CN109797491A - A kind of color nano fiber non-woven and its preparation method and application - Google Patents
A kind of color nano fiber non-woven and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of color nano fiber non-wovens and its preparation method and application, red, orange, yellow, green, blue, blue, purple color dyestuff are mixed with spinning material, and prepare color nano fiber non-woven by electrostatic spinning technique.And the coloured nano-fiber for production of non-woven of secondary colour can also be obtained using the double spray head blend spinnings of two different colors of spinning solution progress.Preparation process compared with traditional printing technology, have can operate continuously, is high-quality, steady performance.Prepared coloured nano-fiber material even dyeing, color are bright and beautiful firm, which can be used for the every field such as art work processing, packaging, dress ornament, colour development material.
Description
Technical field
The present invention relates to the preparation technical fields of color nano fiber non-woven, and in particular to color nano fiber is non-to be knitted
Cloth and preparation method and application is made, is mixed by dye molecule with high molecular material, is prepared by electrostatic spinning technique color
Color nano-fiber for production of non-woven；Secondary colour can also be obtained by carrying out double spray head blend spinnings using two different colors of spinning solution
Coloured nano-fiber for production of non-woven, and be used for the every field such as art work processing, packaging, dress ornament, colour development material.
Background technique
Aesthetic feeling can be assigned using color material to cloth or packaging material and the art work, promote sale, color identification,
Improve the value of the art work or commodity, therefore, color on these materials using extremely important, also very universal.Preparation is color
Color material can be there are two types of mode: first is that dyed again after preparing material, including cloth, drawing (be equivalent to paper, thin,tough silk silks etc. into
Row dyeing), printing and dyeing of packaging material etc.；Another way is processed again after exactly mixing dyestuff with material, including needle
It knits, spinning, press mold, the modes such as casting.No matter which kind of preparation method, require being sufficiently mixed and forming for dyestuff and rapidoprint
Stability.Such as cloth, beautiful decorative pattern is not only obtained, but also fuel and original fiber will combine closely, and be allowed to
Can be subjected to after use washing and it is colour-fast.
Electrostatic spinning nano fiber technology is a kind of technology for preparing non-woven nano-fiber cloth developed in recent years.It is main
If being prepared into diameter in sub-micron or the fiber of Nano grade, and in fibre by polymer solution under the action of extra electric field
It is collected in the case where the random accumulation of dimension and obtains the nano fibrous membrane of three-dimensional net structure.Its main feature is exactly specific surface area
Greatly, porosity is high, aperture and fibre diameter are adjustable etc., is commonly used for preparing air and sewage purification film, organizational project, strengthening material
Material, sensor etc..
As Chinese patent application CN201710431871 discloses a kind of system of colored fiber based on Cellulose nanocrystal
Preparation Method, comprising the following steps: (1) CNC solution is extracted from plant material using acid-hydrolyzed method；(2) CNC solution is taken,
Stirring is concentrated by evaporation, is made into liquid before spinning；(3) liquid before the spinning of step (2) is placed in organic media and carries out wet spinning,
Obtain purpose product colored fiber.Compared with prior art, using CNC solution as raw material, by the polymerization that different content is added
The regulation to composite fibre optical property may be implemented in object.
Separately there is Chinese patent application CN201220475043 to disclose a kind of polyester modified short fibre of honeycomb uvioresistant
It ties up, disperse dyes can contaminate cationic dye capable of dyeing under (dyeing temperature≤125 DEG C) or normal temperature and pressure, the bee under high temperature and pressure
The surface and inside of nest structure uvioresistant polyester modified short fiber have irregular multi-cellular structure, mutually pass through between each micropore
It is logical, and to be evenly equipped with uvioresistant nano oxidized for the outer surface of the whole fiber, surface layer, the surface of inside and each micropore and inside
Titanium composite micro-powder.The staple fiber of the utility model is prepared under conditions of pore former is not added, and can have strong reflection to ultraviolet light
And shielding action, ultraviolet energy can be converted into thermal energy or other harmless low energy forms, discharged or consumed, had simultaneously
The multiple functions such as hydroscopic fast-drying can be used for spinning various textiles.
It is combined with electrostatic spinning technique with dye techniques to prepare the technology of non-woven color nano fiber cloth and also rarely have
Report, compared with traditional printing technology, have can operate continuously, is high-quality, steady performance.Obtained colour is received
Rice fiber non-woven has overturned the pattern and performance of conventional woven cloth, can both assign non-woven cloth with the particularity of nano material
Can, and color and processing performance with conventional woven cloth, it can be in art work processing, packaging material, dress materials, colour development material
Equal fields are widely used.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provide a kind of color nano fiber non-woven and
Dyestuff is mixed with spinning material, is prepared yellowish green with blood orange by using electrostatic spinning nano fiber technology by preparation method
The nanofiber composite non-weaving cloth of the various colorss such as ultramarine purple, and regulate and control the ginseng such as fibre diameter by changing preparation condition
Number is allowed to for every field such as art work processing, packaging material, dress materials, colour development materials.
To achieve the above object, the invention adopts the following technical scheme:
A kind of color nano fiber non-woven, including be combined by one or more nanofibers, at least contain a kind of coloured silk
Color nanofiber, the color nano fiber are mixed with dyestuff and spinning material, are prepared by electrostatic spinning technique.
In some examples, the nanofiber is natural-nanometer fiber or synthesis nanofiber or combinations thereof；It is described
Natural-nanometer fiber include various native protein nanofibers, natural polysaccharide nanofiber, natural inorganic nanofiber, day
Right organic nanofibers, natural polymer nanofiber or combinations thereof；The synthesis nanofiber includes Inorganic synthese nanometer
Fiber, organic synthesis nanofiber, Polymer Synthesizing nanofiber or combinations thereof；The Polymer Synthesizing nanofiber includes
But it is not limited to polyethylene, polypropylene, polystyrene, polysulfones, polyether sulfone, Kynoar, polyvinyl chloride, polyvinyl alcohol, gathers
The nanofibers such as acrylonitrile, polyamide, polyimides, cellulose, nitrocellulose, cellulose acetate or combination.
In some examples, the color nano fiber is the nanofiber for including the colors such as the presentation yellowish green ultramarine purple of blood orange
Or combinations thereof.
In some examples, the color nano fiber is mixed with dyestuff and spinning material, passes through electrostatic spinning technique
It is prepared；The dyestuff is including including environmentally friendly green (G-1018), environmentally friendly red (G-1013), environmental protection indigo plant (G-1019), environmental protection
Dyestuffs such as yellow (G-1017) or combinations thereof；The electrostatic spinning technique includes single nozzle spinning, double spray head spinning, the spinning of more spray heads
One or more of silk, melt spinning, solution-polymerized SBR.
In some examples, the mass ratio of dyestuff and spinning material in color nano fiber non-woven is 0.001-
99.9%；It is preferred that the mass ratio of dyestuff and spinning material in color nano fiber non-woven is lower than 8%；More preferably 2%.
In some examples, the parameter of solution spinning includes that the concentration of spinning solution is 5%~30%；Spinning voltage be 5kV~
30kV；The distance of spinning head to receiver is 5cm~50cm；It is 1 μ of μ L/min~50 L/min that spinning solution, which injects speed,.
In some examples, the solvent of spinning material includes dimethylformamide, dimethyl acetamide, two in solution spinning
Or mixtures thereof methyl sulfoxide, chloroform, methylene chloride, toluene, benzene, tetrahydrofuran, acetonitrile, water；More preferably dimethyl formyl
Amine.
In some examples, the diameter of the color nano fiber is 0.001-10 microns, more preferably 200 nanometers；It is long
Degree is 100 nanometers -1000 meters；With a thickness of 0.001-10 millimeters, more preferably 100 microns.
In some examples, the brightness of the color nano fiber is 1-99.9%, chromaticity coordinate value (red green direction and Huang
Blue party to) between -100-100.
The present invention also protects the color nano fiber non-woven for art work processing, packaging material, clothes material
The field of material, colour development material.
Compared with prior art, the beneficial effects of the present invention are:
(1) take the lead in preparing color static spinning nano fibre, and regulate and control the color of the fiber cloth, coloration, fibre diameter, porosity,
A variety of properties such as stability are washed, the color static spinning nano fibre being had excellent performance.
(2) preparation method is simple, is easy to amplify production, promotes the industrialization of color nano fiber.
(3) the color nano fiber non-woven obtained by can be used successfully to art work processing, packaging, dress ornament, colour developing
Etc. every field.
Detailed description of the invention
It is further described with reference to the accompanying drawing:
Fig. 1 is the infrared spectrogram of color static spinning nanometer fiber membrane.(a) PAN 10%, (b) green 2%, (c) red 2%, (d)
Yellow 2%, (e) blue 2%；
Fig. 2 is respectively the PAN10% electrospinning film that (A) does not add dyestuff, 2% electrospinning film of (B) green, 2% electrospinning film water of (C) green
Scanning electron microscope (SEM) photograph of washing that treated；
Fig. 3 is the reflectance spectrum figure of the electrospinning film of various concentration green dye and PAN10% preparation；
Fig. 4 is the optical photograph of the electrospinning film of various concentration green dye and PAN10% preparation；
Fig. 5 be various colors spinning solution individually and mixing electrospinning preparation nano fibrous membrane photo；
Fig. 6 is various colors analogous diagram.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, without structure
At limitation of the present invention.
Example one: the preparation of electrostatic spinning liquid.(1) it takes 10g PAN powder that 90g DMF is added and stirs 2 angels at 60 DEG C
It is sufficiently dissolved, be cooled to room temperature with mass fraction be 10% PAN solution.(2) it prepares green concentration gradient spinning solution: taking
Appropriate 10% PAN solution, being added relative to PAN material quality score is 0.4 %, 0.8 %, 2 %, the green (ring of 4 %, 8 %
Protect green G-1018) dyestuff mixing is placed in vial, and it is slowly stirred after 1 h to take out under 90 DEG C of water bath conditions and is cooled to room temperature,
Obtain the green dye PAN solution of various concentration.Red (the red G- of environmental protection that dye strength is 2% is prepared under identical condition
1013), blue (environmentally friendly indigo plant G-1019), yellow (environmentally friendly Huang G-1017) PAN10% solution.
Example two: using double nozzle electrospinning devices, the green PAN solution of appropriate various concentration is taken to be put in left and right respectively
In syringe on (A, B) two infusing devices, speed V is injectedA = VB= 20μL/min；The connection of two syringe needles (internal diameter 0.6mm)
The voltage of 20 kV, while electrospinning；One surface coats the grounded metal roller (revolving speed is 60 r/min) of aluminium foil as reception dress
It sets；Two spinning heads are from Rotation of receiver roll spacing from respectively DA = DB = 12 cm；Two infusing devices are by motor control simultaneously along vertical
Horizontal reciprocating movement directly is done in receiving roll direction of rotation, 10 cm of moving range, 1 h of electrospinning are to obtain the green of different content
Electrospun nano-fibers film.The Nanowire of different colours is obtained by red, yellow, the blue spinning solution of two sprinkler selection one or two
Tie up film.
Example three: coloured electrospinning film composition analysis.Use 8700 type Fourier Transform Infrared Spectrometer of Nicolet, decay
Total reflection method (ATR-FTIR) respectively obtains the electrospinning film infrared absorpting light spectra of kind of color.As shown in Figure 1, wherein each spectrogram is distinguished
For (a) PAN 10%, (b) green 2%, (c) red 2%, (d) yellow 2%, (e) blue 2% electrospinning film.Wherein by being unstained
PAN10% spinning solution prepared by electrospinning film infrared spectrogram (A), 3628 cm-1With 3531 cm-1Place be respectively it is free and with
Hydrogen bond association hydroxyl absorption peak, hydroxyl are probably derived from sample as the moisture for eliminating or absorbing, 2933 cm-1With 2869 cm-1
Place is the C-H stretching vibration absworption peak in methyl and methylene, 2243 cm-1Locate sharp Qiang Fengwei cyano C ≡ N stretching vibration
Absorption peak, 1450 cm-1Place is methylene deformation vibration the absworption peak, 1372 cm-1 Place is methoxycarbonyl group (CH3OOC methyl in)
Deformation vibration the absworption peak.And in orchil electrospinning film, there may be amide structures: in 1534 cm-1For NH deformation vibration absorption
Peak, 732 cm-1Place is-NH2Bending vibration absorption peak.It is analyzed according to other spectrogram peak positions, it can in green, yellow and blue dyes
Aromatic amine, nitro and fatty ether structure can all be contained.Wherein corresponding peak position may be: 3280 cm-1For amino N H stretching vibration
Absorption peak, 1330 cm-1For aromatic amine CN stretching vibration absworption peak, and at 1497 it is phenyl ring skeleton C=C vibration absorption peak；
1557cm-1Place is nitro NO stretching vibration absworption peak, in 814cm-1Place is CN stretching vibration absworption peak；1158cm-1Place is ethers
CO stretching vibration absworption peak.
Example four: environmental microbes are observed using JSM-7800F field emission scanning electron microscope (SEM).Make
50 fiber measurement its average diameters are chosen from the SEM image of Fig. 2 with Lycra software (Leica).Membrane porosity is by following formula meter
It calculates, whereinρThe apparent density for representing film is calculated by film quality divided by membrane volume；ρ 0 The ontology for representing component film raw material is close
Degree.
The maximum diameter of hole of film, most probable pore size fenestra analysis-e/or determining PAN10% electrospinning membrane fiber compound with regular structure.And add
Most of fiber still keeps compound with regular structure after entering 2% green dye, but part bends and winds.Green 2% after washing
Bending deformation slightly occurs for electrospinning film, and has the phenomenon that contraction, but whole pattern does not change much.Table 1 is dye
Material concentration is that the electrospinning film water that the spinning solution of green 2% is prepared washes front and back relevant characterization data.
Pattern, the structural characterization of 1 color nano tunica fibrosa of table
PVA10% 193 ± 27nm of average fibre diameter is calculated based on SEM picture, fiber is average straight after 2% green dye is added
Diameter slightly reduces, and becomes 170 ± 40nm.And water-washing process influences less its diameter, washing rear average diameter is 166 ± 22nm.
Electrospinning membrane porosity after dyestuff is added substantially has no change, and film thickness and maximum diameter of hole, average pore size all reduce.
Example five: the photochrome of each membrane sample is shot using Nikon D7200 camera；Use HunterLab company
ColorQuest XE type beam splitting type colorimeter carries out characterization, available CIE L*a*b* color space to each electrospinning film
Coordinate value, reflectance spectrum figure and color analogous diagram.Fig. 3 is the electrospinning film reflectance spectrum for adding the preparation of various concentration green dye
Figure, wherein each spectral line is respectively (a) PAN10%, (b) green 0.4%, (c) green 0.8%, (d) green 2%, (e) green
4%, (f) green 8% electrospinning film.Curve (a) is the electro spinning nanometer fiber membrane without adding the PAN10% spinning solution preparation of dyestuff,
It is can see in visible-range almost to any light wave reflection rate all close to 100%, so it should show white, this
It is consistent with visually observing.And other spectral lines, with the increase of green dye mass fraction, to 400-500nm, 600-
Light wave reflection rate within the scope of 700nm gradually decreases, this is because increasing with the increase of dyestuff to the light wave uptake of this wave band
Add.
Example six: the photochrome of each membrane sample is shot using Nikon D7200 camera.Add various concentration green dye
The Static Spinning film of various colors is prepared, as shown in Figure 4.It can be seen that green 0.2% and green 0.4% color are shallower, green 2% is just
It can obtain the significantly green electrospinning film of color.With the increase of spinning solution Green dye content, electro spinning nanometer fiber membrane
Color is gradually deepened, and specific value of chromatism will be indicated by subsequent coloration and color space coordinate.But as concentration continues to increase
Greatly, for example green 8% is increased to, pigment and PAN powder dispersibility and the uniformity in DMF solvent substantially reduce, and influence electrospinning mistake
Journey, obtained electro spinning nano fiber poor quality.Therefore, continue subsequent research for adding amount of dye 2%.
(A) red 2%(B obtained by the solution that double nozzle electrospinning devices prepare same color) blue 2%, (C)
2% nano fibrous membrane of yellow.Meanwhile by using two spray heads the spinning solution of different colours to carry out blend spinning, preparation respectively
The nano fibrous membrane of more colors out obtains the mixed effect of different colours nanofiber, as shown in Figure 5.Wherein dye strength
Available (D) purple for the 2% double spray head blend spinnings of red and blue PAN solution, blue 2% and yellow 2% can obtain
To greeny (E).According to the data that ColorQuest XE type beam splitting type colorimeter is collected, the face of each film is obtained using software
Color analogous diagram 6.Wherein corresponding 1-PAN10%, 2- green 0.4% of each number, 3- green 0.8%, 4- green 2%, 5- green 4%, 6- are green
Color 8%, 7- red 2%, 8- yellow 2%, 9- blue 2%, 10 red 2%+ indigo plants 2%, 11- Huang 2%+ are blue, 12- green 2% washes electrospun nanofiber
Tunica fibrosa.
Seven: CIE L*a*b* colorimetry model of example is one of the colour space of measurement object color general at present, is by state
Border illuminates the committee (CIE) in formulation in 1976.It is to be gone out a kind of color digital representation with mono- group of data of L*, a*, b*
Come, one group of L*a*b* value forms one-to-one relationship with a kind of color.Wherein L* value indicates brightness, and a*, b* value are chromaticity coordinate
Value.A* value indicates red green direction color change, and+a* indicates to change to red direction, and-a* is indicated to green direction change.B* table
Show champac direction change ,+b* indicates that yellow direction change ,-b* is indicated to blue direction change.
2 color nano fiber CIE L*a*b* color space coordinate value of table
The color difference of two kinds of colors indicates that △ L*, △ a*, △ b* are respectively L*, a*, b* difference of two kinds of colors with △ E.Then have
△ECIE L*a*b = [(△L*)2+(△a*)2+(△b*)2]1/2, △ L* △ a* △ b*.On the basis of green 2%, yellow is calculated to obtain
2%+ blue 2% and its value of chromatism (E=5.91 △) very little.That is environmental protection Huang (G-1017) 2% and environmental protection indigo plant (G-1019) 2%
Blended film color is green, and the color of close green 2% electrospinning film.In order to probe into the resistance to of coloured electro spinning nanometer fiber membrane color
Washing property simulates cloth washing process, and 2 % electrospinning films of green are clipped among two pieces of cottons and are placed in 500 mL deionized waters,
72 h are slowly stirred at a room temperature, change a water every 24 h.As shown in table 2 and Fig. 6, its color space coordinate base of washing front and back
This is constant, and value of chromatism (E=1.43 △) is very small, that is to say, that the processing Jing Guo the test condition, green electro spinning nano fiber
Film color is basically unchanged, and washing color fastness is very high.
Following embodiment will be helpful to those skilled in the art and further understand the present invention, but not limit in any form
The present invention.It should be pointed out that those skilled in the art, without departing from the inventive concept of the premise, also
Several modifications and improvements can be made.These are all within the scope of protection of the present invention.
Claims (10)
1. a kind of color nano fiber non-woven, which is characterized in that including being combined by one or more nanofibers, until
Contain a kind of color nano fiber less, the color nano fiber is mixed with dyestuff and spinning material, passes through electrostatic spinning skill
Art is prepared.
2. color nano fiber non-woven according to claim 1, which is characterized in that the nanofiber is natural
Nanofiber or synthesis nanofiber or combinations thereof；The natural-nanometer fiber includes various native protein Nanowires
Dimension, natural polysaccharide nanofiber, natural inorganic nanofiber, natural organic nanofibers, natural polymer nanofiber or its
Combination；The synthesis nanofiber includes Inorganic synthese nanofiber, organic synthesis nanofiber, Polymer Synthesizing Nanowire
Dimension or combinations thereof；The Polymer Synthesizing nanofiber include but is not limited to polyethylene, polypropylene, polystyrene, polysulfones,
Polyether sulfone, Kynoar, polyvinyl chloride, polyvinyl alcohol, polyacrylonitrile, polyamide, polyimides, cellulose, cellulose nitrate
The nanofibers such as element, cellulose acetate or combination.
3. color nano fiber non-woven according to claim 1, which is characterized in that the color nano fiber is
Including nanofibers of colors such as the yellowish green ultramarine purple of blood orange or combinations thereof are presented.
4. color nano fiber non-woven according to claim 1, which is characterized in that the color nano fiber is
It is mixed with dyestuff and spinning material, is prepared by electrostatic spinning technique；The dyestuff includes including the green (G- of environmental protection
1018), environmentally friendly red (G-1013), environmental protection blue (G-1019), environmental protection yellow (G-1017) or combinations thereof；The electrostatic spinning technique
Including one or more of single nozzle spinning, double spray head spinning, more spray head spinning, melt spinning, solution-polymerized SBR.
5. color nano fiber non-woven according to claim 4, which is characterized in that color nano fiber non-woven
In dyestuff and spinning material mass ratio be 0.001-99.9%；It is preferred that dyestuff and spinning in color nano fiber non-woven
The mass ratio of wire material is lower than 8%；More preferably 2%.
6. color nano fiber non-woven according to claim 4, which is characterized in that the parameter of solution spinning includes
The concentration of spinning solution is 5%~30%；Spinning voltage is 5kV~30kV；The distance of spinning head to receiver is 5cm~50cm；It spins
It is 1 μ of μ L/min~50 L/min that silk liquid, which injects speed,.
7. color nano fiber non-woven according to claim 4, which is characterized in that spinning material in solution spinning
Solvent include dimethylformamide, dimethyl acetamide, dimethyl sulfoxide, chloroform, methylene chloride, toluene, benzene, tetrahydro furan
It mutters, or mixtures thereof acetonitrile, water；More preferably dimethylformamide.
8. color nano fiber non-woven according to claim 4, which is characterized in that the color nano fiber
Diameter is 0.001-10 microns, more preferably 200 nanometers；Length is 100 nanometers -1000 meters；With a thickness of 0.001-10 millimeters, more
Preferably 100 microns.
9. color nano fiber non-woven according to claim 4, which is characterized in that the color nano fiber
Brightness is 1-99.9%, and on red green direction and champac direction, chromaticity coordinate value is between -100-100.
10. color nano fiber non-woven of any of claims 1-9 for art work processing, packaging material,
The field of dress materials, colour development material.
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