CN107419514A - Rare earth upconversion nano material layers self assembly cotton fiber - Google Patents
Rare earth upconversion nano material layers self assembly cotton fiber Download PDFInfo
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- CN107419514A CN107419514A CN201710836621.7A CN201710836621A CN107419514A CN 107419514 A CN107419514 A CN 107419514A CN 201710836621 A CN201710836621 A CN 201710836621A CN 107419514 A CN107419514 A CN 107419514A
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- nayf
- bafta
- aqueous solution
- cotton fabric
- deionized water
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 53
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 9
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 8
- 238000001338 self-assembly Methods 0.000 title claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 239000004744 fabric Substances 0.000 claims abstract description 35
- TZYULTYGSBAILI-UHFFFAOYSA-M trimethyl(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC=C TZYULTYGSBAILI-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 229920000962 poly(amidoamine) Polymers 0.000 claims abstract description 11
- 229920000587 hyperbranched polymer Polymers 0.000 claims description 33
- 239000007864 aqueous solution Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 29
- 229910021641 deionized water Inorganic materials 0.000 claims description 29
- 125000003368 amide group Chemical group 0.000 claims description 18
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 230000004048 modification Effects 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- -1 allyl chlorine Chemical compound 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000000908 ammonium hydroxide Substances 0.000 claims 1
- 230000009881 electrostatic interaction Effects 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 4
- MLGWTHRHHANFCC-UHFFFAOYSA-N prop-2-en-1-amine;hydrochloride Chemical compound Cl.NCC=C MLGWTHRHHANFCC-UHFFFAOYSA-N 0.000 description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 4
- 229910001948 sodium oxide Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 229920000433 Lyocell Polymers 0.000 description 1
- 241000124033 Salix Species 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000985 reactive dye Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/17—Halides of elements of Groups 3 or 13 of the Periodic Table
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- 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
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
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- 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
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- Engineering & Computer Science (AREA)
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses rare earth upconversion nano material layers self assembly cotton fiber and preparation method thereof, obtains the bafta that is cationized using sodium hydroxide, trimethylallylammonium chloride, PAMAM modified cotton fabrics, then utilizes electronegative NaYF4:Yb, Er/Tm and positively charged NaYF4:Electrostatic interaction between Yb, Er/Tm, cationization bafta determines surface of cotton fabric NaYF as needed as film forming motive force4:The number of plies that Yb, Er/Tm are arranged, the excellent up-conversion fluorescence performance of providing cotton fabric and washing fastness.
Description
Technical field
The present invention relates to rare earth upconversion nano material layers self assembly cotton fiber, category fibrous material field.
Background technology
Cotton fiber is with the performance such as its excellent moisture absorption, ventilative, comfortable, soft, warming, renewable, degradable by vast
Consumer's likes.But compared with synthetic fibers, the feature of cotton fiber still has deficiency.Therefore it is fine in order to fully excavate cotton
The potential function of dimension, the technology content and added value of product of cotton fiber are improved, carrying out functional modification to cotton fiber turns into one
Important research direction（The preparation of dissaving polymer and functional modification [D] the University Of Suzhou to cotton fiber, 2009）.
Rare earth upconversion nano luminescent material（UCNPs）Can be by two-photon or multi-photon mechanism the long amplitude of low energy
Penetrate and be converted into high-energy shortwave radiation, it possesses, and toxicity is low, chemical stability is high, photostability is strong, signal to noise ratio is high, emission band
Light penetration depth narrow, fluorescence lifetime is long, anti-Stokes displacement is big, larger, without photobleaching, without background fluorescence and to biology
Many advantages, such as organizing not damaged, controls in immunoassay, biomarker, bio-sensing, bio-imaging, pharmaceutical carrier, light power
The fields such as treatment, photo-thermal therapy, photoconductive switch, information storage, food safety detection, photocatalysis and solar cell have extensively
Research and application.Wherein NaYF4:Yb, Er/Tm are one of luminous efficiency highest UCNPs.
201410701957.9 a kind of salix monogolica regenerated celulose fibre of Chinese invention patent and preparation method thereof, China
A kind of fluorescence Lyocell fiber of patent of invention 201410702142.2 and preparation method thereof, Chinese invention patent
UCNPs is added in spinning solution by 201410702118.9 a kind of Static Spinning fluorescence PVA nano fibrous membranes and preparation method thereof, leads to
Cross efficiently blending, wet spinning technology and the fiber with excellent fluorescence property is prepared.But co-blended spinning method is only applicable to
Synthetic fibers, be not suitable for the natural fibers such as cotton, hair, silk, fiber crops.It yet there are no and arrange UCNPs to the document on natural fiber
Report.
The content of the invention
In view of the above problems, the present invention provides rare earth upconversion nano material layers self assembly cotton fiber and its preparation side
Method.
The technical scheme is that：
（1）Bafta is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reaction 120min, are used
Deionized water is washed till neutrality repeatedly, and sodium hydroxide modified cotton fabric is obtained after drying；Then by sodium hydroxide modified cotton fabric weight
Newly it is scattered in deionized water, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethylallylammonium chloride and hydrogen
The mass ratio of sodium oxide molybdena modified cotton fabric is 1:5-1:10,60-80 DEG C of reaction 1-24h, are cleaned, after drying repeatedly with deionized water
Obtain trimethylallylammonium chloride modified cotton fabric；By trimethylallylammonium chloride modified cotton fabric be scattered in again from
In sub- water, bath raio 1:50, it is slowly added to the 1-100g/L polyamide-amide PAMAM aqueous solution, the PAMAM aqueous solution and front three
The volume ratio of the base allyl ammonium chloride modified cotton fabric aqueous solution is 1:5-1:10,75-95 DEG C of reaction 60-120min, after taking-up
Cleaning, drying obtains the bafta that is cationized；（2）Hyperbranched Polymer with Terminal Amido is modified into NaYF4:Yb, Er/Tm and terminal hydroxy group
Dissaving polymer modifies NaYF4:Yb, Er/Tm are configured to the 0.1-5g/L aqueous solution respectively, and will then be cationized bafta
It is immersed in 80 DEG C of Hyperbranched Polymer with Terminal Hydroxyl modification NaYF4:10-60min in Yb, the Er/Tm aqueous solution, bath raio 1:10, take
Rinsed, dried repeatedly with deionized water after going out；Then the Hyperbranched Polymer with Terminal Amido for above-mentioned bafta being immersed in 80 DEG C is repaiied
Adorn NaYF4:10-60min in Yb, the Er/Tm aqueous solution, bath raio 1:10, rinsed, dried, so far repeatedly with deionized water after taking-up
By one layer of NaYF4:Yb, Er/Tm arrange the surface to bafta, are then modified successively in Hyperbranched Polymer with Terminal Hydroxyl
NaYF4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Amido modification NaYF4:Aforesaid operations are repeated in Yb, Er/Tm dressing liquid, according to
Need to determine surface of cotton fabric NaYF4:The number of plies that Yb, Er/Tm are arranged.
The synthesis of Hyperbranched Polymer with Terminal Amido refers to following open source literatures：Hyperbranched Polymer with Terminal Amido and its quaternary ammonium
The preparation of salt and performance [J] polymer material sciences and engineering, 2009,25 (8): 141-144；CN200710020794.8
A kind of super-branching reactive dye salt-free dyeing auxiliary；Coloration Technology, 2007, 123(6): 351-357；
AATCC Review, 2010, 10(6): 56-60；Biomacromolecules, 2010, 11(1): 245-251；
Chemical Research in Chinese Universities, 2005, 21(3): 345-354。
The synthesis of Hyperbranched Polymer with Terminal Hydroxyl refers to following open source literatures：The such as Yang Baoping, Zhang Pengfei, Cui Jinfeng ends
The study on the modification of hydroxyl dissaving polymer and its application [J] the China coating in coating, 2011,26 (3):53-57；King
River is learned, the Hyperbranched Polymer with Terminal Hydroxyl such as Hu Yanxin, Zheng Shujie is to Fe3+Absorption behavior studies [J] New Chemical Materials,
2011,39(9):26-29,47；The synthesis of the strong Hyperbranched Polymer with Terminal Hydroxyl such as torrential, Zhang Guoguo, Wang Xuechuan and modification [J]
Daily chemical industry, 2012,42 (6):413-417.
Hyperbranched Polymer with Terminal Amido modifies NaYF4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Hydroxyl modification NaYF4:Yb,
Er/Tm preparation processes refer to document：A kind of water-soluble upper conversion nano particles of Chinese invention patent CN201410701945.6
And preparation method thereof.
Compared with prior art, the advantage of the invention is that：Modified using electronegative Hyperbranched Polymer with Terminal Hydroxyl
NaYF4:The Hyperbranched Polymer with Terminal Amido of Yb, Er/Tm and positively charged modifies NaYF4:Yb, Er/Tm, cationization bafta it
Between electrostatic interaction as film forming motive force, bafta is immersed in Hyperbranched Polymer with Terminal Hydroxyl modification NaYF successively4:Yb,
The Er/Tm aqueous solution and Hyperbranched Polymer with Terminal Amido modification NaYF4:In Yb, the Er/Tm aqueous solution, determine that cotton is knitted as needed
Thing surface NaYF4:The number of plies that Yb, Er/Tm are arranged, providing cotton fabric up-conversion fluorescence performance and washing fastness.
Embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1：
（1）Bafta is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reaction 120min, are used
Deionized water is washed till neutrality repeatedly, and sodium hydroxide modified cotton fabric is obtained after drying；Then by sodium hydroxide modified cotton fabric weight
Newly it is scattered in deionized water, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethylallylammonium chloride and hydrogen
The mass ratio of sodium oxide molybdena modified cotton fabric is 1:5,60 DEG C of reaction 1h, are cleaned, trimethyl are obtained after drying repeatedly with deionized water
Allyl ammonium chloride modified cotton fabric；Trimethylallylammonium chloride modified cotton fabric is scattered in deionized water again, bathed
Than 1:50, it is slowly added to the 10g/L polyamide-amide PAMAM aqueous solution, wherein the PAMAM aqueous solution and trimethyl allyl chlorination
The volume ratio of the ammonium modified cotton fabric aqueous solution is 1:5,75 DEG C reaction 60min, after taking-up cleaning, drying obtain be cationized cotton knit
Thing；（2）Hyperbranched Polymer with Terminal Amido is modified into NaYF4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Hydroxyl modification NaYF4:Yb,
Er/Tm is configured to the 0.1g/L aqueous solution respectively, and the bafta that is cationized then is immersed in 80 DEG C of superbrnaching end-hydroxy and gathered
Compound modifies NaYF4:10min in Yb, the Er/Tm aqueous solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；So
The Hyperbranched Polymer with Terminal Amido that above-mentioned bafta is immersed in 80 DEG C afterwards modifies NaYF4:10min in Yb, the Er/Tm aqueous solution,
Bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up.
Embodiment 2：
（1）Bafta is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reaction 120min, are used
Deionized water is washed till neutrality repeatedly, and sodium hydroxide modified cotton fabric is obtained after drying；Then by sodium hydroxide modified cotton fabric weight
Newly it is scattered in deionized water, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethylallylammonium chloride and hydrogen
The mass ratio of sodium oxide molybdena modified cotton fabric is 1:7,70 DEG C of reaction 6h, are cleaned, trimethyl are obtained after drying repeatedly with deionized water
Allyl ammonium chloride modified cotton fabric；Trimethylallylammonium chloride modified cotton fabric is scattered in deionized water again, bathed
Than 1:50, it is slowly added to the 50g/L polyamide-amide PAMAM aqueous solution, wherein the PAMAM aqueous solution and trimethyl allyl chlorination
The volume ratio of the ammonium modified cotton fabric aqueous solution is 1:8,80 DEG C reaction 90min, after taking-up cleaning, drying obtain be cationized cotton knit
Thing；（2）Hyperbranched Polymer with Terminal Amido is modified into NaYF4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Hydroxyl modification NaYF4:Yb,
Er/Tm is configured to the 1g/L aqueous solution respectively, and the bafta that is cationized then is immersed in 80 DEG C of superbrnaching end-hydroxy and polymerize
Thing modifies NaYF4:30min in Yb, the Er/Tm aqueous solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；Then
Above-mentioned bafta is immersed in 80 DEG C of Hyperbranched Polymer with Terminal Amido and modifies NaYF4:30min in Yb, the Er/Tm aqueous solution, bath
Than 1:10, rinsed, dried, so far by one layer of NaYF repeatedly with deionized water after taking-up4:Yb, Er/Tm are arranged and are arrived bafta
Surface, then modify NaYF in Hyperbranched Polymer with Terminal Hydroxyl successively4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Amido modification
NaYF4:Aforesaid operations in triplicate in Yb, Er/Tm dressing liquid.
Embodiment 3：
（1）Bafta is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reaction 120min, are used
Deionized water is washed till neutrality repeatedly, and sodium hydroxide modified cotton fabric is obtained after drying；Then by sodium hydroxide modified cotton fabric weight
Newly it is scattered in deionized water, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethylallylammonium chloride and hydrogen
The mass ratio of sodium oxide molybdena modified cotton fabric is 1:10,80 DEG C of reaction 24h, are cleaned, front three are obtained after drying repeatedly with deionized water
Base allyl ammonium chloride modified cotton fabric；Trimethylallylammonium chloride modified cotton fabric is scattered in deionized water again,
Bath raio 1:50, it is slowly added to the 100g/L polyamide-amide PAMAM aqueous solution, wherein the PAMAM aqueous solution and trimethyl allyl chlorine
The volume ratio for changing the ammonium modified cotton fabric aqueous solution is 1:10,90 DEG C of reaction 120min, cleaning, drying is cationized after taking-up
Bafta；（2）Hyperbranched Polymer with Terminal Amido is modified into NaYF4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Hydroxyl modification NaYF4:
Yb, Er/Tm are configured to the 5g/L aqueous solution respectively, and the bafta that is cationized then is immersed in 80 DEG C of superbrnaching end-hydroxy and gathered
Compound modifies NaYF4:60min in Yb, the Er/Tm aqueous solution, bath raio 1:10, rinsed, dried repeatedly with deionized water after taking-up；So
The Hyperbranched Polymer with Terminal Amido that above-mentioned bafta is immersed in 80 DEG C afterwards modifies NaYF4:60min in Yb, the Er/Tm aqueous solution,
Bath raio 1:10, rinsed, dried, so far by one layer of NaYF repeatedly with deionized water after taking-up4:Yb, Er/Tm are arranged and are arrived bafta
Surface, then successively Hyperbranched Polymer with Terminal Hydroxyl modify NaYF4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Amido modification
NaYF4:Six aforesaid operations are repeated in Yb, Er/Tm dressing liquid.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is amplified out still in protection scope of the present invention.
Claims (3)
1. the preparation method of rare earth upconversion nano material layers self assembly cotton fiber, it is characterised in that：
Step 1：Bafta is placed in the sodium hydroxide solution that mass fraction is 20%, bath raio 1:50,90 DEG C of reactions
120min, neutrality is washed till repeatedly with deionized water, sodium hydroxide modified cotton fabric is obtained after drying；Then sodium hydroxide is modified
Bafta is scattered in deionized water again, bath raio 1:50, add trimethylallylammonium chloride, wherein trimethyl allyl chlorine
The mass ratio for changing ammonium and sodium hydroxide modified cotton fabric is 1:5-1:10,60-80 DEG C are reacted 1-24h, repeatedly clear with deionized water
Wash, trimethylallylammonium chloride modified cotton fabric is obtained after drying；By trimethylallylammonium chloride modified cotton fabric again
It is scattered in deionized water, bath raio 1:50, it is slowly added to the 1-100g/L polyamide-amide PAMAM aqueous solution, 75-95 DEG C of reaction
60-120min, cleaning, drying obtains the bafta that is cationized after taking-up；
Step 2：Hyperbranched Polymer with Terminal Amido is modified into NaYF4:Yb, Er/Tm and Hyperbranched Polymer with Terminal Hydroxyl modification
NaYF4:Yb, Er/Tm are configured to the 0.1-5g/L aqueous solution respectively, and the bafta that is cationized then is immersed in 80 DEG C of end hydroxyl
Base dissaving polymer modifies NaYF4:10-60min in Yb, the Er/Tm aqueous solution, bath raio 1:10, it is anti-with deionized water after taking-up
It is multiple to rinse, drying；Then the Hyperbranched Polymer with Terminal Amido for above-mentioned bafta being immersed in 80 DEG C modifies NaYF4:Yb,Er/Tm
10-60min in the aqueous solution, bath raio 1:10, rinsed, dried, so far by one layer of NaYF repeatedly with deionized water after taking-up4:Yb,
Er/Tm arranges the surface to bafta, then modifies NaYF in Hyperbranched Polymer with Terminal Hydroxyl successively4:Yb, Er/Tm and end ammonia
Base dissaving polymer modifies NaYF4:Aforesaid operations are repeated in Yb, Er/Tm dressing liquid, determine surface of cotton fabric as needed
NaYF4:The number of plies that Yb, Er/Tm are arranged.
2. the preparation method of rare earth upconversion nano material layers self assembly cotton fiber according to claim 1, its feature
It is, the volume ratio of the PAMAM aqueous solution and the trimethylallylammonium chloride modified cotton fabric aqueous solution is 1:5-1:10.
3. the rare earth upconversion nano material layers self assembly cotton fiber obtained by claim 1 preparation method.
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| CN111206414A (en) * | 2020-01-16 | 2020-05-29 | 南通纺织丝绸产业技术研究院 | Fluorescent fiber based on rare earth doped up-conversion nano material and preparation method thereof |
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