CN106192038A - The preparation method of blue light luminous fiber - Google Patents
The preparation method of blue light luminous fiber Download PDFInfo
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- CN106192038A CN106192038A CN201610577112.2A CN201610577112A CN106192038A CN 106192038 A CN106192038 A CN 106192038A CN 201610577112 A CN201610577112 A CN 201610577112A CN 106192038 A CN106192038 A CN 106192038A
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- luminous fiber
- blue light
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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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
-
- 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
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
- D01F6/06—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins from polypropylene
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
Abstract
The present invention relates to the preparation method of a kind of blue light luminous fiber, comprise the following steps: (1) is by 0.1～0.5 weight portion triphenyl iodine hexafluoro antimonate light trigger and 5～10 weight portion SrAl2O4: Eu2+, Dy3+Luminescent material, 20～40 weight portion fibre-forming polymer base material mixing, use dual-screw pelletizer pelletize, obtain spinning noctilucence master batch；(2) the predrying rear melt spinning of spinning noctilucence master batch step (1) obtained, obtains described blue light luminous fiber.The luminous fiber that the present invention obtains absorbs visible ray 10 minutes, the most sustainable luminous more than 10 hours；Luminosity reaches as high as 1.5 ~ 3cd/m2；430 ~ 450nm the blue light sent is the one of three primary colours, the luminous fiber that just can prepare any secondary color compounding with the one or two kinds of in red luminous fiber and green luminous fiber, can expand the application of luminous fiber.
Description
Technical field
The present invention relates to the preparation method of a kind of blue light luminous fiber, especially one and can send 430 in the dark
～the preparation method of the blue light luminous fiber of 450nm, belong to function textile material manufacturing technology field.
Background technology
Rare earth aluminic acid strontium luminous fiber is a kind of novel environmental protection and energy saving fiber type, mainly utilizes rare earth material as luminescence
Body is made through extraordinary spinning technique, because it in the dark or has good luminescent properties night and be used widely.But
Being that its wavelength of transmitted light is positioned at 520～540nm, spectral distribution is in yellow-green light district, and it is one big that glow color dullness becomes application
Problem.The primary raw material of current existing blue light luminous fiber has metal sulfide and silicate luminescent material, relative to aluminum
Its initial after-glow brightness of the luminescent material of silicate system is relatively low.Research shows, traditional with SrAl2O4: Eu2+, Dy3+For luminous material
The green light luminous fiber of material and red light luminous fiber have been developed exploitation, but up to the present have no that report uses
SrAl2O4: Eu2+, Dy3+Can be with the luminous fiber of blue light-emitting for luminescent substance preparation.
Therefore, finding one can be by the long wave (SrAl of jaundice green light2O4: Eu2+, Dy3+Luminous fiber) be converted to shortwave
(the SrAl of the coloured light that turns blue2O4: Eu2+, Dy3+Luminous fiber) lower transition material there is important researching value and realistic meaning.
Wherein, triphenyl iodine hexafluoro antimonate light trigger is a kind of sensitive material with excellent light conversion properties energy, it is possible to absorb spoke
Penetrate energy, cause electronics generation transition, SrAl can be realized2O4: Eu2+, Dy3+Luminous fiber turns blue the purpose of coloured light in the dark.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that the preparation side of a kind of blue light luminous fiber
Method, the luminous fiber obtained can send the blue light that wavelength is 430～450nm.
The technical scheme provided according to the present invention, the preparation method of described blue light luminous fiber, feature is, including following
Step:
(1) by 0.1～0.5 weight portion triphenyl iodine hexafluoro antimonate light trigger and 5～10 weight portion SrAl2O4: Eu2 +, Dy3+Luminescent material, 20～40 weight portion fibre-forming polymer base material mixing, use dual-screw pelletizer pelletize, obtain spinning use
Noctilucence master batch；The structural formula of described triphenyl iodine hexafluoro antimonate light trigger is:
(2) the predrying rear melt spinning of spinning noctilucence master batch step (1) obtained, obtains described blue light noctilucence
Fiber.
In a detailed description of the invention, described triphenyl iodine hexafluoro antimonate light trigger uses following steps to prepare:
By 10～15 weight portion potassium iodate, 16～20 weight portion benzene, 23～27 pbw of acetic anhydride and the mixing of 5～10 parts by weight solvent,
The reactant liquor obtained is down to-5～-10 DEG C, after being slowly added to 10～15 weight portion concentrated sulphuric acids, reacts 2～4h, then in room temperature
Adding hexafluoro-antimonic acid aqueous solutions of potassium after lower stirring 46～48h, hexafluoro antimonate aqueous solutions of potassium is by 10～15 weight portion hexafluoro-antimonic acids
Potassium and 50～55 weight parts waters are mixed to get；By above-mentioned reactant liquor through sucking filtration, wash and be recrystallized to give diphenyl iodine hexafluoro
Stibate white crystal；20～25 weight portion benzene sulfur are added in 5～10 weight portion diphenyl iodine hexafluoro antimonate white crystals
Ether and 6～10 part by weight of catalyst, by reaction vessel rushing full nitrogen and being warming up to 100～120 DEG C of reactions 2～4h, the coldest
It is precipitated thing the most afterwards, through sucking filtration, washing and recrystallization, obtains triphenyl iodine hexafluoro antimonate white crystal.
In a detailed description of the invention, described step (1) uses concretely comprising the following steps of dual-screw pelletizer pelletize: will
Fibre-forming polymer base material after 100～120 DEG C predrying 20～24h, with triphenyl iodine hexafluoro antimonate light trigger and
SrAl2O4: Eu2+, Dy3+Luminescent material mixes, and uses dual-screw pelletizer pelletize, obtains spinning noctilucence master batch.
In a detailed description of the invention, the employing polyester of described fibre-forming polymer base material, polypropylene or polyamide section.
In a detailed description of the invention, described solvent uses anhydrous acetonitrile.
In a detailed description of the invention, described catalyst uses Salicylaldoxime.
The invention have the advantages that the luminous fiber that the present invention obtains absorbs visible ray 10 minutes, in the dark state
Sustainable luminous more than 10 hours；Luminosity reaches as high as 1.5～3cd/m2；430～the 450nm blue lights sent are three primary colours
One, compounding with the one or two kinds of in red luminous fiber and green luminous fiber just can prepare any one again
The luminous fiber of color, can expand the application of luminous fiber.
Accompanying drawing explanation
The scanning electron microscope (SEM) photograph of the triphenyl iodine hexafluoro antimonate light trigger that Fig. 1-1 is prepared for the present invention.
Fig. 1-2 is the scanning electron microscope (SEM) photograph of blue luminous fiber prepared by the present invention.
Fig. 1-3 prepares SrAl for the present invention2O4: Eu2+, Dy3+The scanning electron microscope (SEM) photograph of luminescent material.
Fig. 2 is the fluorescence spectrum figure of the luminous fiber of blue light-emitting prepared by the present invention.
Fig. 3 is the light-initiated schematic diagram of the luminous fiber of blue light-emitting prepared by the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Triphenyl iodine hexafluoro antimonate has space charge force height and the feature of heat-resistant stable, can cause by being blended
Rare earth aluminic acid strontium luminous fiber produces blue light.It causes principle to be containing conjugation high score in triphenyl iodine hexafluoro-antimonic acid molecules of salt
The material of subsystem, they can absorb luminous energy and transit to excited state, and the molecule being in excited state can be by unnecessary energy transmission
To the molecule of fluorescent material；Due to the specific electronic configuration of rare earth ion, they can accept energy from conjugated polymer system
Amount transits to excited state, launches the characteristic fluorescence of each ion when electronics returns to ground state from excited state.There is conjugated system
Triphenyl iodine hexafluoro antimonate plays one " antenna effect ", its emission spectrum and receptor (rare earth ion) as energy donor
Absorption spectrum should have good overlap, luminous energy or electronics can migrate in whole conjugated system, therefore, can be shifted by energy
Realize SrAl2O4: Eu2+, Dy3+The blue shift of luminous fiber emission spectrum.As in figure 2 it is shown, the night of the blue light-emitting prepared for the present invention
The fluorescence spectrum figure of fiber optics；Abscissa is wavelength, and unit is nm；Vertical coordinate is relative intensity, and unit is counting s-1。
As it is shown on figure 3, the light-initiated schematic diagram of the luminous fiber of the blue light-emitting prepared for the present invention: triphenyl iodine hexafluoro antimony
In hydrochlorate, conjugated polymer donor (S) arrives SrAl2O4: Eu2+, Dy3+The energy transfer of luminescent material receptor (A) causes fluorescent emission
Blue shift.
Embodiment 1: the preparation method of a kind of blue light luminous fiber, comprises the following steps:
(1) prepare triphenyl iodine hexafluoro antimonate light trigger, use following steps: by 10 weight portion potassium iodate, 16 weights
Amount part benzene, 23 pbw of acetic anhydride and the mixing of 5 weight portion anhydrous acetonitriles, be down to-5 DEG C by the reactant liquor obtained, be slowly added to 10
Reacting 2h after weight portion concentrated sulphuric acid, then be stirred at room temperature addition hexafluoro-antimonic acid aqueous solutions of potassium after 46h, hexafluoro antimonate potassium is water-soluble
Liquid is mixed to get by 10 weight portion potassium hexafluoroantimonate and 50 weight parts waters；By above-mentioned reactant liquor through sucking filtration, washing and recrystallization
Obtain diphenyl iodine hexafluoro antimonate white crystal；20 weights are added in 5 weight portion diphenyl iodine hexafluoro antimonate white crystals
Amount part diphenyl sulfide and 6 weight portion Salicylaldoximes, by reaction vessel rushing full nitrogen and being warming up to 100 DEG C of reaction 2h, the coldest
It is precipitated thing the most afterwards, through sucking filtration, washing and recrystallization, obtains triphenyl iodine hexafluoro antimonate white crystal；
(2) by 20 weight portion fibre-forming polymer base materials after 100 DEG C of predrying 20h, with 0.1 weight portion triphenyl iodine hexafluoro
Stibate light trigger and 5 weight portion SrAl2O4: Eu2+, Dy3+Luminescent material mixes, and uses dual-screw pelletizer pelletize, obtains
Spinning noctilucence master batch；The employing polyester of described fibre-forming polymer base material, polypropylene or polyamide section；
(3) the predrying rear melt spinning of spinning noctilucence master batch step (2) obtained, obtains described blue light noctilucence
Fiber.
Embodiment 2: the preparation method of a kind of blue light luminous fiber, comprises the following steps:
(1) prepare triphenyl iodine hexafluoro antimonate light trigger, use following steps: by 13 weight portion potassium iodate, 18 weights
Amount part benzene, 25 pbw of acetic anhydride and the mixing of 7 weight portion anhydrous acetonitriles, be down to-7 DEG C by the reactant liquor obtained, be slowly added to 13
Reacting 3h after weight portion concentrated sulphuric acid, then be stirred at room temperature addition hexafluoro-antimonic acid aqueous solutions of potassium after 47h, hexafluoro antimonate potassium is water-soluble
Liquid is mixed to get by 13 weight portion potassium hexafluoroantimonate and 53 weight parts waters；By above-mentioned reactant liquor through sucking filtration, washing and recrystallization
Obtain diphenyl iodine hexafluoro antimonate white crystal；23 weights are added in 7 weight portion diphenyl iodine hexafluoro antimonate white crystals
Amount part diphenyl sulfide and 8 weight portion Salicylaldoximes, by reaction vessel rushing full nitrogen and being warming up to 110 DEG C of reaction 3h, the coldest
It is precipitated thing the most afterwards, through sucking filtration, washing and recrystallization, obtains triphenyl iodine hexafluoro antimonate white crystal；
(2) by 30 weight portion fibre-forming polymer base materials after 110 DEG C of predrying 22h, with 0.3 weight portion triphenyl iodine hexafluoro
Stibate light trigger and 7 weight portion SrAl2O4: Eu2+, Dy3+Luminescent material mixes, and uses dual-screw pelletizer pelletize, obtains
Spinning noctilucence master batch；The employing polyester of described fibre-forming polymer base material, polypropylene or polyamide section；
(3) the predrying rear melt spinning of spinning noctilucence master batch step (2) obtained, obtains described blue light noctilucence
Fiber.
Embodiment 3: the preparation method of a kind of blue light luminous fiber, comprises the following steps:
(1) prepare triphenyl iodine hexafluoro antimonate light trigger, use following steps: by 15 weight portion potassium iodate, 20 weights
Amount part benzene, 27 pbw of acetic anhydride and the mixing of 10 weight portion anhydrous acetonitriles, be down to-10 DEG C by the reactant liquor obtained, be slowly added to
React 4h after 15 weight portion concentrated sulphuric acids, then be stirred at room temperature addition hexafluoro-antimonic acid aqueous solutions of potassium after 48h, hexafluoro antimonate potassium water
Solution is mixed to get by 15 weight portion potassium hexafluoroantimonate and 55 weight parts waters；Above-mentioned reactant liquor through sucking filtration, washing and is heavily tied
Crystalline substance obtains diphenyl iodine hexafluoro antimonate white crystal；25 are added in 10 weight portion diphenyl iodine hexafluoro antimonate white crystals
Weight portion diphenyl sulfide and 10 weight portion Salicylaldoximes, by reaction vessel rushing full nitrogen and being warming up to 120 DEG C of reaction 4h, natural
It is precipitated thing after cooling, through sucking filtration, washing and recrystallization, obtains triphenyl iodine hexafluoro antimonate white crystal；
(2) by 40 weight portion fibre-forming polymer base materials after 120 DEG C of predrying 24h, with 0.5 weight portion triphenyl iodine hexafluoro
Stibate light trigger and 10 weight portion SrAl2O4: Eu2+, Dy3+Luminescent material mixes, and uses dual-screw pelletizer pelletize, obtains
Spinning noctilucence master batch；The employing polyester of described fibre-forming polymer base material, polypropylene or polyamide section；
(3) the predrying rear melt spinning of spinning noctilucence master batch step (2) obtained, obtains described blue light noctilucence
Fiber.
As shown in Fig. 1-1, Fig. 1-2, Fig. 1-3, triphenyl iodine hexafluoro antimonate light trigger that respectively prepared by the present invention,
Blue luminous fiber and SrAl2O4: Eu2+, Dy3+The scanning electron microscope (SEM) photograph of luminescent material.
Claims (6)
1. a preparation method for blue light luminous fiber, is characterized in that, comprises the following steps:
(1) by 0.1～0.5 weight portion triphenyl iodine hexafluoro antimonate light trigger and 5～10 weight portion SrAl2O4: Eu2+, Dy3+
Luminescent material, 20～40 weight portion fibre-forming polymer base material mixing, use dual-screw pelletizer pelletize, obtain spinning noctilucence female
Grain；
(2) the predrying rear melt spinning of spinning noctilucence master batch step (1) obtained, obtains described blue light noctilucence fine
Dimension.
2. the preparation method of blue light luminous fiber as claimed in claim 1, is characterized in that: described triphenyl iodine hexafluoro-antimonic acid
Salt light trigger uses following steps to prepare: by 10～15 weight portion potassium iodate, 16～20 weight portion benzene, 23～27 weight portion second
Anhydride and the mixing of 5～10 parts by weight solvent, be down to-5～-10 DEG C by the reactant liquor obtained, be slowly added to 10～15 weight portions
React 2～4h after concentrated sulphuric acid, then add hexafluoro-antimonic acid aqueous solutions of potassium, hexafluoro antimonate potassium water after being stirred at room temperature 46～48h
Solution is mixed to get by 10～15 weight portion potassium hexafluoroantimonate and 50～55 weight parts waters；By above-mentioned reactant liquor through sucking filtration, wash
Wash and be recrystallized to give diphenyl iodine hexafluoro antimonate white crystal；To 5～10 weight portion diphenyl iodine hexafluoro antimonate whites
Crystal adds 20～25 weight portion diphenyl sulfides and 6～10 part by weight of catalyst, reaction vessel will rush full nitrogen and be warming up to
100 ~ 120 DEG C of reactions 2～4h, are precipitated thing, through sucking filtration, washing and recrystallization, obtain triphenyl iodine six after natural cooling
Fluorine antimonate white crystal.
3. the preparation method of blue light luminous fiber as claimed in claim 1, is characterized in that: use double in described step (1)
Concretely comprising the following steps of screw pelletizer pelletize: by fibre-forming polymer base material after 100～120 DEG C predrying 20～24h, with triphen
Base iodine hexafluoro antimonate light trigger and SrAl2O4: Eu2+, Dy3+Luminescent material mixes, and uses dual-screw pelletizer pelletize, obtains
Spinning noctilucence master batch.
4. the preparation method of the blue light luminous fiber as described in claim 1 or 3, is characterized in that: described fibre-forming polymer base
The employing polyester of material, polypropylene or polyamide section.
5. the preparation method of blue light luminous fiber as claimed in claim 2, is characterized in that: described solvent uses anhydrous second
Nitrile.
6. the preparation method of blue light luminous fiber as claimed in claim 2, is characterized in that: described catalyst uses anhydrous vinegar
Acid copper.
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Cited By (4)
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| CN108381955A (en) * | 2018-02-27 | 2018-08-10 | 西南科技大学 | A kind of preparation method of plastic scintillant fiber array |
| CN109021964A (en) * | 2018-07-06 | 2018-12-18 | 宁波大学 | A kind of preparation method of organic salt/rare earth aluminic acid strontium composite blue light material |
| CN109763183A (en) * | 2019-01-14 | 2019-05-17 | 河南凯辉实业有限公司 | A kind of polypropylene wool top and preparation method thereof of giving out light certainly |
| CN112941660A (en) * | 2021-02-04 | 2021-06-11 | 宁波大学 | Preparation method of spectrum blue-shifted noctilucent fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108381955A (en) * | 2018-02-27 | 2018-08-10 | 西南科技大学 | A kind of preparation method of plastic scintillant fiber array |
| CN108381955B (en) * | 2018-02-27 | 2020-04-14 | 西南科技大学 | Preparation method of plastic scintillator fiber array |
| CN109021964A (en) * | 2018-07-06 | 2018-12-18 | 宁波大学 | A kind of preparation method of organic salt/rare earth aluminic acid strontium composite blue light material |
| CN109763183A (en) * | 2019-01-14 | 2019-05-17 | 河南凯辉实业有限公司 | A kind of polypropylene wool top and preparation method thereof of giving out light certainly |
| CN112941660A (en) * | 2021-02-04 | 2021-06-11 | 宁波大学 | Preparation method of spectrum blue-shifted noctilucent fiber |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106192038B (en) | 2018-09-21 |
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