CN103361764A - Rare-earth-silicate long-red-afterglow colored polyester fiber - Google Patents

Rare-earth-silicate long-red-afterglow colored polyester fiber Download PDF

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Publication number
CN103361764A
CN103361764A CN 201210086916 CN201210086916A CN103361764A CN 103361764 A CN103361764 A CN 103361764A CN 201210086916 CN201210086916 CN 201210086916 CN 201210086916 A CN201210086916 A CN 201210086916A CN 103361764 A CN103361764 A CN 103361764A
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China
Prior art keywords
afterglow
rare earth
magnesium silicate
fiber
luminescent
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CN 201210086916
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Chinese (zh)
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罗军
高大海
李永贵
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Jiangnan University
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Jiangnan University
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Priority to CN 201210086916 priority Critical patent/CN103361764A/en
Publication of CN103361764A publication Critical patent/CN103361764A/en
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Abstract

The invention relates to rare-earth-silicate long-red-afterglow colored polyester fiber and a preparation method thereof. The fiber is characterized by being prepared from the following raw materials in percentage by weight: 89-96% of polyester spinning raw material, 3-10% of rare-earth magnesium silicate luminescent material, 0.6-1.0% of color master batch and a trace amount of functional assistants; and POY (Pre-Oriented Yarn) is prepared through proportionally mixing the raw materials, 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 polyester fiber prepared by the method disclosed by the invention has the advantages that various colors are shown without dyeing, red afterglow with the wavelength of 600-750 nm is emitted after the polyester fiber is irradiated by sunlight or fluorescent light for 1-10 min, the initial brightness of the afterglow is 2-3cd/m<2>, and the service life of the afterglow reaches 4-6 h; and the luminescent fiber is non-toxic and harmless and is free of any adverse effect on human bodies and environment.

Description

Rare earth silicate red long-afterglow color polyester
Technical field
The present invention relates to textile product and technical field, specifically a kind of rare earth magnesium silicate red long-afterglow colorful polyester fiber and preparation method thereof.
Background technology
Long-persistence luminous fiber also claims luminous fiber, is a kind of take terylene, polyamide fibre or polypropylene fibre 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 method of rare earth silicate red long-afterglow colorful polyester fiber, and utilize the method to prepare rare earth magnesium silicate red long-afterglow color polyester.This fiber need not dyeing can present shades of colour, and behind daylight or fluorescence irradiation 1~10min, sending wavelength is the red twilight sunset of 600~750nm, and the twilight sunset life-span reaches 4~6 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 stated polyesters section under 100~120 ℃ the temperature behind 15~25 hours drying, by the ratio adding particle diameter of the 20~35wt% MgSiO less than 10um 3: Eu 2+, Dy 3+, Mn 2+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 240~260 ℃ 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 Masterbatch, polyester slice are mixed with spinning material in proportion, so that contain the rare earth magnesium silicate luminescent material of 3~10wt% and the Masterbatch of 0.8~1.0wt%, the polyester composition of 89~96wt% in the final spinning material, under 100~120 ℃ the temperature behind 15~25 hours drying, in screw extruder with 280~300 ℃ melt temperature, 3000~3300 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 polyester 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 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 luminescent material as the light emitting source of fiber.Rare earth magnesium silicate 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 stated polyesters section under 120 ℃ the temperature behind 15 hours drying, ratio in 20wt% adds rare earth magnesium silicate 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 245 ℃ 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 spinning special polyester chip of above-mentioned manufacturing are mixed with spinning material by 1: 4 mass ratio, and the Masterbatch of adding 0.6wt%, under 120 ℃ the temperature behind 15 hours drying, in screw extruder with 280 ℃ melt temperature, 3200 m/mins winding speed carries out spinning silk winding, makes rare earth luminous POY long filament.
Embodiment two
With stated polyesters section under 110 ℃ the temperature behind 20 hours drying, ratio in 25wt% adds rare earth magnesium silicate 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 250 ℃ 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;
The luminous master batch of above-mentioned manufacturing is mixed with spinning material with large bright yarn section by 1: 3.5 mass ratio, the Masterbatch that adds 0.8wt%, under 110 ℃ the temperature behind 20 hours drying, in screw extruder with 290 ℃ melt temperature, 3100 m/mins winding speed carries out spinning silk winding, 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 polyester DTY long filament.
Embodiment three
With stated polyesters section under 100 ℃ the temperature behind 25 hours drying, ratio in 30wt% adds rare earth magnesium silicate 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 255 ℃ 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;
The luminous master batch of above-mentioned manufacturing is mixed with spinning material with large bright yarn section by 1: 3 mass ratio, and the Masterbatch of adding 1.0wt%, under 100 ℃ the temperature behind 25 hours drying, in screw extruder with 285 ℃ melt temperature, 3000 m/mins winding speed carries out spinning silk winding, makes rare earth luminous POY long filament.

Claims (6)

1. rare earth magnesium silicate red long-afterglow color polyester, it is characterized in that: this fiber is made of the Direct-spinning of PET Fiber raw material of 89~96wt%, the rare earth magnesium silicate luminescent material of 3~10wt%, Masterbatch and the micro-function additive of 0.6~1.0wt%; This fiber need not dyeing and namely presents shades of colour, through daylight or fluorescence excitation, sends red twilight sunset, and this luminescent fibre is nontoxic, without radiocontamination, to human body and environment without any harmful effect.
2. color polyester luminescent fibre according to claim 1, it is characterized in that: described rare earth magnesium silicate luminescent material is MgSiO 3: Eu 2+, Dy 3+, Mn 2+, matrix is the magnesium silicate crystalline phase, particle diameter is less than 10um.
3. terylene 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. terylene 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 250nm~500nm.
5. according to claim 1 with 4, described terylene luminescent fibre can be by behind daylight or the fluorescence irradiation 1~10min, and sending wavelength is the red twilight sunset of 500~750nm, and its twilight sunset initial strength is 2~3cd/m 2, the twilight sunset life-span is 4~6 hours.
6. according to claim 1,2,3, a kind of preparation method of rare earth magnesium silicate red long-afterglow color polyester, it is characterized in that: with stated polyesters section under 100~120 ℃ of temperature behind 15~25 hours drying, ratio in 20~35wt% adds rare earth magnesium silicate luminescent material, add various nanoscale function additives in the described ratio of claim 3 again, then luminous master batch is made in melting under 240~260 ℃ temperature, Cast Strip, pelletizing.
Above-mentioned luminous master batch and Masterbatch, polyester slice are prepared in proportion, so that contain the rare earth magnesium silicate luminescent material of 3~10wt%, the Masterbatch of 0.6~1.0wt% and the polyester composition of 89~96wt% in the final spinning material, under 100~120 ℃ of temperature behind 15~25 hours drying, in screw extruder, carry out spinning silk winding with 280~300 ℃ melt temperature, 3000~3300 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.
CN 201210086916 2012-03-29 2012-03-29 Rare-earth-silicate long-red-afterglow colored polyester fiber Pending CN103361764A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104404648A (en) * 2014-12-17 2015-03-11 浙江华峰氨纶股份有限公司 Preparation method of rare earth aluminate polyurethane elastic fiber capable of emitting long blue afterglow
CN106758149A (en) * 2016-12-01 2017-05-31 西南大学 The preparation method of long afterglow emitting red light dacron

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104404648A (en) * 2014-12-17 2015-03-11 浙江华峰氨纶股份有限公司 Preparation method of rare earth aluminate polyurethane elastic fiber capable of emitting long blue afterglow
CN106758149A (en) * 2016-12-01 2017-05-31 西南大学 The preparation method of long afterglow emitting red light dacron

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Application publication date: 20131023