CN103361760A - Rare-earth-silicate long-blue-afterglow luminescent polyamide fiber and preparation process thereof - Google Patents
Rare-earth-silicate long-blue-afterglow luminescent polyamide fiber and preparation process thereof Download PDFInfo
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- CN103361760A CN103361760A CN 201210086891 CN201210086891A CN103361760A CN 103361760 A CN103361760 A CN 103361760A CN 201210086891 CN201210086891 CN 201210086891 CN 201210086891 A CN201210086891 A CN 201210086891A CN 103361760 A CN103361760 A CN 103361760A
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Abstract
The invention relates to rare-earth-silicate long-blue-afterglow polyamide fiber and a preparation method thereof. The fiber is characterized by being prepared from the following raw materials in percentage by weight: 90-96% of polyamide spinning raw material, 3-10% of rare-earth magnesium/strontium silicate luminescent material and lower than 1% of nano functional assistants; and POY (Pre-Oriented Yarn) is prepared through proportionally mixing luminescent master batch, prepared from the raw materials, with polyamide slices, baking for a certain time at certain temperature, using a special spinning process and carrying out spinning winding by using a screw extruder, and DTY (Draw Textured Yarn) or FDY (Fully Drawn Yarn) can be prepared from the POY through draw texturing or drawing. The polyamide fiber prepared by the method disclosed by the invention has the advantages that blue afterglow with the wavelength of 435-500 nm can be emitted after the polyamide fiber is irradiated by sunlight or fluorescent light, the initial strength of the afterglow is 2-3cd/m<2>, and the service life of the afterglow can reach 10-15 h; and the luminescent fiber is non-toxic and harmless and is free of any adverse effect on human bodies and environment.
Description
Technical field
The present invention relates to textile product and technical field, specifically a kind of rare earth magnesium silicate strontium blue long afterflow polyamide luminescent fibre and preparation technology thereof.
Background technology
Long-persistence luminous fiber also claims luminous fiber, is a kind of take terylene, polyamide fibre or nylon resin as base material, by adding rare earth long-afterglow luminescent material, nanoscale function additive, and the photic accumulating type luminescent fibre of making through special spinning technique.This fiber green, environmental protection, energy-conservation can be widely used in the fields such as aviation and navigation, national defense industry, building decoration, communications and transportation, night work and dress ornament.The luminous fiber of commercially producing at present mainly is the rare earth aluminate luminescent fibre, this fibrid has good long afterglow performance, chemical property is more stable, but shortcoming also clearly: resistance to water is relatively poor, glow color is more single, and the after-treatment of light-emitting particles (coating such as the surface) is increased cost, affects luminous efficiency.Therefore, the application of rare earth aluminate luminous fiber is subject to larger restriction.
Development along with rare earth long-afterglow luminescent material research, the afterglow property of silicates luminescent material is near aluminate, and present from blue light luminous to ruddiness continually varying multiple color, the scope of exciting light reaches 200nm～500nm, the silicate long-afterglow material has good chemical stability, water-fast dissolubility and heat endurance in addition, low price, cost is low, therefore, exploitation rare earth silicate luminous fiber can effectively remedy the deficiency of aluminate luminous fiber, greatly expands the range of application of RE luminous fiber.
Summary of the invention
The objective of the invention is to seek a kind of preparation technology of rare earth silicate polyamide luminescent fibre, and under this technique, prepare rare earth magnesium silicate strontium blue long afterflow polyamide fiber.This fiber can be behind daylight or fluorescence irradiation 1～10min, and sending wavelength is the blue twilight sunset of 435～500nm, and the twilight sunset life-span reaches 10～15 hours.And this fiber is nontoxic, and human body and environment without any harm, are belonged to the environment-friendly and green fiber.
The main technical schemes of its preparation is: with the special-purpose polyamide section of spinning under 100～120 ℃ the temperature behind 15～20 hours drying, by the ratio adding particle diameter of the 20～35wt% Sr less than 10um
2MgSi
2O
7: Eu
2+, Dy
3+Luminescent material, add again flow stabilizing agent 0.01～0.03wt%, oxidation stabilizers 0.02～0.04wt%, antioxidant 0.01～0.05wt%, crosslinking agent 0.03～0.04wt%, dispersant 0.1～0.5wt%, then melting under 180～220 ℃ temperature, Cast Strip, pelletizing, make master batch, the stabilizing agent that wherein flows, oxidation stabilizers, antioxidant, crosslinking agent, dispersant are the nanoscale auxiliary agent.
Above-mentioned luminous master batch and polyamide section are mixed with spinning material in proportion, so that contain the rare earth magnesium silicate strontium luminescent material of 3～10wt% and the polyamide composition of 90～96wt% in the final spinning material, under 100～120 ℃ the temperature behind 15～20 hours drying, in screw extruder with 220～280 ℃ melt temperature, 2500～3000 m/mins winding speed carries out spinning silk winding, make rare earth luminous POY long filament, this POY silk can be made the DTY silk or make the FDY silk through drawing-off through adding bullet.
Rare earth magnesium silicate strontium polyamide fiber of the present invention belongs to a kind of photic accumulating type luminescent fibre, and its principle of luminosity is: rare earth luminescent fiber under visible light or ultraviolet excitation, the Eu in the rare earth material
2+The 4f of ion
7The ground state electronics is excited to 4f
65d
1Upper state, excite stop after, be subjected to magnesium silicate strontium lattice heat disturbance action, electronics in a large amount of shallow trap energy levels is escaped rapidly and is returned ground state, form initial twilight sunset (luminous), and the electron number in the deep trap energy level is few, Escape Probability is little, finally forms the long afterglow phenomenon.
The invention has the advantages that:
(1) adopt rare earth magnesium silicate strontium luminescent material as the light emitting source of fiber.Rare earth magnesium silicate strontium luminescent material has good chemical stability, water-fast dissolubility and heat endurance than aluminate luminescent material, as raw-material high-purity Si O
2Low price, be easy to get, preparation cost is low, and this material is "dead", and is harmless to human-body safety.
Adding nanoscale function additive and particle diameter are the ultra-fine luminescent powder of 1～10um when (2) making luminous master batch, make each component have good dispersiveness and stable in luminous master batch, have guaranteed the continuous spinnability of fiber.
(3) when preparation POY silk, adopted conventional lower melt temperature, reduced the impact that long-chain molecule in the fiber is subjected to high temperature degradation, guaranteed the mechanical mechanics property of fiber.
The specific embodiment
Embodiment one
With polyamide section under 100 ℃ the temperature behind 19 hours drying, ratio in 30wt% adds rare earth magnesium silicate strontium luminescent powder, add again the stabilizing agent glycerine monofatty ester 0.03% that flows, oxidation stabilizers triphenyl phosphite 0.04%, ultraviolet (UV) resistant agent benzotriazole 0.05%, crosslinking agent trimethylol-propane trimethacrylate 0.04%, dispersant barium stearate 0.3%, then melting under 200 ℃ temperature, the Cast Strip, pelletizing, make master batch, wherein by mobile stabilizing agent, oxidation stabilizers, ultraviolet (UV) resistant agent, the auxiliary agent that crosslinking agent forms is nanoscale;
Luminous master batch and the polyamide section of above-mentioned manufacturing are mixed with spinning material by 1: 3 mass ratio, under 100 ℃ the temperature behind 19 hours drying, with 260 ℃ melt temperature, 2900 m/mins winding speed carries out spinning silk winding in screw extruder, makes rare earth luminous POY long filament.
Embodiment two
With polyamide section under 110 ℃ the temperature behind 17 hours drying, ratio in 25wt% adds rare earth magnesium silicate strontium luminescent powder, add again the stabilizing agent glycerine monofatty ester 0.02% that flows, oxidation stabilizers triphenyl phosphite 0.03%, ultraviolet (UV) resistant agent benzotriazole 0.03%, crosslinking agent trimethylol-propane trimethacrylate 0.03%, dispersant barium stearate 0.2%, then melting under 190 ℃ temperature, the Cast Strip, pelletizing, make master batch, wherein by mobile stabilizing agent, oxidation stabilizers, ultraviolet (UV) resistant agent, the auxiliary agent that crosslinking agent forms is nanoscale;
Luminous master batch and the polyamide section of above-mentioned manufacturing are mixed with spinning material by 1: 3.5 mass ratio, under 110 ℃ the temperature behind 17 hours drying, with 240 ℃ melt temperature, 2700 m/mins winding speed carries out spinning silk winding in screw extruder, makes rare earth luminous POY long filament.
Again above-mentioned POY fiber is processed at high-speed stretch yarn machine, wherein going up heater temperature is 180 ℃, lower heater temperature is 160 ℃, and owing doubly is 1.65, and false twisting friction plate speed is 1.8 with the ratio of silk speed, the speed of a motor vehicle is 600 m/mins, one underfeed is that-8.5%, two underfeeds are-5%, and the oil tanker rotating speed is 1.8 rev/mins, false twister is combined as in the situation of 1-6-1 and adds bullet, makes polyamide DTY long filament.
Embodiment three
With the special-purpose polyamide section of spinning under 120 ℃ the temperature behind 15 hours drying, ratio in 20wt% adds rare earth magnesium silicate strontium luminescent powder, add again the stabilizing agent glycerine monofatty ester 0.01% that flows, oxidation stabilizers triphenyl phosphite 0.02%, ultraviolet (UV) resistant agent benzotriazole 0.01%, crosslinking agent trimethylol-propane trimethacrylate 0.03%, dispersant barium stearate 0.1%, then melting under 185 ℃ temperature, the Cast Strip, pelletizing, make master batch, wherein by mobile stabilizing agent, oxidation stabilizers, ultraviolet (UV) resistant agent, the auxiliary agent that crosslinking agent forms is nanoscale;
Luminous master batch and the polyamide section of above-mentioned manufacturing are mixed with spinning material by 1: 4 mass ratio, under 120 ℃ the temperature behind 15 hours drying, with 220 ℃ melt temperature, 2500 m/mins winding speed carries out spinning silk winding in screw extruder, makes rare earth luminous POY long filament.
Claims (6)
1. rare earth magnesium silicate strontium blue long afterflow polyamide fiber, it is characterized in that: this fiber consists of by the rare earth magnesium silicate strontium luminescent material of the polyamide spinning material of 90～96wt%, 3～10wt% and less than the nano functional auxiliary agent of 1wt%, this fiber can be through daylight or fluorescence excitation, send blue long afterflow, and this luminescent fibre is nontoxic, without radiocontamination, to human body and environment without any harmful effect.
2. polyamide luminescent fibre according to claim 1, it is characterized in that: described rare earth magnesium silicate strontium luminescent material is Sr
2MgSi
2O
7: Eu
2+, Dy
3+, matrix is magnesium silicate strontium crystalline phase, particle diameter is less than 10um.
3. polyamide luminescent fibre according to claim 1 is characterized in that: the nano functional auxiliary agent in the luminous master batch comprises flow stabilizing agent 0.01～0.03wt%, oxidation stabilizers 0.02～0.04wt%, antioxidant 0.01～0.05wt%, crosslinking agent 0.03～0.04wt%, dispersant 0.1～0.5wt%.
4. polyamide luminescent fibre according to claim 1, it is characterized in that: the excitation wavelength of described luminescent fibre is positioned at the Uv and visible light scope of 300nm～500nm.
5. according to claim 1 with 4, described polyamide luminescent fibre can be by behind daylight or the fluorescence irradiation 1～10min, and sending wavelength is the blue twilight sunset of 435～500nm, and its twilight sunset initial strength is 2～3cd/m
2, the twilight sunset life-span is 10～15 hours.
6. according to claim 1,2,3, a kind of preparation method of rare earth magnesium silicate strontium blue long afterflow polyamide fiber, it is characterized in that: with the special-purpose polyamide section of spinning under 100～120 ℃ of temperature behind 15～20 hours drying, ratio in 20～35wt% adds rare earth magnesium silicate strontium luminescent material, add various nanoscale function additives in the described ratio of claim 3 again, then luminous master batch is made in melting under 180～220 ℃ temperature, Cast Strip, pelletizing.
With above-mentioned luminous master batch and in proportion preparation of polyamide section, so that contain the rare earth magnesium silicate strontium luminescent material of 3～10wt% and the polyamide composition of 90～96wt% in the final spinning material, under 100～120 ℃ of temperature behind 15～20 hours drying, in screw extruder, carry out spinning silk winding with 220～280 ℃ melt temperature, 2500～3000 m/mins winding speed, make the POY silk, this POY silk can be made the DTY silk or make the FDY silk through drawing-off through adding bullet.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882556A (en) * | 2014-03-18 | 2014-06-25 | 闽江学院 | Composite noctilucent fiber with skin-core structure and preparation method of composite noctilucent fiber |
| CN104164082A (en) * | 2014-06-30 | 2014-11-26 | 江苏旭华圣洛迪建材有限公司 | Preparing method of light-storage type luminescent wood-plastic composite |
| CN109913972A (en) * | 2019-03-07 | 2019-06-21 | 苏州经贸职业技术学院 | A kind of luminous composite fibre and preparation method thereof, a kind of luminous work clothes |
| CN114808188A (en) * | 2022-04-11 | 2022-07-29 | 闽江学院 | Blue-green double-color spontaneous optical fiber and preparation method thereof |
-
2012
- 2012-03-29 CN CN 201210086891 patent/CN103361760A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103882556A (en) * | 2014-03-18 | 2014-06-25 | 闽江学院 | Composite noctilucent fiber with skin-core structure and preparation method of composite noctilucent fiber |
| CN104164082A (en) * | 2014-06-30 | 2014-11-26 | 江苏旭华圣洛迪建材有限公司 | Preparing method of light-storage type luminescent wood-plastic composite |
| CN109913972A (en) * | 2019-03-07 | 2019-06-21 | 苏州经贸职业技术学院 | A kind of luminous composite fibre and preparation method thereof, a kind of luminous work clothes |
| CN114808188A (en) * | 2022-04-11 | 2022-07-29 | 闽江学院 | Blue-green double-color spontaneous optical fiber and preparation method thereof |
| CN114808188B (en) * | 2022-04-11 | 2023-12-15 | 闽江学院 | Blue-green double-color self-luminous fiber and preparation method thereof |
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Application publication date: 20131023 |