CN111497398A - Extrusion type flexible end point light-emitting optical fiber and preparation method thereof - Google Patents
Extrusion type flexible end point light-emitting optical fiber and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
- B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
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- B32B1/00—Layered products having a general shape other than plane
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular 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
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/18—Homopolymers or copolymers or tetrafluoroethene
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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
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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
- G02B6/036—Optical fibres with cladding with or without a coating core or cladding comprising multiple layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2011/00—Optical elements, e.g. lenses, prisms
- B29L2011/0075—Light guides, optical cables
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/418—Refractive
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/558—Impact strength, toughness
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention discloses an extrusion type flexible end point luminous fiber and a preparation method thereof, the extrusion type flexible end point luminous fiber consists of a core layer, a skin layer and an outer skin layer, wherein the base material of the core layer is optical acrylic, an acrylic monomer is added as a toughening material, so that the acrylic is changed from hard to soft into modified acrylic, the skin layer is fluoroplastic, and a light stabilizer, a light diffusant and a photoresist are synthesized, the core layer and the skin layer are jointed and formed through an asynchronous co-extrusion process, and then the outer surface of the skin layer material is wrapped by the core layer, and the outer skin layer is made of thermoplastic resin, so that infinite length automatic extrusion production can be realized. The prepared extrusion type flexible end point luminous optical fiber is good in flexibility and toughness, can be bent and molded at will, and is not easy to break due to the fact that the diameter of the extrusion type flexible end point luminous optical fiber does not influence the toughness. Meanwhile, the heat resistance is strong, and the heat-resistant material is also suitable for high-temperature and low-temperature working environments; the optical refractive index is high, the LED is particularly suitable for the field of illumination and luminescence, yellowing is avoided, and the performance is stable.
Description
Technical Field
The invention relates to the technical field of optical fibers, in particular to an extrusion type flexible end point light-emitting optical fiber and a preparation method thereof.
Background
The end point light-emitting optical fiber is an optical fiber with one end connected to any light end, the other end point emitting light and the middle not emitting light. The existing endpoint light-emitting optical fiber mainly uses acrylic as a base material, but the acrylic material is hard, so that the optical fiber cannot be bent, the product is easy to crack, and the optical fiber is easy to break when the diameter is larger.
The existing endpoint light-emitting optical fiber is generally a perfusion type optical fiber and has low yield.
However, the existing filling type optical fiber has the following defects:
(1) the structure is a layered structure, so that the use process is easy to layer, and the performance and the service life are influenced;
(2) poor environmental tolerance, easy yellowing and no temperature resistance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an extruded flexible end point light-emitting optical fiber and a preparation method thereof. Meanwhile, the heat resistance is strong, and the heat-resistant material is also suitable for high-temperature and low-temperature working environments; the optical refractive index is high, the LED is particularly suitable for the field of illumination and luminescence, yellowing is avoided, and the performance is stable.
The purpose of the invention is realized by adopting the following technical scheme:
an extrusion type flexible end point light-emitting optical fiber comprises an outer skin layer, a core layer and a skin layer which are integrally formed; the skin layer wraps the core layer, and the outer skin layer wraps the skin layer; the skin layer is prepared from fluororesin, a light stabilizer, a light diffusant and photoresist; the core layer is prepared from acrylic and acrylic monomers; the material of the outer skin layer is thermoplastic resin.
The acrylic and acrylic monomers are fully sheared and mixed at a low temperature to a high temperature in the mixing screw rod, so that after the acrylic and acrylic monomers are effectively polymerized, the hardness of the acrylic can be effectively reduced, and the acrylic and acrylic monomers are softened, namely, the core layer is a flexible core layer.
The light stabilizer is used for shielding or absorbing the energy of ultraviolet rays, so that the possibility of photochemical reaction can be eliminated or slowed down and the photoaging process can be prevented or delayed under the irradiation of light to achieve the purpose of prolonging the service life of the high molecular polymer product. The light diffusant can increase light scattering and transmission, shield a luminous source and a glaring light source, and enable the whole endpoint luminous fiber to transmit softer and more beautiful light, thereby achieving the comfortable effect of light transmission and opaqueness. The photoresist, also called as photoresist and photoresist (photoresist), is a corrosion-resistant film material with the solubility changed by the illumination or radiation of ultraviolet light, deep ultraviolet light, electron beam, ion beam, X-ray, etc., is a key material in the photoetching process, and realizes the visual effect that when a light source irradiates from one end and enters into an end point light-emitting optical fiber, the middle part is not bright, and the other end is bright.
Further, the thermoplastic resin is polyvinyl chloride and/or polyethylene.
And the core layer further comprises ethyl acetate and butyl acetate, the transparency of the core layer can be changed after the ethyl acetate and the butyl acetate are added, and the weight ratio of the ethyl acetate to the butyl acetate to the extruded flexible end point light-emitting fiber is 2-4 wt%.
Furthermore, the fluororesin is fluorinated ethylene propylene, and the weight ratio of the fluororesin to the extruded flexible end-point light-emitting optical fiber is 9-15 wt%.
Furthermore, the weight ratio of the acrylic to the extruded flexible body endpoint light-emitting optical fiber is 60-80 wt%, and the mass ratio of the acrylic to the acrylic monomer is 100: 5 to 7.
Further, the light stabilizer is polyvinylidene fluoride and tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, and the mixing ratio of the polyvinylidene fluoride to the tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer is 1: 2; the light stabilizer accounts for 2-4 wt% of the extruded flexible body endpoint light-emitting fiber.
Further, the light diffusing agent is barium sulfate, calcium carbonate and organic silicon modified acrylic resin, and the mixing ratio of the barium sulfate, the calcium carbonate and the organic silicon modified acrylic resin is 1.5-2: 2-2.5: 1.3 to 3.3; the light diffusant accounts for 1-2 wt% of the extruded flexible end point light-emitting optical fiber.
Further, the photoresist is phenol resin, diazonaphthoquinone, organic silicon resin and acrylic, and the mixing ratio of the phenol resin, the diazonaphthoquinone, the organic silicon resin and the acrylic is 3-5: 1: 4: 90-92; the photoresist accounts for 1-2 wt% of the extruded flexible end point light-emitting fiber.
The preparation method of the extruded flexible end point light-emitting optical fiber comprises the following steps:
1) fusing acrylic monomers and acrylic monomers at high temperature in a multi-screw exhaust type extruder to obtain a modified acrylic core layer material; the acrylic and acrylic monomers are fully fused in a multi-section mixing screw and an exhaust type charging barrel in a multi-screw exhaust type extruder, so that the hardness of the acrylic is reduced.
2) Polymerizing fluororesin, a light stabilizer, a light diffusant and photoresist at high temperature, then conveying the polymer into another extruder, and then conveying the polymer into a flow dividing die head in the multi-screw exhaust type extruder in the step 1) to be synchronously attached and molded with the core layer material of the modified acrylic obtained in the step 1) to obtain a material with a skin layer wrapping the core layer;
3) wrapping the outer skin layer on the outer surface of the material of the skin layer wrapping core layer obtained in the step 2) to obtain the extrusion type flexible body endpoint light-emitting optical fiber. In particular, the outer skin layer may be separately processed into various colors and sizes, and the processed size may range from 1.0mm to 20 mm.
Further, in the step 1), the polymerization temperature is 200-400 ℃, preferably 300 ℃, and the fusion time is 2-5 min, preferably 3 min; in the step 2), the polymerization temperature is 400-500 ℃, preferably 420 ℃, and the fusion time is 1-3 min.
Compared with the prior art, the invention has the beneficial effects that:
the extrusion type flexible end point luminous optical fiber consists of a core layer, a skin layer and an outer skin layer, wherein the base material of the core layer is optical acrylic, and then an acrylic monomer is added to serve as a toughening material, so that the acrylic is changed from hard to soft into modified acrylic, the skin layer is formed by compounding fluoroplastic with a light stabilizer, a light diffusant and photoresist, the core layer and the skin layer are attached and formed through an asynchronous co-extrusion process, then the outer skin layer is made of thermoplastic resin on the outer surface of the skin layer wrapped by the core layer, and automatic extrusion production with infinite length can be realized. The prepared extrusion type flexible end point luminous optical fiber is good in flexibility and toughness, can be bent and molded at will, and is not easy to break due to the fact that the diameter of the extrusion type flexible end point luminous optical fiber does not influence the toughness. Meanwhile, the heat resistance is strong, and the heat-resistant material is also suitable for high-temperature and low-temperature working environments; the optical refractive index is high, the LED is particularly suitable for the field of illumination and luminescence, yellowing is avoided, and the performance is stable.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
Example 1
The preparation method of the extruded flexible end point light-emitting optical fiber comprises the following steps:
1) feeding 100g of acrylic, 9g of acrylic monomer, 6.5g of butyl acetate and 6.4g of ethyl acetate into a multi-screw exhaust type extruder together, and fully fusing the acrylic monomer and the ethyl acetate for 3min at 300 ℃ in a multi-section mixing screw and an exhaust type charging barrel in the multi-screw exhaust type extruder to obtain a modified acrylic core layer material;
2) polymerizing 24.4g of fluororesin, 9.8g of light stabilizer, 3.2g of light diffusant and 3.2g of photoresist for 3min at 420 ℃, then conveying the polymer into another extruder, and then conveying the polymer into a flow distribution die head in the multi-screw exhaust type extruder in the step 1) to synchronously attach and mold the polymer with the modified acrylic core layer material obtained in the step 1), so as to obtain a material with a skin layer wrapping the core layer;
3) wrapping the outer skin layer on the outer surface of the material of the skin layer wrapping core layer obtained in the step 2) to obtain the extrusion type flexible body endpoint light-emitting optical fiber.
Specifically, the light stabilizer is polyvinylidene fluoride and tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, and the mixing ratio of the polyvinylidene fluoride to the tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer is 1: 2; the light diffusant is barium sulfate, calcium carbonate and organic silicon modified acrylic resin, and the mixing ratio of the barium sulfate, the calcium carbonate and the organic silicon modified acrylic resin is 2: 2.5: 3.3; the photoresist is phenolic resin, diazonaphthoquinone, organic silicon resin and acrylic, and the mixing ratio of the phenolic resin, the diazonaphthoquinone, the organic silicon resin and the acrylic is 5: 1: 4: 90, respectively;
the diameter of the extruded flexible end point light-emitting fiber obtained in example 1 was 5 mm.
Example 2
The preparation method of the extruded flexible end point light-emitting optical fiber comprises the following steps:
1) feeding 100g of acrylic, 3.7g of acrylic monomer, 2.5g of butyl acetate and 2.5g of ethyl acetate into a multi-screw exhaust type extruder together, and fully fusing the acrylic monomer, the butyl acetate and the ethyl acetate for 3min at 300 ℃ in a multi-section mixing screw and an exhaust type charging barrel in the multi-screw exhaust type extruder to obtain a modified acrylic core layer material;
2) polymerizing 11.25g of fluororesin, 2.5g of light stabilizer, 1.2g of light diffusant and 1.3g of photoresist at 360 ℃ for 3min, then conveying the polymer into another extruder, and then conveying the polymer into a flow distribution die head in the multi-screw exhaust type extruder in the step 1) to synchronously attach and mold the polymer with the modified acrylic core layer material obtained in the step 1), so as to obtain a material with a skin layer wrapping the core layer;
3) wrapping the outer skin layer on the outer surface of the material of the skin layer wrapping core layer obtained in the step 2) to obtain the extrusion type flexible body endpoint light-emitting optical fiber.
Specifically, the light stabilizer is polyvinylidene fluoride and tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, and the mixing ratio of the polyvinylidene fluoride to the tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer is 1: 2; the light diffusant is barium sulfate, calcium carbonate and organic silicon modified acrylic resin, and the mixing ratio of the barium sulfate, the calcium carbonate and the organic silicon modified acrylic resin is 1.5: 2: 1.3; the photoresist is phenolic resin, diazonaphthoquinone, organic silicon resin and acrylic, and the mixing ratio of the phenolic resin, the diazonaphthoquinone, the organic silicon resin and the acrylic is 3: 1: 4: 92;
the diameter of the extruded flexible end point light-emitting fiber obtained in example 2 was 2 mm.
Comparative example 1
Comparative example 1, which omits step 1), the other steps are the same as in example 1. The finished product obtained in comparative example 1 was 5mm in diameter.
Effect evaluation and Performance detection
Experiment 1 the high temperature resistance, low temperature resistance, rocking frequency, optical refractive index and yellowing tests were performed on the finished products of examples 1-2 and comparative example 1 to obtain data as shown in table 1.
TABLE 1 test data for high temperature resistance, low temperature resistance, rocking frequency, optical refractive index and yellowing of the finished products of examples 1-2 and comparative example 1
| High temperature resistance | Low temperature resistance | Number of swings | Optical refractive index | Yellow stain | |
| Example 1 | 120℃ | -30℃ | 100 | 97.5％ | More than 48 months |
| Example 2 | 100℃ | 20℃ | 80 | 96.8％ | Over 36 months |
| Comparative example 1 | 80℃ | 10℃ | 30 | 95％ | 28 months old |
As can be seen from the data in Table 1, the high temperature resistance and the low temperature resistance of examples 1-2 are better than those of comparative example 1, which shows that examples 1-2 have strong temperature resistance and are also suitable for high temperature and low temperature working environments. The working temperature of the sample 1 is-30 ℃. Compared with the comparative example 1, the core layer, the skin layer and the outer skin layer are not easy to separate, the swing service life is long, and the swing times of the example 1 are 3.3 times that of the comparative example 1; meanwhile, the optical refractive indexes of the embodiment 1-2 are higher than those of the comparative example, and reach more than 96 percent, so that the light-emitting diode is particularly suitable for the field of illumination and luminescence. The yellowing time of the examples 1-2 at normal temperature is far longer than that of the comparative example, which shows that the examples 1-2 are not easy to yellow and have stable performance.
Experiment 2 the finished products of examples 1-2 and comparative example 1 were subjected to a flexibility experiment
TABLE 2 flexibility data for the finished products of examples 1-2 and comparative example 1
As is clear from the above table, the tensile strength, elongation at break, flexural strength, impact strength and hardness of examples 1-2 are all superior to those of comparative example 1, and in examples 1-2, the diameter 5mm of example 1 is larger than 2mm of example 2, indicating that the larger the diameter, the better the flexibility.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. An extrusion type flexible end point light-emitting optical fiber is characterized by comprising an outer skin layer, and a core layer and a skin layer which are integrally formed; the skin layer wraps the core layer, and the outer skin layer wraps the skin layer; the skin layer is prepared from fluororesin, a light stabilizer, a light diffusant and photoresist; the core layer is prepared from acrylic and acrylic monomers; the material of the outer skin layer is thermoplastic resin.
2. The extruded flexible end-point emitting fiber of claim 1, wherein the thermoplastic resin is polyvinyl chloride and/or polyethylene.
3. The extruded flexible end point light-emitting fiber of claim 1, wherein the core layer further comprises ethyl acetate and butyl acetate, and the weight ratio of the ethyl acetate to the butyl acetate is 2-4 wt% of the extruded flexible end point light-emitting fiber.
4. The extruded flexible end-point light-emitting fiber of claim 1, wherein the fluororesin is fluorinated ethylene propylene, and the weight ratio of the fluororesin to the extruded flexible end-point light-emitting fiber is 9 to 15 wt%.
5. The extruded flexible endpoint light-emitting fiber of claim 1, wherein the weight ratio of the acrylic to the extruded flexible endpoint light-emitting fiber is 60-80 wt%, and the mass ratio of the acrylic to the acrylic monomer is 100: 5 to 7.
6. The extruded flexible end-point light emitting fiber of claim 1, wherein the light stabilizer is polyvinylidene fluoride and tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, and the mixing ratio of the polyvinylidene fluoride to the tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer is 1: 2; the light stabilizer accounts for 2-4 wt% of the extruded flexible body endpoint light-emitting fiber.
7. The extruded flexible endpoint light-emitting fiber of claim 1, wherein the light diffuser is barium sulfate, calcium carbonate and silicone modified acrylic resin, and the mixing ratio of the barium sulfate, the calcium carbonate and the silicone modified acrylic resin is 1.5-2: 2-2.5: 1.3 to 3.3; the light diffusant accounts for 1-2 wt% of the extruded flexible end point light-emitting optical fiber.
8. The extruded flexible endpoint light-emitting fiber of claim 1, wherein the photoresist is phenolic resin, diazonaphthoquinone, silicone resin and acrylic, and the mixing ratio of phenolic resin, diazonaphthoquinone, silicone resin and acrylic is 3-5: 1: 4: 90-92; the photoresist accounts for 1-2 wt% of the extruded flexible end point light-emitting fiber.
9. The method of making an extruded flexible end-point light emitting fiber of any of claims 1-8, comprising the steps of:
1) fusing acrylic monomers and acrylic monomers at high temperature in a multi-screw exhaust type extruder to obtain a modified acrylic core layer material;
2) polymerizing fluororesin, a light stabilizer, a light diffusant and photoresist at high temperature, then conveying the polymer into another extruder, and then conveying the polymer into a flow dividing die head in the multi-screw exhaust type extruder in the step 1) to be synchronously attached and molded with the core layer material of the modified acrylic obtained in the step 1) to obtain a material with a skin layer wrapping the core layer;
3) wrapping the outer skin layer on the outer surface of the material of the skin layer wrapping core layer obtained in the step 2) to obtain the extrusion type flexible body endpoint light-emitting optical fiber.
10. The method for preparing the extruded flexible end point light-emitting fiber according to claim 9, wherein in the step 1), the polymerization temperature is 200-400 ℃, and the fusion time is 2-5 min; in the step 2), the polymerization temperature is 400-500 ℃, and the fusion time is 1-3 min.
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