CN105780169A - Preparation method of long afterglow fluorescent fibers emitting red light - Google Patents
Preparation method of long afterglow fluorescent fibers emitting red light Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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Abstract
The invention relates to a preparation method of long afterglow fluorescent fibers emitting red light. The method is characterized by comprising the following steps: (1) mixing a titanate coupling agent, anhydrous alcohol, a light conversion agent of a xanthene structure and a fluorescent material, conducting heating and reaction in the high-speed dispersion state, filtering after reacting, fully washing with the anhydrous alcohol, drying and crushing to obtain a light conversion agent/fluorescent material composite; (2) drying PET powder in a vacuum oven to be premixed with the light conversion agent/fluorescent material composite to obtain a fluorescence fiber masterbatch material; (3) after the fluorescence fiber masterbatch material is dried, using a double-screw extruder to carry out melting and granulating to manufacture spinning masterbatches; (4) uniformly mixing PET masterbatches with the spinning masterbatches, carrying out melt spinning after drying, extruding, drafting and winding to prepare the long afterglow fluorescent fibers which can emit red light. According to the invention, the bonding force with PET macromolecules as fiber base materials is increased and the fiber material which has good dispersion and long afterglow fluorescence and emits the red light is obtained.
Description
Technical field
The preparation method that the present invention relates to a kind of long-afterglow fluorescent fiber that glows, belongs to function textile material technical field.
Background technology
Along with the development of science and technology, the fibrous raw material of single performance can not meet the demand of the growing functional textile of people, and the safety of fiber itself simultaneously and the feature of environmental protection are also increasingly subject to people's attention.The development leading national textile industry economizes, as weaving is big, in Jiangsu Province, in recent years, along with developing rapidly of our province industry, the maturation of perfect and the spinning technique, equipment of the abundant and performance of long-afterglow material kind, RE luminous fiber arises at the historic moment and achieves certain achievement in research.Luminous fiber is a kind of novel functional fiber material, and it is high in technological content, self sends light when unglazed photograph.RE luminous fiber is with fibre-forming polymer for base material, adds luminescent material and colored pigment and spin finish aid, adopt the new type functional fiber with storage light-lighting function that melt spinning method is prepared from spinning process.RE luminous fiber luminescence process mainly absorbs luminous energy-luminous energy storage-luminous energy release, and when excitation light irradiation to fiber surface, the luminescent material of fibrous inside absorbs luminous energy, and rare earth ion outer-shell electron transits to excited state and stored by luminous energy；Removing excitation source, the energy of absorption, to ground state, is discharged by electron transition in the form of light, produces to launch light.The luminescent material that production luminous fiber adopts is alkaline earth aluminate persistent luminescent material, and this luminescent material has excellent luminescent properties, and does not have radioactivity, and human body and environment will not produce harm.Luminous fiber is used for garment for children, the safety that child walked at night can be improved, also can increase the children's interesting of garment for children simultaneously；Luminous fiber is used for the work clothes of night work, the such as working clothing of mine workman, the work for the personnel of working at night provides convenience, and when peril occurs, the self light emission function of luminous fiber is easy to the expansion of search-and-rescue work, offers help for rescue work；Luminous fiber being used for the exploitation of embroidery product, is the perfect adaptation of high-tech and traditional handicraft, the innovation for tradition embroidery product proposes new approaches, is conducive to improving industrial art and the reserve value of embroidery product；Luminous fiber is used for down toy, improves the enjoying nature of down toy, significantly widen the selling market of down toy.Luminous fiber can be used for the aspects such as all kinds of daily life, amusement and recreation and transportation, provides living condition more convenient, abundant for the mankind.
The development of luminous fiber can trace back to 1998 the earliest, a company of Germany developed in the first a kind of without the fiber launching green glow under light conditions, employing zinc sulfide is luminescent material, luminescent material, spin finish aid etc. are added in spinning base material and be prepared from, but adopt fiber original intensity prepared by the method too short for higher persistence, and placement is easy to aging in atmosphere, therefore this fiber is not widely used.2002, a company of the U.S. is for covering the shortage, adopting the zinc sulfide adding radiosiotope hard iron 147 is luminescent material, make a kind of luminous fiber, the luminosity of luminous fiber obtains a degree of raising, but human body and environment are created corresponding harm by the interpolation of radioelement, therefore this luminous fiber is also without well being studied application.From (2000) at the beginning of 21 century, the research and development of luminous fiber are made that significant contribution by the researcher of Japan, 2004, E.Shim have developed a kind of sheath-core bicomponent luminous fiber, this fiber does core composition or shell component with luminescent material, do shell component or core composition with fibre substrate, made the luminous fiber of skin-core structure by extraordinary spinning, and the luminescent properties and mechanical performance to this fiber has been studied.Also the not luminous component of the luminous fiber of skin-core structure is dyeed by some Japanese scholars so that fiber presents colourful color when there being illumination, but the brightness after this stock-dye reduces to a great extent.
At home, within 2003, department's spring thunder have employed thermoplastic polypropylene and rare earth aluminate luminescent material is blended, and the method for melt spinning is prepared for long persistence luminous polypropylene fiber.Result of study shows: this fiber has good luminescent properties, and persistence can reach more than 10 hours；In fiber, light-storing material content increases, and its physical and mechanical properties declines, and persistence and brightness increase；When light-storing material content is 5%, properties is better, but has no report subsequently.Southern Yangtze University in 2004 combines with Jiangsu Guo Da company and successfully have developed RE luminous fiber, and industrialization, is widely used research subsequently.Pointing out that light can optionally be absorbed by inorganic pigment by studying, the emission spectrum causing fiber is different.The absorption that selects of light can be affected the light propagation at fibrous inside and SrAl in fiber by transparent inorganic pigment2O4:Eu2+, Dy3+Rare earth luminescent material is different from the active force of pigment, causes that the spectral radiation curves adding the fiber of different colours there are differences.Research and development along with luminous fiber, fiber Photochromic Properties becomes main study subject, the impact of luminous fiber Photochromic Properties is concluded that the color form and aspect of luminous fiber are determined by the tone of the pigment added by studying pigment by Yan Yanhong etc., and yellow is similar with green luminous fiber brightness value.Degree about luminescent fibre pigment color hatching effect is more high more big on luminosity impact；Pigment color is more deep, and the luminosity of luminescent fibre is more low；Pigment color is more shallow, and luminosity is more high.The photochromic form and aspect of luminous fiber are affected inconspicuous by colored pigment, are still yellow-green light.The compound that luminous fiber photochromic is based on yellow-green light is photochromic, and excitation is all relatively low, and color developing is better.
Owing to the addition of colored pigment in spinning process, luminous fiber can present colourful color when there being illumination, and at dark place, the luminescence of luminous fiber and Photochromic Properties depend on the performance of the luminescent material used.Current luminous fiber luminescent material has Sr2MgSi2O7:Eu2+, Dy3+、SrAl2O4:Eu2+, Dy3+Two kinds, mainly send blue light and green glow, and the low-energy ransition of the effect of red illuminating material parent lattice structure and rare earth ion outer-shell electron causes that its luminescent properties is poor, do not reach the performance requirement for preparing luminous fiber.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, the preparation method that a kind of long-afterglow fluorescent fiber that glows is provided, adopt the mode that master batch adds, and change the complex method of red light flourescent material, add and the adhesion of fiber base material PET macromole, it is thus achieved that favorable dispersibility and there is long afterglow HONGGUANG fluorescent fiber material.
According to technical scheme provided by the invention, the preparation method of a kind of long-afterglow fluorescent fiber that glows, it is characterized by, comprises the following steps that:
(1) preparation of photothermal converting agent/fluorescent material complex: by titanate coupling agent, dehydrated alcohol, the photothermal converting agent of oxygen anthracene structure and fluorescent material 0.5～1.5:60 in mass ratio～80:0.03～0.07:10 mixing, it is heated to 50～80 DEG C under closing, high speed dispersion state, reaction 20～60min, filter after completion of the reaction, and fully wash with dehydrated alcohol, dry, prepare photothermal converting agent/fluorescent material complex；
(2) grinding of photothermal converting agent/fluorescent material complex: photothermal converting agent/fluorescent material complex is pulverized, obtains the powder body of particle diameter 10～200nm；
(3) carrying out premix by dried in vacuum drying oven for PET powder body with photothermal converting agent/fluorescent material complex, the premixing machine that employing rotating speed is 50～500r/min carries out batch mixing, obtains fluorescent fiber agglomerate material；Wherein the mass percent of photothermal converting agent/fluorescent material complex is 10～40%；
(4), after being dried by fluorescent fiber agglomerate material, double screw extruder melt pelletization is adopted to make spinning master batch；
(5) spinning master batch Homogeneous phase mixing PET master batch and step (4) obtained, wherein the mass percent of the spinning master batch that step (4) obtains is 2～20%；Carrying out melt spinning after drying, during spinning, melt temperature is 270～290 DEG C, makes, through extruding, drawing-off, winding, the long-afterglow fluorescent fiber that glows.
In a detailed description of the invention, described fluorescent material is SrAl2O4:Eu2+, Dy3+。
In a detailed description of the invention, described step (2) photothermal converting agent/fluorescent material complex is pulverized by mechanical milling method and comminution by gas stream.
In a detailed description of the invention, in described step (3), PET powder drying temperature is 110～120 DEG C, and drying time is 2～4h.
In a detailed description of the invention, in described step (4), the drying temperature of fluorescent fiber agglomerate material is 110～120 DEG C, and drying time is 2～10h.
In a detailed description of the invention, in described step (4), the extruder temperature of double screw extruder is 260～290 DEG C, and screw speed is 200-600r/min.
In a detailed description of the invention, in described step (5), mixing apparatus adopts rotating speed to be the premixing machine of 50～500r/min.
In a detailed description of the invention: in described step (5), baking temperature is 110～120 DEG C, and drying time is 10～24h.
In a detailed description of the invention, the photothermal converting agent of described oxygen anthracene structure is
The preparation method of the long-afterglow fluorescent fiber that glows of the present invention, do not damaging the problem that PET can not glow that not only solves on the basis of PET process based prediction model, more changed the complex method of red-emitting fluorescent material and photothermal converting agent by the mode of chemical modification, while adding fiber added value, also extend its application within the scope of weaving.
Accompanying drawing explanation
Figure 1A and Figure 1B is the SEM figure of photothermal converting agent/fluorescent material complex, and the scale length in Figure 1A is unit 20 μm, and the scale length of Figure 1B is 10 μm.
Fig. 2 is luminous fiber decay curve figure；Abscissa is the time, and unit is s；Vertical coordinate is brightness, and unit is cd m-2。
Fig. 3 is luminous fiber spectral radiation curves；Abscissa is wavelength, and unit is nm；Vertical coordinate is relative intensity, and unit is a.u..
Detailed description of the invention
Below in conjunction with concrete drawings and Examples, the invention will be further described.
Fluorescent material used in the present invention is SrAl2O4:Eu2+, Dy3+.The photothermal converting agent of oxygen anthracene structure of the present invention is
Embodiment 1: the preparation method of a kind of long-afterglow fluorescent fiber that glows, comprises the following steps that:
(1) preparation of photothermal converting agent/fluorescent material complex: by titanate coupling agent, dehydrated alcohol, the photothermal converting agent of oxygen anthracene structure and fluorescent material 1:70:0.05:10 in mass ratio mixing, it is heated to 70 DEG C under closing, high speed dispersion state, reaction 40min, filter after completion of the reaction, and fully wash with dehydrated alcohol, dry, prepare photothermal converting agent/fluorescent material complex；
(2) grinding of photothermal converting agent/fluorescent material complex: photothermal converting agent/fluorescent material complex is pulverized by mechanical milling method and comminution by gas stream, obtains the powder body of particle diameter 60nm；
(3) being dried in vacuum drying oven by PET powder body, baking temperature is 110 DEG C, and drying time is 3h；Dried and photothermal converting agent/fluorescent material complex carries out premix, and the premixing machine adopting rotating speed to be 200r/min carries out batch mixing, obtains fluorescent fiber agglomerate material；Wherein the mass percent of photothermal converting agent/fluorescent material complex is 25%；
(4) being dried by fluorescent fiber agglomerate material, drying temperature is 110 DEG C, and drying time is 5h；Adopting double screw extruder melt pelletization to make spinning master batch after drying, the extruder temperature of double screw extruder is 275 DEG C, and screw speed is 400r/min；
(5) spinning master batch Homogeneous phase mixing PET master batch and step (4) obtained, wherein the mass percent of the spinning master batch that step (4) obtains is 10%, and mixing apparatus adopts rotating speed to be the premixing machine of 200r/min；Carrying out melt spinning after drying, baking temperature is 110 DEG C, and drying time is 18h；During spinning, melt temperature is 285 DEG C, makes, through extruding, drawing-off, winding, the long-afterglow fluorescent fiber that glows.
Performance test:
(1) scanning electron microscope: embodiment 1 step (2) is obtained photothermal converting agent/fluorescent material complex and is scanned Electronic Speculum test, from Figure 1A, Figure 1B, can be seen that light transforming agent/fluorescent material complex interface cohesion is good, forming complex surface topography, the fine particle particle diameter of attachment in 60nm size and is evenly distributed.
(2) the long-afterglow fluorescent fiber that glows embodiment 1 obtained carries out long afterglow and fluorescent emission test test, and its result is as shown in Figures 2 and 3.As in figure 2 it is shown, afterglow intensity is 0.1/cd m when decay curve tends towards stability2, this value is much larger than the afterglow intensity 0.001/cd m of eye recognition2, therefore can meet the needs of fluorescent product.As it is shown on figure 3, the maximum emission wavelength of fluorescence is at about 600nm, here for red light district, the fiber that therefore prepared by the present invention is red long-afterglow fluorescent fiber.
Embodiment 2: the preparation method of a kind of long-afterglow fluorescent fiber that glows, comprises the following steps that:
(1) preparation of photothermal converting agent/fluorescent material complex: by titanate coupling agent, dehydrated alcohol, the photothermal converting agent of oxygen anthracene structure and fluorescent material 0.5:60:0.03:10 in mass ratio mixing, it is heated to 50 DEG C under closing, high speed dispersion state, reaction 60min, filter after completion of the reaction, and fully wash with dehydrated alcohol, dry, prepare photothermal converting agent/fluorescent material complex；
(2) grinding of photothermal converting agent/fluorescent material complex: photothermal converting agent/fluorescent material complex is pulverized by mechanical milling method and comminution by gas stream, obtains the powder body of particle diameter 10nm；
(3) being dried in vacuum drying oven by PET powder body, baking temperature is 110 DEG C, and drying time is 4h；Dried and photothermal converting agent/fluorescent material complex carries out premix, and the premixing machine adopting rotating speed to be 50r/min carries out batch mixing, obtains fluorescent fiber agglomerate material；Wherein the mass percent of photothermal converting agent/fluorescent material complex is 10%；
(4) being dried by fluorescent fiber agglomerate material, drying temperature is 110 DEG C, and drying time is 10h；Adopting double screw extruder melt pelletization to make spinning master batch after drying, the extruder temperature of double screw extruder is 260 DEG C, and screw speed is 200r/min；
(5) spinning master batch Homogeneous phase mixing PET master batch and step (4) obtained, wherein the mass percent of the spinning master batch that step (4) obtains is 2%, and mixing apparatus adopts rotating speed to be the premixing machine of 50r/min；Carrying out melt spinning after drying, baking temperature is 110 DEG C, and drying time is 24h；During spinning, melt temperature is 270 DEG C, makes, through extruding, drawing-off, winding, the long-afterglow fluorescent fiber that glows.
Embodiment 3: the preparation method of a kind of long-afterglow fluorescent fiber that glows, comprises the following steps that:
(1) preparation of photothermal converting agent/fluorescent material complex: by titanate coupling agent, dehydrated alcohol, the photothermal converting agent of oxygen anthracene structure and fluorescent material 1.5:80:0.07:10 in mass ratio mixing, it is heated to 80 DEG C under closing, high speed dispersion state, reaction 20min, filter after completion of the reaction, and fully wash with dehydrated alcohol, dry, prepare photothermal converting agent/fluorescent material complex；
(2) grinding of photothermal converting agent/fluorescent material complex: photothermal converting agent/fluorescent material complex is pulverized by mechanical milling method and comminution by gas stream, obtains the powder body of particle diameter 200nm；
(3) being dried in vacuum drying oven by PET powder body, baking temperature is 120 DEG C, and drying time is 2h；Dried and photothermal converting agent/fluorescent material complex carries out premix, and the premixing machine adopting rotating speed to be 500r/min carries out batch mixing, obtains fluorescent fiber agglomerate material；Wherein the mass percent of photothermal converting agent/fluorescent material complex is 40%；
(4) being dried by fluorescent fiber agglomerate material, drying temperature is 120 DEG C, and drying time is 2h；Adopting double screw extruder melt pelletization to make spinning master batch after drying, the extruder temperature of double screw extruder is 290 DEG C, and screw speed is 600r/min；
(5) spinning master batch Homogeneous phase mixing PET master batch and step (4) obtained, wherein the mass percent of the spinning master batch that step (4) obtains is 20%, and mixing apparatus adopts rotating speed to be the premixing machine of 500r/min；Carrying out melt spinning after drying, baking temperature is 120 DEG C, and drying time is 10h；During spinning, melt temperature is 290 DEG C, makes, through extruding, drawing-off, winding, the long-afterglow fluorescent fiber that glows.
Embodiment 4: the preparation method of a kind of long-afterglow fluorescent fiber that glows, comprises the following steps that:
(1) preparation of photothermal converting agent/fluorescent material complex: by titanate coupling agent, dehydrated alcohol, the photothermal converting agent of oxygen anthracene structure and fluorescent material 0.6:65:0.04:10 in mass ratio mixing, it is heated to 60 DEG C under closing, high speed dispersion state, reaction 30min, filter after completion of the reaction, and fully wash with dehydrated alcohol, dry, prepare photothermal converting agent/fluorescent material complex；
(2) grinding of photothermal converting agent/fluorescent material complex: photothermal converting agent/fluorescent material complex is pulverized by mechanical milling method and comminution by gas stream, obtains the powder body of particle diameter 100nm；
(3) being dried in vacuum drying oven by PET powder body, baking temperature is 115 DEG C, and drying time is 3h；Dried and photothermal converting agent/fluorescent material complex carries out premix, and the premixing machine adopting rotating speed to be 250r/min carries out batch mixing, obtains fluorescent fiber agglomerate material；Wherein the mass percent of photothermal converting agent/fluorescent material complex is 20%；
(4) being dried by fluorescent fiber agglomerate material, drying temperature is 115 DEG C, and drying time is 3h；Adopting double screw extruder melt pelletization to make spinning master batch after drying, the extruder temperature of double screw extruder is 270 DEG C, and screw speed is 300r/min；
(5) spinning master batch Homogeneous phase mixing PET master batch and step (4) obtained, wherein the mass percent of the spinning master batch that step (4) obtains is 5%, and mixing apparatus adopts rotating speed to be the premixing machine of 150r/min；Carrying out melt spinning after drying, baking temperature is 115 DEG C, and drying time is 12h；During spinning, melt temperature is 280 DEG C, makes, through extruding, drawing-off, winding, the long-afterglow fluorescent fiber that glows.
Claims (9)
1. glow the preparation method of long-afterglow fluorescent fiber, it is characterized in that, comprises the following steps that:
(1) preparation of photothermal converting agent/fluorescent material complex: by titanate coupling agent, dehydrated alcohol, the photothermal converting agent of oxygen anthracene structure and fluorescent material 0.5～1.5:60 in mass ratio～80:0.03～0.07:10 mixing, it is heated to 50～80 DEG C under closing, high speed dispersion state, reaction 20～60min, filter after completion of the reaction, and fully wash with dehydrated alcohol, dry, prepare photothermal converting agent/fluorescent material complex；
(2) grinding of photothermal converting agent/fluorescent material complex: photothermal converting agent/fluorescent material complex is pulverized, obtains the powder body of particle diameter 10～200nm；
(3) carrying out premix after PET powder drying with photothermal converting agent/fluorescent material complex, the premixing machine adopting rotating speed to be 50～500r/min carries out batch mixing, obtains fluorescent fiber agglomerate material；Wherein the mass percent of photothermal converting agent/fluorescent material complex is 10～40%；
(4), after being dried by fluorescent fiber agglomerate material, double screw extruder melt pelletization is adopted to make spinning master batch；
(5) spinning master batch Homogeneous phase mixing PET master batch and step (4) obtained, wherein the mass percent of the spinning master batch that step (4) obtains is 2～20%；Carrying out melt spinning after drying, during spinning, melt temperature is 270～290 DEG C, makes, through extruding, drawing-off, winding, the long-afterglow fluorescent fiber that glows.
2. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: described fluorescent material is SrAl2O4:Eu2+, Dy3+。
3. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: described step (2) photothermal converting agent/fluorescent material complex is pulverized by mechanical milling method and comminution by gas stream.
4. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: in described step (3), PET powder drying temperature is 110～120 DEG C, and drying time is 2～4h.
5. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: in described step (4), the drying temperature of fluorescent fiber agglomerate material is 110～120 DEG C, and drying time is 2～10h.
6. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: in described step (4), the extruder temperature of double screw extruder is 260～290 DEG C, and screw speed is 200-600r/min.
7. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: in described step (5), mixing apparatus adopts rotating speed to be the premixing machine of 50～500r/min.
8. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: in described step (5), baking temperature is 110～120 DEG C, and drying time is 10～24h.
9. glow the preparation method of long-afterglow fluorescent fiber as claimed in claim 1, it is characterized in that: the photothermal converting agent of described oxygen anthracene structure is
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| CN108822830A (en) * | 2018-05-21 | 2018-11-16 | 江南大学 | A kind of preparation method and products thereof of rare earth aluminic acid alkali composite red color luminescent material |
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