CN101544046A - Method for preparing sidelight plastic fibers by continuous reaction coextrusion method - Google Patents
Method for preparing sidelight plastic fibers by continuous reaction coextrusion method Download PDFInfo
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- CN101544046A CN101544046A CN200910059260A CN200910059260A CN101544046A CN 101544046 A CN101544046 A CN 101544046A CN 200910059260 A CN200910059260 A CN 200910059260A CN 200910059260 A CN200910059260 A CN 200910059260A CN 101544046 A CN101544046 A CN 101544046A
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Abstract
The invention provides a method for preparing sidelight plastic fibers with luminous effect. The method comprises the following steps: fusing and extruding a semitransparent cladding which is prepared from at least two different materials through copolymerization and has shore hardness of less than or equal to 90A and a soft sandwich layer of which the shore hardness is less than or equal to 90A, the refractive index is larger than that of the cladding and the light transmittance is more than or equal to 93 percent into a cladding area and a sandwich layer area in a coextrusion die respectively to form strip extrudates with concentric circular cross sections; and cooling the extrudates to obtain the sidelight plastic fibers with entire-body luminous effect. The method can produce the sidelight plastic fibers with high flexibility, high sidelight evenness and low light loss continuously and stably.
Description
Technical field:
The invention belongs to light transferring material field, relevant with method by preparing sidelight plastic fibers by continuous reaction coextrusion.
Background technology:
Decorative lighting comprises two kinds of end light type and side light types with plastic optical fiber, and end light plastic optical fiber is that optical fiber end is luminous, is applicable to that by a light be the decorative lighting field that elementary cell constitutes various art pattern effects, shown in figure one; The side light type plastic optical fiber is that optical fiber side is luminous, or be called entirely lighting, linear luminous, be applicable to that by linear light be the decorative lighting field that elementary cell constitutes various art pattern effects, be specially adapted to build that profile sketches the contours, advertising signboard, do not have the emergency lighting of electricity, fields such as decorative art of special-effect under water.
The method of producing the sidelight plastic optical fiber of illumination effect at present both at home and abroad has following several:
1, monomer perfusion:
This method is present modal method, it is to adopt fluororesin tube, as perfluoroethylene-propylene (F46, FEP), flexible acrylic ester or methyl acrylic ester resin after perfusion is purified therein, the back polymerization forming of the pressurization of heating, lateral emitting is a semi-crystalline character of utilizing the F46 material, makes light reach the effect of lateral emitting in the inscattering of covering scope.Because F46 materials processing temperature is higher near 300 ℃, differ bigger with acrylate or methyl acrylic ester resinous polymer processing temperature (180～220 ℃), be not suitable for adopting coextruding method production, can only adopt first moulding F46 pipe, pour into the monomer polymerization moulding again, the defective of the product that this method is produced has: 1) after the high out of doors low temperature circulation in sandwich layer covering interface, occur interface debonding easily, form hollow bubble, have a strong impact on result of use; 2) the F46 material is harder, makes the fibre-optical bending difficulty, and design and construction are subjected to certain limitation; 3) method for filling is not suitable for the optical fiber of diameter less than 3mm; 4) method for filling is intermittent fixed length production, random length production continuously.
2) stranded method:
This method is that (0.5～1.0mm) by stranded twisting, makes optical fiber produce crooked scattering, forms lateral emitting with many minor diameter plastic optical fibers.The defective of this method has: it is on the weak side that 1) light-receiving area reduces to cause sidelight brightness; 2) the sidelight uniformity is relatively poor.
3) boundary defect method:
This method is to make sandwich layer covering interface defective occur, and light forms the sidelight effect in the fault location scattering.The defective of this method has: 1) stability of Sheng Chaning is lower, causes sidelight brightness batch difference to occur.
4) special auxiliary agent method:
This method is to add the material that makes light scattering at the interface at fiber core layer or covering or core bag, as glass microballoon, pearl essence, fluorescer etc.The defective of this method has: 1) sidelight poor effect, and do not have matured product at present and come out.
In view of there are various drawbacks in present sidelight plastic optical fiber, the special this method that proposes, but sidelight plastic optical fiber pliability height, sidelight good uniformity, long, the wide continuous and stable production random length of fibre diameter specification limit of biography light length of using this method to produce.
Summary of the invention:
The objective of the invention is method for the sidelight plastic optical fiber that a kind of continuous and stable production high flexibility, high sidelight uniformity, low optical loss are provided.
The present invention is achieved like this:
The method of preparing sidelight plastic fibers by continuous reaction coextrusion of the present invention, this method be translucent covering that at least two kinds of different materials copolymerization are formed and shore hardness≤90A, refractive index with shore hardness≤90A greater than covering and light transmittance 〉=93% flexible core respectively fusion clamp-on the clad region and the sandwich layer district of co-extruding mould, form the strip extrudate in concentric circles cross section, promptly make sidelight plastic optical fiber after the cooling with entirely lighting effect.
Above-mentioned method comprises the steps:
1) preparation covering:
A. prepare burden in proportion:
Covering is made up of at least two kinds of clad materials, and by mass percentage concentration, every kind of clad material comprises following component:
Radical initiator 0～0.4%
Chain-transferring agent 0～0.6%
Covering monomer surplus.
B. prepare covering:
After the above-mentioned various clad materials that are made into are purified respectively respectively under 60～160 ℃ of pre-polymerization temperature respectively pre-polymerization carry out continuous prepolymerization reaction again after being 5～20% to conversion ratio, heating-up temperature is 60～160 ℃ and makes the pre-polymerization conversion ratio and reach 10～50% mixed prepolymer, mixed prepolymer is sent into extruder, its conversion ratio is reached 80～90%, take off single granulation and promptly make required covering;
2) preparation sandwich layer:
A. prepare burden in proportion: by mass percentage concentration, sandwich layer comprises following component:
Sandwich layer monomer 80～100%
Modifier 0～20%
Radical initiator 0～0.4%
Chain-transferring agent 0～0.6%,
B. prepare sandwich layer:
Carry out prepolymerization reaction after said components purified respectively, in heating-up temperature is to make its pre-polymerization conversion ratio reach 10～50% under 60～160 ℃, the prepolymer that pre-polymerization is obtained is sent into and is made its conversion ratio reach 80～90% in the extruder, takes off single fusion and make sandwich layer in extruder.
3), preparation sidelight plastic optical fiber
The sandwich layer that will take off single fusion is expressed into the sandwich layer district in the co-extruding mould, covering is melt extruded clad region in the co-extruding mould through the covering extruder that is connected with co-extruding mould, form the strip extrudate in concentric circles cross section, promptly make sidelight plastic optical fiber after the cooling with entirely lighting effect.
Above-mentioned covering monomer is fluorine-containing class monomer or acrylic monomer, and the sandwich layer monomer is an acrylic monomer.
Radially count in the above-mentioned optical fiber, cladding thickness is 5～100: 1000 with the core layer thickness ratio.
At first, covering selection pliability of the present invention is good, the material of shore hardness＜90A, and cladding index should be less than the sandwich layer refractive index, so that meet the total reflection law.Make optical fiber side luminous, need light when sandwich layer transmits, be refracted in the covering, part light total reflection is got back to sandwich layer, continue transmission forward, another part light scatters covering at the covering place along any direction, enters into optical fiber air in addition, and the effect that shows is exactly the optical fiber side entirely lighting.Therefore covering should have the function of diffuse light, among the present invention is to adopt to produce softness (shore hardness＜90A), translucent (light transmittance is 50～70%), refractive index realizes less than the polymer of sandwich layer refractive index.
Covering can be made up of two kinds of clad materials among the present invention, clad material component A wherein: can adopt fluorine-containing class monomer, as trifluoroethyl methacrylate 3FEM, refractive index polymer n=1.41, shore hardness=80A, light transmittance=91%, prescription also comprises radical initiator, material is azo class such as azodiisobutyronitrile AIBN, or peroxidating class initator such as dibenzoyl peroxide BPO, di-t-butyl peroxide DTBP etc., mass concentration is 0～0.4%, chain-transferring agent, material is the thio-alcohol material, such as n-butyl mercaptan, and n-octyl mercaptan, mass concentrations such as positive lauryl mercaptan are 0～0.6%; Clad material B component: can adopt acrylic monomer such as methyl methacrylate MMA, refractive index polymer is 1.491, shore hardness〉100A, light transmittance=93%, prescription comprises that also radical initiator, material are azo class or peroxidating class initator, mass concentration is 0～0.4%, chain-transferring agent, material are the thio-alcohol material, and mass concentration is 0～0.6%.
Monomer material required among the present invention all need be purified, and method of purification is conventional decompression distillation, filtration etc., to remove impurity, improves purity, and main monomer purity needs〉99.99%.
Secondly, the technology of the present invention's employing is successive reaction polymerisation in bulk coextrusion process.Usually polymerization technique comprises substance law, solwution method, suspension method, the back all need add solvent to take away a large amount of heats that reaction produces for two kinds, therefore the material purity that polymerize is not high, and be intermittence type polymerization, there is some difference for product quality between batch, in order to reduce mass discrepancy, usually producing is large chemical complex, and retort is hundred tons and arrives kiloton, invests huge, cost is higher, and body method of the present invention is same monomer material, can obtain highly purified polymer, but can't take away heat rapidly because of substance law, be difficult to stable control production technology, industrial seldom employing.The present invention adopts successive reaction polymerisation in bulk extrusion molding, can take away the heat that reaction produces at any time, and the control reaction speed is carried out stable reaction, simultaneously owing to carry out polymerization continuously and extrude, and the difference between having reduced batch, and input cost is less.The present invention can adopt outsourcing still formula pre-polymerization device, continuous pre-polymerization device, extruder.Still formula pre-polymerization device is the reactor of band heating jacket and agitator, to component A and B component pre-polymerization simultaneously respectively, 60～160 ℃ of pre-polymerization temperature, pre-polymerization conversion ratio 5～20% is transported to then in the continuous pre-polymerization device and carries out continuous prepolymerization reaction, and the pre-polymerization device can be series connection still formula structure continuously, it also can be the pipeline structure of band heating jacket, its function is that pre-collecting process is carried out continuously, and heating-up temperature can be set at 60～160 ℃, makes the pre-polymerization conversion ratio reach 10～50%.Because component A and B are through having had some polymer poly trifluoroethyl methacrylate and polymethyl methacrylates separately after the pre-polymerization respectively, mixing back two kinds of polymer more can not mix, it is translucent that thereby the material that makes last polymerization presents, control pre-polymerization conversion ratio separately, the light transmittance that can obtain final polymer is 50～70%, and the anaclasis that enters into optical fiber can present uniform entire body side illumination effect behind translucent covering.The conversion ratio that continuous pre-polymerization is obtained is that 10～50% prepolymer is sent in the extruder, continue to improve conversion ratio and reach 80～90%, in extruder, take off single extruding pelletization then, obtain the translucent polymethylacrylic acid trifluoro ethyl ester after the modification, light transmittance 50～70%, refractive index n=1.423, shore hardness=85A seals up for safekeeping standby.Extruder can adopt the double-screw type structure, also can adopt the single-screw structure.
Clad material also can adopt above-mentioned technology to produce with other fluorochemical monomer, comprise methacrylic acid hexafluoro butyl ester (6FBMA, refractive index polymer n=1.40, light transmittance〉90%, shore hardness＜60A), tetrafluoropropyl propyl ester (4FPM, refractive index polymer n=1.42, light transmittance〉90%, shore hardness＜70A), perhaps adopt other translucent polyvinyl fluoride resinoid utilizes and carries out light scattering with semi-crystalline region in the polyvinyl fluoride resinoid, as Kynoar (PVDF), refractive index n=1.42, light transmittance 50%, shore hardness〉100A.
Center core layer material of the present invention can be selected acrylic monomer such as butyl methacrylate (BMA, refractive index polymer n=1.48, shore hardness=60A, light transmittance=93%), mass concentration 80～100%, the modifier methyl methacrylate (MMA, refractive index polymer are 1.491, shore hardness〉100A, light transmittance=93%), mass concentration 0～20%, prescription comprises that also radical initiator, material are azo class or peroxidating class initator, mass concentration is 0～0.4%, chain-transferring agent, material are the thio-alcohol material, and mass concentration is 0～0.6%.
Monomer material required among the present invention all need be purified, and method of purification is conventional decompression distillation, filtration etc., to remove impurity, improves purity, and main monomer purity needs〉99.99%.
The present invention's employing is similar to aforesaid method and carries out continuous bulk polymerization coextrusion sidelight plastic optical fiber.Comprise a continuous pre-polymerization device in this technology, an extruder.Component behind the prescription is delivered in the continuous pre-polymerization device and carried out continuous prepolymerization reaction, the pre-polymerization device can be series connection still formula structure continuously, it also can be the pipeline structure of band heating jacket, its function is that pre-collecting process is carried out continuously, heating-up temperature can be set at 60～160 ℃, makes the pre-polymerization conversion ratio reach 10～50%.The prepolymer that continuous pre-polymerization obtains is sent in the extruder, continue to improve conversion ratio and reach 80～90%, in extruder, take off then and singly melt extrude in a co-extruding mould, this co-extruding mould opposite side is connected with a single screw rod covering extruder, seal aforementioned preparation up for safekeeping standby translucent polymethylacrylic acid trifluoro ethyl ester (light transmittance 50～70%, refractive index n=1.423, shore hardness=85A) melt extrude in co-extruding mould by this covering extruder, form the strip extrudate in concentric circles cross section, go up dish by cooling and shaping rear haulage coiling, obtain the sidelight plastic optical fiber of entirely lighting effect.
It is as follows to adopt sidelight plastic optical fiber that above-mentioned method prepares and perfusion to compare the result:
| The continuous reaction coextrusion method | Perfusion | |
| Characterize flexible bending radius (D is a fibre diameter) | <5D | 20～30D |
| Light transmittance | >93％ | 90～91％ |
| Effectively pass light length | 60～80m | 30～40m |
| -40～70 ℃ high low temperature circulation 72h | Sandwich layer covering interface is not stratified | Layering is wanted at sandwich layer covering interface, influences result of use |
| Production efficiency | Produce efficient height, but production random length continuously | Batch production, efficient is lower, can only produce according to F46 length of tube fixed length |
| Fibre diameter | 0.25～35mm | 3～25mm |
The inventive method can solve that the pliability of existing sidelight plastic optical fiber is poor, the easy layering of cold cycling rear interface plays hollow bubble out of doors, influence result of use, service life and defective such as lacks; Simultaneously production efficiency height, production cost are low.The sidelight plastic optical fiber that the inventive method is produced is applicable in the indoor outer decorative lighting field and sketches the contours fields such as profile, underwater lighting, artistic lamp-ornaments.
Description of drawings:
Fig. 1 is a sidelight plastic optical fiber structural representation.
The specific embodiment:
Embodiment of the invention preparing sidelight plastic fibers by continuous reaction coextrusion comprise the steps:
1, produce covering: the purification monomer component, the mixed solution of formulation components A: (by mass percentage concentration) peroxidating class initator DTBP0.1%, mercaptan type chain transfer agent n-butyl mercaptan 0.4%, fluorine monomer solution 3FEA surplus, dispose the mixed solution of B component again: (by mass percentage concentration) peroxidating class initator 0.1%, mercaptan type chain transfer agent n-butyl mercaptan 0.4%, methyl methacrylate MMA surplus, the conversion ratio of difference pre-polymerization to 10% under 100 ℃ in continuous pre-polymerization device, mix pre-polymerization again and reach 60% to conversion ratio, be transported to again and further be aggregated to conversion ratio 80% in the double screw extruder, slough unreacted monomer then, make content of monomer be controlled at＜0.3%, extrude the traction granulation obtain covering fluororesin polymethylacrylic acid trifluoro ethyl ester, seal up for safekeeping standby.
The key technical indexes:
Light transmittance 50～70%
Refractive index n=1.423
Shore hardness=85A
2, produce sandwich layer:
Purification sandwich layer monomer component, preparation sandwich layer monomer solution butyl methacrylate BMA, peroxidating class initator DTBP0.1%, the mixed solution of mercaptan type chain transfer agent n-butyl mercaptan 0.4%, 100 ℃ of following pre-polymerizations reach 60% to conversion ratio in continuous pre-polymerization device, are transported to by Melt Pump and further are aggregated to conversion ratio 80% in the double screw extruder, slough unreacted monomer then, make content of monomer be controlled at＜0.3%, promptly obtain sandwich layer
3, produce the sidelight plastic optical fiber
Sandwich layer is melt extruded sandwich layer district in the co-extruding mould, simultaneously covering fluororesin polymethylacrylic acid trifluoro ethyl ester is melt extruded sandwich layer district in the co-extruding mould by another extruder, it is the bar shaped optical fiber in concentric circles cross section that two kinds of materials converge coextrusion cross section, back, and drawn cooling rear haulage is reeled to go up to coil and obtained the sidelight plastic optical fiber.
The sidelight plastic optical fiber leading indicator that adopts this kind method to produce:
Light loss consumption:＜0.3dB/m
Bending radius: 3D
Diameter: φ 0.25mm～35mm
-40～70 ℃ high low temperature circulation 72h: optical fibre interface is not stratified
Radially count in the optical fiber, cladding thickness is 5～100: 1000 with the core layer thickness ratio.
The sidelight plastic optical fiber structural representation of Fig. 1 for adopting said method to produce.Comprise sandwich layer 1, be coated on the covering 2 of sandwich layer periphery.
The foregoing description is that foregoing of the present invention is further described, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to the foregoing description.All technology that realizes based on foregoing all belong to scope of the present invention.
Claims (4)
1, the method for preparing sidelight plastic fibers by continuous reaction coextrusion, this method be translucent covering that at least two kinds of different materials copolymerization are formed and shore hardness≤90A, refractive index with shore hardness≤90A greater than the flexible core of cladding index and light transmittance 〉=93% respectively fusion clamp-on the clad region and the sandwich layer district of co-extruding mould, form the strip extrudate in concentric circles cross section, promptly make sidelight plastic optical fiber after the cooling with entirely lighting effect.
2, the method for preparing sidelight plastic fibers by continuous reaction coextrusion as claimed in claim 1 is characterized in that this method comprises the steps:
1) preparation covering:
A. prepare burden in proportion:
Covering is made up of at least two kinds of clad materials, and by mass percentage concentration, every kind of clad material comprises following component:
Radical initiator 0～0.4%
Chain-transferring agent 0～0.6%
Covering monomer surplus,
B. prepare covering:
After the above-mentioned various clad materials that are made into are purified respectively respectively under 60～160 ℃ of pre-polymerization temperature respectively pre-polymerization carry out continuous prepolymerization reaction again after being 5～20% to conversion ratio, heating-up temperature is 60～160 ℃ and makes the pre-polymerization conversion ratio and reach 10～50% mixed prepolymer, mixed prepolymer is sent into extruder, its conversion ratio is reached 80～90%, take off single granulation and promptly make required covering;
2) preparation sandwich layer:
A. prepare burden in proportion: by mass percentage concentration, sandwich layer comprises following component:
Sandwich layer monomer 80～100%
Modifier 0～20%
Radical initiator 0～0.4%
Chain-transferring agent 0～0.6%,
B. prepare sandwich layer:
Carry out prepolymerization reaction after said components purified respectively, in heating-up temperature is to make its pre-polymerization conversion ratio reach 10～50% under 60～160 ℃, the prepolymer that pre-polymerization is obtained is sent into and is made its conversion ratio reach 80～90% in the extruder, takes off single fusion and make sandwich layer in extruder;
3), preparation sidelight plastic optical fiber:
The sandwich layer that will take off single fusion is expressed into the sandwich layer district in the co-extruding mould, covering is melt extruded clad region in the co-extruding mould through the covering extruder that is connected with co-extruding mould, form the strip extrudate in concentric circles cross section, promptly make sidelight plastic optical fiber after the cooling with entirely lighting effect.
3, the method for preparing sidelight plastic fibers by continuous reaction coextrusion as claimed in claim 2 is characterized in that the covering monomer is fluorine-containing class monomer or acrylic monomer, and the sandwich layer monomer is an acrylic monomer.
4, as the method for the described preparing sidelight plastic fibers by continuous reaction coextrusion of one of claim 1～3, it is characterized in that radially counting in the optical fiber, cladding thickness is 5～100: 1000 with the core layer thickness ratio.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105885319A (en) * | 2016-05-13 | 2016-08-24 | 江西大圣塑料光纤有限公司 | Preparation method for surface light-emitting plastic optical fiber |
| CN106019466A (en) * | 2016-06-03 | 2016-10-12 | 江西大圣塑料光纤有限公司 | Method of producing large diameter flexible solid state core side surface light-emitting type plastic optical fiber |
| CN109402758A (en) * | 2018-09-30 | 2019-03-01 | 镇江微芯光子科技有限公司 | The preparation method of polymer optical fiber |
| CN109669234A (en) * | 2019-02-27 | 2019-04-23 | 南宁旭越光纤有限责任公司 | A kind of light-strip of entirely lighting and preparation method thereof |
| CN111118658A (en) * | 2019-12-06 | 2020-05-08 | 湖北森沃光电科技有限公司 | Extrusion type super-flexible side light-emitting optical fiber and preparation method thereof |
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| CN2365681Y (en) * | 1999-04-21 | 2000-02-23 | 樊邦弘 | Optical fibre (crystal optical fibre) |
| CN1221374C (en) * | 2003-08-22 | 2005-10-05 | 四川汇源光通信股份有限公司 | Continuous reaction and coextrusion process of preparing stepped plastic fiber |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105885319A (en) * | 2016-05-13 | 2016-08-24 | 江西大圣塑料光纤有限公司 | Preparation method for surface light-emitting plastic optical fiber |
| CN106019466A (en) * | 2016-06-03 | 2016-10-12 | 江西大圣塑料光纤有限公司 | Method of producing large diameter flexible solid state core side surface light-emitting type plastic optical fiber |
| CN106019466B (en) * | 2016-06-03 | 2018-09-18 | 江西大圣塑料光纤有限公司 | A kind of preparation method of large-diameter flexible solid core entirely lighting plastic optical fiber |
| CN109402758A (en) * | 2018-09-30 | 2019-03-01 | 镇江微芯光子科技有限公司 | The preparation method of polymer optical fiber |
| CN109669234A (en) * | 2019-02-27 | 2019-04-23 | 南宁旭越光纤有限责任公司 | A kind of light-strip of entirely lighting and preparation method thereof |
| CN111118658A (en) * | 2019-12-06 | 2020-05-08 | 湖北森沃光电科技有限公司 | Extrusion type super-flexible side light-emitting optical fiber and preparation method thereof |
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