CN104674361A - Preparation method of noctilucent fibers capable of emitting red light in darkness - Google Patents
Preparation method of noctilucent fibers capable of emitting red light in darkness Download PDFInfo
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- CN104674361A CN104674361A CN201510039602.2A CN201510039602A CN104674361A CN 104674361 A CN104674361 A CN 104674361A CN 201510039602 A CN201510039602 A CN 201510039602A CN 104674361 A CN104674361 A CN 104674361A
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Abstract
The invention discloses a preparation method of noctilucent fibers capable of emitting red light in darkness. The preparation method comprises the following steps: mixing 2-hydroxybenzaldehyde with 3-hydroxyl-N,N-dimethylaniline which can be dissolved in water to obtain a mixture, heating the mixture, mixing the mixture with anhydrous zinc chloride and sulfuric acid to obtain a mixture I, and carrying out the reaction on the mixture I to obtain a light conversion agent; mixing the light conversion agent with SrAl2O4:Eu<2+>, Dy<3+> and a fiber forming polymer base material to obtain a mixture II, smelting the mixture II, and granulating to obtain noctilucent particles for spinning; and drying the noctilucent particles, then smelting the noctilucent particles and spinning to obtain the noctilucent fibers. The red light emitted by the noctilucent fibers prepared by adopting the preparation method can be maintained for more than ten hours, the highest luminance can reach 3.0cd/m<2>, the emitted red light is one of three basic colors, and the noctilucent fibers can be compounded with one or two of blue light noctilucent fibers and green light noctilucent fibers to prepare luminous colorful noctilucent fibers, so that the important significance can be realized.
Description
Technical field
The present invention relates to function textile fabric processing and manufacturing field, particularly relate to a kind of preparation method that can send the luminous fiber of ruddiness at dark place.
Background technology
Luminous fiber is a kind of tencel that can send light in night or dark, and because of the luminescent properties that it is excellent, obtain in recent years and apply comparatively widely, main application fields has building decoration, communications and transportation, night work and navigation aviation etc.1998, German a company developed a kind of luminous fiber that can send green glow using fiber as base material under UV-irradiation condition.2002, You Liang company of the U.S. developed luminous fiber.From 2000 so far, Japanese researchers successively have developed the luminous fiber of skin-core structure, and core composition (or shell component) made by luminescent material, shell component made by polyester fiber (or core composition) in employing.The luminous fiber that can send ruddiness is at present mainly that luminescent substance is prepared from copper sulfide, relative blue light and its luminosity of green glow is lower is no more than 1.0 cd/m
2and persistence is very short, only has dozens of minutes.Traditional twilight sunset more than sustainable ten hours luminous fibers only have blue light luminous fiber (with Sr
2mgSi
2o
7: Eu
2+, Dy
3+for luminescent substance) and green glow luminous fiber (with SrAl
2o
4: Eu
2+, Dy
3+for luminescent substance), and there is no the luminous fiber that can send ruddiness.RE luminous fiber is have developed at first at home, SrAl by Southern Yangtze University
2o
4: Eu
2+, Dy
3+for luminescent substance, mainly send green glow.But up to the present have no report and use SrAl
2o
4: Eu
2+, Dy
3+luminescent substance preparation can send the luminous fiber of ruddiness.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method that can send the luminous fiber of ruddiness at dark place, and the luminous fiber luminosity obtained is higher, and persistence is longer.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide a kind of preparation method that can send the luminous fiber of ruddiness at dark place, comprising step is:
(1) to water-soluble 3-hydroxy-n, in accelerine, add Benzaldehyde,2-hydroxy, heat up and add anhydrous zinc chloride and H
2sO
4, be obtained by reacting photothermal converting agent;
(2) by described photothermal converting agent and SrAl
2o
4: Eu
2+, Dy
3+, the granulation of fibre-forming polymer base material mixed melting, obtain spinning noctilucence particle;
(3) described noctilucence particle is dry, then the luminous fiber that can send ruddiness at dark place is obtained through melt spinning.
In a preferred embodiment of the present invention, the concrete steps of step (1) are: to water-soluble 3-hydroxy-n under the condition stirred and heat gradually, add Benzaldehyde,2-hydroxy, add anhydrous zinc chloride and H when temperature rises to 50 DEG C in accelerine
2sO
4, sealed thermostat reaction 18-20 hour, obtains photothermal converting agent.
In a preferred embodiment of the present invention, the concrete steps of step (1) are: by 3-hydroxy-n, accelerine 1 ~ 7 part adds in the container that deionized water 30 ~ 50 parts is housed, mixing speed is 500-600 rev/min and stirs, under heating condition gradually, add Benzaldehyde,2-hydroxy 1 ~ 7 part, when temperature rises to 50 DEG C, add anhydrous zinc chloride 0.02 ~ 0.1 part and H
2sO
40.02 ~ 0.1 part, by seal of vessel, under constant temperature 50 DEG C, stirring condition, react 18-20 hour, open container, constantly stir moisture evaporate to dryness, dry under 110 DEG C of conditions and obtain photothermal converting agent half an hour.
In a preferred embodiment of the present invention, described in step (2), fibre-forming polymer base material is polyethylene terephthalate, polycaprolactam or polypropylene.
In a preferred embodiment of the present invention, be by described photothermal converting agent 0.1 ~ 0.2 part and SrAl in step (2)
2o
4: Eu
2+, Dy
3+5 ~ 10 parts, 20 ~ 30 parts of mixed melting granulations of fibre-forming polymer base material.
In a preferred embodiment of the present invention, noctilucence particle described in step (3) wants first dry at 140 DEG C ~ 160 DEG C, makes its moisture content reach below 25ppm and carries out spinning again.
The invention has the beneficial effects as follows: the preparation method that can send the luminous fiber of ruddiness at dark place of the present invention, the luminous fiber ruddiness twilight sunset more than sustainable ten hours obtained, luminosity is the highest can reach 3.0 cd/m
2, the ruddiness sent is the one of three primary colours, and a kind of or two kinds of composite luminous fibers just can preparing any one glow color with blue light luminous fiber and green glow luminous fiber, are significant.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings, wherein:
Fig. 1 is the molecular structural formula figure of photothermal converting agent prepared by the present invention;
Fig. 2 is the luminous fiber figure glowed prepared by the present invention, and wherein a is the surface configuration of luminous fiber, and b is luminous fiber in the dark state photochromic, and in figure, elongated strip is the ruddiness sent out;
Fig. 3 is smooth transfer principle figure of the present invention;
Fig. 4 is the luminous fiber light wave figure glowed prepared by the present invention.
Detailed description of the invention
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment one:
There is provided a kind of preparation method that can send the luminous fiber of ruddiness at dark place, comprising step is:
(1) preparation of photothermal converting agent:
By 3-hydroxy-n, accelerine 1 part adds in the container that deionized water 30 parts is housed, and stirs (mixing speed 500 revs/min), adds Benzaldehyde,2-hydroxy 1 part, add anhydrous zinc chloride 0.02 part and H when temperature rises to 50 DEG C under heating condition gradually
2sO
40.02 part.By seal of vessel, react 18 hours under constant temperature 50 DEG C, stirring condition.Open container, constantly stir moisture evaporate to dryness.Finally under 110 DEG C of conditions, dry half an hour, obtain photothermal converting agent.
(2) noctilucence particle preparation:
The photothermal converting agent 0.1 part obtained by step 1 and SrAl
2o
4: Eu
2+, Dy
3+5 parts, polyethylene terephthalate 20 parts of mixed melting granulations, make noctilucence particle.
(3) the noctilucence particle that step (2) is obtained is baked drying under the condition of 140 DEG C, make its moisture content reach below 25ppm, then obtain the described luminous fiber that can send ruddiness at dark place through melt spinning.
Embodiment two:
There is provided a kind of preparation method that can send the luminous fiber of ruddiness at dark place, comprising step is:
(1) preparation of photothermal converting agent:
By 3-hydroxy-n, accelerine 3 parts adds in the container that deionized water 40 parts is housed, and stirs (mixing speed 550 revs/min), adds Benzaldehyde,2-hydroxy 3 parts, add anhydrous zinc chloride 0.07 part and H when temperature rises to 50 DEG C under heating condition gradually
2sO
40.07 part.By seal of vessel, react 19 hours under constant temperature 50 DEG C, stirring condition.Open container, constantly stir moisture evaporate to dryness.Finally under 110 DEG C of conditions, dry half an hour, obtain photothermal converting agent.
(2) noctilucence particle preparation:
The photothermal converting agent 0.15 part obtained by step (1) and SrAl
2o
4: Eu
2+, Dy
3+7 parts, polycaprolactam 26 parts of mixed melting granulations, make noctilucence particle.
(3) the noctilucence particle that step (2) is obtained is baked drying under the condition of 150 DEG C, make its moisture content reach below 25ppm, then obtain the described luminous fiber that can send ruddiness at dark place through melt spinning.
Embodiment three:
There is provided a kind of preparation method that can send the luminous fiber of ruddiness at dark place, comprising step is:
(1) preparation of photothermal converting agent:
By 3-hydroxy-n, accelerine 7 parts adds in the container that deionized water 50 parts is housed, and stirs (mixing speed 600 revs/min), adds Benzaldehyde,2-hydroxy 7 parts, add anhydrous zinc chloride 0.1 part and H when temperature rises to 50 DEG C under heating condition gradually
2sO
40.1 part.By seal of vessel, react 20 hours under constant temperature 50 DEG C, stirring condition.Open container, constantly stir moisture evaporate to dryness.Finally under 110 DEG C of conditions, dry half an hour, obtain photothermal converting agent.
(2) noctilucence particle preparation:
By photothermal converting agent 0.2 part obtained for step (1) and SrAl2O4:Eu2+, Dy3+ 10 parts, polypropylene 30 parts of mixed melting granulations, make noctilucence particle.
(3) the noctilucence particle that step (2) is obtained is baked drying under the condition of 160 DEG C.Make its moisture content reach below 25ppm, then obtain the described luminous fiber that can send ruddiness at dark place through melt spinning.
Refer to Fig. 1 and 2, photothermal converting agent in the present invention is a kind of light-converting material, and a kind of light of wavelength can be transformed into the light of another kind of wavelength by it, can change the luminescent properties of luminous fiber by adding photothermal converting agent, its emission spectrum is moved to ruddiness direction, sends red light.SrAl is found by studying us
2o
4: Eu
2+, Dy
3+wavelength corresponding to spectral radiation curves be 460-550 nm, the wavelength that the excitation spectrum curve of photothermal converting agent is corresponding is 440-550 nm, and two curves are overlapping between 460-550 nm, as shown in Figure 3.At fibrous inside, SrAl
2o
4: Eu
2+, Dy
3+the illumination sending 460-550nm is mapped to photothermal converting agent surface, photothermal converting agent can absorb the light of 460-550nm, the Electron absorption energy of photothermal converting agent inside, by ground state transition to excitation state and by energy storage, when ground state is returned in electron transition, the fault offset will stored in the form of light, sends characteristic light, its electron transition path of photothermal converting agent prepared by the present invention is more, makes the wavelength that its emission peak is corresponding larger.The wavelength that luminous fiber emission peak prepared by the present invention is corresponding is mainly positioned at about 610 nm, is positioned at red light region, as shown in Figure 4.
The preparation method that can send the luminous fiber of ruddiness at dark place of the present invention is with SrAl
2o
4: Eu
2+, Dy
3+as luminescent substance, obtained by the photothermal converting agent adding preparation, this luminous fiber ruddiness twilight sunset more than sustainable ten hours, luminosity is the highest can reach 3.0 cd/m
2, the ruddiness sent is the one of three primary colours, with traditional blue light luminous fiber (with Sr
2mgSi
2o
7: Eu
2+, Dy
3+for luminescent substance) and green glow luminous fiber (with SrAl
2o
4: Eu
2+, Dy
3+for luminescent substance) in a kind of or two kinds of composite luminous fibers just can preparing any one glow color, therefore significant.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. can send a preparation method for the luminous fiber of ruddiness at dark place, it is characterized in that, comprising step is:
(1) to water-soluble 3-hydroxy-n, in accelerine, add Benzaldehyde,2-hydroxy, heat up and add anhydrous zinc chloride and H
2sO
4, be obtained by reacting photothermal converting agent;
(2) by described photothermal converting agent and SrAl
2o
4: Eu
2+, Dy
3+, the granulation of fibre-forming polymer base material mixed melting, obtain spinning noctilucence particle;
(3) described noctilucence particle is dry, then the luminous fiber that can send ruddiness at dark place is obtained through melt spinning.
2. preparation method according to claim 1, it is characterized in that, the concrete steps of step (1) are: to water-soluble 3-hydroxy-n under the condition stirred and heat gradually, add Benzaldehyde,2-hydroxy, add anhydrous zinc chloride and H when temperature rises to 50 DEG C in accelerine
2sO
4, sealed thermostat reaction 18-20 hour, obtains photothermal converting agent.
3. preparation method according to claim 2, it is characterized in that, the concrete steps of step (1) are: by 3-hydroxy-n, accelerine 1 ~ 7 part adds in the container that deionized water 30 ~ 50 parts is housed, mixing speed is 500-600 rev/min and stirs, under heating condition gradually, add Benzaldehyde,2-hydroxy 1 ~ 7 part, when temperature rises to 50 DEG C, add anhydrous zinc chloride 0.02 ~ 0.1 part and H
2sO
40.02 ~ 0.1 part, by seal of vessel, under constant temperature 50 DEG C, stirring condition, react 18-20 hour, open container, constantly stir moisture evaporate to dryness, dry under 110 DEG C of conditions and obtain photothermal converting agent half an hour.
4. preparation method according to claim 1, is characterized in that, described in step (2), fibre-forming polymer base material is polyethylene terephthalate, polycaprolactam or polypropylene.
5. preparation method according to claim 1, is characterized in that, is by described photothermal converting agent 0.1 ~ 0.2 part and SrAl in step (2)
2o
4: Eu
2+, Dy
3+5 ~ 10 parts, 20 ~ 30 parts of mixed melting granulations of fibre-forming polymer base material.
6. preparation method according to claim 1, is characterized in that, noctilucence particle described in step (3) wants first dry at 140 DEG C ~ 160 DEG C, makes its moisture content reach below 25ppm and carries out spinning again.
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| CN201510039602.2A CN104674361B (en) | 2015-01-27 | 2015-01-27 | Preparation method of noctilucent fibers capable of emitting red light in darkness |
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| CN104674361B CN104674361B (en) | 2017-04-26 |
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Cited By (6)
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| CN105780169A (en) * | 2016-03-09 | 2016-07-20 | 江南大学 | Preparation method of long afterglow fluorescent fibers emitting red light |
| CN106012069A (en) * | 2016-06-28 | 2016-10-12 | 江南大学 | Preparation method of yellow luminescent fiber |
| CN106010532A (en) * | 2016-06-03 | 2016-10-12 | 江南大学 | Method for preparing high-brightness red light long afterglow luminous material |
| CN106192038A (en) * | 2016-07-21 | 2016-12-07 | 江南大学 | The preparation method of blue light luminous fiber |
| CN107418555A (en) * | 2017-03-27 | 2017-12-01 | 江苏弘盛新材料股份有限公司 | The preparation method and system of a kind of luminous chinlon 6 section of Europium |
| CN107841797A (en) * | 2017-11-10 | 2018-03-27 | 江阴金盟纺织有限公司 | A kind of Novel luminous long filament and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105780169A (en) * | 2016-03-09 | 2016-07-20 | 江南大学 | Preparation method of long afterglow fluorescent fibers emitting red light |
| CN105780169B (en) * | 2016-03-09 | 2017-11-28 | 江南大学 | Glow the preparation method of long-afterglow fluorescent fiber |
| CN106010532A (en) * | 2016-06-03 | 2016-10-12 | 江南大学 | Method for preparing high-brightness red light long afterglow luminous material |
| CN106010532B (en) * | 2016-06-03 | 2018-05-08 | 江南大学 | The preparation method of high brightness red light long afterglow luminous material |
| CN106012069A (en) * | 2016-06-28 | 2016-10-12 | 江南大学 | Preparation method of yellow luminescent fiber |
| CN106012069B (en) * | 2016-06-28 | 2022-02-01 | 江南大学 | Preparation method of yellow noctilucent fiber |
| CN106192038A (en) * | 2016-07-21 | 2016-12-07 | 江南大学 | The preparation method of blue light luminous fiber |
| CN106192038B (en) * | 2016-07-21 | 2018-09-21 | 江南大学 | The preparation method of blue light luminous fiber |
| CN107418555A (en) * | 2017-03-27 | 2017-12-01 | 江苏弘盛新材料股份有限公司 | The preparation method and system of a kind of luminous chinlon 6 section of Europium |
| CN107841797A (en) * | 2017-11-10 | 2018-03-27 | 江阴金盟纺织有限公司 | A kind of Novel luminous long filament and preparation method thereof |
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| CN104674361B (en) | 2017-04-26 |
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Effective date of registration: 20220913 Address after: No. 1-3, Daizhuang Road, Gaoyou Street, Gaoyou City, Yangzhou City, Jiangsu Province 225600 Patentee after: Yangzhou Jianghui Textile Technology Co.,Ltd. Address before: 215000 Building 1, No.8, Jindu Road, Southeast Economic Development Zone, Changshu City, Suzhou City, Jiangsu Province Patentee before: CHANGSHU JIANGHUI FIBER PRODUCTS TECHNOLOGY CO.,LTD. |