CN112941660A - Preparation method of spectrum blue-shifted noctilucent fiber - Google Patents
Preparation method of spectrum blue-shifted noctilucent fiber Download PDFInfo
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- CN112941660A CN112941660A CN202110157846.6A CN202110157846A CN112941660A CN 112941660 A CN112941660 A CN 112941660A CN 202110157846 A CN202110157846 A CN 202110157846A CN 112941660 A CN112941660 A CN 112941660A
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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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- 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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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
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- Luminescent Compositions (AREA)
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Abstract
The invention provides a preparation method of a spectrum blue-shift noctilucent fiber, which comprises the following steps: (1) activation treatment: mixing SrAl2O4:Eu2+，Dy3+Mixing the luminescent powder and the luminescent reinforcing agent according to the weight ratio of 0.5-5: 1, baking in a microwave calcining furnace to obtain composite powder, and activating the composite powder by using a coupling agent; (2) preparing the luminescent composite master batch: 10-90 parts by weight of PET polyester chip, 1-20 parts by weight of photosensitive color-changing powder and 1-30 parts by weight of activated SrAl2O4:Eu2+，Dy3+Mixing luminescent powder and 0.5-1.5 parts by weight of functional auxiliary agent, and granulating by adopting a double-screw granulator; (3) and (3) preparing the luminescent composite fiber. The luminous composite fiber obtained by the invention has double-emission spectrum phenomenon which is respectively positioned at 425nm and 520nm, the wavelength is positioned in a blue region of about 480nm after the double-spectrum superposition, and the luminous fiber with spectrum blue shift is obtainedThe light composite fiber has good washing resistance, and the afterglow brightness of the light composite fiber after washing is only slightly reduced.
Description
Technical Field
The invention relates to the technical field of functional textile material manufacturing, in particular to a preparation method of spectrum blue-shifted noctilucent fiber.
Background
With the continuous change of market demand and the consumption level of people, the original fiber raw material with single performance cannot meet the increasing personalized and diversified demands of people. Therefore, in order to solve the problem of technical innovation of luminescent functional fibers in the development of textile industry in China, continuous innovation from the aspect of fiber preparation raw materials needs to be tried, natural fibers or chemical fibers are subjected to functional modification through process treatment or functional additive addition, new technical products are actively developed, the development strength of high-performance, functional and differential fibers is increased, the application of the high-performance, functional and differential fibers in key fields such as functional textiles is expanded, and the added value of products is improved by means of technological contribution rate. The rare earth strontium aluminate luminous fiber is a novel environment-friendly energy-saving fiber, is mainly prepared by taking a rare earth material as a luminous body through a special spinning process, and is widely applied due to good luminous performance in the dark or at night. However, the wavelength of the emitted light is 520 to 540nm, the spectrum is distributed in a yellow-green light region, and the monotonous emission color becomes a big problem in application.
Disclosure of Invention
The invention aims to disclose a preparation method of a spectrum blue-shift noctilucent fiber, which is respectively positioned at 425nm and 520nm, and the wavelength of the overlapped double spectrums is positioned in a blue area about 480nm, so that the spectrum blue-shift noctilucent fiber is obtained, the application field of the noctilucent fiber is expanded, the spectrum blue-shift noctilucent fiber can be used for blue light material products, in addition, the washing resistance of the luminescent composite fiber is better, and the afterglow brightness of the washed luminescent composite fiber is only slightly reduced.
In order to achieve the purpose, the invention provides a preparation method of a spectrum blue-shift noctilucent fiber, which comprises the following steps:
(1) activation treatment: mixing SrAl2O4：Eu2+，Dy3+Mixing luminescent powder and luminescent reinforcing agent according to the weight ratio of 0.5-5: 1, baking in a microwave calcining furnace to obtain composite powder, and then using relative SrAl2O4：Eu2+，Dy3+Activating the composite powder by a coupling agent accounting for 5-20% of the weight of the luminescent powder to obtain activated SrAl2O4：Eu2+，Dy3+Luminescent powder;
(2) preparing the luminescent composite master batch: 10-90 parts by weight of PET polyester chip, 1-20 parts by weight of photosensitive color-changing powder and 1-30 parts by weight of activated SrAl2O4：Eu2+，Dy3+Mixing luminescent powder and 0.5-1.5 parts by weight of functional auxiliary agent, and granulating by adopting a double-screw granulator to obtain luminescent composite master batch for spinning;
(3) preparing the luminescent composite fiber: and (3) pre-drying the luminous composite master batch, and then carrying out melt spinning to obtain the spectrum blue-shift noctilucent fiber.
In some embodiments, in the first step, the baking temperature in the microwave calcining furnace is 300-500 ℃ and the baking time is 1-3 h.
In some embodiments, in the first step, the luminescence enhancer is one or more of rice hull carbon powder, volcanic powder and coconut shell carbon powder, and the particle size of the luminescence enhancer is 50-1000 nm.
In some embodiments, in step one, the coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560, and a silane coupling agent KH 570.
In some embodiments, in step two, the functional auxiliary agent is one or more of an antioxidant, a dispersant, and a heat stabilizer.
In some embodiments, in the second step, the photosensitive variable toner is a photosensitive variable blue powder.
In some embodiments, in the third step, the luminescent composite master batch and the PET polyester chip are mixed and dried according to the weight ratio of 1: 5-20, then melt-spun at the temperature of 220-280 ℃, and finally drawn and wound to obtain the spectrum blue-shift noctilucent fiber.
Compared with the prior art, the invention has the beneficial effects that: the luminous composite fiber obtained by the invention has double-emission spectrum phenomenon, is respectively positioned at 425nm and 520nm, and the wavelength is positioned in a blue region about 480nm after the double-spectrum superposition, so that the luminous fiber with spectrum blue shift is obtained, the application field of the luminous fiber is expanded, the luminous fiber can be used for blue light material products, in addition, the luminous composite fiber has better water washing resistance, and the afterglow brightness of the luminous composite fiber after water washing is only slightly reduced.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph of the emission spectrum of a spectrally blue-shifted luminescent fiber of the present invention;
FIG. 3 is a CIE 1931 chromaticity diagram;
FIG. 4 is the afterglow luminance graph before and after the water washing of the spectrum blue-shifted luminous fiber of the invention.
Detailed Description
The present invention is described in detail with reference to the embodiments shown in the drawings, but it should be understood that these embodiments are not intended to limit the present invention, and those skilled in the art should understand that functional, methodological, or structural equivalents or substitutions made by these embodiments are within the scope of the present invention.
The first embodiment is as follows:
the embodiment discloses a preparation method of a spectrum blue-shift noctilucent fiber, which comprises the following steps:
(1) activation treatment: mixing SrAl2O4：Eu2+，Dy3+Mixing luminescent powder and luminescent reinforcing agent according to the weight ratio of 0.5: 1, baking in a microwave calcining furnace to obtain composite powder, and then using relative SrAl2O4：Eu2+，Dy3+The coupling agent accounting for 5 percent of the weight of the luminescent powder is used for activating the composite powder to obtain activated SrAl2O4：Eu2+，Dy3+Luminescent powder.
Specifically, the baking temperature in the microwave calciner is 300 ℃, and the baking time is 1 h. The luminescence reinforcing agent is rice hull carbon powder, and the grain size of the luminescence reinforcing agent is 50 nm. The coupling agent is a silane coupling agent KH 550.
(2) Preparing the luminescent composite master batch: 10 parts by weight of PET polyester chip, 1 part by weight of photosensitive color-changing powder and 1 part by weight of activated SrAl2O4：Eu2+，Dy3+And mixing the luminescent powder and 0.5 part by weight of functional auxiliary agent, and granulating by adopting a double-screw granulator to obtain the luminescent composite master batch for spinning.
Specifically, the functional auxiliary agent is an antioxidant. The photosensitive color-changing powder is photosensitive blue-changing powder.
(3) Preparing the luminescent composite fiber: and (3) pre-drying the luminous composite master batch, and then carrying out melt spinning to obtain the spectrum blue-shift noctilucent fiber.
Specifically, the luminous composite master batch and the PET polyester chip are mixed and dried according to the weight ratio of 1: 5, then melt spinning is carried out at the temperature of 220 ℃, and finally drafting and winding are carried out to obtain the spectrum blue shift noctilucent fiber.
Example two:
the embodiment discloses a preparation method of a spectrum blue-shift noctilucent fiber, which comprises the following steps:
(1) activation treatment: mixing SrAl2O4：Eu2+，Dy3+Mixing luminescent powder and luminescent reinforcing agent according to the weight ratio of 3: 1, baking in a microwave calcining furnace to obtain composite powder, and then using relative SrAl2O4：Eu2+，Dy3+Activating the composite powder by a coupling agent accounting for 10 percent of the weight of the luminescent powder to obtain activated SrAl2O4：Eu2+，Dy3+Luminescent powder.
Specifically, the baking temperature in the microwave calcining furnace is 400 ℃, and the baking time is 2 h. The luminescence enhancer is volcano powder, and the particle size of the luminescence enhancer is 500 nm. The coupling agent is a silane coupling agent KH 560.
(2) Preparing the luminescent composite master batch: 50 parts by weight of PET polyester chip, 10 parts by weight of photosensitive toner and 15 parts by weight of activated SrAl2O4：Eu2+，Dy3+And mixing the luminescent powder and 1 part by weight of functional auxiliary agent, and granulating by using a double-screw granulator to obtain the luminescent composite master batch for spinning.
Specifically, the functional auxiliary agent is a dispersant. The photosensitive color-changing powder is photosensitive blue-changing powder.
(3) Preparing the luminescent composite fiber: and (3) pre-drying the luminous composite master batch, and then carrying out melt spinning to obtain the spectrum blue-shift noctilucent fiber.
Specifically, the luminous composite master batch and the PET polyester chip are mixed and dried according to the weight ratio of 1: 10, then melt spinning is carried out at the temperature of 250 ℃, and finally drafting and winding are carried out to obtain the spectrum blue shift noctilucent fiber.
Example three:
the embodiment discloses a preparation method of a spectrum blue-shift noctilucent fiber, which comprises the following steps:
(1) activation treatment: mixing SrAl2O4：Eu2+，Dy3+Mixing luminescent powder and luminescent reinforcing agent according to the weight ratio of 5: 1, baking in a microwave calcining furnace to obtain composite powder, and then using relative SrAl2O4：Eu2+，Dy3+The coupling agent accounting for 20 percent of the weight of the luminescent powder is used for activating the composite powder to obtain activated SrAl2O4：Eu2+，Dy3+Luminescent powder.
Specifically, the baking temperature in the microwave calciner is 500 ℃, and the baking time is 3 h. The luminescence reinforcing agent is coconut shell carbon powder, and the grain size of the luminescence reinforcing agent is 1000 nm. The coupling agent is a silane coupling agent KH 570.
(2) Preparing the luminescent composite master batch: 90 parts by weight of PET polyester chip, 20 parts by weight of photosensitive toner and 30 parts by weight of activated SrAl2O4：Eu2+，Dy3+And mixing the luminescent powder and 1.5 parts by weight of functional auxiliary agent, and granulating by using a double-screw granulator to obtain the luminescent composite master batch for spinning.
Specifically, the functional auxiliary agent is a heat stabilizer. The photosensitive color-changing powder is photosensitive blue-changing powder.
(3) Preparing the luminescent composite fiber: and (3) pre-drying the luminous composite master batch, and then carrying out melt spinning to obtain the spectrum blue-shift noctilucent fiber.
Specifically, the luminous composite master batch and the PET polyester chip are mixed and dried according to the weight ratio of 1: 20, then melt spinning is carried out at the temperature of 280 ℃, and finally drafting and winding are carried out to obtain the spectrum blue shift noctilucent fiber.
The luminescent composite fiber obtained by the invention can emit blue light for the following reasons:
one, composed of SrAl2O4：Eu2+，Dy3+The yellow-green light emitting center of the luminescent powder and the blue light emitting center of the photosensitive color powder are generated by overlapping the luminescent colors, and the light color obtained by matching the yellow-green light and the blue light by the light color addition principle belongs to a blue light area;
second, SrAl in the luminescent composite fiber2O4：Eu2+，Dy3+Luminescent powder and luminous powder both belong to inorganic substance and coupling agentIs an organosilicon compound containing an inorganophilic group on the surface, SrAl is treated with a coupling agent2O4：Eu2+，Dy3+After being activated, the luminescent powder is blended and spun with the photochromic powder, so that the adhesion and the dispersibility of the mixture can be improved, and a molecular bridge function can be realized, so that the energy transfer between two different types of electronic transitions in the luminescent composite fiber after being illuminated is caused, and the blue shift phenomenon of the spectrum is indirectly influenced.
Specifically, the emission spectrum of the photosensitive color-changing powder is well overlapped with the absorption spectrum of the rare earth ions, photosensitive molecular bonds in the photosensitive color-changing powder absorb light energy to open and jump to an excited state, and molecules in the excited state have redundant energy; due to the specific electronic configuration of the rare earth ions, the rare earth ions can receive energy from the photochromic powder and jump to an excited state, when electrons return to a ground state from the excited state, the characteristic fluorescence of each ion is emitted, and different spectra can achieve the purpose of adjusting the spectrum of the noctilucent fiber after superposition interference.
And (3) analyzing experimental data and results:
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is a graph showing the comparison between the emission spectrum of the luminescent composite fiber of the present invention and the emission spectrum of the luminescent fiber (without adding photosensitive color-changing powder), and fig. 3 is a graph showing the light color coordinates of the luminescent composite fiber and the luminescent fiber of the present invention. The observation shows that the light color area of the luminescent composite fiber is blue, the luminescent composite fiber has double-emission spectrum phenomena which are respectively positioned at 425nm and 520nm, and the wavelength of the superposed double-spectrum is positioned in the blue area of about 480nm, thereby further verifying that the spectrum of the luminescent composite fiber generates blue shift.
FIG. 4 is a graph showing afterglow luminance of the luminescent conjugate fiber before and after washing with water. It is observed that the afterglow brightness of the composite fiber after washing is slightly lowered owing to the organosilicon compound as the coupling agent and the inorganic radical contained in the surface of the fiber, and the coupling agent to SrAl2O4：Eu2+，Dy3+Activating the luminous powder and mixing with photosensitive color-changing powderThe blended spinning can not only improve the adhesiveness and the dispersibility between the mixtures, but also play a role of a molecular bridge, has larger bonding force, and SrAl2O4：Eu2+，Dy3+The luminescent powder and the photosensitive color-changing powder are not easy to fall off.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A preparation method of a spectrum blue-shift noctilucent fiber is characterized by comprising the following steps:
(1) activation treatment: mixing SrAl2O4：Eu2+，Dy3+Mixing luminescent powder and luminescent reinforcing agent according to the weight ratio of 0.5-5: 1, baking in a microwave calcining furnace to obtain composite powder, and then using relative SrAl2O4：Eu2+，Dy3+Activating the composite powder by a coupling agent accounting for 5-20% of the weight of the luminescent powder to obtain activated SrAl2O4：Eu2+，Dy3+Luminescent powder;
(2) preparing the luminescent composite master batch: 10-90 parts by weight of PET polyester chip, 1-20 parts by weight of photosensitive color-changing powder and 1-30 parts by weight of activated SrAl2O4：Eu2+，Dy3+Mixing luminescent powder and 0.5-1.5 parts by weight of functional auxiliary agent, and granulating by adopting a double-screw granulator to obtain luminescent composite master batch for spinning;
(3) preparing the luminescent composite fiber: and (3) pre-drying the luminous composite master batch, and then carrying out melt spinning to obtain the spectrum blue-shift noctilucent fiber.
2. The method for preparing the luminous fiber with the blue-shifted spectrum according to claim 1, wherein in the first step, the baking temperature in the microwave calcining furnace is 300-500 ℃ and the baking time is 1-3 h.
3. The preparation method of the spectrum blue-shift noctilucent fiber according to claim 1, wherein in the first step, the luminescence enhancer is one or more of rice hull carbon powder, volcanic powder and coconut shell carbon powder, and the particle size of the luminescence enhancer is 50-1000 nm.
4. The method for preparing the noctilucent fiber with blue-shifted spectrum according to claim 1, wherein in the first step, the coupling agent is one or more of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
5. The method for preparing the noctilucent fiber with blue shift of spectrum according to claim 1, wherein in the second step, the functional auxiliary agent is one or more of antioxidant, dispersant and heat stabilizer.
6. The method for preparing the spectrum blue-shift noctilucent fiber according to claim 1, wherein in the second step, the photosensitive color-changing powder is photosensitive blue-changing powder.
7. The method for preparing the noctilucent fiber with the spectrum blue shift as claimed in claim 1, wherein in the third step, the luminescent composite mother particle and the PET polyester chip are mixed and dried according to the weight ratio of 1: 5-20, then melt-spun at the temperature of 220-280 ℃, finally drawn and wound to obtain the noctilucent fiber with the spectrum blue shift.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102493017A (en) * | 2011-12-08 | 2012-06-13 | 江南大学 | Rare-earth silicate blue long-afterglow polyester fiber and preparation method thereof |
| CN103361763A (en) * | 2012-03-29 | 2013-10-23 | 江南大学 | Rare-earth-silicate long-blue-afterglow colored polyester fiber and preparation method thereof |
| CN105019049A (en) * | 2014-04-22 | 2015-11-04 | 上海纽恩特实业有限公司 | Luminous fiber-forming polymer |
| CN106192038A (en) * | 2016-07-21 | 2016-12-07 | 江南大学 | The preparation method of blue light luminous fiber |
| CN111155196A (en) * | 2020-01-03 | 2020-05-15 | 浙江颖诺泰材料科技有限公司 | Luminescent fiber based on recycled polyester material and preparation method thereof |
-
2021
- 2021-02-04 CN CN202110157846.6A patent/CN112941660A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102493017A (en) * | 2011-12-08 | 2012-06-13 | 江南大学 | Rare-earth silicate blue long-afterglow polyester fiber and preparation method thereof |
| CN103361763A (en) * | 2012-03-29 | 2013-10-23 | 江南大学 | Rare-earth-silicate long-blue-afterglow colored polyester fiber and preparation method thereof |
| CN105019049A (en) * | 2014-04-22 | 2015-11-04 | 上海纽恩特实业有限公司 | Luminous fiber-forming polymer |
| CN106192038A (en) * | 2016-07-21 | 2016-12-07 | 江南大学 | The preparation method of blue light luminous fiber |
| CN111155196A (en) * | 2020-01-03 | 2020-05-15 | 浙江颖诺泰材料科技有限公司 | Luminescent fiber based on recycled polyester material and preparation method thereof |
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