CN110373738A - A kind of preparation method of warm colour light luminescent fibre - Google Patents
A kind of preparation method of warm colour light luminescent fibre Download PDFInfo
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- CN110373738A CN110373738A CN201910765498.3A CN201910765498A CN110373738A CN 110373738 A CN110373738 A CN 110373738A CN 201910765498 A CN201910765498 A CN 201910765498A CN 110373738 A CN110373738 A CN 110373738A
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- preparation
- warm colour
- color conversion
- colour light
- conversion agent
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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
- D01F6/90—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 polyamides
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Luminescent Compositions (AREA)
Abstract
It is choice of powder shape spinning-grade polyamide fibre PA6 as fiber base material, by itself and SrAl the invention discloses a kind of preparation method of warm colour light luminescent fibre2O4:Eu2+,Dy3+Luminescent material and the Coumarins Color Conversion agent for using tetraethyl orthosilicate (TEOS) to coat are sufficiently mixed, the warm colour light luminescent fibre is made through melt spinning, it can obtain a variety of photochromic warm colour luminescent fibres by adjusting the mass ratio of Color Conversion agent and PA6.
Description
Technical field
The invention belongs to fibrous material preparation fields, and in particular to a kind of preparation method of warm colour light luminescent fibre.
Background technique
SrAl2O4:Eu2+, Dy3+The most mature long afterglow of best, preparation process as luminescent properties currently on the market
Luminescent material is the most important luminescent material source of current luminescent fibre.But SrAl2O4:Eu2+, Dy3+It is photochromic predominantly Huang
It is photochromic to belong to cool colour for green.With the development of textile and apparel enterprise, the luminescent fibre of single yellow green is no longer satisfied people
For different photochromic textiles demand, people prefer the color of the warm colours such as yellow, orange, red, it is desirable to have
A variety of photochromic luminescent fibres are available.Although researcher attempts by using new synthesis technology, new rare earth addition
Material prepares the rare earth long-afterglow luminescent material of different warm colour light.But mostly light emission luminance is low, and persistence is short, Wu Faman
The production application requirement of sufficient luminescent fibre.Therefore, the warm colour light luminescent fibre for preparing good luminescence property is still the fibre that shines at present
Dimension field urgent need to solve the problem.
Summary of the invention
Against the above technical problems, the present invention proposes a kind of preparation method of warm colour light luminescent fibre.The present invention is with luminous energy
Conversion and photochromic synergistic effect are theoretical foundation, in SrAl2O4:Eu2+, Dy3+ On the basis of luminescent fibre, during the spinning process
Pass through Color Conversion agent by different proportion and SrAl2O4:Eu2+, Dy3+Luminescent material is blended, and can prepare with a variety of warm colours
The luminescent fibre of fluorescence.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of warm colour light luminescent fibre comprising following preparation step:
(1) TEOS of certain mass the preparation of tetraethyl orthosilicate (TEOS) solution: is dissolved in dehydrated alcohol and deionized water
In mixed solution, after stirring 20-30 minutes under room temperature, the dilution heat of sulfuric acid that 1mol/L is added adjusts pH value to 3-4；
(2) it is molten that the TEOS that step (1) is prepared the cladding of Color Conversion agent: is added in the Coumarins Color Conversion agent of certain mass
In liquid, it is transferred in three-necked flask, 60-70 DEG C of heating water bath stirs 1.5-2 hours, to filter after reaction, products therefrom
It is washed with deionized 3-4 times, 60-70 DEG C is dried for standby；
(3) preparation of spinning raw material: weighing the PA6 powder of certain mass, is placed in 100-110 DEG C of vacuum drying oven dry
10-12 hours, after taking-up with SrAl2O4:Eu2+,Dy3+Luminescent material and step (2) the Color Conversion agent obtained coated
It is sufficiently mixed, and adds a certain amount of low molecule wax class dispersing agent；
(4) melt spinning: the spinning raw material that step (3) are prepared are added melt spinning machine and carry out melt spinning, obtain described
Warm colour light luminescent fibre.By adjusting the mass ratio of Color Conversion agent and PA6, the luminous fibre of a variety of photochromic warm colours can be obtained
Dimension.
The molar ratio of TEOS used, dehydrated alcohol and deionized water are 1:(30-35 in step (1)): (15-20).
The mass ratio of Coumarins Color Conversion agent used and TEOS are 1:(5-7 in step (2)).
PA6 powder and SrAl used in step (3)2O4:Eu2+,Dy3+Luminescent material, the Color Conversion agent coated matter
Amount is than being 100:8:(0.1-1.4).Wherein, the SrAl2O4:Eu2+,Dy3+The partial size of luminescent material is 6-8 μm, the cladding
The partial size of good Color Conversion agent is 2-3 μm, and the specification of the PA6 powder is spinning-grade.Low-molecular-weight wax class dispersing agent be added
Amount be three kinds of material total weights 0.1%-0.2%.
A kind of warm colour light luminescent fibre prepared by the present invention has excellent luminescent properties.By adjust PA6 powder with
SrAl2O4:Eu2+,Dy3+Luminescent material and the mass ratio of Color Conversion agent can be prepared with a variety of different warm colour fluorescence
Luminescent fibre.
Detailed description of the invention
Fig. 1 is the launching light spectrogram of warm colour light luminescent fibre obtained by 1-4 of the embodiment of the present invention.
Fig. 2 is the luminous photo of warm colour light luminescent fibre in a dark environment obtained by 1-4 of the embodiment of the present invention.
Fig. 3 is the fluorescence color chromaticity coordinate of warm colour light luminescent fibre obtained by 1-4 of the embodiment of the present invention.
Fig. 4 is the decay of afterglow curve of warm colour light luminescent fibre obtained by 1-4 of the embodiment of the present invention.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1:
A kind of preparation method of warm colour light luminescent fibre, comprising the following steps:
(1) it is 1:30:15 by the molar ratio of TEOS and dehydrated alcohol and water, TEOS is dissolved in the mixed of dehydrated alcohol and deionized water
It closes in solution, is stirred under room temperature after twenty minutes, adjust its pH value to 3 with the dilution heat of sulfuric acid of 1mol/L；
It (2) is what 1:5 prepared Coumarins Color Conversion agent addition step (1) by the mass ratio of Color Conversion agent and TEOS
It in TEOS solution, is transferred in three-necked flask, 60 DEG C of heating water baths stir 2 hours, to filter after reaction, and use deionization
After water washing 3 times, 60 DEG C are dried for standby；
(3) weigh PA6 powder, be placed in 100 DEG C of vacuum drying oven it is 12 hours dry, after taking-up by PA6 powder with
SrAl2O4:Eu2+,Dy3+Luminescent material and the mass ratio of Color Conversion agent are 100:8:0.1, by PA6 powder and SrAl2O4:
Eu2+,Dy3+The Color Conversion agent of luminescent material and step (2) preparation coated is sufficiently mixed, while the gross weight that adds materials
The low molecule wax class dispersing agent of amount 0.1%；
(4) the spinning raw material for preparing step (3) are added melt spinning machine and carry out melt spinning, and it is luminous to obtain a kind of warm colour light
Fiber is denoted as 1#(0.1%).
Embodiment 2:
A kind of preparation method of warm colour light luminescent fibre, comprising the following steps:
(1) it is 1:35:20 by the molar ratio of TEOS and dehydrated alcohol and water, TEOS is dissolved in the mixed of dehydrated alcohol and deionized water
It closes in solution, is stirred under room temperature after twenty minutes, adjust its pH value to 4 with the dilution heat of sulfuric acid of 1mol/L；
It (2) is what 1:6 prepared Coumarins Color Conversion agent addition step (1) by the mass ratio of Color Conversion agent and TEOS
In TEOS solution, be transferred in three-necked flask, 70 DEG C of heating water baths stir 1.5 hours, to filter after reaction, and spend from
After sub- water washing 4 times, 70 DEG C are dried for standby；
(3) weigh PA6 powder, be placed in 100 DEG C of vacuum drying oven it is 12 hours dry, after taking-up by PA6 powder with
SrAl2O4:Eu2+,Dy3+Luminescent material and the mass ratio of Color Conversion agent are 100:8:0.6, by PA6 powder and SrAl2O4:
Eu2+,Dy3+The Color Conversion agent of luminescent material and step (2) preparation coated is sufficiently mixed, while the gross weight that adds materials
Measure 0.1% low molecule wax class dispersing agent；
(4) the spinning raw material for preparing step (3) are added melt spinning machine and carry out melt spinning, and it is luminous to obtain a kind of warm colour light
Fiber is denoted as 2#(0.6%).
Embodiment 3:
A kind of preparation method of warm colour light luminescent fibre, comprising the following steps:
(1) it is 1:30:20 by the molar ratio of TEOS and dehydrated alcohol and water, TEOS is dissolved in the mixed of dehydrated alcohol and deionized water
It closes in solution, after stirring 30 minutes under room temperature, adjusts its pH value to 3 with the dilution heat of sulfuric acid of 1mol/L；
It (2) is what 1:7 prepared Coumarins Color Conversion agent addition step (1) by the mass ratio of Color Conversion agent and TEOS
It in TEOS solution, is transferred in three-necked flask, 60 DEG C of heating water baths stir 2 hours, to filter after reaction, and use deionization
After water washing 3 times, 70 DEG C are dried for standby；
(3) weigh PA6 powder, be placed in 110 DEG C of vacuum drying oven it is 11 hours dry, after taking-up by PA6 powder with
SrAl2O4:Eu2+,Dy3+Luminescent material and the mass ratio of Color Conversion agent are 100:8:1.0, by PA6 powder and SrAl2O4:
Eu2+,Dy3+The Color Conversion agent of luminescent material and step (2) preparation coated is sufficiently mixed, while the gross weight that adds materials
Measure 0.3% low molecule wax class dispersing agent；
(4) the spinning raw material for preparing step (3) are added melt spinning machine and carry out melt spinning, and it is luminous to obtain a kind of warm colour light
Fiber is denoted as 3#(1.0%).
Embodiment 4:
A kind of preparation method of warm colour light luminescent fibre, comprising the following steps:
(1) it is 1:35:15 by the molar ratio of TEOS and dehydrated alcohol and water, TEOS is dissolved in the mixed of dehydrated alcohol and deionized water
It closes in solution, after stirring 30 minutes under room temperature, adjusts its pH value to 4 with the dilution heat of sulfuric acid of 1mol/L；
It (2) is what 1:7 prepared Coumarins Color Conversion agent addition step (1) by the mass ratio of Color Conversion agent and TEOS
It in TEOS solution, is transferred in three-necked flask, 70 DEG C of heating water baths stir 2 hours, to filter after reaction, and use deionization
After water washing 4 times, 60 DEG C are dried for standby；
(3) weigh PA6 powder, be placed in 110 DEG C of vacuum drying oven it is 10 hours dry, after taking-up by PA6 powder with
SrAl2O4:Eu2+,Dy3+Luminescent material and the mass ratio of Color Conversion agent are 100:8:1.4, by PA6 powder and SrAl2O4:
Eu2+,Dy3+The Color Conversion agent of luminescent material and step (2) preparation coated is sufficiently mixed, while the gross weight that adds materials
Measure 0.3% low molecule wax class dispersing agent；
(4) the spinning raw material for preparing step (3) are added melt spinning machine and carry out melt spinning, and it is luminous to obtain a kind of warm colour light
Fiber is denoted as 4#(1.4%).
Fig. 1 is a kind of launching light spectrogram of warm colour light luminescent fibre obtained by embodiment 1-4.It can be seen that with photochromic
The increase of conversion agent adding proportion, maximum emission wavelength gradually red shift.When the mass fraction of Color Conversion agent is respectively 0.1%,
0.6%, 1.0%, when 1.4%, corresponding emission maximum optical wavelength is respectively 578nm, 591nm, 596nm, 600nm.
Fig. 2 is a kind of luminous photo of warm colour light luminescent fibre of embodiment 1-4 gained in a dark environment.By can in figure
See, the luminescent color of 4 groups of luminescent fibres in a dark environment is respectively pale yellow, yellow, pink, orange red.
Fig. 3 is a kind of fluorescence color chromaticity coordinate of warm colour light luminescent fibre obtained by embodiment 1-4.It can be seen that 4 groups
The chromaticity coordinate of luminescent fibre is located at pale yellow coloured light area, sodium yellow area, pink area, orange-red light area.
Fig. 4 is a kind of decay of afterglow curve of warm colour light luminescent fibre obtained by embodiment 1-4.It can be seen that with light
The initial luminous brightness of the increase of color conversion agent adding proportion, 4 groups of warm colour fiber optics is gradually reduced.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (5)
1. a kind of preparation method of warm colour light luminescent fibre, it is characterised in that: including following preparation step:
(1) tetraethyl orthosilicate of certain mass the preparation of tetraethyl orthosilicate solution: is dissolved in dehydrated alcohol and deionized water
Mixed solution in, after stirring 20-30 minutes under room temperature, the dilution heat of sulfuric acid that 1mol/L is added adjusts pH value to 3-4；
(2) the positive silicic acid that step (1) is prepared the cladding of Color Conversion agent: is added in the Coumarins Color Conversion agent of certain mass
In tetrem ester solution, 60-70 DEG C of heating water bath is stirred 1.5-2 hours, to filter after reaction, products therefrom deionized water
Washing 3-4 times, 60-70 DEG C is dried for standby；
(3) preparation of spinning raw material: weighing the PA6 powder of certain mass, is placed in 100-110 DEG C of vacuum drying oven dry
10-12 hours, after taking-up with SrAl2O4:Eu2+,Dy3+Luminescent material and step (2) the Color Conversion agent obtained coated
It is sufficiently mixed, and adds a certain amount of low molecule wax class dispersing agent；
(4) melt spinning: the spinning raw material that step (3) are prepared are added melt spinning machine and carry out melt spinning, obtain described
Warm colour light luminescent fibre.
2. a kind of preparation method of warm colour light luminescent fibre as described in claim 1, it is characterised in that: used in step (1)
The molar ratio of tetraethyl orthosilicate, dehydrated alcohol and deionized water is 1:(30-35): (15-20).
3. a kind of preparation method of warm colour light luminescent fibre as described in claim 1, it is characterised in that: used in step (2)
The mass ratio of the agent of Coumarins Color Conversion and tetraethyl orthosilicate is 1:(5-7).
4. a kind of preparation method of warm colour light luminescent fibre as described in claim 1, it is characterised in that: used in step (3)
PA6 powder and SrAl2O4:Eu2+,Dy3+Luminescent material, the Color Conversion agent coated mass ratio be 100:8:(0.1-1.4)；
The amount of low-molecular-weight wax class dispersing agent be added is the 0.1%-0.2% of above-mentioned three kinds of material total weights.
5. a kind of preparation method of warm colour light luminescent fibre as described in claim 1 or 4, it is characterised in that: described
SrAl2O4:Eu2+,Dy3+The partial size of luminescent material is 6-8 μm, and the partial size of the Color Conversion agent coated is 2-3 μm, institute
The specification for stating PA6 powder is spinning-grade.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910765498.3A CN110373738B (en) | 2019-08-19 | 2019-08-19 | Preparation method of warm color light emitting optical fiber |
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| CN201910765498.3A CN110373738B (en) | 2019-08-19 | 2019-08-19 | Preparation method of warm color light emitting optical fiber |
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| CN110373738B CN110373738B (en) | 2021-12-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113213931A (en) * | 2021-05-08 | 2021-08-06 | 南通大学 | Transparent ceramic optical fiber preparation method based on Isobam gel and melt spinning technology |
| CN115557780A (en) * | 2022-10-21 | 2023-01-03 | 苏州璋驰光电科技有限公司 | Color-adjustable light-storing ceramic and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1488790A (en) * | 2003-08-07 | 2004-04-14 | 东华大学 | Long-persistence/mminous polyamide fiber and preparing method thereof |
| CN105780169A (en) * | 2016-03-09 | 2016-07-20 | 江南大学 | Preparation method of long afterglow fluorescent fibers emitting red light |
| CN106010532A (en) * | 2016-06-03 | 2016-10-12 | 江南大学 | Method for preparing high-brightness red light long afterglow luminous material |
-
2019
- 2019-08-19 CN CN201910765498.3A patent/CN110373738B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1488790A (en) * | 2003-08-07 | 2004-04-14 | 东华大学 | Long-persistence/mminous polyamide fiber and preparing method thereof |
| CN105780169A (en) * | 2016-03-09 | 2016-07-20 | 江南大学 | Preparation method of long afterglow fluorescent fibers emitting red light |
| CN106010532A (en) * | 2016-06-03 | 2016-10-12 | 江南大学 | Method for preparing high-brightness red light long afterglow luminous material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113213931A (en) * | 2021-05-08 | 2021-08-06 | 南通大学 | Transparent ceramic optical fiber preparation method based on Isobam gel and melt spinning technology |
| CN115557780A (en) * | 2022-10-21 | 2023-01-03 | 苏州璋驰光电科技有限公司 | Color-adjustable light-storing ceramic and preparation method thereof |
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| CN110373738B (en) | 2021-12-03 |
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