CN102094254B - Preparation method of seven-color fluorescent rare-earth ion/polymer nanometer composite fibers - Google Patents
Preparation method of seven-color fluorescent rare-earth ion/polymer nanometer composite fibers Download PDFInfo
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- CN102094254B CN102094254B CN2010106027724A CN201010602772A CN102094254B CN 102094254 B CN102094254 B CN 102094254B CN 2010106027724 A CN2010106027724 A CN 2010106027724A CN 201010602772 A CN201010602772 A CN 201010602772A CN 102094254 B CN102094254 B CN 102094254B
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Abstract
The invention relates to a preparation method of composite fibers, aiming to provide a preparation method of seven-color fluorescent rare-earth ion/polymer nanometer composite fibers. The preparation method comprises the following steps: 1, dissolving Eu(NO3)3 in water, then adding zinc powder, centrifugally concentrating, and adding polyvinyl alcohol to obtain a spinning solution a; 2, dissolving Tb(NO3)3 or Eu(NO3)3 in water, and adding polyvinyl alcohol to obtain a spinning solution b or c; 3, mixing any two of spinning solutions a, b and c to obtain a spinning solution d, e, f or g; and 4, spinning fibers from the spinning solution obtained in the step 3 with a spinning process, thereby obtaining the composite fibers. After being measured by a fluorescence spectrometer, the fibers prepared in the invention have corresponding characteristic peaks and high fluorescence intensity, and the preparation method is simple in operation and can be used for preparing the fibers with diverse fluorescent light colors.
Description
Technical field
The invention belongs to the preparation field of polymer fluorescent fiber, be specifically related to a kind of composite fibre preparation method.
Background technology
Rare earth element all is f because of its ground state and excitation state
nElectron configuration, and the f track is effectively shielded by outer s and p track, causes the f-f transition to present sharp-pointed wire bands of a spectrum, rare earth ion has characteristics such as light, electricity, magnetic just because of the electronic structure that has this uniqueness, be described as the treasure-house of new material.In decades in the past, owing to contain the complex (RE of trivalent rare earth ions
3+) possess excellent fluorescence; Aspects such as fluoremetry, fluorescence labeling, ultraviolet detector, electroluminescent device and molecular biosciences (as: can be used for high quick time resolved fluoro-immunoassay and explore on the life inhereditary material structure) have been widely applied to; But the less stable of self has limited its practical application.
The luminosity and the high molecular good mechanical performance that have bibliographical information to cross rare earth ion combine, and (the NO with Eu is also arranged
3)
3Be compound in polyvinylpyrrolidone (PVP) or the polyacrylonitrile and prepare high polymer nanometer fiber through electrostatic spinning.Because of the nano material dimensional effect makes its character at aspects such as light, heat, magnetic, electricity obviously different with the body material, so the research of nano material has received material scholar's great attention.Wherein the research of nanofiber becomes the focus of Recent study especially.The maximum characteristics of nanofiber are exactly that specific area is big, thereby cause its surface energy and active increase, are created in the specificity of chemistry, physical property aspect, make it be widely used in fields such as clothes, food, medicine, the energy, electronics, papermaking, aviation.At present; As a kind of important function fiber; Fluorescent fiber also is widely used in aspects such as anti-fake product, label, ornament, and its research and development is highly visible always, and the research of rare earth fluorescent fiber has become an important component part of fluorescent fiber research.
Although the development of fluorescent fiber grows stronger day by day, the fluorescence color of fiber also is only limited to the fluorescence color of the rare earth ion of being selected for use, also is not reported about the preparation of colorful fluorescent fiber.
Summary of the invention
The objective of the invention is for the preparation method of a kind of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is provided.
The preparation method of the present invention's seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution a; Two, through spinning technique the spinning solution a that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following: one, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution c; Two, through spinning technique spinning solution b or the spinning solution c that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution a; Two, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution c; Three, spinning solution a is mixed according to 1: 30 volume ratio with spinning solution b, obtain Eu
2+And Tb
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution d; Four, spinning solution a is mixed according to 1: 10 volume ratio with spinning solution c, obtain Eu
2+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution e; Five, spinning solution b is mixed according to 1: 4 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution f; Six, spinning solution b is mixed according to 1: 15 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution g; Seven, through spinning technique spinning solution d, spinning solution e, spinning solution f or the spinning solution g that step 3 to six obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
Above-mentioned spinning technique is fiber elongation method, rotary spinning or electrostatic spinning; Copper wire is as anode in the above-mentioned electrostatic spinning, and aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm～20cm, electrostatic spinning under 12kv～20kv voltage.
The present invention adopts three primary colours fluorescent rare earth ion/polymer manufacture nano-composite fiber, and the trichromatic rare-earth solion obtains multiple fluorescence color mixed rare earth ionic solution through mutual mixing, through electrostatic spinning technique multiple fluorescence color spinning solution is spun into colorful fiber; Record through XRF; This fiber has corresponding characteristic peak, and fluorescence intensity is high, compares with existing fluorescent fiber preparation method; This method is simple to operate, and prepared fiber fluorescence color is various.
Description of drawings
Fig. 1 is the fluorescence spectrum figure of spinning solution b in the specific embodiment ten; Fig. 2 is the fluorescence spectrum figure of spinning solution c in the specific embodiment 11; Fig. 3 is the fluorescence spectrum figure of spinning solution g in the specific embodiment 12; Fig. 4 is the fluorescence spectrum figure of spinning solution f in the specific embodiment 13; Fig. 5 is the fluorescence spectrum figure of spinning solution e in the specific embodiment 14; Fig. 6 is the fluorescence spectrum figure of gained seven color fluorescent rare earth ion/polymer nanocomposite composite fibres in the specific embodiment ten; Fig. 7 is the fluorescence spectrum figure of gained seven color fluorescent rare earth ion/polymer nanocomposite composite fibres in the specific embodiment 11; Fig. 8 is the fluorescence spectrum figure of gained seven color fluorescent rare earth ion/polymer nanocomposite composite fibres in the specific embodiment 12.
The specific embodiment
Technical scheme of the present invention is not limited to the following cited specific embodiment, also comprises the combination in any between each specific embodiment.
The specific embodiment one: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution a; Two, through spinning technique the spinning solution a that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution a water white transparency of gained has blue-fluorescence in this embodiment step 2 under uviol lamp.
The specific embodiment two: what this embodiment and the specific embodiment one were different is that said spinning technique is fiber elongation method, rotary spinning or electrostatic spinning.Other is identical with the specific embodiment one.
The specific embodiment three: what this embodiment and the specific embodiment two were different is that copper wire is as anode in the said electrostatic spinning, and aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm～20cm, electrostatic spinning under 12kv～20kv voltage.Other is identical with the specific embodiment two.
The specific embodiment four: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution c; Two, through spinning technique spinning solution b or the spinning solution c that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution b water white transparency of gained has green fluorescence in this embodiment step 2 under uviol lamp.
The spinning solution c water white transparency of gained has red fluorescence in this embodiment step 2 under uviol lamp.
The specific embodiment five: what this embodiment and the specific embodiment four were different is that said spinning technique is fiber elongation method, rotary spinning or electrostatic spinning.Other is identical with the specific embodiment four.
The specific embodiment six: what this embodiment and the specific embodiment five were different is that copper wire is as anode in the said electrostatic spinning, and aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm～20cm, electrostatic spinning under 12kv～20kv voltage.Other is identical with the specific embodiment five.
The specific embodiment seven: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution a; Two, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution c; Three, spinning solution a is mixed according to 1: 30 volume ratio with spinning solution b, obtain Eu
2+And Tb
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution d; Four, spinning solution a is mixed according to 1: 10 volume ratio with spinning solution c, obtain Eu
2+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution e; Five, spinning solution b is mixed according to 1: 4 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution f; Six, spinning solution b is mixed according to 1: 15 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution g; Seven, through spinning technique spinning solution d, spinning solution e, spinning solution f or the spinning solution g that step 3 to six obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution d water white transparency of step 3 gained has cyan fluorescence in this embodiment under uviol lamp.
The spinning solution e water white transparency of step 4 gained has purple fluorescence in this embodiment under uviol lamp.
The spinning solution f water white transparency of step 5 gained has yellow fluorescence in this embodiment under uviol lamp.
The spinning solution g water white transparency of step 6 gained has fluorescent orange in this embodiment under uviol lamp.
The specific embodiment eight: what this embodiment and the specific embodiment seven were different is that said spinning technique is fiber elongation method, rotary spinning or electrostatic spinning.Other is identical with the specific embodiment seven.
The specific embodiment nine: what this embodiment and the specific embodiment eight were different is that copper wire is as anode in the said electrostatic spinning, and aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm～20cm, electrostatic spinning under 12kv～20kv voltage.Other is identical with the specific embodiment eight.
The specific embodiment ten: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Tb (NO
3)
3The water-soluble Tb that is made into
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution b; Two, through spinning technique the spinning solution b that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution b water white transparency of gained has green fluorescence in this embodiment step 2 under uviol lamp.
The specific embodiment 11: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3The water-soluble Eu that is made into
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution c; Two, through spinning technique the spinning solution c that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution c water white transparency of gained has red fluorescence in this embodiment step 2 under uviol lamp.
The specific embodiment 12: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Tb (NO
3)
3The water-soluble Tb that is made into
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution b; Two, with Eu (NO
3)
3The water-soluble Eu that is made into
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution c; Three, spinning solution b is mixed according to 1: 15 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution g; Four, through spinning technique the spinning solution g that step 3 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution g water white transparency of step 4 gained has fluorescent orange in this embodiment under uviol lamp.
The specific embodiment 13: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Tb (NO
3)
3The water-soluble Tb that is made into
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution b; Two, with Eu (NO
3)
3The water-soluble Eu that is made into
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution c; Three, spinning solution b is mixed according to 1: 4 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution f; Four, through spinning technique the spinning solution f that step 3 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution f water white transparency of step 3 gained has yellow fluorescence in this embodiment under uviol lamp.
The specific embodiment 14: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution a; Two, with Eu (NO
3)
3The water-soluble Eu that is made into
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution c; Three, spinning solution a is mixed according to 1: 30 volume ratio with spinning solution c, obtain Eu
2+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 10% spinning solution e; Four, through spinning technique the spinning solution e that step 3 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The spinning solution e water white transparency of step 3 gained has purple fluorescence in this embodiment under uviol lamp.
The specific embodiment 15: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution a; Two, through spinning technique the spinning solution a that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The specific embodiment 16: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution a; Two, through spinning technique the spinning solution a that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The specific embodiment 17: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution c; Two, through spinning technique spinning solution b or the spinning solution c that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The specific embodiment 18: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution c; Two, through spinning technique spinning solution b or the spinning solution c that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The specific embodiment 19: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution a; Two, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution c; Three, spinning solution a is mixed according to 1: 30 volume ratio with spinning solution b, obtain Eu
2+And Tb
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution d; Four, spinning solution a is mixed according to 1: 10 volume ratio with spinning solution c, obtain Eu
2+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution e; Five, spinning solution b is mixed according to 1: 4 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution f; Six, spinning solution b is mixed according to 1: 15 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8% spinning solution g; Seven, through spinning technique spinning solution d, spinning solution e, spinning solution f or the spinning solution g that step 3 to six obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
The specific embodiment 20: the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following in this embodiment: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution a; Two, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution c; Three, spinning solution a is mixed according to 1: 30 volume ratio with spinning solution b, obtain Eu
2+And Tb
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution d; Four, spinning solution a is mixed according to 1: 10 volume ratio with spinning solution c, obtain Eu
2+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution e; Five, spinning solution b is mixed according to 1: 4 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution f; Six, spinning solution b is mixed according to 1: 15 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 20% spinning solution g; Seven, through spinning technique spinning solution d, spinning solution e, spinning solution f or the spinning solution g that step 3 to six obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
Claims (6)
1. the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is characterized in that the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution a; Two, through spinning technique the spinning solution a that step 1 obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
2. according to the preparation method of claim 1 said seven color fluorescent rare earth ion/polymer nanocomposite composite fibres, it is characterized in that said spinning technique is fiber elongation method, rotary spinning or electrostatic spinning.
3. according to the preparation method of claim 2 said seven color fluorescent rare earth ion/polymer nanocomposite composite fibres; It is characterized in that copper wire is as anode in the said electrostatic spinning; Aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm～20cm, electrostatic spinning under 12kv～20kv voltage.
4. the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is characterized in that the preparation method of seven color fluorescent rare earth ion/polymer nanocomposite composite fibres is following: one, with Eu (NO
3)
3Water-soluble wiring solution-forming adds zinc powder, then with Eu
3+Restore All is Eu
2+, centrifugal concentrating obtains Eu
2+Concentration is the aqueous solution of 1mol/L, adds polyvinyl alcohol again, obtains Eu
2+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution a; Two, with Tb (NO
3)
3Or Eu (NO
3)
3The water-soluble Tb that is made into
3+Or Eu
3+Concentration is the solution of 1mol/L, adds polyvinyl alcohol again, promptly gets Tb
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution b or Eu
3+Concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution c; Three, spinning solution a is mixed according to 1: 30 volume ratio with spinning solution b, obtain Eu
2+And Tb
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution d; Four, spinning solution a is mixed according to 1: 10 volume ratio with spinning solution c, obtain Eu
2+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution e; Five, spinning solution b is mixed according to 1: 4 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution f; Six, spinning solution b is mixed according to 1: 15 volume ratio with spinning solution c, obtain Tb
3+And Eu
3+Total concentration is that 1mol/L, polyvinyl alcohol mass concentration are 8%～20% spinning solution g; Seven, through spinning technique spinning solution d, spinning solution e, spinning solution f or the spinning solution g that step 3 to six obtains is spun into fiber; Promptly get seven color fluorescent rare earth ion/polymer nanocomposite composite fibres.
5. according to the preparation method of claim 4 said seven color fluorescent rare earth ion/polymer nanocomposite composite fibres, it is characterized in that said spinning technique is fiber elongation method, rotary spinning or electrostatic spinning.
6. according to the preparation method of claim 5 said seven color fluorescent rare earth ion/polymer nanocomposite composite fibres; It is characterized in that copper wire is as anode in the said electrostatic spinning; Aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm～20cm, electrostatic spinning under 12kv～20kv voltage.
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| DE3434971A1 (en) * | 1984-09-24 | 1986-03-27 | Wakita Nenshi Co., Ltd., Bisai, Aichi | Luminescent fibre |
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| CN1752306A (en) * | 2004-09-23 | 2006-03-29 | 北京大学 | Rere-earth compound modified polyurethane fibre and preparing process thereof |
| CN101067229A (en) * | 2007-06-12 | 2007-11-07 | 江苏盛虹化纤有限公司 | Flashlight multicolour polyster fibre |
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| KR20020096229A (en) * | 2001-06-19 | 2002-12-31 | 주식회사 효성 | Method for manufacturing sea-island type luminent conjugate fiber having high brightness, abrasion-resistance and good strength and the sea-island type luminent conjugate fiber |
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