CN105038220A - High-toughness aramid composite material optical fiber reinforced core and preparation method thereof - Google Patents
High-toughness aramid composite material optical fiber reinforced core and preparation method thereof Download PDFInfo
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- CN105038220A CN105038220A CN201510347152.3A CN201510347152A CN105038220A CN 105038220 A CN105038220 A CN 105038220A CN 201510347152 A CN201510347152 A CN 201510347152A CN 105038220 A CN105038220 A CN 105038220A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino-carboxylic acids or of polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1477—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The invention discloses a high-toughness aramid composite material optical fiber reinforced core which is prepared from an aramid fiber, a resin substrate, two or more fillers, and one or two mold release agents. The resin substrate comprises the following substances in parts by weight: 20-45 parts of liquid epoxy resin, 11-30 parts of N,N'-diphenylmethane bismaleimide, 9-23 parts of a curing agent, 5-15 parts of furfuryl amine and 0-2 parts of an accelerating agent. A preparation method of the aramid composite material optical fiber reinforced core comprises two stages: (a) pultrusion forming: conducting drying-tunnel preheating, gum dipping, mold forming, drying-tunnel curing, rolling-up and other processes on the aramid fiber; (b) self-repairing of the reinforced core composite material: carrying out heating in a drying oven. The aramid composite material optical fiber reinforced core has the advantages that through addition of furan and imide structures in the resin substrate, the cross-linking density of the resin substrate is increased, and thus such mechanical properties as the toughness and the tensile strength of the aramid composite material optical fiber reinforced core can be improved; besides, part of the interlaminar crack damage can be repaired, so that the purpose of further improving the toughness and the tensile strength of the aramid composite material optical fiber reinforced core can be fulfilled.
Description
Technical field
The present invention relates to the nonmetal reinforced composite of a kind of optical fiber, specifically a kind of high tenacity aramid fiber composite material optical fiber strengthens core and preparation method thereof.
Background technology
Along with popularizing of fiber entering household (FTTH) overall situation, bring opportunity to the development of optical fiber strongthener upgrading.Traditional optical fiber strengthens core and is made of metal, therefore has 1), self is heavier, transportation cost is high; 2) chemical stability is poor, is easily corroded, and greatly reduces the work-ing life of optical fiber; 3), easily produce electrostatic, have the shortcomings such as interference at thunderstorm weather to signal.Now gradually substitute by nonmetallic composite.Early stage non-metallic optical fiber cables strengthens core and is mainly glass fibre and thermosetting resin compound, although have high-strength light, the advantage such as corrosion-resistant, antistatic, but glass fibre self is more crisp, cause its pultrusion rate-constrained, just cannot re-use once generation fracture, scrap rate is high, and finished product bending radius is large, and complex indoor environment wiring is difficult.
In recent years, the reversible addition reaction of Di Ersi-Alder (Diels-Alder) diene is one of focus of research matrix material selfreparing.By introduce in reaction system needed for Diels-Alder reaction containing the carbon-carbon double bond group of closed loop, utilize under this low temperature reaction, under Diene-addition and heating condition, the reversible repairing effect that reversed reaction realizes material occur.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of high tenacity, high strength, good heat resistance aramid fiber composite material optical fiber strengthen core and preparation method thereof.
The present invention adopts following technical scheme: a kind of high tenacity aramid fiber composite material optical fiber strengthens core, is made up of aramid fiber, matrix resin, filler and releasing agent, and described matrix resin is the hybrid resin containing epoxy resin, comprises the material of following weight part:
Liquid epoxies 20-45 part,
N, N'-diphenyl methane dimaleimide 11-30 part,
Solidifying agent 9-23 part,
Chaff amine 5-15 part,
Promotor 0-2 part.
Wherein, described liquid epoxies is bis-phenol A glycidyl ether type epoxy resin, and epoxy equivalent (weight) is 163g/mol-188g/mol.
Preferably, described solidifying agent is HHPA or methyl hexahydrophthalic anhydride.
Preferably, described promotor is DMP-30 or triethylamine.
Preferably, described aramid fiber is 60-80 part, and matrix resin is 15-30 part, and filler is 2-8 part, and releasing agent is 1-3 part.
Preferably, described filler is at least two kinds in calcium carbonate, aluminium hydroxide, barium sulfate, magnesium hydroxide, aluminum oxide, is preferably two to three kinds.Appropriate mineral filler can strengthen toughness and the hardness of resin, and hydroxide addition aluminium, magnesium hydroxide also have fire retardation.
Preferably, described releasing agent is one or both in tung oil, methyl-silicone oil, aluminum stearate, calcium stearate.Suitable releasing agent can promote pultrusion speed, extends the pultrusion time, improve production efficiency and conforming product rate, and core surfaces is more smooth, smooth.
Above-mentioned high tenacity aramid fiber composite material optical fiber strengthens the preparation method of core, is divided into two stages: a) pultrusion stage of completing through techniques such as drying tunnel preheating, impregnation, mould shape, drying tunnel solidification, rollings of aramid fiber; B) via baking oven for heating, the enhancing core matrix material selfreparing stage completed; Specifically comprise the following steps: 1) 20-45 part liquid epoxies is placed in container, is heated to 50 DEG C, stir, slow dropping 5-15 part chaff amine, control temperature of reaction 45 DEG C-75 DEG C, after reaction 1-3h, add 11-30 part N, N'-diphenyl methane dimaleimide, 9-23 part solidifying agent, 0-2 part promotor, continues to be uniformly mixed, obtain the high tenacity of pultrusion molding process after cooling, there is the matrix resin of reversible repairing effect; 2) in 15-30 part matrix resin, 2-8 part filler is added, 1-3 part releasing agent, electric blender stirs 30min, pour into after stirring in steeping vat, by 60-80 part aramid fiber after drying tunnel prewarming baking, pass through steeping vat, shape through mould Procuring after complete viscose glue, drying tunnel solidifies completely, eventually passes pressure roller traction, winder rolling; 3) optical fiber pultrusion gone out strengthens core and is positioned in the baking oven of 220 DEG C-300 DEG C, baking 4h-7h, after naturally cooling cooling, obtains high tenacity aramid fiber composite material optical fiber and strengthens core.
Wherein, step 2) in aramid fiber preheating drying tunnel temperature be 75 DEG C-115 DEG C, steeping vat temperature is 30 DEG C-60 DEG C, and die temperature is 95 DEG C-130 DEG C, and the temperature of solidification drying tunnel is 220 DEG C-260 DEG C, and rolling speed is 300mm/min-500mm/min.
In the present invention program, chaff amine is added to introduce furan group in matrix resin, N, N'-diphenyl methane dimaleimide introduces imide group, add the active group in substrate ring epoxy resin system, thus increase the cross-linking density of resin crosslinks system, Diels-Alder thermal reversion can be there is between the furan group simultaneously introduced and imide group react, under low temperature there is Diene-addition in the two, then reversed reaction is there is under heating condition, repair and produce, Crack Damage in the reinforced partly core architecture that transportation produces, the toughness that aramid fiber composite material Fiber Composites strengthens core is improved to reach, draw high the object of intensity and thermotolerance.
In addition, utilize aramid fiber for strongthener, thermosetting resin is matrix resin, and the aramid fiber composite material optical fiber shaping through pultrude process strengthens core, compared to enhancing core before, there is stronger mechanical property, tensile strength >=1800MPa, even if fracture still has the intensity of 1000MPa, bending radius is less simultaneously, be about 30mm, quality is lighter, is about the half that glass fiber cable strengthens core, so it is one of desirable optical cable strengthening core that aramid fiber composite material optical fiber strengthens core.
Tool of the present invention has the following advantages: high tenacity aramid fiber composite material optical fiber prepared by the present invention strengthens core, adds chaff amine and N, N'-diphenyl methane dimaleimide introduces furan group and imide group in matrix resin.On the one hand, the active group added can increase the cross-linking density after matrix resin solidification, thus promotes its mechanical property such as toughness, tensile strength; On the other hand, the thermal reversion selfreparing group of increase, at aramid fiber composite material after pultrude process hot setting, can repair Crack Damage between part layer, again reaches the object promoting toughness and tensile strength.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is further described, but protection scope of the present invention is not limited thereto.
Embodiment 1
1) be equipped with at 250ml in the there-necked flask of mechanical stirring, thermometer, constant pressure funnel and nitrogen gatherer and add 43g liquid epoxies, limit is stirred and is warming up to 50 DEG C, constant pressure funnel is utilized slowly to be added drop-wise in liquid epoxies by 5.5g chaff amine in 40min, temperature of reaction controls at about 65 DEG C, isothermal reaction 2h.Continue to add N, N'-diphenyl methane dimaleimide 11.2g, methyl hexahydrophthalic anhydride 13.2g, DMP-30 promotor 0.2g, continue isothermal reaction 0.5h, cooling obtain preparing high tenacity aramid fiber composite material optical fiber strengthen core high tenacity, can the matrix resin of selfreparing.
Adopt the 60g matrix resin of above-mentioned preparation, add the aluminium hydroxide of 2g, the activated Calcium carbonate of 2g, the aluminum stearate of 2g.Pour into after electric blender stirs in glue groove.DuPontKevlarK291500D type aramid fiber 150g is selected to be strongthener, after 90 DEG C of bakings, successively through steeping vat impregnation, mould molding, drying tunnel solidification, pressure roller traction and winder rolling flow process.Wherein, steeping vat temperature is 50 DEG C, and die temperature is 115 DEG C, solidification drying tunnel temperature is 240 DEG C, and pulling speed is 300mm/min, and it is 0.52mm that the aramid fiber composite material tentatively prepared strengthens core diameter, its tensile strength is 1860MPa, and minimum bend diameter is 15mm.
Tentatively obtained aramid fiber composite material is strengthened core to be positioned in the baking oven of 240 DEG C, and naturally cooling after continuation baking 5h, make high tenacity aramid fiber composite material optical fiber and strengthen core, its tensile strength can be increased to 1985MPa, and minimum bend diameter is lower than 10mm.
Embodiment 2
Be equipped with at 250ml in the there-necked flask of mechanical stirring, thermometer, constant pressure funnel and nitrogen gatherer and add 43g liquid epoxies, limit is stirred and is warming up to 50 DEG C, constant pressure funnel is utilized slowly to be added drop-wise in liquid epoxies by 8g chaff amine in 40min, temperature of reaction controls at about 65 DEG C, isothermal reaction 2h.Continue to add N, N'-diphenyl methane dimaleimide 14.8g, methyl hexahydrophthalic anhydride 9.1g, DMP-30 promotor 0.2g, continue isothermal reaction 0.5h, cooling obtain preparing high tenacity aramid fiber composite material optical fiber strengthen core high tenacity, can the matrix resin of selfreparing.
Adopt the 60g matrix resin of above-mentioned preparation, add the aluminium hydroxide of 2g, the activated Calcium carbonate of 2g, the aluminum stearate of 4g.Pour in glue groove after electric blender stirs, DuPontKevlarK291500D type aramid fiber 160g is selected to be strongthener, after 90 DEG C of bakings, successively through steeping vat impregnation, mould molding, drying tunnel solidification, pressure roller traction and winder rolling flow process.Wherein, steeping vat temperature is 50 DEG C, and die temperature is 115 DEG C, and drying tunnel temperature is 240 DEG C, and pulling speed is 300mm/min, and it is 0.52mm that the aramid fiber composite material tentatively prepared strengthens core diameter, and its tensile strength is 1920MPa, and minimum bend diameter is 12mm.
Tentatively obtained aramid fiber composite material is strengthened core to be positioned in the baking oven of 240 DEG C, and naturally cooling after continuation baking 5h, make high tenacity aramid fiber composite material optical fiber and strengthen core, its tensile strength can be increased to 2034MPa, and minimum bend diameter is lower than 10mm.
Embodiment 3
Be equipped with at 250ml in the there-necked flask of mechanical stirring, thermometer, constant pressure funnel and nitrogen gatherer and add 20g liquid epoxies, limit is stirred and is warming up to 50 DEG C, constant pressure funnel is utilized slowly to be added drop-wise in liquid epoxies by 5g chaff amine in 40min, temperature of reaction controls at about 65 DEG C, isothermal reaction 1h.Continue to add N, N'-diphenyl methane dimaleimide 11g, methyl hexahydrophthalic anhydride 9g, continue isothermal reaction 1h, cooling obtain preparing high tenacity aramid fiber composite material optical fiber strengthen core high tenacity, can the matrix resin of selfreparing.
Adopt the 30g matrix resin of above-mentioned preparation, add the aluminium hydroxide of 4g, the activated Calcium carbonate of 4g, the aluminum stearate of 6g.Pour in glue groove after electric blender stirs, DuPontKevlarK291500D type aramid fiber 120g is selected to be strongthener, after 75 DEG C of bakings, successively through steeping vat impregnation, mould molding, drying tunnel solidification, pressure roller traction and winder rolling flow process.Wherein, steeping vat temperature is 30 DEG C, and die temperature is 95 DEG C, and drying tunnel temperature is 220 DEG C, and pulling speed is 400mm/min, and it is 0.53mm that the aramid fiber composite material tentatively prepared strengthens core diameter, and its tensile strength is 1900MPa, and minimum bend diameter is 13mm.
Tentatively obtained aramid fiber composite material is strengthened core to be positioned in the baking oven of 220 DEG C, and naturally cooling after continuation baking 4h, make high tenacity aramid fiber composite material optical fiber and strengthen core, its tensile strength can be increased to 2010MPa, and minimum bend diameter is lower than 10mm.
Embodiment 4
Be equipped with at 250ml in the there-necked flask of mechanical stirring, thermometer, constant pressure funnel and nitrogen gatherer and add 45g liquid epoxies, limit is stirred and is warming up to 50 DEG C, constant pressure funnel is utilized slowly to be added drop-wise in liquid epoxies by 15g chaff amine in 40min, temperature of reaction controls at about 65 DEG C, isothermal reaction 2h.Continue to add N, N'-diphenyl methane dimaleimide 30g, HHPA 23g, triethylamine promotor 2g, continue isothermal reaction 0.5h, cooling obtain preparing high tenacity aramid fiber composite material optical fiber strengthen core high tenacity, can the matrix resin of selfreparing.
Adopt the 60g matrix resin of above-mentioned preparation, add the aluminium hydroxide of 12g, the activated Calcium carbonate of 12g, the aluminum stearate of 6g.Pour in glue groove after electric blender stirs, DuPontKevlarK291500D type aramid fiber 240g is selected to be strongthener, after 115 DEG C of bakings, successively through steeping vat impregnation, mould molding, drying tunnel solidification, pressure roller traction and winder rolling flow process.Wherein, steeping vat temperature is 60 DEG C, and die temperature is 130 DEG C, and drying tunnel temperature is 260 DEG C, and pulling speed is 500mm/min, and it is 0.52mm that the aramid fiber composite material tentatively prepared strengthens core diameter, and its tensile strength is 1980MPa, and minimum bend diameter is 11mm.
Tentatively obtained aramid fiber composite material is strengthened core to be positioned in the baking oven of 300 DEG C, and naturally cooling after continuation baking 7h, make high tenacity aramid fiber composite material optical fiber and strengthen core, its tensile strength can be increased to 2080MPa, and minimum bend diameter is lower than 10mm.
High tenacity aramid fiber composite material optical fiber prepared by the present invention strengthens core, DuPontKevlar1500D aramid fiber is adopted to be strongthener, prepared matrix material strengthens drawing high intensity and can reaching 2080MPa of core, the 1800MPa that group strengthens core is repaired relative to not adding, improve nearly 15.5%, interlaminar shear strength reaches as high as 71.2MPa, and minimum bend diameter is lower than 10mm.
Claims (9)
1. high tenacity aramid fiber composite material optical fiber strengthens a core, and be made up of aramid fiber, matrix resin, filler and releasing agent, it is characterized in that, described matrix resin comprises the material of following weight part:
Liquid epoxies 20-45 part,
N, N'-diphenyl methane dimaleimide 11-30 part,
Solidifying agent 9-23 part,
Chaff amine 5-15 part,
Promotor 0-2 part.
2. a kind of high tenacity aramid fiber composite material optical fiber according to claim 1 strengthens core, and it is characterized in that, described liquid epoxies is bis-phenol A glycidyl ether type epoxy resin, and epoxy equivalent (weight) is 163g/mol-188g/mol.
3. a kind of high tenacity aramid fiber composite material optical fiber according to claim 1 strengthens core, and it is characterized in that, described solidifying agent is HHPA or methyl hexahydrophthalic anhydride.
4. a kind of high tenacity aramid fiber composite material optical fiber according to claim 1 strengthens core, and it is characterized in that, described promotor is DMP-30 or triethylamine.
5. a kind of high tenacity aramid fiber composite material optical fiber according to claim 1 strengthens core, and it is characterized in that, described aramid fiber is 60-80 part, and matrix resin is 15-30 part, and filler is 2-8 part, and releasing agent is 1-3 part.
6. a kind of high tenacity aramid fiber composite material optical fiber strengthens core according to claim 1 or 5, and it is characterized in that, described filler is at least two kinds in calcium carbonate, aluminium hydroxide, barium sulfate, magnesium hydroxide, aluminum oxide.
7. a kind of high tenacity aramid fiber composite material optical fiber strengthens core according to claim 1 or 5, it is characterized in that, described releasing agent is one or both in tung oil, methyl-silicone oil, aluminum stearate, calcium stearate.
8. the preparation method of a high tenacity aramid fiber composite material optical fiber enhancing core, it is characterized in that, comprise the following steps: 1) in 20-45 part liquid epoxies, add 5-15 part chaff amine, after reaction 1-3h, add 11-30 part N, N'-diphenyl methane dimaleimide, 9-23 part solidifying agent, 0-2 part promotor, obtains matrix resin after continuing to be uniformly mixed; 2) 2-8 part filler is added in the matrix resin obtained in 15-30 part step 1), 1-3 part releasing agent, pour into after stirring in steeping vat, by 60-80 part aramid fiber after drying tunnel prewarming baking, by steeping vat, through mould Procuring sizing after complete viscose glue, drying tunnel solidifies completely, eventually pass pressure roller traction, winder rolling; 3) by step 2) optical fiber that goes out of pultrusion strengthens core and is positioned in the baking oven of 220 DEG C-300 DEG C, baking 4h-7h, after naturally cooling cooling, obtain aramid fiber composite material optical fiber and strengthen core.
9. a kind of high tenacity aramid fiber composite material optical fiber according to claim 8 strengthens the preparation method of core, it is characterized in that, step 2) in aramid fiber preheating drying tunnel temperature be 75 DEG C-115 DEG C, steeping vat temperature is 30 DEG C-60 DEG C, die temperature is 95 DEG C-130 DEG C, the temperature of solidification drying tunnel is 220 DEG C-260 DEG C, and rolling speed is 300mm/min-500mm/min.
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| CN106896459A (en) * | 2017-03-21 | 2017-06-27 | 海安南京大学高新技术研究院 | Selfreparing optical cable enhancing core containing microcapsules and preparation method thereof |
| CN107037550A (en) * | 2017-03-21 | 2017-08-11 | 海安南京大学高新技术研究院 | Aramid fiber enhancing core of self-repair function and preparation method thereof |
| CN107955306A (en) * | 2017-11-22 | 2018-04-24 | 郑州天舜电子技术有限公司 | A kind of plastic optical fiber and its preparation method and application |
| CN108559224A (en) * | 2016-12-12 | 2018-09-21 | 苏州大学 | Self-repair type can remold the preparation method of the multiple deformation thermoset shape memory resin system of shape |
| CN109505131A (en) * | 2018-11-29 | 2019-03-22 | 安徽牡东通讯光缆有限公司 | A kind of optical cable selfreparing aramid fiber strengthening core and preparation method thereof |
| CN109518466A (en) * | 2018-11-29 | 2019-03-26 | 安徽牡东通讯光缆有限公司 | A kind of optical cable strengthening core and preparation method thereof |
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| CN113831688A (en) * | 2021-09-30 | 2021-12-24 | 山东天畅环保科技股份有限公司 | Door and window profile made of aramid fiber reinforced composite material |
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| CN109505131B (en) * | 2018-11-29 | 2021-10-08 | 安徽牡东通讯光缆有限公司 | Self-repairing aramid fiber reinforced core for optical cable and preparation method thereof |
| CN113930047A (en) * | 2020-07-14 | 2022-01-14 | 北京化工大学 | Hot-weldable heat-recoverable epoxy fireproof plate and preparation method thereof |
| CN113930047B (en) * | 2020-07-14 | 2022-07-29 | 北京化工大学 | Heat-weldable heat-repairable epoxy fireproof plate and preparation method thereof |
| CN112048905A (en) * | 2020-07-24 | 2020-12-08 | 福建创立佳科技有限公司 | Environment-resistant aramid fiber composite core and preparation method thereof |
| CN113831688A (en) * | 2021-09-30 | 2021-12-24 | 山东天畅环保科技股份有限公司 | Door and window profile made of aramid fiber reinforced composite material |
| CN113897028A (en) * | 2021-10-22 | 2022-01-07 | 中国林业科学研究院林产化学工业研究所 | Tung oil-based interpenetrating network type shape memory polymer and preparation method thereof |
| CN113897028B (en) * | 2021-10-22 | 2024-04-16 | 中国林业科学研究院林产化学工业研究所 | Tung oil-based interpenetrating network shape memory polymer and preparation method thereof |
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