CN108589287A - A kind of in-situ preparation method of fluorescence cotton fiber - Google Patents
A kind of in-situ preparation method of fluorescence cotton fiber Download PDFInfo
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- CN108589287A CN108589287A CN201810285351.XA CN201810285351A CN108589287A CN 108589287 A CN108589287 A CN 108589287A CN 201810285351 A CN201810285351 A CN 201810285351A CN 108589287 A CN108589287 A CN 108589287A
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- cotton
- cotton fiber
- fluorescence
- solution
- situ preparation
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
The invention belongs to fluorescent material preparation fields, and in particular to a kind of in-situ preparation method of fluorescence cotton fiber.Specific method is：（1）Fixanol is dissolved in aqueous solution under room temperature, obtains transparent clear precursor solution；（2）The cotton of certain mass is immersed in above-mentioned solution, certain density strong base solution is added after cotton is soaked completely；（3）It is slowly stirred a period of time, cotton is taken out from solution, and centrifuges the aqueous solution in removal cotton；（4）Cotton fiber is cleaned to neutrality with clear water, and removes the Fixanol of remained unreacted, can be obtained the cotton fiber with uniform green fluorescence after dry.The preparation method of the present invention is simple, low production cost, and fluorescence cotton fiber obtained is stablized, and does not change the intensity of cotton, is had potential application in field of textiles.
Description
Technical field
The invention belongs to fluorescent fiber preparation field, more particularly to a kind of in-situ preparation method of fluorescence cotton fiber.
Background technology
Fluorescent fiber is a kind of fiber that fluorescence can be sent out under visible light or ultraviolet light, after light disappears its
Fluorescence also disappears, and is restored to original color.Currently, inorganic or organic fluorescence materials are mainly blended or are modified by fluorescent fiber
On fiber, or dispersion is in a polymer matrix, and the fluorescent fiber material with fluorescent emission is obtained by spining technology.It is glimmering
Luminescent material has preferable anti-fake effect and warning function, and therefore, the product made of fluorescent fiber can be applied widely
In the multiple fields such as road, traffic and the protective garment of working at height, warning sign, daily necessities, anti-fake material.
Currently used for manufacturing the main organic and/or inorganic materials of fluorescent material of fluorescent fiber（As terres rares fluorescent material, quantum dot,
Metal complex etc.）With organic fluorescence small molecule, high molecular fluorescent compound etc..But it should not be melted since inorganic fluorescent material has
Melt, easily reunite, difficult the features such as disperseing, therefore limiting its application in terms of fluorescent fiber preparation；Organic fluorescence molecule although
There is stronger fluorescence quantum yield, and have the characteristics that preferable dispersibility in the solution, but its maximum deficiency is exactly light
Stability is bad, is irradiated by long-time light, photobleaching phenomenon easily occurs, fluorescence weakens or disappears significantly, therefore also limits
It is widely applied.
Cotton fiber is a kind of natural plant fiber and the primary raw material of textile industry, due to its preferable moisture absorption
Property and gas permeability, there is preferable snugness of fit with its clothing for making of weaving.However, most of with reflective or glimmering at present
Protective garment of luminescent material etc. is by synthetic fibers（Such as polyesters, polypropylene）It prepares, this kind of textile is due to gas permeability
It is poor, smell is easy tod produce after dressing the long period, causes the discomfort of wearing.
The present invention is prepared in situ using cheap Fixanol as fluorescent material presoma on natural cotton fiber
Nano-sized carbon fluorescent material with green-fluorescent emission.Technology, the fluorescent material of fiber surface is prepared in situ due to using
It is not easily to fall off with higher adhesive ability；In addition, due to chemical property and optical property that fluorescence carbon nanomaterial is stablized,
Make the fluorescence cotton fiber that there is stronger fluorescent emission and anti-light bleaching power.In addition, this technology carries out at normal temperatures and pressures,
Simple to equipment requirement, cost is relatively low, is suitable for promoting and applying.
Invention content
The present invention provides a kind of in-situ preparation methods of fluorescence cotton fiber, are shone with solving conventional polymeric fluorescent fiber
It is uneven, stability is poor, is also easy to produce the problems such as photobleaching.
A kind of in-situ preparation method of fluorescence cotton fiber provided by the invention, includes the following steps：
（1）Fixanol and water are mixed, transparent clear precursor solution is stirred to get；
（2）The cotton of certain mass is totally submerged in above-mentioned solution, strong base solution is added after cotton is soaked completely；
（3）It is slowly stirred a period of time under room temperature or heating condition, cotton is taken out from solution, and centrifuges in removal cotton
Solution；
（4）Cotton fiber is washed with water, unreacted Fixanol is removed, the cotton that green fluorescence is can be obtained after dry is fine
Dimension.
Above-mentioned steps（1）Described in Fixanol be dococylpyridinium, tetradecylpyridinium, cetyl pyridinium
One or more of hydrochloride or bromate.
Above-mentioned steps（1）Described in Fixanol concentration be more than 10 mmol/L.
Above-mentioned steps（2）Described in strong base solution be NaOH, KOH, Ca (OH)2One or more of solution.
Above-mentioned steps（2）Described in strong base solution concentration be more than 0.1 mol/L.
Above-mentioned steps（3）Described in heating temperature range be 20 ~ 100 degrees Celsius.
Above-mentioned steps（3）Described in mixing time >=0.5 hour.
Above-mentioned steps（4）In, cotton fiber is washed with water to ranging from 6.5≤pH≤8 pH）.
Above-mentioned steps（4）Described in drying be drying at room temperature or vacuum drying.
The present invention is fluorescence presoma using Fixanol that is of low cost and being easy to get, using the method system being prepared in situ
Standby fluorescence cotton fiber, whole process carries out under normal temperature and pressure conditions, easy to operate, relatively low to equipment requirement, therefore, this side
Method production cost is relatively low, and pole prepares fluorescence cotton fiber suitable for high-volume scale.
Fluorescence cotton fiber prepared by the present invention shines uniformly, has stronger fluorescent emission and preferable photostability,
Its textile has in the multiple fields such as road, traffic and the protective garment of working at height, warning sign, daily necessities, anti-fake material
It is widely applied foreground.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the cotton fiber (A) and fluorescence cotton fiber (B) used in the present invention.
Fig. 2 is fluorescence picture of the fluorescence cotton fiber of the invention prepared under the ultra violet lamp of 365nm.
Specific implementation mode
Following embodiments are the further explanations for the content of present invention, using as the explanation to the technology of the present invention content,
But the present invention substantive content be not limited in described in following embodiments, those skilled in the art can with and should know
Any simple change or replacement based on true spirit should all belong to protection domain of the presently claimed invention.
Embodiment 1
（1）0.5370 g hexadecylpyridinium chlorides are added in the deionized water of 100 mL under room temperature, stir to get clarification
Aqueous solution, a concentration of 15 mmol/L of cetyl pyridinium salt；
（2）The cotton of 10 g is totally submerged in above-mentioned solution, the NaOH that 10 mL, 2 mol/L are added after soaking completely is molten
Liquid；
（3）It is slowly stirred 10 hours, cotton is taken out from solution, clean cotton fiber to weakly acidic pH with clear water, be then centrifuged for
The moisture of cotton absorption is removed, can be obtained the cotton fiber with uniform green fluorescence after drying at room temperature.
Embodiment 2
（1）1.2078 g dococylpyridinium hydrochlorides are added in the deionized water of 200 mL under room temperature, are stirred to get clear
Clear aqueous solution, a concentration of 20 mmol/L of dococylpyridinium salt；
（2）The cotton of 30 g is totally submerged in above-mentioned solution, the KOH solution of 20 mL, 2 mol/L is added after soaking completely；
（3）It is slowly stirred 5 hours, cotton is taken out from solution, clean cotton fiber to weakly acidic pH with clear water, be then centrifuged for
Except the moisture of cotton absorption, the cotton fiber with uniform green fluorescence can be obtained after drying at room temperature.
Embodiment 3
（1）1.2102 g dococylpyridinium hydrochlorides are added in the deionized water of 200 mL under room temperature, are stirred to get clear
Clear aqueous solution, a concentration of 20 mmol/L of dococylpyridinium salt；
（2）The cotton of 30 g is totally submerged in above-mentioned solution, the KOH solution of 20 mL, 2 mol/L is added after soaking completely；
（3）80 degrees Celsius are heated to, is slowly stirred 1 hour, cotton is taken out from solution, cotton fiber is cleaned to close with clear water
Neutrality is then centrifuged for the moisture of removal cotton absorption, can be obtained the cotton fiber with homogeneous yellow fluorescence after drying at room temperature.
Evaluation further illustrates the present invention reached effect by experiment test.
Fluorescence cotton fiber prepared by above-described embodiment 1 is scanned Electronic Speculum test characterization, and the cotton fibre before preparation
Dimension is compared, and pattern does not change（Fig. 1）, it was demonstrated that the preparation process of fluorescence cotton fiber does not have shadow to its fibre structure
It rings.
Under the irradiation of ultraviolet lamp（Wavelength：365nm）, fluorescence cotton fiber prepared by above-described embodiment 2 is with stronger
Yellow-green fluorescence（Fig. 2）, and it is uniform to shine, it was demonstrated that fluorescence cotton fiber fluorescence property prepared by the present invention is excellent.
Claims (9)
1. a kind of in-situ preparation method of fluorescence cotton fiber, includes the following steps：
（1）Fixanol and water are mixed, transparent clear precursor solution is stirred to get；
（2）The cotton of certain mass is totally submerged in above-mentioned solution, strong base solution is added after cotton is soaked completely；
（3）It is slowly stirred a period of time under room temperature or heating condition, cotton is taken out from solution, and centrifuges in removal cotton
Solution；
（4）Cotton fiber is washed with water, unreacted Fixanol is removed, the cotton that green fluorescence is can be obtained after dry is fine
Dimension.
2. a kind of in-situ preparation method of fluorescence cotton fiber according to claim 1, it is characterised in that step（1）Middle institute
The Fixanol stated is one kind in dococylpyridinium, tetradecylpyridinium, cetyl pyridinium hydrochloride or bromate
Or it is several.
3. a kind of in-situ preparation method of fluorescence cotton fiber according to claim 1 or 2, it is characterised in that step（1）
Described in Fixanol concentration be more than 10 mmol/L.
4. according to a kind of in-situ preparation method of fluorescence cotton fiber of claim 1-3 any one of them, it is characterised in that step
Suddenly（2）Described in strong base solution be NaOH, KOH, Ca (OH)2One or more of solution.
5. according to a kind of in-situ preparation method of fluorescence cotton fiber of claim 1-4 any one of them, it is characterised in that step
Suddenly（2）Described in strong base solution concentration be more than 0.1 mol/L.
6. according to a kind of in-situ preparation method of fluorescence cotton fiber of claim 1-5 any one of them, it is characterised in that step
Suddenly（3）Described in heating temperature range be 20 ~ 100 degrees Celsius.
7. according to a kind of in-situ preparation method of fluorescence cotton fiber of claim 1-6 any one of them, it is characterised in that step
Suddenly（3）Described in mixing time >=0.5 hour.
8. according to a kind of in-situ preparation method of fluorescence cotton fiber of claim 1-7 any one of them, it is characterised in that step
Suddenly（4）In, cotton fiber is washed with water to ranging from 6.5≤pH≤8 pH.
9. according to a kind of in-situ preparation method of fluorescence cotton fiber of claim 1-8 any one of them, it is characterised in that step
Suddenly（4）Described in drying be drying at room temperature or vacuum drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810285351.XA CN108589287A (en) | 2018-04-03 | 2018-04-03 | A kind of in-situ preparation method of fluorescence cotton fiber |
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| CN201810285351.XA CN108589287A (en) | 2018-04-03 | 2018-04-03 | A kind of in-situ preparation method of fluorescence cotton fiber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266315A (en) * | 2018-10-17 | 2019-01-25 | 中北大学 | A kind of preparation method of carbon dots base photothermal conversion materiat |
| CN109453748A (en) * | 2018-12-05 | 2019-03-12 | 四川大学 | The modified iodine adsorbent material of efficiently reversible fat-soluble carbon dots, preparation and application |
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| EP1479797A1 (en) * | 2003-05-22 | 2004-11-24 | Landqart | Photoluminescent fibre, security paper and other security articles |
| CN101173272A (en) * | 2007-10-12 | 2008-05-07 | 中国农业科学院棉花研究所 | Cotton DNA fibre hybridization in situ technique |
| WO2012012813A1 (en) * | 2010-07-27 | 2012-02-02 | Lenzing Ag | Fluorescent fibres and their use |
| CN104591129A (en) * | 2015-01-12 | 2015-05-06 | 四川大学 | Method for preparing hydrophobic carbon quantum dots on large scale under ambient temperature condition |
| CN107747212A (en) * | 2017-11-24 | 2018-03-02 | 福州大学 | A kind of preparation method of the fluorescent fiber based on perovskite quantum dot |
-
2018
- 2018-04-03 CN CN201810285351.XA patent/CN108589287A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1479797A1 (en) * | 2003-05-22 | 2004-11-24 | Landqart | Photoluminescent fibre, security paper and other security articles |
| CN101173272A (en) * | 2007-10-12 | 2008-05-07 | 中国农业科学院棉花研究所 | Cotton DNA fibre hybridization in situ technique |
| WO2012012813A1 (en) * | 2010-07-27 | 2012-02-02 | Lenzing Ag | Fluorescent fibres and their use |
| CN104591129A (en) * | 2015-01-12 | 2015-05-06 | 四川大学 | Method for preparing hydrophobic carbon quantum dots on large scale under ambient temperature condition |
| CN107747212A (en) * | 2017-11-24 | 2018-03-02 | 福州大学 | A kind of preparation method of the fluorescent fiber based on perovskite quantum dot |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266315A (en) * | 2018-10-17 | 2019-01-25 | 中北大学 | A kind of preparation method of carbon dots base photothermal conversion materiat |
| CN109266315B (en) * | 2018-10-17 | 2020-11-03 | 中北大学 | Preparation method of carbon dot-based photothermal conversion material |
| CN109453748A (en) * | 2018-12-05 | 2019-03-12 | 四川大学 | The modified iodine adsorbent material of efficiently reversible fat-soluble carbon dots, preparation and application |
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