CN106087246A - A kind of superfine fibre strengthens hyaline membrane and preparation method thereof - Google Patents
A kind of superfine fibre strengthens hyaline membrane and preparation method thereof Download PDFInfo
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- CN106087246A CN106087246A CN201610615691.5A CN201610615691A CN106087246A CN 106087246 A CN106087246 A CN 106087246A CN 201610615691 A CN201610615691 A CN 201610615691A CN 106087246 A CN106087246 A CN 106087246A
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- superfine fibre
- polyurethane
- polyacrylonitrile
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
Abstract
The invention discloses a kind of superfine fibre and strengthen hyaline membrane, described superfine fibre strengthens the composite that hyaline membrane is made up of superfine fibre reinforcement and the polyurethane matrix of a diameter of 50nm 2 μm, wherein said superfine fibre is piled up in polyurethane matrix as reinforcement is random, and the described Composite material transparent degree being prepared as is high.Its preparation method comprises the steps: to mix polyacrylonitrile with polyurethane to be dissolved in N, N dimethylformamide is made uniform spinning liquid, obtain the random polyacrylonitrile/polyurethane composite ultrafine fiber perforated membrane piled up together by electrostatic spinning, be then passed through heat treatment step and form polyacrylonitrile superfine fibre enhancing polyurethane transparent film.It is good that superfine fibre prepared by the present invention strengthens hyaline membrane mechanical property, and transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Description
Technical field
The present invention relates to a kind of superfine fibre and strengthen hyaline membrane and preparation method thereof, belong to functional film material and preparation thereof
Technical field.
Background technology
Along with the fast development of membrane technology, the requirement to membrane material and film properties is more and more higher.Apply (such as electricity in many
Son, packaging) in, use the film with sufficient transparency critically important, for some functional device (such as temperature sensing color changing sensor),
The transparency of material be it is also proposed the highest requirement.The novel film materials researching and developing function admirable for this has become as one
The very important research topic of item.Polyacrylonitrile (PAN) has chemistry, heat and the mechanical stability of excellence, after PAN wiring solution-forming
In electrostatic spinning, good spinnability, the fibre forming obtained is good, for raw material conventional during electrostatic spinning.Polyurethane
By the materials synthesis such as polyhydric alcohol, diisocyanate, there is the hard and soft chain segment block structure of uniqueness, can be by regulation polyurethane soft or hard
Segment components ratio changes its elasticity, hardness, hydrophilic etc., designs the product of different properties, and meanwhile, the goods of polyurethane have
The high resiliency of uniqueness, wettability, pliability, wearability, glossiness, before therefore having a wide range of applications in the preparation of various films
Scape.
About using fiber or fabric as reinforcement, resin is by pouring or hot rolling becomes the method preparation weaving of matrix
The technology of structural composite material is gradually improved, also has in a large number about the theoretical research in textile structural composite materials preparation process
Document is reported.Electrostatic spinning is a kind of simple method efficiently preparing continuous superfine fibre.Traditional electrostatic spinning one
As use single spraying head spinning, production efficiency is low.Many shower nozzles and the appearance without nozzle electrospinning technology, as Czech Elmarco is public
The nanometer Aranea that department produces, has promoted the industrialization process of electrostatic spinning technique significantly.
Electrostatic spinning principle: traditional electrostatic spinning device is typically by high voltage power supply, spinning electrode (spinning head) and reception dress
Put 3 part compositions.Being loaded by high polymeric solution in device for storing liquid, device for storing liquid and spinning head connect.To spinning head plus high pressure
Electrostatic, in the surface tension of the suffered in the electric field electric field force of the charged drop of spinning head end with polymer solution when just starting
Being in balance, drop is in steady statue at spinning head end, and along with the increasing of voltage, drop is gradually elongated formation cone
(i.e. Taylor cone).When electric field increases to a marginal value, charge repulsion is more than surface tension, and jet sprays from Taylor poppet surface
Go out.Jet first passes through a stable section moved along a straight line after taylor cone sprays, and then bends at certain point jet, shape
Curl " whip moves ", bending from jet starting no longer to attenuate to jet is unstable section, in jet motor process
Solvent volatilization, solidification, the fiber of formation solidifies on the reception device with the form of lack of alignment, obtains the most on the reception device
Fibrous membrane (net or felt).
Static Spinning superfine fibre film has the advantages such as porosity is high, specific surface area is big, absorption property is good, is widely used in
Biomedical (such as artificial blood vessel, tissue engineering bracket, wound dressing, operation suture thread etc.), photocatalysis, filtration, sensor etc.
Field.Owing in the fibrous membrane that electrostatic spinning device prepares, superfine fibre is usually and arranges with unordered shape, fibrous membrane mechanical property
Difference limit its in microelectronics and the device fabrication of photon, the use in the fields such as biological engineering, therefore produce and there is certain orientation
One of the Static Spinning superfine fibre of arrangement or the fibre bundle focus becoming electrostatic spinning technique current research.
Summary of the invention
Object of the present invention is to provide a kind of superfine fibre and strengthen hyaline membrane and preparation method thereof, prepared by the present invention
It is good that superfine fibre strengthens hyaline membrane mechanical property, and transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
For reaching above-mentioned purpose, the technical scheme is that
A kind of superfine fibre strengthens hyaline membrane, and it is surpassing by a diameter of 50nm-2 μm that described superfine fibre strengthens hyaline membrane
Fine fibre reinforcement and the composite of polyurethane matrix composition, wherein said superfine fibre is as the random heap of reinforcement
Building in polyurethane matrix, the described Composite material transparent degree being prepared as is high.
A kind of superfine fibre strengthens the preparation method of hyaline membrane, comprises the steps: to mix polyacrylonitrile with polyurethane
It is dissolved in DMF and makes uniform spinning liquid, by electrostatic spinning, polyacrylonitrile/polyurethane composite superfine is fine
Tie up random piling up and form perforated membrane together, be then passed through heat treatment step and form polyacrylonitrile superfine fibre enhancing polyurethane
Hyaline membrane.
Described step particularly as follows:
1) spinning liquid is prepared
Polyacrylonitrile (being purchased from Hangzhou Wan acrylon company limited (PAN, Mw=140000)) and polyurethane (are purchased from Shanghai moral
Science and Technology Ltd. of class (PU, Mw=500000)) material, dissolves in DMF solvent and (is purchased from Hangzhou Gao Jingjing
Thin Chemical Co., Ltd. (DMF, ρ=0.94g/cm3, analytical pure)), continuously stirred, until obtain the polyacrylonitrile of homogeneous transparent/
Polyurethane blend spinning liquid；
2) electrostatic spinning
By step 1) polyacrylonitrile/polyurethane blend spinning liquid of obtaining is encased in device for storing liquid and passes through Micro-metering Pumps
The spinning head being transported on spinning-drawing machine, under the effect of high voltage electric field, obtains polyacrylonitrile/polyurethane on the reception device and is combined
Superfine fiber porous membrane；
3) polyacrylonitrile superfine fibre strengthens the preparation of polyurethane transparent film
By step 2) polyacrylonitrile/polyurethane composite ultrafine fiber perforated membrane of obtaining puts in conventional heating equipment and carries out
Heat treatment, heat treatment temperature is 180-250 DEG C, and the process time is 60-120min, makes fusing point in composite superfine fibre membrane relatively low
Phase polyurethane melts, and the higher heterophasic polypropylene nitrile superfine fibre shape of fusing point is held essentially constant, and obtains superfine fibre and strengthens
Hyaline membrane.
In solute, the mass ratio of different high polymer materials strengthens hyaline membrane impact significantly to follow-up superfine fibre of preparing, and poly-third
Alkene nitrile content too much can not form continuous print polyurethane matrix, with the presence of air in matrix, affects transparency and the mechanics of material
Performance；Polyacrylonitrile content is very few, and polyacrylonitrile superfine fibre can not keep continuous in melted polyurethane matrix, affects
The mechanical property of whole material and shaping.So described step 1) in spinning liquid solid content be 10-20%, wherein polyacrylonitrile and
The mass ratio of polyurethane is 30:70-50:50.
Described polyacrylonitrile and the mass ratio of polyurethane are preferably 40:60.
Described polyacrylonitrile can be replaced with politef, poly(isophthaloyl metaphenylene diamine).
Described step 2) in spinning head use more than 1；When using spinning head as spinning electrode, described spray
Silk head is connected with DC high voltage electric field, and voltage is positive 10-40kV.
The thickness of film prepared by electrostatic spinning is determined by amount of solution used: too much by amount of solution, film is blocked up, heat treatment caudacoria
Poor transparency；Very few by amount of solution, lepthymenia, the poor mechanical property of heat treatment caudacoria.
Described step 2) in load device for storing liquid polyacrylonitrile/polyurethane blend spinning liquid measure be 2-6ml.
Described polyacrylonitrile/polyurethane blend spinning liquid measure is preferably 3ml.
Described step 3) in heat treatment temperature be preferably 180-200 DEG C, heat treatment time is preferably 80-100min, its
Described in polyacrylonitrile superfine fibre intersect in melted polyurethane, formed formability get well and have fracture strength with
The superfine fibre that transparency is high strengthens hyaline membrane.Temperature is too high or overlong time is all easily caused by step 2) polypropylene that obtains
In nitrile/polyurethane composite superfine fibre membrane, polyurethane decomposes, and the inclined brown of film color that processing obtains, film dynamic performance is poor, temperature
Too low or the time is too short, and to be all easily caused melt polyurethane in composite superfine fibre membrane insufficient, and the inclined yellow of film color is opaque.
The invention has the beneficial effects as follows: present invention employs the electrostatic spinning technique reached its maturity at present, steady in conjunction with tradition
Fixed heat treatment method is prepared superfine fibre and is strengthened hyaline membrane.The present invention initially with electrospinning process by two kinds of high polymer materials
Material is uniformly combined with each other, and makes high polymer presented in superfine fibre；Then heat treatment method is used to make wherein fusing point
Low Polymers Phase melts, and the Polymers Phase making fusing point high maintains a relatively stable state and plays enhancing and shaping effect.By
In heat treatment process, together with the Polymers Phase that low-melting Polymers Phase is high with fusing point, it is evenly distributed on superfine fibre at random
In, therefore when heat treatment, this Polymers Phase easily melts, and is easily uniformly distributed.Superfine fibre prepared by the present invention strengthens thoroughly
Bright film dynamic performance is good, and transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Accompanying drawing explanation
Fig. 1 is polyacrylonitrile in the embodiment of the present invention 1/polyurethane composite superfine fibre membrane scanning electron microscope (SEM) photograph；
Fig. 2 is that in the embodiment of the present invention 1, polyacrylonitrile superfine fibre strengthens polyurethane transparent film scanning electron microscope (SEM) photograph；
Fig. 3 is that in the embodiment of the present invention 1, polyacrylonitrile superfine fibre strengthens polyurethane transparent film pictorial diagram；
Fig. 4 is the fracture strength figure of different samples in the embodiment of the present invention 1, and wherein abscissa is sample, and sample a is poly-third
Alkene nitrile superfine fibre film, b is polyurethane superfine fiber film, and c is polyacrylonitrile/polyurethane composite superfine fibre membrane, and d is polypropylene
Nitrile superfine fibre strengthens polyurethane transparent film；Vertical coordinate is fracture strength；
Fig. 5 is the breaking strain figure of different samples in the embodiment of the present invention 1, and wherein abscissa is sample, and sample a is poly-
Acrylonitrile superfine fibre film, b is polyurethane superfine fiber film, and c is polyacrylonitrile/polyurethane composite superfine fibre membrane, and d is poly-third
Alkene nitrile superfine fibre strengthens polyurethane transparent film；Vertical coordinate is breaking strain；
Fig. 6 is that in the embodiment of the present invention 1, polyacrylonitrile superfine fibre strengthens polyurethane transparent film light transmittance figure.
Form explanation
Table 1 is parameters data synopsis in embodiment of the present invention 1-7.
Detailed description of the invention
Embodiment 1
A kind of superfine fibre of the present embodiment strengthens the preparation method of hyaline membrane, as shown in table 1, comprises the steps: to claim
Take the polyacrylonitrile powder of 0.3108g, the little granule of polyurethane of 0.4662g, pour into equipped with in the spinning liquid reagent bottle of Magnetitum, measure
Take the DMF of 5ml, pour in bottle, will be equipped with using adhesive tape good seal after the reagent bottle spinning solution is built,
It is placed on Magnetitum agitator, magnetic stirrer stirs 12 hours；Polyacrylonitrile/polyurethane that taking-up has stirred 12 hours is molten
Liquid, gets out the clean reservoir being dried and spinning head, is connected to spinning head on reservoir carry out remove impurity dredging, is fallen by solution
Enter in reservoir.Finally reservoir is fixed on spinning-drawing machine draw-in groove, the parameters of electrostatic spinning is set.The solution of electrostatic spinning
Amount is 3ml, and the flow velocity of spinning is 0.6ml/h.Then regulation spinning head is 18cm to the distance of reception device, the stannum that will cut
Foil paper is fixed on receiving screen, and HV generator voltage is slowly adjusted to 20kV, starts electrostatic spinning machine and starts spinning, knot
Shu Houhui forms the polyacrylonitrile/polyurethane composite superfine fibre membrane of one layer of smooth white on masking foil；Weigh the most respectively
0.777g polyacrylonitrile solution and polyurethane solutions, use same method to prepare polyacrylonitrile superfine fibre film and polyurethane surpass
Fine fibre film.As it is shown in figure 1, it is good to can get polyacrylonitrile/polyurethane composite ultrafine fiber pattern from Fig. 1, fiber is the most mixed and disorderly
Being stacked to form perforated membrane, average fibre diameter is 250nm.Composite superfine fibre membrane is flattened on Noah's ark, uses resistance to height
The corner of composite superfine fibre membrane is tightly fixed by the adhesive tape of temperature, then puts it in electric heating constant-temperature blowing drying box,
Heat treatment 90min at 200 DEG C, obtains the polyacrylonitrile superfine fibre that average diameter is 370nm and makees as reinforcement and polyurethane
Superfine fibre for matrix strengthens hyaline membrane；As shown in figures 2-6, each sample that in Fig. 4, abscissa obtains during being embodiment
Product, wherein a is polyacrylonitrile superfine fibre film, and b is polyurethane superfine fiber film, and c is that polyacrylonitrile/polyurethane composite superfine is fine
Dimension film, d is that polyacrylonitrile superfine fibre strengthens polyurethane transparent film；Vertical coordinate represents the fracture strength of each sample；Horizontal stroke in Fig. 5
Coordinate is each sample obtained during embodiment, and wherein a is polyacrylonitrile superfine fibre film, and b is polyurethane superfine fiber
Film, c is polyacrylonitrile/polyurethane composite superfine fibre membrane, and d is that polyacrylonitrile superfine fibre strengthens polyurethane transparent film；Vertical seat
Mark represents the breaking strain of each sample.During Fig. 2 is embodiment, polyacrylonitrile shown in Fig. 1/polyurethane composite ultrafine fiber
Film is after Overheating Treatment, although polyurethane is melt into matrix mutually in composite superfine fibre membrane, polyacrylonitrile keeps fiber condition, but
Polyacrylonitrile is heated swell, and fibre diameter increases.Fig. 3 shows that the polyacrylonitrile superfine fibre prepared when the present embodiment strengthens poly-ammonia
When ester hyaline membrane is placed on the paper being printed on ZSTU English alphabet, clearly can see these 4 English words of ZSTU through hyaline membrane
Mother, hyaline membrane transparency is high.Fig. 4 and Fig. 5 shows in embodiment, the polyacrylonitrile superfine fibre film that obtained by electrostatic spinning,
Polyurethane superfine fiber film and polyacrylonitrile/polyurethane composite superfine fibre membrane, fracture strength is followed successively by polyurethane superfine fiber
Film and polyacrylonitrile/polyurethane composite superfine fibre membrane ＞ polyacrylonitrile superfine fibre film ＞ polyurethane superfine fiber film, fracture
Strain is followed successively by polyurethane superfine fiber film ＞ polyacrylonitrile/polyurethane composite superfine fibre membrane ＞ polyacrylonitrile superfine fibre
Film, polyacrylonitrile/polyurethane composite superfine fibre membrane is after Overheating Treatment, due to the polyurethane melted hyaline membrane that formed mutually, transparent
Film fracture strength is the highest in 4 kinds of films, and breaking strain remains above pure polyacrylonitrile superfine fibre film.Prepared by the present embodiment super
It is good that fine fibre strengthens hyaline membrane mechanical property, and transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Embodiment 2
A kind of superfine fibre of the present embodiment strengthens the preparation method of hyaline membrane, as shown in table 1, comprises the steps: to claim
Take the polyacrylonitrile powder of 0.2590g, the little granule of polyurethane of 0.5180g, pour into equipped with in the spinning liquid reagent bottle of Magnetitum, measure
Take the DMF of 5ml, pour in bottle, will be equipped with using adhesive tape good seal after the reagent bottle spinning solution is built,
It is placed on Magnetitum agitator, magnetic stirrer stirs 12 hours；Polyacrylonitrile/polyurethane that taking-up has stirred 12 hours is molten
Liquid, gets out the clean reservoir being dried and spinning head, is connected to spinning head on reservoir carry out remove impurity dredging, is fallen by solution
Enter in reservoir.Finally reservoir is fixed on spinning-drawing machine draw-in groove, the parameters of electrostatic spinning is set.The solution of electrostatic spinning
Amount is 3ml, and the flow velocity of spinning is 0.6ml/h.Then regulation spinning head is 18cm to the distance of reception device, the stannum that will cut
Foil paper is fixed on receiving screen, and HV generator voltage is slowly adjusted to 20kV, starts electrostatic spinning machine and starts spinning, knot
Shu Houhui forms the polyacrylonitrile/polyurethane composite superfine fibre membrane of one layer of smooth white on masking foil.Composite superfine is fine
Dimension film is flattened on Noah's ark, is tightly fixed the corner of composite superfine fibre membrane with resistant to elevated temperatures adhesive tape, then puts it into
In electric heating constant-temperature blowing drying box, heat treatment 90min at 200 DEG C, obtain polyacrylonitrile superfine fibre and as reinforcement and gather
Urethane strengthens hyaline membrane as the superfine fibre of matrix.It is good that superfine fibre prepared by the present embodiment strengthens hyaline membrane mechanical property,
Transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Embodiment 3
A kind of superfine fibre of the present embodiment strengthens the preparation method of hyaline membrane, as shown in table 1, comprises the steps: to claim
Take the polyacrylonitrile powder of 0.3496g, the little granule of polyurethane of 0.4274g, pour into equipped with in the spinning liquid reagent bottle of Magnetitum, measure
Take the DMF of 5ml, pour in bottle, will be equipped with using adhesive tape good seal after the reagent bottle spinning solution is built,
It is placed on Magnetitum agitator, magnetic stirrer stirs 12 hours；Polyacrylonitrile/polyurethane that taking-up has stirred 12 hours is molten
Liquid, gets out the clean reservoir being dried and spinning head, is connected to spinning head on reservoir carry out remove impurity dredging, is fallen by solution
Enter in reservoir.Finally reservoir is fixed on spinning-drawing machine draw-in groove, the parameters of electrostatic spinning is set.The solution of electrostatic spinning
Amount is 3ml, and the flow velocity of spinning is 0.6ml/h.Then regulation spinning head is 18cm to the distance of reception device, the stannum that will cut
Foil paper is fixed on receiving screen, and HV generator voltage is slowly adjusted to 20kV, starts electrostatic spinning machine and starts spinning, knot
Shu Houhui forms the polyacrylonitrile/polyurethane composite superfine fibre membrane of one layer of smooth white on masking foil.Composite superfine is fine
Dimension film is flattened on Noah's ark, is tightly fixed the corner of composite superfine fibre membrane with resistant to elevated temperatures adhesive tape, then puts it into
In electric heating constant-temperature blowing drying box, heat treatment 90min at 200 DEG C, obtain polyacrylonitrile superfine fibre and as reinforcement and gather
Urethane strengthens hyaline membrane as the superfine fibre of matrix.It is good that superfine fibre prepared by the present embodiment strengthens hyaline membrane mechanical property,
Transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Embodiment 4
A kind of superfine fibre of the present embodiment strengthens the preparation method of hyaline membrane, as shown in table 1, comprises the steps: to claim
Take the polyacrylonitrile powder of 0.3108g, the little granule of polyurethane of 0.4662g, pour into equipped with in the spinning liquid reagent bottle of Magnetitum, measure
Take the DMF of 5ml, pour in bottle, will be equipped with using adhesive tape good seal after the reagent bottle spinning solution is built,
It is placed on Magnetitum agitator, magnetic stirrer stirs 12 hours；Polyacrylonitrile/polyurethane that taking-up has stirred 12 hours is molten
Liquid, gets out the clean reservoir being dried and spinning head, is connected to spinning head on reservoir carry out remove impurity dredging, is fallen by solution
Enter in reservoir.Finally reservoir is fixed on spinning-drawing machine draw-in groove, the parameters of electrostatic spinning is set.Electrostatic spinning molten
Liquid measure is 3ml, and the flow velocity of spinning is 0.6ml/h.Then regulation spinning head is 18cm to the distance of reception device, by cut
Masking foil is fixed on receiving screen, and HV generator voltage is slowly adjusted to 20kV, starts electrostatic spinning machine and starts spinning,
Polyacrylonitrile/polyurethane the composite superfine fibre membrane of one layer of smooth white can be formed on masking foil after end.By composite superfine
Fibrous membrane is flattened on Noah's ark, is tightly fixed the corner of composite superfine fibre membrane with resistant to elevated temperatures adhesive tape, is then put
Enter in electric heating constant-temperature blowing drying box, heat treatment 110min at 190 DEG C, obtain polyacrylonitrile superfine fibre as reinforcement and
Polyurethane strengthens hyaline membrane as the superfine fibre of matrix.Superfine fibre prepared by the present embodiment strengthens hyaline membrane mechanical property
Good, transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Embodiment 5
A kind of superfine fibre of the present embodiment strengthens the preparation method of hyaline membrane, as shown in table 1, comprises the steps: to claim
Take the polyacrylonitrile powder of 0.3108g, the little granule of polyurethane of 0.4662g, pour into equipped with in the spinning liquid reagent bottle of Magnetitum, measure
Take the DMF of 5ml, pour in bottle, will be equipped with using adhesive tape good seal after the reagent bottle spinning solution is built,
It is placed on Magnetitum agitator, magnetic stirrer stirs 12 hours；Polyacrylonitrile/polyurethane that taking-up has stirred 12 hours is molten
Liquid, gets out the clean reservoir being dried and spinning head, is connected to spinning head on reservoir carry out remove impurity dredging, is fallen by solution
Enter in reservoir.Finally reservoir is fixed on spinning-drawing machine draw-in groove, the parameters of electrostatic spinning is set.The solution of electrostatic spinning
Amount is 3ml, and the flow velocity of spinning is 0.6ml/h.Then regulation spinning head is 18cm to the distance of reception device, the stannum that will cut
Foil paper is fixed on receiving screen, and HV generator voltage is slowly adjusted to 20kV, starts electrostatic spinning machine and starts spinning, knot
Shu Houhui forms the polyacrylonitrile/polyurethane composite superfine fibre membrane of one layer of smooth white on masking foil.Composite superfine is fine
Dimension film is flattened on Noah's ark, is tightly fixed the corner of composite superfine fibre membrane with resistant to elevated temperatures adhesive tape, then puts it into
In electric heating constant-temperature blowing drying box, heat treatment 70min at 240 DEG C, obtain polyacrylonitrile superfine fibre and as reinforcement and gather
Urethane strengthens hyaline membrane as the superfine fibre of matrix.It is good that superfine fibre prepared by the present embodiment strengthens hyaline membrane mechanical property,
Transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Embodiment 6
A kind of superfine fibre of the present embodiment strengthens the preparation method of hyaline membrane, as shown in table 1, comprises the steps: to claim
Take the polyacrylonitrile powder of 0.3108g, the little granule of polyurethane of 0.4662g, pour into equipped with in the spinning liquid reagent bottle of Magnetitum, measure
Take the DMF of 5ml, pour in bottle, will be equipped with using adhesive tape good seal after the reagent bottle spinning solution is built,
It is placed on Magnetitum agitator, magnetic stirrer stirs 12 hours；Polyacrylonitrile/polyurethane that taking-up has stirred 12 hours is molten
Liquid, gets out the clean reservoir being dried and spinning head, is connected to spinning head on reservoir carry out remove impurity dredging, is fallen by solution
Enter in reservoir.Finally reservoir is fixed on spinning-drawing machine draw-in groove, the parameters of electrostatic spinning is set.The solution of electrostatic spinning
Amount is 5ml, and the flow velocity of spinning is 0.6ml/h.Then regulation spinning head is 18cm to the distance of reception device, the stannum that will cut
Foil paper is fixed on receiving screen, and HV generator voltage is slowly adjusted to 20kV, starts electrostatic spinning machine and starts spinning, knot
Shu Houhui forms the polyacrylonitrile/polyurethane composite superfine fibre membrane of one layer of smooth white on masking foil.Composite superfine is fine
Dimension film is flattened on Noah's ark, is tightly fixed the corner of composite superfine fibre membrane with resistant to elevated temperatures adhesive tape, then puts it into
In electric heating constant-temperature blowing drying box, heat treatment 90min at 200 DEG C, obtain polyacrylonitrile superfine fibre and as reinforcement and gather
Urethane strengthens hyaline membrane as the superfine fibre of matrix.It is good that superfine fibre prepared by the present embodiment strengthens hyaline membrane mechanical property,
Transparency is high, has that processing technique is simple, flow process is short, the feature of low cost.
Table 1
Claims (10)
1. a superfine fibre strengthens hyaline membrane, it is characterised in that it is by a diameter of that described superfine fibre strengthens hyaline membrane
The superfine fibre reinforcement of 50nm-2 μm and the composite of polyurethane matrix composition, wherein said superfine fibre is as enhancing
Body is random to be piled up in polyurethane matrix, and the described Composite material transparent degree being prepared as is high.
2. the preparation method of a superfine fibre as claimed in claim 1 enhancing hyaline membrane, it is characterised in that include walking as follows
Rapid: to mix with polyurethane to be dissolved in DMF by polyacrylonitrile and make uniform spinning liquid, will by electrostatic spinning
Random the piling up of polyacrylonitrile/polyurethane composite ultrafine fiber forms perforated membrane together, is then passed through heat treatment step and is formed
Polyacrylonitrile superfine fibre strengthens polyurethane transparent film.
A kind of superfine fibre the most as claimed in claim 2 strengthens the preparation method of hyaline membrane, it is characterised in that described step
Rapid particularly as follows:
1) spinning liquid is prepared
By polyacrylonitrile and polyurethane material, dissolve in DMF solvent, continuously stirred, until obtaining the most thoroughly
Bright polyacrylonitrile/polyurethane blend spinning liquid；
2) electrostatic spinning
Polyacrylonitrile step 1) obtained/polyurethane blend spinning liquid is encased in device for storing liquid by micro-measurement transport pump
Spinning head on spinning-drawing machine, under the effect of high voltage electric field, obtains polyacrylonitrile/polyurethane composite superfine on the reception device
Fiber multihole film；
3) polyacrylonitrile superfine fibre strengthens the preparation of polyurethane transparent film
By step 2) polyacrylonitrile/polyurethane composite ultrafine fiber perforated membrane of obtaining puts into and carries out in conventional heating equipment at heat
Reason, heat treatment temperature is 180-250 DEG C, and the process time is 60-120min, makes the gathering that fusing point in composite superfine fibre membrane is relatively low
Urethane melts, and the higher heterophasic polypropylene nitrile superfine fibre shape of fusing point is held essentially constant, and obtains superfine fibre and strengthens transparent
Film.
A kind of superfine fibre the most according to claim 3 strengthens the preparation method of hyaline membrane, it is characterised in that described step
Rapid 1) in, spinning liquid solid content is 10-20%, and wherein the mass ratio of polyacrylonitrile and polyurethane is 30:70-50:50.
A kind of superfine fibre the most according to claim 4 strengthens the preparation method of hyaline membrane, it is characterised in that described is poly-
The mass ratio of acrylonitrile and polyurethane is 40:60.
6. strengthen the preparation method of hyaline membrane according to a kind of superfine fibre described in claim 3 or 4 or 5, it is characterised in that institute
The polyacrylonitrile stated can be replaced with politef, poly(isophthaloyl metaphenylene diamine).
A kind of superfine fibre the most according to claim 3 strengthens the preparation method of hyaline membrane, it is characterised in that described step
Rapid 2) polyacrylonitrile/polyurethane blend spinning liquid measure loading device for storing liquid in is 2-6ml.
A kind of superfine fibre the most according to claim 7 strengthens the preparation method of hyaline membrane, it is characterised in that described is poly-
Acrylonitrile/polyurethane blend spinning liquid measure is 3ml.
A kind of superfine fibre the most according to claim 3 strengthens the preparation method of hyaline membrane, it is characterised in that described step
Rapid 2) spinning head in uses more than 1；When using spinning head as spinning electrode, described spinning head and DC high-voltage
Field is connected, and voltage is positive 10-40kV.
A kind of superfine fibre the most according to claim 3 strengthens the preparation method of hyaline membrane, it is characterised in that described
In step 3), heat treatment temperature is 180-200 DEG C, and heat treatment time is 80-100min, the ultra-fine fibre of wherein said polyacrylonitrile
Dimension intersect in melted polyurethane, formed formability get well and have fracture strength and transparency high superfine fibre enhancing
Hyaline membrane.
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