CN106084610A - A kind of preparation method of high accuracy graded index plastic light pricker - Google Patents
A kind of preparation method of high accuracy graded index plastic light pricker Download PDFInfo
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- CN106084610A CN106084610A CN201610636299.9A CN201610636299A CN106084610A CN 106084610 A CN106084610 A CN 106084610A CN 201610636299 A CN201610636299 A CN 201610636299A CN 106084610 A CN106084610 A CN 106084610A
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- discharging
- optical fiber
- graded index
- plastic optical
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
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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
- G02B6/02033—Core or cladding made from organic material, e.g. polymeric material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to the preparation method of a kind of high accuracy graded index plastic light pricker, belong to plastic optical fiber preparing technical field.After methyl methacrylate and siloxanes are carried out distillation process by the present invention, distillation raffinate is carried out Hybrid Heating with materials such as azodiisobutyronitriles and pressurizes, then lowers the temperature, discharging, obtain discharging thing, then it is mixed homogeneously with Yttrium trinitrate, freezing discharging, filter, obtain core material base material, finally it is drawn, and put into fluorination stove carries out fluorination parcel, i.e. available high accuracy graded index plastic optical fiber.High accuracy graded index plastic optical fiber bandwidth prepared by the present invention is high, and bandwidth is not less than 1.5GHz 100m, can be widely applied to the higher light pricker of bandwidth requirement to message areas such as family LAN, industry control LANs that volume of transmitted data is bigger；And high accuracy graded index plastic optical fiber refractive index is high, refractive index is more than 1.62.
Description
Technical field
The present invention relates to the preparation method of a kind of high accuracy graded index plastic light pricker, belong to plastic optical fiber technology of preparing
Field.
Background technology
Plastic optical fiber is as sandwich layer by high transparency polymer such as polystyrene, polymethyl methacrylate, Merlon
Material, PMMA, fluoroplastics etc. are as a type optical fiber of cortical material.Different materials has different attenuation performance and temperature
Range of application.Plastic optical fiber may not only be applied to last 100～1000 meters of access network, it is also possible to for various automobiles, aircraft, etc.
On vehicle, it has, and fibre core footpath is big, be easily worked, pliability is good, it is easy to installs and safeguards and the feature of low cost, and
The copper stranded conductor medium high hundreds of times that its bandwidth ratio is traditional, are the first-selected transmission mediums of LAN and fiber entering household, the most various
High performance plastics optical fiber develops rapidly.
Existing plastic optical fiber preparation method is mainly surface fluorination method and co-extrusion process, wherein co-extrusion process, this
Method is first to prepare the optical fiber high transparency polymeric material of different refractivity, is reflected according in center by multiple stage extruder
The Distribution Principles that rate is the highest, radially successively decrease, melt extrudes the polymeric material of different refractivity respectively, by multi-layer co-extruded mould
Tool melt extrudes, and draws drawing and forming.The shortcoming of this method is: (1) belongs to multistage plastic optical fiber, and index distribution is rank
Ladder type, bandwidth is the highest；(2) number of plies is the fewest, and bandwidth is the lowest；(3) generally only have 5～30 μm, the therefore numbers of plies due to every a layer thickness
The most, control difficulty the biggest, yield rate is the lowest, it is difficult to stably produce the high bandwidth plastic optical fiber that batch is qualified.
Summary of the invention
The technical problem to be solved: the highest for the plastic light pricker bandwidth utilizing co-extrusion process to prepare, folding
The problem that rate of penetrating is low, after methyl methacrylate and siloxanes are carried out distillation process by the present invention, will distillation raffinate and azo
The materials such as bis-isobutyronitrile carry out Hybrid Heating and pressurize, then lower the temperature, discharging, obtain discharging thing, then it are carried out with Yttrium trinitrate
Mix homogeneously, freezing discharging, filter, obtain core material base material, finally it is drawn, and put in fluorination stove and be fluorinated
Parcel, i.e. available high accuracy graded index plastic optical fiber.High accuracy graded index plastic light fibre ribbons prepared by the present invention
Width is higher, can be widely applied to the higher light pricker of bandwidth requirement to family LAN, industry control LAN etc. that volume of transmitted data is bigger
Message area.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
(1) count by weight, take 60～70 parts of methyl methacrylates, 14～18 parts of azodiisobutyronitriles, 13～16 part ten
Dialkyl group mercaptan and 8～12 parts of siloxanes, first put in distilling apparatus by methyl methacrylate and siloxanes, uses nitrogen
Protection, naturally cools to room temperature after 120～130 DEG C of distillations 20～30min, then pours distillation raffinate into glass reaction still
In, the most successively azodiisobutyronitrile, lauryl mercaptan are put in glass reaction still；
(2) after above-mentioned lauryl mercaptan puts into glass reaction still, gaseous mixture is used to be discharged by the air in glass reaction still,
And boosting to 0.3～0.6MPa, design temperature is 74～78 DEG C, after 200r/min stirring prepolymerization reaction 24～28min, with 12
DEG C/h is warming up to 98～106 DEG C, with 300r/min stirring reaction 42～52h, described gaseous mixture is that nitrogen, tritium gas and helium are by body
Amass and mix than 8:2:1；
(3) after above-mentioned reaction terminates, be cooled to 60～65 DEG C, discharging while hot, collect discharging thing, and with discharging material amount 1.2
～the Yttrium trinitrate mix homogeneously of 1.6%, to put in liquid nitrogen flash freezer machine, design temperature is-5～0 DEG C, freezing discharging 10～15min,
Filter again, collect filtering residue and warm naturally to room temperature, obtaining core material base material；
(4) putting in fiber drawing tower by the core material base material of above-mentioned gained, design temperature is 170～180 DEG C, is drawn into diameter
Be the filament of 350～400 μm, then the fluorination stove that the volumetric concentration that filament is put into xenon difluoride is 4～7%, be set as 82～
84 DEG C, insulation reaction 20～24h, high accuracy graded index plastic optical fiber.
High accuracy graded index plastic optical fiber light transmittance prepared by the present invention is more than 98%, and bandwidth is not less than 1.5GHz
100m, light loss is less than 0.15dB/m(650nm), refractive index is more than 1.62, and life-time service temperature is less than 120 DEG C.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the high accuracy graded index plastic optical fiber bandwidth that prepared by the present invention is high, and bandwidth is not less than 1.5GHz 100m, can be wide
The general higher light pricker of bandwidth requirement that is applied to is to message areas such as family LAN, industry control LANs that volume of transmitted data is bigger；
(2) the high accuracy graded index plastic optical fiber refractive index that prepared by the present invention is high, and refractive index is more than 1.62；
(3) preparation process of the present invention is simple, required low cost.
Detailed description of the invention
Count the most by weight, take 60～70 parts of methyl methacrylates, 14～18 parts of azodiisobutyronitriles, 13～16
Part lauryl mercaptan and 8～12 parts of siloxanes, first put in distilling apparatus by methyl methacrylate and siloxanes, uses
Nitrogen is protected, and naturally cools to room temperature, then pour distillation raffinate into glass reaction after 120～130 DEG C of distillations 20～30min
In still, the most successively azodiisobutyronitrile, lauryl mercaptan are put in glass reaction still；Put at above-mentioned lauryl mercaptan
After entering glass reaction still, use gaseous mixture to be discharged by the air in glass reaction still, and boost to 0.3～0.6MPa, set temperature
Degree is 74～78 DEG C, after 200r/min stirring prepolymerization reaction 24～28min, is warming up to 98～106 DEG C with 12 DEG C/h, with
300r/min stirring reaction 42～52h, described gaseous mixture is that nitrogen, tritium gas and helium 8:2:1 by volume mixes；Upper
State after reaction terminates, be cooled to 60～65 DEG C, discharging while hot, collect discharging thing, and with discharging material amount 1.2～the nitre of 1.6%
Acid yttrium mix homogeneously, puts in liquid nitrogen flash freezer machine, and design temperature is-5～0 DEG C, freezing discharging 10～15min, then filters,
Collect filtering residue and warm naturally to room temperature, obtaining core material base material；Finally the core material base material of above-mentioned gained is put into drawing optical fibers
In tower, design temperature is 170～180 DEG C, is drawn into the filament of a diameter of 350～400 μm, then filament is put into xenon difluoride
Volumetric concentration is the fluorination stove of 4～7%, is set as 82～84 DEG C, insulation reaction 20～24h, high accuracy gradient refractive index
Rate plastic optical fiber.
Example 1
Count the most by weight, take 70 parts of methyl methacrylates, 18 parts of azodiisobutyronitriles, 16 parts of lauryl mercaptans and
12 parts of siloxanes, first put in distilling apparatus by methyl methacrylate and siloxanes, use nitrogen protection, 130 DEG C of steamings
Naturally cool to room temperature after evaporating 30min, then distillation raffinate is poured in glass reaction still, the most successively by azo two isobutyl
Nitrile, lauryl mercaptan are put in glass reaction still；After above-mentioned lauryl mercaptan puts into glass reaction still, use gaseous mixture
Being discharged by air in glass reaction still, and boost to 0.6MPa, design temperature is 78 DEG C, stirs prepolymerization reaction with 200r/min
After 28min, being warming up to 106 DEG C with 12 DEG C/h, with 300r/min stirring reaction 52h, described gaseous mixture is nitrogen, tritium gas and helium
8:2:1 mixes by volume；After above-mentioned reaction terminates, be cooled to 65 DEG C, discharging while hot, collect discharging thing, and with go out
The Yttrium trinitrate mix homogeneously of material material amount 1.6%, puts in liquid nitrogen flash freezer machine, and design temperature is 0 DEG C, freezing discharging 15min, then
Filter, collect filtering residue and warm naturally to room temperature, obtaining core material base material；Finally the core material base material of above-mentioned gained is put into
In fiber drawing tower, design temperature is 180 DEG C, is drawn into the filament of a diameter of 400 μm, then filament is put into the body of xenon difluoride
Volume concentrations is the fluorination stove of 7%, is set as 84 DEG C, insulation reaction 24h, high accuracy graded index plastic optical fiber.
After testing, high accuracy graded index plastic optical fiber light transmittance prepared by the present invention is 98.2%, carries a width of
1.5GHz 100m, light loss is 0.14dB/m(650nm), refractive index is 1.63, and life-time service temperature is 115 DEG C.
Example 2
Count the most by weight, take 60 parts of methyl methacrylates, 14 parts of azodiisobutyronitriles, 13 parts of lauryl mercaptans and
8 parts of siloxanes, first put in distilling apparatus by methyl methacrylate and siloxanes, use nitrogen protection, 120 DEG C of distillations
Naturally cool to room temperature after 20min, then distillation raffinate poured in glass reaction still, the most successively by azodiisobutyronitrile,
Lauryl mercaptan is put in glass reaction still；After above-mentioned lauryl mercaptan puts into glass reaction still, use gaseous mixture will
Air in glass reaction still is discharged, and boosts to 0.3MPa, and design temperature is 74 DEG C, stirs prepolymerization reaction with 200r/min
After 24min, being warming up to 98 DEG C with 12 DEG C/h, with 300r/min stirring reaction 42h, described gaseous mixture is nitrogen, tritium gas and helium
8:2:1 mixes by volume；After above-mentioned reaction terminates, be cooled to 60 DEG C, discharging while hot, collect discharging thing, and with go out
The Yttrium trinitrate mix homogeneously of material material amount 1.2%, puts in liquid nitrogen flash freezer machine, and design temperature is-5 DEG C, freezing discharging 10min,
Filter again, collect filtering residue and warm naturally to room temperature, obtaining core material base material；Finally the core material base material of above-mentioned gained is put
Entering in fiber drawing tower, design temperature is 170 DEG C, is drawn into the filament of a diameter of 350 μm, then filament is put into xenon difluoride
Volumetric concentration is the fluorination stove of 4%, is set as 82 DEG C, insulation reaction 20h, high accuracy graded index plastic optical fiber.
After testing, high accuracy graded index plastic optical fiber light transmittance prepared by the present invention is 98.3%, carries a width of
1.6GHz 100m, light loss is 0.14dB/m(650nm), refractive index is 1.65, and life-time service temperature is 115 DEG C.
Example 3
Count the most by weight, take 65 parts of methyl methacrylates, 15 parts of azodiisobutyronitriles, 14 parts of lauryl mercaptans and
10 parts of siloxanes, first put in distilling apparatus by methyl methacrylate and siloxanes, use nitrogen protection, 125 DEG C of steamings
Naturally cool to room temperature after evaporating 25min, then distillation raffinate is poured in glass reaction still, the most successively by azo two isobutyl
Nitrile, lauryl mercaptan are put in glass reaction still；After above-mentioned lauryl mercaptan puts into glass reaction still, use gaseous mixture
Being discharged by air in glass reaction still, and boost to 0.5MPa, design temperature is 75 DEG C, stirs prepolymerization reaction with 200r/min
After 25min, being warming up to 100 DEG C with 12 DEG C/h, with 300r/min stirring reaction 50h, described gaseous mixture is nitrogen, tritium gas and helium
8:2:1 mixes by volume；After above-mentioned reaction terminates, be cooled to 62 DEG C, discharging while hot, collect discharging thing, and with go out
The Yttrium trinitrate mix homogeneously of material material amount 1.4%, puts in liquid nitrogen flash freezer machine, and design temperature is-4 DEG C, freezing discharging 12min,
Filter again, collect filtering residue and warm naturally to room temperature, obtaining core material base material；Finally the core material base material of above-mentioned gained is put
Entering in fiber drawing tower, design temperature is 175 DEG C, is drawn into the filament of a diameter of 370 μm, then filament is put into xenon difluoride
Volumetric concentration is the fluorination stove of 6%, is set as 83 DEG C, insulation reaction 22h, high accuracy graded index plastic optical fiber.
After testing, high accuracy graded index plastic optical fiber light transmittance prepared by the present invention is 99%, carries a width of
1.55GHz 100m, light loss is 0.14dB/m(650nm), refractive index is 1.65, and life-time service temperature is 110 DEG C.
Claims (1)
1. the preparation method of a high accuracy graded index plastic optical fiber, it is characterised in that concrete preparation process is:
(1) count by weight, take 60～70 parts of methyl methacrylates, 14～18 parts of azodiisobutyronitriles, 13～16 part ten
Dialkyl group mercaptan and 8～12 parts of siloxanes, first put in distilling apparatus by methyl methacrylate and siloxanes, uses nitrogen
Protection, naturally cools to room temperature after 120～130 DEG C of distillations 20～30min, then pours distillation raffinate into glass reaction still
In, the most successively azodiisobutyronitrile, lauryl mercaptan are put in glass reaction still；
(2) after above-mentioned lauryl mercaptan puts into glass reaction still, gaseous mixture is used to be discharged by the air in glass reaction still,
And boosting to 0.3～0.6MPa, design temperature is 74～78 DEG C, after 200r/min stirring prepolymerization reaction 24～28min, with 12
DEG C/h is warming up to 98～106 DEG C, with 300r/min stirring reaction 42～52h, described gaseous mixture is that nitrogen, tritium gas and helium are by body
Amass and mix than 8:2:1；
(3) after above-mentioned reaction terminates, be cooled to 60～65 DEG C, discharging while hot, collect discharging thing, and with discharging material amount 1.2
～the Yttrium trinitrate mix homogeneously of 1.6%, to put in liquid nitrogen flash freezer machine, design temperature is-5～0 DEG C, freezing discharging 10～15min,
Filter again, collect filtering residue and warm naturally to room temperature, obtaining core material base material；
(4) putting in fiber drawing tower by the core material base material of above-mentioned gained, design temperature is 170～180 DEG C, is drawn into diameter
Be the filament of 350～400 μm, then the fluorination stove that the volumetric concentration that filament is put into xenon difluoride is 4～7%, be set as 82～
84 DEG C, insulation reaction 20～24h, high accuracy graded index plastic optical fiber.
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| CN201610636299.9A CN106084610A (en) | 2016-08-05 | 2016-08-05 | A kind of preparation method of high accuracy graded index plastic light pricker |
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| CN201610636299.9A CN106084610A (en) | 2016-08-05 | 2016-08-05 | A kind of preparation method of high accuracy graded index plastic light pricker |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415982A (en) * | 2002-11-22 | 2003-05-07 | 四川汇源光通信有限公司 | Plastic optical fiber with fluorizated packet-layer and its prepn. method |
| CN1415985A (en) * | 2002-12-05 | 2003-05-07 | 上海交通大学 | Method for preparing prefabricated rod of gradation type plastic optical fiber |
| CN101015959A (en) * | 2006-12-29 | 2007-08-15 | 上海高分子材料研究开发中心 | Manufacture method of visible light curing gradient type plastic optical fiber prefabricated stick |
-
2016
- 2016-08-05 CN CN201610636299.9A patent/CN106084610A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415982A (en) * | 2002-11-22 | 2003-05-07 | 四川汇源光通信有限公司 | Plastic optical fiber with fluorizated packet-layer and its prepn. method |
| CN1415985A (en) * | 2002-12-05 | 2003-05-07 | 上海交通大学 | Method for preparing prefabricated rod of gradation type plastic optical fiber |
| CN101015959A (en) * | 2006-12-29 | 2007-08-15 | 上海高分子材料研究开发中心 | Manufacture method of visible light curing gradient type plastic optical fiber prefabricated stick |
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