CN109762073A - The preparation method of fluorescent fiber element nanofiber - Google Patents
The preparation method of fluorescent fiber element nanofiber Download PDFInfo
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- CN109762073A CN109762073A CN201910028293.7A CN201910028293A CN109762073A CN 109762073 A CN109762073 A CN 109762073A CN 201910028293 A CN201910028293 A CN 201910028293A CN 109762073 A CN109762073 A CN 109762073A
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- fiber element
- fluorescent fiber
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Abstract
It is that cellulosic material is added in reaction solution the invention discloses the preparation method of fluorescent fiber element nanofiber, oil bath heating is condensed back the reaction regular hour, and cellulose surface is made to be grafted upper specific functional group；Then mixture washed, filtered, collect solid product, then be dried, fluorescent fiber element nanofiber powder is made.Preparation method of the present invention is simple, and operation is easy, mild condition, and agents useful for same corrodes small, no pollution to the environment to equipment, and fluorescent fiber element nanofiber yield is high, and fluorescence efficiency is high, and stability is good, biodegradable, good biocompatibility.
Description
Technical field
The invention belongs to natural polymers and field of textiles, and in particular to the preparation method of fluorescent fiber element nanofiber.
Background technique
Currently, the preparation method of fluorescent fiber mainly in fibre substrate be added fluorescent powder be blended, then again into
Row spinning.There are many types, including inorganic particle, small organic molecule, rare earth fluorescent compounds and organic macromolecule for fluorescent material
Fluorescent chemicals.Although inorganic particle fluorescence property is preferable, their dispersion performances in fibre substrate are poor, are easy shape
At reunion；Although good dispersion of the organic compound in fibre-forming polymer, their fluorescence efficiency are lower.Many researchs
Rare earth fluorescent compounds are added in fibre substrate by person, prepare fluorescent fiber using melt spinning or wet therapy forming process.This
Although the fluorescent fiber prepared a bit has certain fluorescence property, because the fluorescent material used is only dispersed in fiber
Stromal surface does not form firm Covalent bonding together with fiber, therefore when by outside stimulus such as chemical reagent, radiation, glimmering
Fiber optics is easy to lose fluorescence property.Compel so developing the fluorescent nano-fiber that novel fluorescence efficiency is high, stability is good
The eyebrows and eyelashes.
Cellulose nano-fibrous is from natural polymer -- the nanofiber with nanoscale extracted in cellulose,
It has high intensity, high-crystallinity, high transparency, high reaction activity, and light weight, biodegradable.Cellulose Nanowire
More high activity hydroxyl is contained in dimension table face, therefore its reactivity is high, it is easy in its surface grafting functional group.With fiber
Plain nanofiber is matrix, the specific fluorophor on its surface grafting, so that it may assign fiber with fluorescence property, while this is glimmering
Light nanofiber has cellulose nano-fibrous high-intensitive and good biocompatibility, can be applied to bio-imaging, biology
The fields such as detection.
Summary of the invention
The present invention is to solve the deficiency of existing fluorescent fiber performance and preparation method, provides fluorescent fiber element nanofiber
Preparation method.This method process is simple, operation be easy, mild condition, agents useful for same to equipment corrode it is small, to environment without dirt
Dye, fluorescent fiber element nanofiber yield is high, and fluorescence efficiency is high, and stability is good, biodegradable, good biocompatibility.
To achieve the above object, the present invention adopts the following technical scheme:
The preparation method of fluorescent fiber element nanofiber, comprising the following steps:
(1) preparation of reaction solution: serine being added in aqueous solution with citric acid and is sufficiently mixed, 60 DEG C of heating water bath stirrings, shape
At homogeneous and transparent solution；
(2) cellulosic material is added in reaction solution, oil bath heating, is condensed back the reaction regular hour, makes cellulose table
Face is grafted upper specific functional group；
(3) mixture that step (2) obtains washed with deionized water, filtered, collect solid product；
(4) solid product in step (3) is put into drying box and is dried, obtain fluorescent fiber element nano-cellulose powder
End.
The molar ratio of serine described in step (1) and citric acid is 1:1-1:10, and serine and citric acid are in aqueous solution
In final concentration of 2-6 mol/L, the mixing time be 10-50 min.
Cellulosic material described in step (2) includes nano-cellulose, nano cellulose crystal, microcrystalline cellulose, nanometer
Crystal fibre element in any one.
The mass fraction of cellulosic material is 1-5% in reaction solution described in step (2).Oil bath described in step (2) adds
Hot temperature is 80-120 DEG C, and the condensing reflux reaction time is 1-10h.Drying temperature in step (4) is 70-100 DEG C, when dry
Between be 5-12h.
Remarkable advantage of the invention:
(1) process of the present invention is simple, and operation is easy, and preparation condition is mild, corrodes small, no pollution to the environment to equipment；
(2) fluorescent fiber element nanofiber yield prepared by the present invention is high, and fluorescence efficiency is high, and stability is good, biodegradable, raw
Object compatibility is good.
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
The preparation of reaction solution: 0.2mol serine being added in 200mL aqueous solution with 0.2mol citric acid and is uniformly mixed, and 60 DEG C
30min is sufficiently stirred in heating water bath, forms homogeneous and transparent solution.
2g nano-cellulose is added in 50g reaction solution, 80 DEG C of condensing refluxes react 9h, then spend reaction product
Ionized water is washed, is filtered, and solid product is collected；The solid product of collection is put into drying box, 80 DEG C of dry 11h are obtained
To fluorescent fiber element nanofiber.The yield of fluorescent fiber element nanofiber is 80%, diameter 5-10nm, length 100-300nm.
Embodiment 2
The preparation of reaction solution: 1mol serine being added in 500mL aqueous solution with 2mol citric acid and is uniformly mixed, 60 DEG C of water-baths
50min is sufficiently stirred in heating, forms homogeneous and transparent solution.
5g nanocrystal cellulose is added in 200g reaction solution, 100 DEG C of condensing refluxes react 8h, then produce reaction
Object is washed with deionized water, is filtered, and solid product is collected；The solid product of collection is put into drying box, 90 DEG C of dryings
7h obtains fluorescent fiber element nanofiber.The yield of fluorescent fiber element nanofiber is 78%, diameter 10-20nm, length 200-
500nm。
Embodiment 3
The preparation of reaction solution: 0.5mol serine being added in 600mL aqueous solution with 2mol citric acid and is uniformly mixed, 60 DEG C of water
25min is sufficiently stirred in bath heating, forms homogeneous and transparent solution.
3g nano cellulose crystal is added in 100g reaction solution, 110 DEG C of condensing refluxes react 3h, then produce reaction
Object is washed with deionized water, is filtered, and solid product is collected；The solid product of collection is put into drying box, 100 DEG C of dryings
5h obtains fluorescent fiber element nanofiber.The yield of fluorescent fiber element nanofiber is 85%, diameter 5-7nm, length 100-
150nm。
Embodiment 4
The preparation of reaction solution: 0.1mol serine being added in 300mL aqueous solution with 1mol citric acid and is uniformly mixed, 60 DEG C of water
40min is sufficiently stirred in bath heating, forms homogeneous and transparent solution.
2.5g microcrystalline cellulose is added in 150g reaction solution, 90 DEG C of condensing refluxes react 7h, then by reaction product
It washed, filtered with deionized water, collect solid product；The solid product of collection is put into drying box, 70 DEG C of dryings
12h obtains fluorescent fiber element nanofiber.The yield of fluorescent fiber element nanofiber is 82%, diameter 15-25nm, length 250-
350nm。
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 (6)
1. the preparation method of fluorescent fiber element nanofiber, it is characterised in that: the following steps are included:
(1) preparation of reaction solution: serine being added in aqueous solution with citric acid and is sufficiently mixed, 60 DEG C of heating water bath stirrings, shape
At homogeneous and transparent solution；
(2) cellulosic material is added in reaction solution, oil bath heating, is condensed back the reaction regular hour, makes cellulose table
Face is grafted upper specific functional group；
(3) mixture that step (2) obtains washed with deionized water, filtered, collect solid product；
(4) solid product in step (3) is put into drying box and is dried, obtain fluorescent fiber element nano-cellulose powder
End.
2. the preparation method of fluorescent fiber element nanofiber according to claim 1, it is characterised in that: in step (1)
The molar ratio of the serine and citric acid is 1:1-1:10, serine and the final concentration of 2-6 of citric acid in aqueous solution
Mol/L, the mixing time are 10-50 min.
3. the preparation method of fluorescent fiber element nanofiber according to claim 1, it is characterised in that: in step (2)
The cellulosic material includes nano-cellulose, nano cellulose crystal, microcrystalline cellulose, any in nanocrystal cellulose
It is a kind of.
4. the preparation method of fluorescent fiber element nanofiber according to claim 1, it is characterised in that: in step (2)
The mass fraction of cellulosic material is 1-5% in the reaction solution.
5. the preparation method of fluorescent fiber element nanofiber according to claim 1, it is characterised in that: in step (2)
The oil bath heating temperature is 80-120 DEG C, and the condensing reflux reaction time is 1-10h.
6. the preparation method of fluorescent fiber element nanofiber according to claim 1, it is characterised in that: in step (4)
Drying temperature be 70-100 DEG C, drying time 5-12h.
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| CN201910028293.7A CN109762073A (en) | 2019-01-11 | 2019-01-11 | The preparation method of fluorescent fiber element nanofiber |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110066408A (en) * | 2019-05-22 | 2019-07-30 | 闽江学院 | A kind of preparation method of nanofiber fluorescent film |
| CN110220879A (en) * | 2019-07-03 | 2019-09-10 | 闽江学院 | A kind of preparation method of the biomass fiber fluorescence probe for calcium ion detection |
| CN111410696A (en) * | 2020-05-06 | 2020-07-14 | 闽江学院 | Method for preparing fluorescent nano-cellulose by one-pot method |
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| CN103343001A (en) * | 2013-07-10 | 2013-10-09 | 福建农林大学 | Method for preparing pH fluorescent response nano cellulose |
| CN105968215A (en) * | 2016-03-31 | 2016-09-28 | 北京理工大学 | Method for grafting nano-crystalline cellulose with amino acid |
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| EP0637594A2 (en) * | 1993-08-03 | 1995-02-08 | Nippon Shokubai Co., Ltd. | Water-absorbent resins and manufacturing methods thereof |
| CN103343001A (en) * | 2013-07-10 | 2013-10-09 | 福建农林大学 | Method for preparing pH fluorescent response nano cellulose |
| CN105968215A (en) * | 2016-03-31 | 2016-09-28 | 北京理工大学 | Method for grafting nano-crystalline cellulose with amino acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110066408A (en) * | 2019-05-22 | 2019-07-30 | 闽江学院 | A kind of preparation method of nanofiber fluorescent film |
| CN110066408B (en) * | 2019-05-22 | 2021-12-03 | 闽江学院 | Preparation method of nanofiber fluorescent film |
| CN110220879A (en) * | 2019-07-03 | 2019-09-10 | 闽江学院 | A kind of preparation method of the biomass fiber fluorescence probe for calcium ion detection |
| CN111410696A (en) * | 2020-05-06 | 2020-07-14 | 闽江学院 | Method for preparing fluorescent nano-cellulose by one-pot method |
| CN111410696B (en) * | 2020-05-06 | 2022-03-08 | 闽江学院 | Method for preparing fluorescent nano-cellulose by one-pot method |
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Application publication date: 20190517 |