CN103866419A - Europium-doped yttrium oxysulfide red long afterglow color terylene - Google Patents
Europium-doped yttrium oxysulfide red long afterglow color terylene Download PDFInfo
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- CN103866419A CN103866419A CN201210524074.6A CN201210524074A CN103866419A CN 103866419 A CN103866419 A CN 103866419A CN 201210524074 A CN201210524074 A CN 201210524074A CN 103866419 A CN103866419 A CN 103866419A
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- yttrium oxysulfide
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Abstract
The invention relates to a rare earth yttrium oxysulfide red long afterglow color fiber and a preparation method. The rare earth yttrium oxysulfide red long afterglow color fiber is composed of 89-96wt% of polyester spinning raw material, 3-10wt% of rare earth yttrium oxysulfide luminescent material, 0.6-1.0wt% of color master batch and microscale nano functional auxiliary agent. The preparation method comprises the following steps: mixing luminescent master batch, color master batch and spinning grade polyester slices in proportion, after drying for a certain time and a certain temperature, using a screw extruder for spinning and reeling through a special spinning technology to prepare POY filament, and texturing the POY filament to prepare DTY filament or preparing the FDY filament through drafting. The polyester fiber prepared by the method can present various colors without dyeing, irradiation for 1-10 minutes through daylight or fluorescence is carried out, the red afterglow with wavelength of 600-720nm is emitted, the afterglow initial intensity is 2-3cd/m<2>, the afterglow life can reach 4-6 hours, the luminescent fiber is innocuous and unpoisonous, and has no adverse influence on human body and environment.
Description
Technical field
The present invention relates to textile product and technical field, specifically a kind of rare earth yttrium oxysulfide red long-afterglow polyester colored 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, 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 producing is at present mainly to send blueness and yellow-green light as main, and the luminescent properties such as its luminosity and persistence have reached the needs of practical application, and have realized suitability for industrialized production.And red long-afterglow fiber is always in development, be mainly that the performance indications such as its persistence and brightness exist larger gap with blue and yellow green material, cannot reach the requirement of practical application.
Along with rare earth long-afterglow luminescent material progress of research, the afterglow property of red long afterglow luminous material has obtained compared with quantum jump, particularly rare earth yttrium oxysulfide luminescent material, its main emission peak is positioned near 627nm, presents pure red luminously, reaches persistence more than 5 hours, the scope of exciting light is also very wide, reach 200nm～500nm, substantially can meet the needs of practical application, and start to commercially produce.Therefore, developing rare-earth red luminous fiber has become possibility, and this kind of photochromic luminous fiber can effectively make up the photochromic deficiency of existing luminous fiber, greatly expands the range of application of RE luminous fiber.
Summary of the invention
The object of the invention is to seek a kind of preparation method of rare earth yttrium oxysulfide red long-afterglow polyester colored fiber, and utilize the method to prepare the colorful fiber of rare earth yttrium oxysulfide red long-afterglow polyester.This fiber can present shades of colour without dyeing, irradiates after 1～10min through daylight or fluorescence, and sending wavelength is the red twilight sunset of 600～720nm, and the twilight sunset life-span reaches 4～6 hours.And this fiber is nontoxic, human body and environment, without any harm, are belonged to environment-friendly and green fiber.
Its main technical schemes of preparing is: by stated polyesters section at the temperature of 100～120 ℃ after the drying of 15～25 hours, add particle diameter to be less than the Y of 10um in the ratio of 20～35wt%
2o
2s:Eu
3+, Mg
2+, Ti
4+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 at the temperature of 240～260 ℃, Cast Strip, pelletizing, make master batch, the stabilizing agent that wherein flows, oxidation stabilizers, antioxidant, crosslinking agent, dispersant are nanoscale auxiliary agent.
Above-mentioned luminous master batch and Masterbatch, polyester slice are mixed with to spinning material in proportion, the rare earth yttrium oxysulfide luminescent material that makes to contain 3～10wt% in final spinning material and the Masterbatch of 0.8～1.0wt%, the polyester composition of 89～96wt%, at the temperature of 100～120 ℃ after the drying of 15～25 hours, in screw extruder with the melt temperature of 280～300 ℃, the winding speed of 3000～3300 ms/min carries out spinning silk winding, make rare earth luminous POY long filament, this POY silk can be made DTY silk or make FDY silk through drawing-off through adding bullet.
Rare earth yttrium oxysulfide 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 ray or ultraviolet excitation, the Eu in rare earth material
2+the 4f of ion
7ground state electronics is excited to 4f
65d
1upper state, after exciting and stopping, being subject to yttrium oxysulfide lattice heat disturbance action, electronics in a large amount of shallow trap energy levels is escaped and is returned to ground state rapidly, forms initial twilight sunset (luminous), and electron number in deep trap energy level is few, short time Escape Probability is little, finally forms long afterglow phenomenon.
The invention has the advantages that:
(1) adopt the light emitting source of rare earth yttrium oxysulfide luminescent material as fiber.The main emission peak of this luminescent material is positioned near 627nm, presents pure red luminously, and the scope of exciting light is wider, reaches 200nm～500nm, and this material is "dead", harmless to human-body safety.
(2) while making luminous master batch, adding nanoscale function additive and particle diameter is the ultra-fine luminescent powder of 1～10um, makes each component in luminous master batch, have good dispersiveness and stability, has guaranteed the continuous spinnability of fiber.
(3) in the time of preparation POY silk, adopt more conventional lower melt temperature, reduced long-chain molecule in fiber and be subject to the impact of high temperature degradation, guaranteed the mechanical mechanics property of fiber.
The specific embodiment
Embodiment mono-
By stated polyesters section at the temperature of 120 ℃ after the drying of 15 hours, add rare earth yttrium oxysulfide luminescent powder in the ratio of 20wt%, 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 at the temperature of 245 ℃, Cast Strip, pelletizing, make master batch, wherein by mobile stabilizing agent, oxidation stabilizers, ultraviolet (UV) resistant agent, the auxiliary agent of crosslinking agent composition is nanoscale,
The luminous master batch of above-mentioned manufacture and spinning special polyester chip are mixed with to spinning material by 1: 4 mass ratio, and add the Masterbatch of 0.7wt%, at the temperature of 120 ℃ after the drying of 15 hours, in screw extruder with the melt temperature of 280 ℃, the winding speed of 3200 ms/min carries out spinning silk winding, makes rare earth luminous POY long filament.
Embodiment bis-
By stated polyesters section at the temperature of 110 ℃ after the drying of 20 hours, add rare earth yttrium oxysulfide luminescent powder in the ratio of 25wt%, 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 at the temperature of 250 ℃, Cast Strip, pelletizing, make master batch, wherein by mobile stabilizing agent, oxidation stabilizers, ultraviolet (UV) resistant agent, the auxiliary agent of crosslinking agent composition is nanoscale,
The luminous master batch of above-mentioned manufacture and large bright yarn section are mixed with to spinning material by 1: 3.5 mass ratio, and add the Masterbatch of 1.0wt%, at the temperature of 110 ℃ after the drying of 20 hours, in screw extruder with the melt temperature of 290 ℃, the winding speed of 3100 ms/min carries out spinning silk winding, makes rare earth luminous POY long filament.
Again above-mentioned POY fiber is processed on high-speed stretch yarn machine, wherein going up heater temperature is 180 ℃, lower heater temperature is 160 ℃, and owing is doubly 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 ms/min, one underfeed is that-8.5%, two underfeeds are-5%, and oil tanker rotating speed is 1.8 revs/min, false twister is combined as in the situation of 1-6-1 and adds bullet, makes polyester DTY long filament.
Embodiment tri-
By stated polyesters section at the temperature of 100 ℃ after the drying of 25 hours, add rare earth yttrium oxysulfide luminescent powder in the ratio of 30wt%, 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 at the temperature of 255 ℃, Cast Strip, pelletizing, make master batch, wherein by mobile stabilizing agent, oxidation stabilizers, ultraviolet (UV) resistant agent, the auxiliary agent of crosslinking agent composition is nanoscale,
The luminous master batch of above-mentioned manufacture and large bright yarn section are mixed with to spinning material by 1: 3 mass ratio, and add the Masterbatch of 0.8wt%, at the temperature of 100 ℃ after the drying of 25 hours, in screw extruder with the melt temperature of 285 ℃, the winding speed of 3000 ms/min carries out spinning silk winding, makes rare earth luminous POY long filament.
Claims (6)
1. a rare earth yttrium oxysulfide color polyester luminescent fibre, is characterized in that: this fiber is made up of the Direct-spinning of PET Fiber raw material of 90～96wt%, the rare earth yttrium oxysulfide luminescent material of 3～10wt%, Masterbatch and the micro-function additive of 0.6～1.0wt%; This fiber presents shades of colour without dyeing, through daylight or fluorescence excitation, sends red long-afterglow, and this luminescent fibre is nontoxic, without radiocontamination, to human body and environment without any harmful effect.
2. colorful polyester luminescent fibre according to claim 1, is characterized in that: described rare earth yttrium oxysulfide luminescent material is Y
2o
2s:Eu
3+, Mg
2+, Ti
4+, matrix is yttrium oxysulfide crystalline phase, particle diameter is less than 10um.
3. colorful polyester luminescent fibre according to claim 1, is characterized in that: the nano functional auxiliary agent in 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. polyester luminescent fibre according to claim 1, is characterized in that: the excitation wavelength of described luminescent fibre is positioned at the Uv and visible light scope of 200nm～500nm.
5. according to claim 1 and 4, described polyester luminescent fibre can be irradiated after 1～10min by daylight or fluorescence, and sending wavelength is the red twilight sunset of 600～720nm, 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 yttrium oxysulfide red long-afterglow polyester colored fiber, it is characterized in that: by stated polyesters section at 100～120 ℃ of temperature after the drying of 15～25 hours, add rare earth yttrium oxysulfide luminescent material in the ratio of 20～35wt%, add various nanoscale function additives in ratio described in claim 3 again, then melting at the temperature of 240～260 ℃, Cast Strip, pelletizing, makes luminous master batch.
Above-mentioned luminous master batch and Masterbatch, polyester slice are prepared in proportion, make the rare earth yttrium oxysulfide luminescent material, the Masterbatch of 0.6～1.0wt% and the polyester composition of 89～96wt% that in final spinning material, contain 3～10wt%, at 100～120 ℃ of temperature after the drying of 15～25 hours, in screw extruder, carry out spinning silk winding with the melt temperature of 280～300 ℃, the winding speed of 3000～3300 ms/min, make POY silk, this POY silk can be made DTY silk or make FDY silk through drawing-off through adding bullet.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210524074.6A CN103866419A (en) | 2012-12-10 | 2012-12-10 | Europium-doped yttrium oxysulfide red long afterglow color terylene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210524074.6A CN103866419A (en) | 2012-12-10 | 2012-12-10 | Europium-doped yttrium oxysulfide red long afterglow color terylene |
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| CN103866419A true CN103866419A (en) | 2014-06-18 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105671676A (en) * | 2016-02-02 | 2016-06-15 | 闽江学院 | Graphene reinforced luminescent polyester fiber and preparation method thereof |
| CN107675322A (en) * | 2017-11-09 | 2018-02-09 | 浙江花小匠网络科技有限公司 | A kind of long-afterglow fluorescent composite filament |
| CN107987277A (en) * | 2017-11-27 | 2018-05-04 | 长沙新材料产业研究院有限公司 | A kind of X-ray luminescence composite polyimide material and preparation method thereof |
| CN108796656A (en) * | 2018-07-06 | 2018-11-13 | 上海曙雀贸易有限公司 | A kind of high-performance of dopen Nano yttrium oxide is anti-fake, can trace to the source yarn |
-
2012
- 2012-12-10 CN CN201210524074.6A patent/CN103866419A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105671676A (en) * | 2016-02-02 | 2016-06-15 | 闽江学院 | Graphene reinforced luminescent polyester fiber and preparation method thereof |
| CN107675322A (en) * | 2017-11-09 | 2018-02-09 | 浙江花小匠网络科技有限公司 | A kind of long-afterglow fluorescent composite filament |
| CN107987277A (en) * | 2017-11-27 | 2018-05-04 | 长沙新材料产业研究院有限公司 | A kind of X-ray luminescence composite polyimide material and preparation method thereof |
| CN108796656A (en) * | 2018-07-06 | 2018-11-13 | 上海曙雀贸易有限公司 | A kind of high-performance of dopen Nano yttrium oxide is anti-fake, can trace to the source yarn |
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Application publication date: 20140618 |