating or microwave carry out prepolymerization, then prepolymer or polymeric solution are pumped into to react in the successive reaction extruder and extrude, discharge and reclaim unreacted monomer and oligomer, form transparent polymer melt or cooling at last and cut into particle;
(2) utilize the successive reaction extruder, adopt step (1) preparation transparent polymer core, utilize another extruder to extrude transparent skin material, it is compound to carry out fusion by co-extruding mould, and traction, stretching, cooling form phase step type plastics optical fibre; Perhaps utilize a successive reaction extruder, adopt the transparent skin material of step (1) preparation, utilize another extruder to extrude the transparent polymer core, it is compound to carry out fusion by co-extruding mould, and traction, stretching, cooling form phase step type plastics optical fibre; Perhaps utilize two successive reaction extruders, adopt step (1) to prepare polymer core and skin material respectively, it is compound to carry out fusion by co-extruding mould, traction, stretching, cooling, form phase step type plastics optical fibre, the core refractive index is higher by 1% than skin material refractive index at least, and polymer of the present invention comprises that monomer whoses such as polyacrylate, polystyrene, Merlon, poly-fluorinated acrylic ester can carry out the various polymer of polymerisation.
Core and skin material refractive index are 1.3~1.6 in the above-mentioned method.
When adopting microwave that polymerization single polymerization monomer is carried out prepolymerization in the above-mentioned method, microwave frequency is 10
8~10
11Hz, microwave power 100~1000W, employing is to the prepolymerization of methylmethacrylate polymer (MMA) microwave, can improve polymerization speed, reduce the pre-polymerization initiator amount, thereby improve polymer purity, light transmission, as adopting thermal polymerization, dibenzoyl peroxide (BPO) initiator content is 0.2%, 50 ℃ of following polymerization methylmethacrylate polymer MMA conversion ratio<10% in the time of 100 minutes; And adopt microwave frequency is that 2450MHz, power are the microwave action of 375W, 50 ℃ of following polymerizations MMA conversion ratio>50% in the time of 20 minutes.
In the above-mentioned method during thermal polymerization initiator content be 0.2~0.4%, initiator content is 0.01~0.1% during the microwave polymerization.
Adopt above-mentioned method to prepare phase step type plastics optical fibre.
Manufacture method of the present invention is utilized successive reaction to extrude coextruding method to prepare phase step type plastics optical fibre, can prepare low-loss plastic optical fiber, simultaneously by adjusting the refractive index of institute's extruded polymer, thereby adjust the numerical aperture of plastic optical fiber, the low-loss plastic optical fiber of preparation special purpose, as the optical illumination plastic optical fiber of high-NA (NA=0.6), and the optic communication high bandwidth plastic optical fiber of low numerical aperture (NA=0.3).This method is serialization production, enhances productivity in addition.
By improving extraneous production environment, improve the transparency of material, can the production loss be 0.1~0.7 low-loss plastic optical fiber near 150dB/km, numerical aperture adjustable extent, realize the industrialization continuous and stable production
Description of drawings:
Fig. 1 phase step type plastics optical fibre production line schematic diagram.
Fig. 2 co-extruding mould schematic diagram.
The specific embodiment:
Fig. 1 is a phase step type plastics optical fibre production line schematic diagram.The core extruder 2 that comprise co-extruding mould 1, communicates, covering extruder 3 with co-extruding mould, laser diameter measuring instrument 4, traction drawing mechanism 5, take-up mechanism 6.
Fig. 2 is the co-extruding mould schematic diagram.Core 7 internal layer runners 8, skin material 9 outer circulation 10 and compound runners 11 are arranged on it.
Embodiment 1:
Methyl methacrylate (MMA) is carried out decompression distillation purifies; add modifier, initator, the chain-transferring agent of purifying then; under the protection of 99.99% high pure nitrogen; at 40~80 ℃ of following prepolymerization 1~24h; make its viscosity suitable, pump in the twin-screw successive reaction extruder of extruding core by measuring pump then.Twin-screw successive reaction extruder temperature is set at 120~200 ℃, reacts under the high pure nitrogen protection and extrudes, and last vacuum is got rid of unreacted monomer, makes residual monomer content less than 1%, extrudes high-purity PMMA polymer core.
To methyl methacrylate (MMA), methacrylic acid-2,3,3; 3-tetrafluoro propyl ester carries out decompression distillation and purifies; MMA, methacrylic acid-2,3 in the solution, 3; the molar concentration of 3-tetrafluoro propyl ester is respectively 21.5%, 78.5%; add initator, the chain-transferring agent of purifying then, under the protection of 99.99% high pure nitrogen, at 40~80 ℃ of following prepolymerization 1~24h; make its viscosity suitable, pump in the twin-screw successive reaction extruder of extruding the skin material by measuring pump then.Twin-screw successive reaction extruder temperature is set at 120~200 ℃; under the high pure nitrogen protection, react and extrude; last vacuum is got rid of unreacted monomer, makes residual monomer content less than 1%, extrudes refractive index and be high-purity fluorinated acrylic ester polymer sheath material of 1.404.
Above-mentioned two twin-screw successive reaction extruders, as shown in Figure 1 with PMMA core and the fluorinated acrylic ester polymer sheath material extruded respectively, extrude by the co-extruding mould as shown in Figure 2 that is attached thereto, traction, stretch, cooling, make numerical aperture and be 0.5 PMMA phase step type plastics optical fibre.
Embodiment 2:
To methyl methacrylate (MMA), methacrylic acid-2; 2, the 2-trifluoro ethyl ester carries out decompression distillation and purifies MMA, methacrylic acid-2 in the solution; 2; 2, the molar concentration of trifluoro ethyl ester is respectively 61.4%, 38.6%, adds initator, the chain-transferring agent of purifying then; under the protection of 99.99% high pure nitrogen; at 40~80 ℃ of following prepolymerization 1~24h, make its viscosity suitable, pump in the twin-screw successive reaction extruder of extruding the skin material by measuring pump then.Twin-screw successive reaction extruder temperature is set at 120~200 ℃; under the high pure nitrogen protection, react and extrude; last vacuum is got rid of unreacted monomer, makes residual monomer content less than 1%, extrudes refractive index and be high-purity fluorinated acrylic ester polymer sheath material of 1.460.
Utilize two twin-screw successive reaction extruders, extrude PMMA core material among the embodiment 1 and the fluorinated acrylic ester polymer sheath material in the present embodiment respectively as Fig. 1, extrude by co-extruding mould as shown in Figure 2, traction, stretch, cooling, make numerical aperture and be the PMMA phase step type plastics optical fibre of 0.3 low numerical aperture.
Can utilize microwave that MMA is carried out prepolymerization in the various embodiments described above.The employing frequency is that 2450MHz, power are the microwave of 375W; Initiator B PO content is 0.02%, and chain-transferring agent (n-butyl mercaptan) content is 0.3%, and temperature was descended 15~20 minutes at 70 ℃, and the MMA conversion ratio is 10~20%.
Claims (4)
1, the continuous reaction coextrusion legal system is equipped with the method for phase step type plastics optical fibre, it is characterized in that comprising the steps:
(1) polymerization single polymerization monomer is purified, the preparation polymeric solution, heating or microwave carry out prepolymerization, then prepolymer are pumped into to react in the successive reaction extruder and extrude, discharge and reclaim unreacted monomer and oligomer, form transparent polymer melt or cooling at last and cut into particle;
(2) utilize the successive reaction extruder, adopt step (1) preparation transparent polymer core, utilize another extruder to extrude transparent skin material, it is compound to carry out fusion by co-extruding mould, and traction, stretching, cooling form phase step type plastics optical fibre; Perhaps utilize a successive reaction extruder, adopt the transparent skin material of step (1) preparation, utilize another extruder to extrude the transparent polymer core, it is compound to carry out fusion by co-extruding mould, and traction, stretching, cooling form phase step type plastics optical fibre; Perhaps utilize two successive reaction extruders, adopt step (1) to prepare transparent polymer core and skin material respectively, it is compound to carry out fusion by co-extruding mould, traction, stretching, cooling, form phase step type plastics optical fibre, above-mentioned core refractive index is higher by 1% than skin material refractive index at least.
2, the described continuous reaction coextrusion legal system of claim 1 is equipped with the method for phase step type plastics optical fibre, it is characterized in that core and skin material refractive index are 1.3~1.6.
3, continuous reaction coextrusion legal system as claimed in claim 1 or 2 is equipped with the method for phase step type plastics optical fibre, and when it is characterized in that adopting the microwave polymerization single polymerization monomer to carry out prepolymerization, microwave frequency is 10
8~10
11Hz, microwave power 100~1000W.
4, continuous reaction coextrusion legal system as claimed in claim 1 or 2 is equipped with the method for phase step type plastics optical fibre, and initiator content is 0.2~0.4% when it is characterized in that thermal polymerization, and initiator content is 0.01~0.1% during the microwave polymerization.
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Cited By (1)
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CN103597239B (en) * | 2011-02-09 | 2016-05-25 | 澳大利亚公司号166970627控股有限公司 | Vibration damping device |
Families Citing this family (7)
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CN101544046B (en) * | 2009-05-12 | 2012-01-11 | 四川汇源塑料光纤有限公司 | Method for preparing sidelight plastic fibers by continuous reaction coextrusion method |
CN102173043A (en) * | 2011-01-21 | 2011-09-07 | 江门市多快好省机械有限公司 | Cast film extruding machine |
CN106182666B (en) * | 2016-09-06 | 2019-05-17 | 深圳市圣诺光电科技有限公司 | Plastic optical fiber and preparation method thereof and preparation facilities |
WO2021001398A1 (en) * | 2019-07-02 | 2021-01-07 | Essilor International | Fdm 3d printing of optical lens with high clarity and mechanical strength |
CN110685027B (en) * | 2019-09-04 | 2020-11-10 | 苏州大学 | Method for preparing polymer optical fiber |
CN110549705B (en) * | 2019-09-04 | 2021-06-01 | 苏州大学 | Polymer optical fiber and luminous fabric |
CN114415299B (en) * | 2022-03-30 | 2022-06-24 | 深圳市埃尔法光电科技有限公司 | Optical fiber signal direct-guiding type optical module |
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Cited By (1)
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CN103597239B (en) * | 2011-02-09 | 2016-05-25 | 澳大利亚公司号166970627控股有限公司 | Vibration damping device |
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