CN104451911A - Electrostatic assisting solution jet spinning device and method - Google Patents
Electrostatic assisting solution jet spinning device and method Download PDFInfo
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- CN104451911A CN104451911A CN201410673678.6A CN201410673678A CN104451911A CN 104451911 A CN104451911 A CN 104451911A CN 201410673678 A CN201410673678 A CN 201410673678A CN 104451911 A CN104451911 A CN 104451911A
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- lace curtaining
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- 238000009987 spinning Methods 0.000 title claims abstract description 178
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000835 fiber Substances 0.000 claims abstract description 78
- 230000005686 electrostatic field Effects 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 229920000642 polymer Polymers 0.000 claims abstract description 12
- 230000001939 inductive effect Effects 0.000 claims description 26
- 230000005684 electric field Effects 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 13
- 238000005096 rolling process Methods 0.000 claims description 13
- 238000003860 storage Methods 0.000 claims description 13
- 239000002121 nanofiber Substances 0.000 claims description 12
- 230000009471 action Effects 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000004020 conductor Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 10
- 230000006698 induction Effects 0.000 abstract 5
- 239000000243 solution Substances 0.000 description 86
- 238000005516 engineering process Methods 0.000 description 11
- 238000010041 electrostatic spinning Methods 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 239000007921 spray Substances 0.000 description 7
- 238000012876 topography Methods 0.000 description 7
- 238000001523 electrospinning Methods 0.000 description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 208000001308 Fasciculation Diseases 0.000 description 2
- 206010028293 Muscle contractions involuntary Diseases 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 210000002950 fibroblast Anatomy 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 150000007523 nucleic acids Chemical class 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920001872 Spider silk Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920003225 polyurethane elastomer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses an electrostatic assisting solution jet spinning device and method. The spinning device comprises a spinneret, an annular induction electrode, a wire, a high-voltage electrostatic generator, a guide roller and a receiving net curtain. The electrostatic field of the spinning device is not directly exerted on a spinneret orifice but exerted on the annular induction electrode and can not directly make a solution electrified but make the solution produce induction charges, and therefore the spinning solution jet flow is stretched. By means of the spinning method, at least one type of polymers are dissolved in at least one type of solution to make a spinning solution; the spinning solution is squeezed out of the spinneret hole of the spinneret, the high-speed jet air flow, sprayed out of an air outlet, of the spinning solution is stretched and thinned, solvents of spinning solution thin flow are volatilized under the effect of the high-speed jet air flow and the effect of the electrostatic field of the annular induction electrode to form micro-nanometer fiber, and the micro-nanometer fiber is collected on the receiving net curtain under the effect of the high-speed get air flow and the effect of the electrostatic field of the annular induction electrode.
Description
Technical field
The present invention relates to micro nanometer fiber technology of preparing, be specially a kind of electrostatic assisted solution jet spinning device and spinning process.
Background technology
The preparation method of current micro nanometer fiber comprises composite spinning technology, centrifugal spinning technology, electrostatic spinning technique and solution jet spinning technology etc.Electrostatic spinning technique is that polymer solution or melt carry out injection stretching and obtain the technology of nano-scale fiber under electrostatic interaction, polymer solution is put on or between melt and gathering-device by high direct voltage, to make on polymer solution or melt band several thousand to volt high-pressure electrostatic up to ten thousand, when electric field force is enough large, charged polymer drop overcomes surface tension and forms injection thread, thread solidifies with solvent evaporation or cooled and solidified in course of injection, finally drop on gathering-device, form the fibrofelt of similar nonwoven fabric, its nanofiber diameter generally tens nanometers (nm) to and micron (μm) between.Along with people are to the extensive concern of nanometer technique, method of electrostatic spinning obtained fast development in the last few years, and for tens kinds of different macromolecules, as electrospinning, the electrospinning of polyurethane elastomer, the electrospinning etc. of mesomorphic rigid macromolecule PPTA of the flexible macromolecules such as polyester, nylon, polyvinyl alcohol.In addition, comprise silk, the large biological molecule such as protein and nucleic acid (DNA) of spider silk also can carry out electrospinning.Filamentary diameter can change with processing conditions, and the diameter of typical electrospinning fibre is 40nm ~ 2 μm.But there is certain technical problem in current electrospinning, the output as current electrostatic spinning machine is very low, and the difficulty of large-scale application is larger in popularization.In recent years, numerous researcher gets down to the research of the technology such as Multi needle Static Spinning, needleless Static Spinning to realizing the extensive preparation of micro nanometer fiber.
Solution jet spinning technology is a kind of novel micro nanometer rice fiber producing processes that Chinese patent (patent No. ZL201110041792.3) discloses, and this technology and electrostatic spinning technique have different fibre forming driving forces.Electrostatic spinning is a kind of known micro nanometer fiber technology of preparing, relies on electrostatic field, carries out slenderizing finally obtain fiber to solution jet.Electrostatic field can make to there is like charges between gained fiber thus improve the uniformity of micro nanometer fiber, and voltage increasing within the specific limits can make the diameter of nanofiber reduce simultaneously.Solution jet spinning technology utilizes high velocity air to carry out ultra-fine stretching to polymer solution thread to prepare micro nanometer fiber; there is higher spinning efficiency; single hole spray silk efficiency can higher than pin hole electrostatic spinning more than ten times; and can spinneret die be used; therefore; the scale preparation of micro nanometer fiber can be realized, developed into one of important method prepared by micro nanometer fiber.
The micro nanometer fiber utilizing solution spraying technique to prepare, owing to being subject to the impact of air-flow in forming process, shows as three-dimensional crimp form, has obvious advantage in a lot of field, as shown the advantage of obvious low filtration resistance when being applied to filtration art.But the irregular wrapped configuration of fiber also makes fiber show necessarily inhomogeneities macroscopically when building up.
Summary of the invention
For the deficiencies in the prior art, the technical problem that quasi-solution of the present invention is determined is, provides a kind of electrostatic assisted solution jet spinning device and spinning process.The electrostatic field of this device for spinning is not directly be added on spinneret orifice, but being added on toroidal inductive electrode, such electrostatic field does not directly contact with spinning solution, will directly make solution charged, but allow solution produce charge inducing, thus spinning solution jet is stretched.This spinning process not only can make spinning security and operability strengthen, and adds the modification scope to electrostatic field size; Effectively can solve the fasciculation of air-flow fibroblast, make to be evenly distributed between fiber, be of value to the application in the direction such as filtration, biological tissue's base material.
The technical scheme that the present invention solve the technical problem is, provides a kind of electrostatic assisted solution jet spinning device, comprises spinning head, wire, HV generator, deflector roll and reception lace curtaining; Described spinning head comprises air inlet, gas outlet, spinneret orifice and liquid storage tank; Gas outlet outlet pressure in described spinning head is 0.2-1.2MPa; Described spinning head is the spinning head at least with a spinneret orifice, and when the number of spinneret orifice is two or more, orifice centre-to-centre spacing is 0.2cm-4cm; Described HV generator carries protective grounding conductor; Described reception lace curtaining is fixed on deflector roll, along with the rolling of deflector roll, receives the nanofiber mats that lace curtaining can export package, receives lace curtaining and pass through wired earth; Described spinning head distance receives the distance range of lace curtaining at 20-140cm, and the order number scope receiving lace curtaining is 40-200 order; It is characterized in that this device also comprises toroidal inductive electrode, described toroidal inductive electrode diameter is 0.1-2cm, and toroidal inductive electrode is positioned at 0-2cm place immediately below spinneret orifice, is connected with HV generator by wire, thus subsidiary high-pressure electrostatic, voltage range is 0-35kV.
The technical scheme that the present invention solve the technical problem is, provide a kind of electrostatic assisted solution jet spinning method, concrete spinning process is as follows:
By at least one polymer dissolution at least one solvent, make spinning solution, spinning solution concentration is between 2-30wt%; By spinning solution through measuring pump metered supply in the liquid storage tank of spinning head, delivery rate is 5-50mL/h hole, spinning solution is extruded from the spinneret orifice of spinning head, the high velocity jet air-flow that spinning solution is ejected by gas outlet is with the angle drawing-off refinement of 5-60 °, high velocity jet air-flow is supplied to spinning head by air inlet, gas outlet outlet pressure is 0.2-1.2MPa, and temperature is room temperature; Spinning solution thread is under high velocity jet air-flow and the effect of toroidal inductive electrode electrostatic field, solvent evaporates forms micro nanometer fiber, micro nanometer fiber is under high velocity jet air-flow and the effect of toroidal inductive electrode electrostatic field, being collected in distance spinning head 20-140cm place receives on lace curtaining, receiving lace curtaining is fixed on deflector roll, along with the rolling of deflector roll, receive the micro nanometer fiber felt that lace curtaining exports package.
Compared with prior art, the invention has the beneficial effects as follows: the electrostatic field that the present invention is formed is different with the electric field of electrostatic spinning, not directly be added on spinneret orifice, directly do not contact with spinning solution, will directly make solution charged, but allow solution produce charge inducing, thus spinning solution jet is stretched.This design not only can make spinning security and operability strengthen, and adds the modification scope to electrostatic field size.Meanwhile, the sub-wire effect of electrostatic effectively can solve the fasciculation of air-flow fibroblast, makes to be evenly distributed between fiber, is of value to the application in the direction such as filtration, biological tissue's base material.The stretching action of electrostatic is also conducive to the slenderizing of solution jet, and the microscopic pattern controllability of fiber is strengthened, and the stretching of electrostatic force simultaneously also makes fibre crystallinity strengthen to some extent within the specific limits, improves fibrous mechanical property.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram of a kind of electrostatic assisted solution of the present invention jet spinning device and spinning process;
Fig. 2 is the surface topography Electronic Speculum figure of spinning process embodiment 1 gained nanofiber of the present invention;
Fig. 3 is the surface topography Electronic Speculum figure of spinning process embodiment 2 gained nanofiber of the present invention;
Fig. 4 is the surface topography Electronic Speculum figure of spinning process embodiment 3 gained nanofiber of the present invention;
Fig. 5 is the surface topography Electronic Speculum figure of spinning process embodiment 4 gained nanofiber of the present invention;
Fig. 6 is the surface topography Electronic Speculum figure of spinning process embodiment 5 gained nanofiber of the present invention;
Fig. 7 is the surface topography Electronic Speculum figure of spinning process embodiment 6 gained nanofiber of the present invention;
Fig. 8 is the surface topography Electronic Speculum figure of spinning process embodiment 7 gained nanofiber of the present invention.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.
Electrostatic assisted solution jet spinning device of the present invention, comprises spinning head 1, toroidal inductive electrode 2, wire 3, HV generator 4, deflector roll 5, receives lace curtaining 6;
Described spinning head 1 comprises air inlet 11, gas outlet 12, spinneret orifice 13 and liquid storage tank 14; Described air inlet 11 is gas accesses, and gas outlet 12 is the ducts producing tangential gas flow; Gas outlet 12 outlet pressure in described spinning head is 0.2-1.2MPa; Described toroidal inductive electrode diameter is 0.1-2cm, and toroidal inductive electrode 2 is positioned at 0-2cm place immediately below spinneret orifice 13, is connected with HV generator 4 by wire 3, thus subsidiary high-pressure electrostatic, voltage range is 0-35kV; Described HV generator 4 carries protective grounding conductor, leaky can not occur; Described reception lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 can export package, receives lace curtaining 6 by wire 3 ground connection; Described spinning head 1 is apart from receiving the distance range of lace curtaining 6 at 20-140cm, and the order number scope receiving lace curtaining 6 is 40-200 order.
Adding of toroidal inductive electrode 2, the electrostatic field that HV generator 4 is produced need not be added on the spinneret orifice 13 of spinning head 1, and electrostatic field does not directly contact with spinning solution, will directly make solution charged, but allow solution produce charge inducing, thus spinning solution jet is stretched.
Spinning head 1 is the spinning head at least with a spinneret orifice, and when the number of spinneret orifice is two or more, orifice centre-to-centre spacing is 0.2cm-4cm.
Described electrostatic assisted solution jet spinning method is as follows:
Prepare spinning solution concentration between 2-30wt%, by spinning solution through measuring pump metered supply in the liquid storage tank 14 of spinning head 1, delivery rate is 5-50mL/h hole, spinning solution is extruded from spinneret orifice 13, the high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 5-60 °, high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is 0.2-1.2MPa, and temperature is room temperature; Spinning solution thread is under high velocity jet air-flow and the effect of toroidal inductive electrode electrostatic field, solvent evaporates forms micro nanometer fiber, micro nanometer fiber is under high velocity jet air-flow and the effect of toroidal inductive electrode electrostatic field, being collected in distance spinning head 20-140cm place receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receive the micro nanometer fiber felt that lace curtaining 6 exports package.
Below provide specific embodiments of the invention, but the claims of patent application is not by the restriction of specific embodiment.
Embodiment 1
The polyurethane being 280,000 by mean molecule quantity (Mw) is dissolved in and dissolves in DMF with the ratio of mass fraction 12%, and stir until mix, make spinning solution, the viscosity of spinning solution is 4300mPs at 25 DEG C.
Be fed in the liquid storage tank 14 of spinning head 1 by spinning solution through measuring pump, delivery rate is 10mL/h hole, and spinning solution is extruded from spinneret orifice 13, and spinning head 1 is single hole spinning head; The high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 30 °, and high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is set as 0.05MPa, and temperature is room temperature.Spinning solution thread is through the electric field action of toroidal inductive electrode 2, voltage is 3kV, ring electrode diameter is 0.5cm, be placed on 0cm place immediately below spinneret orifice, solvent evaporates forms micro nanometer fiber, and micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 18cm place 40 object receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 exports package.
Utilize the micro nanometer fiber that SEM radiographic measurement obtains, the diameter of gained micro nanometer fiber is between 0.5-2 micron, and electric field force sub-wire effect is comparatively obvious, and fiber dispersion is substantially even, without tangling phenomenon (see Fig. 2).
Embodiment 2
The polyacrylonitrile being 350,000 by mean molecule quantity (Mw) dissolves in DMF with the ratio of mass fraction 20%, under agitation until mix, makes spinning solution, and spinning solution viscosity is 14900mPs at 30 DEG C.
By spinning solution through measuring pump metered supply in the liquid storage tank 14 of spinning head 1, delivery rate is 30mL/h hole, and spinning solution is extruded from spinneret orifice 13, and spinning head 1 is four hole spinning heads, hole centre-to-centre spacing 1cm; The high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 60 °, and high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is set as 0.15MPa, and temperature is room temperature.Spinning solution thread is through the electric field action of toroidal inductive electrode 2, voltage is 10kV, ring electrode diameter is 0.9cm, be placed on 0.5cm place immediately below spray silk, solvent evaporates forms micro nanometer fiber, and micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 25cm place 100 object receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 exports package.
Utilize the micro nanometer fiber that SEM radiographic measurement obtains, the diameter of gained micro nanometer fiber is between 0.31-1.2 micron, and electric field force sub-wire successful, fiber dispersion is substantially even, without tangling phenomenon (see Fig. 3).
Embodiment 3
By mean molecule quantity (Mw) be 300,000 poly-(oxirane) be dissolved in deionized water with the ratio of mass fraction 8%, and add the silver nitrate (AgNO relative to poly-(oxirane) quality 2%
3), stir until mix, make spinning solution, spinning solution viscosity is 1800mPs at 50 DEG C.
By spinning solution through measuring pump metered supply in the liquid storage tank 14 of spinning head 1, delivery rate is 20mL/h hole, and spinning solution is extruded from spinneret orifice 13, and spinning head 1 is 6 hole spinning heads, hole centre-to-centre spacing 2.5cm; The high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 40 °, and high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is set as 0.3MPa, and temperature is room temperature.Spinning solution thread is through the electric field action of toroidal inductive electrode 2, voltage is 15kV, ring electrode diameter is 1.4cm, be placed on 1cm place immediately below spray silk, solvent evaporates forms micro nanometer fiber, and micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 30cm place 140 object receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 exports package.
Utilize the micro nanometer fiber that SEM radiographic measurement obtains, the diameter of gained micro nanometer fiber is between 0.08-0.58 micron, and electric field force sub-wire successful, fiber dispersion is substantially even, without tangling phenomenon (see Fig. 4).
Embodiment 4
By the degree of polymerization be 1600 cellulose be dissolved in LiCl/DMAc (lithium chloride/N with the ratio of mass fraction 3%, N-dimethylacetylamide) in, under agitation until mix, and be mixed into the nano-Ag particles that mass fraction content is 0.2%, make spinning solution, spinning solution viscosity is 8400mPs at 45 DEG C.
By spinning solution through measuring pump metered supply in the liquid storage tank 14 of spinning head 1, delivery rate is 18mL/h hole, and spinning solution is extruded from spinneret orifice 13, and spinning head 1 is single hole spinning head; The high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 50 °, and high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is set as 0.65MPa, and temperature is room temperature.Spinning solution thread is through the electric field action of toroidal inductive electrode 2, voltage is 20kV, ring electrode diameter is 1.8cm, be placed on 1.5cm place immediately below spray silk, solvent evaporates forms micro nanometer fiber, and micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 45cm place 180 object receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 exports package.
The micro nanometer fiber non-weaving cloth collected is through washing, remove lithium chloride, after drying, utilize the micro nanometer fiber that SEM radiographic measurement obtains, the diameter of gained micro nanometer fiber is between 0.22-0.92 micron, electric field force sub-wire successful, fiber dispersion is substantially even, without tangling phenomenon (see Fig. 5)
Embodiment 5
In DMF, make the spinning solution of polymer quality mark 12% by the polyurethane described in embodiment 1 and embodiment 2 and polyacrylonitrile raw material with mass ratio 1:3 mixed dissolution, spinning solution viscosity is 7400mPs at 30 DEG C.
By spinning solution through measuring pump metered supply in the liquid storage tank 14 of spinning head 1, delivery rate is 15mL/h hole, and spinning solution is extruded from spinneret orifice 13, and spinning head 1 is nine hole spinning heads, hole centre-to-centre spacing 1.5cm; The high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 30 °, and high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is set as 0.8MPa, and temperature is room temperature.Spinning solution thread is through the electric field action of toroidal inductive electrode 2, voltage is 20kV, ring electrode diameter is 1.8cm, be placed on 1.5cm place immediately below spray silk, solvent evaporates forms micro nanometer fiber, and micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 50cm place 200 object receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 exports package.
Utilize the micro nanometer fiber that SEM radiographic measurement obtains, the diameter of gained micro nanometer fiber is between 0.42-1.81 micron, and electric field force sub-wire successful, fiber dispersion is substantially even, without tangling phenomenon (see Fig. 6).
Embodiment 6
By the polyurethane described in embodiment 1 and embodiment 2 and polyacrylonitrile raw material with mass ratio 1:1 mixed dissolution in N, make the spinning solution of polymer quality mark 10% in dinethylformamide/dimethyl sulfoxide (DMSO) (volume ratio is 4:1), spinning solution viscosity is 5700mPs at 25 DEG C.
By spinning solution through measuring pump metered supply in the liquid storage tank 14 of spinning head 1, delivery rate is 35mL/h hole, and spinning solution is extruded from spinneret orifice 13, and spinning head 1 is single hole spinning head; The high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 40 °, and high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is set as 1.2MPa, and temperature is room temperature.Spinning solution thread is through the electric field action of toroidal inductive electrode 2, voltage is 30kV, ring electrode diameter is 2cm, be placed on 2cm place immediately below spray silk, solvent evaporates forms micro nanometer fiber, and micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 60cm place 160 object receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 exports package.
Utilize the micro nanometer fiber that SEM radiographic measurement obtains, the diameter of gained micro nanometer fiber is between 0.78-1.33 micron, and electric field force sub-wire successful, fiber dispersion is substantially even, without tangling phenomenon (see Fig. 7).
Embodiment 7
By average degree of polymerization be 640 cellulose acetate be dissolved in acetone/N with the ratio of mass fraction 22%, in dinethylformamide (volume ratio 90:10), under agitation until mix, make spinning solution, spinning solution viscosity is 2400mPs at 25 DEG C.
By spinning solution through measuring pump metered supply in the liquid storage tank 14 of spinning head 1, delivery rate is 25mL/h hole, and spinning solution is extruded from spinneret orifice 13, and spinning head 1 is single hole spinning head; The high velocity jet air-flow that spinning solution is ejected by gas outlet 12 is with the angle drawing-off refinement of 35 °, and high velocity jet air-flow is supplied to spinning head 1 by air inlet 11, and gas outlet 12 outlet pressure (expulsion pressure) is set as 1MPa, and temperature is room temperature.Spinning solution thread is through the electric field action of toroidal inductive electrode 2, voltage is 35kV, ring electrode diameter is 2cm, be placed on 2cm place immediately below spray silk, solvent evaporates forms micro nanometer fiber, and micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 70cm place 120 object receives on lace curtaining 6, receiving lace curtaining 6 is fixed on deflector roll 5, along with the rolling of deflector roll 5, receives the micro nanometer fiber felt that lace curtaining 6 exports package.
Utilize the micro nanometer fiber that SEM radiographic measurement obtains, the diameter of gained micro nanometer fiber is between 0.42-0.96 micron, and electric field force sub-wire successful, fiber dispersion is substantially even, without tangling phenomenon (see Fig. 8).
In the above description, preparation method of the present invention adopts method of testing below to determine various listed characterisitic parameter.
1. spinning solution concentration: weigh polymer quality and solvent quality respectively with electronic balance, calculates the percentage that polymer quality accounts for gross mass.
2. spinning solution viscosity: measure on the flow graph being equipped with a 20mm parallel-plate.At 23 DEG C, shear rate rose to 1000s with 4 minutes from 0
-1, Data Collection is got off, and with s
-1under mPs (milli handkerchief second) record.
3. micro nanometer fiber diameter: undertaken observing, measuring by scanning electronic microscope, for each micro nanometer fiber product sample, the diameter measuring 100 fibers provides its average diameter range.
Claims (2)
1. an electrostatic assisted solution jet spinning device, comprises spinning head, wire, HV generator, deflector roll and reception lace curtaining; Described spinning head comprises air inlet, gas outlet, spinneret orifice and liquid storage tank; Gas outlet outlet pressure in described spinning head is 0.2-1.2MPa; Described spinning head is the spinning head at least with a spinneret orifice, and when the number of spinneret orifice is two or more, orifice centre-to-centre spacing is 0.2cm-4cm; Described HV generator carries protective grounding conductor; Described reception lace curtaining is fixed on deflector roll, along with the rolling of deflector roll, receives the nanofiber mats that lace curtaining can export package, receives lace curtaining and pass through wired earth; Described spinning head distance receives the distance range of lace curtaining at 20-140cm, and the order number scope receiving lace curtaining is 40-200 order; It is characterized in that this device also comprises toroidal inductive electrode, described toroidal inductive electrode diameter is 0.1-2cm, and toroidal inductive electrode is positioned at 0-2cm place immediately below spinneret orifice, is connected with HV generator by wire, thus subsidiary high-pressure electrostatic, voltage range is 0-35kV.
2. an electrostatic assisted solution jet spinning method, the method adopts the electrostatic assisted solution jet spinning device described in claim 1, and concrete spinning process is as follows:
By at least one polymer dissolution at least one solvent, make spinning solution, spinning solution concentration is between 2-30wt%; By spinning solution through measuring pump metered supply in the liquid storage tank of spinning head, delivery rate is 5-50mL/h hole, spinning solution is extruded from the spinneret orifice of spinning head, the high velocity jet air-flow that spinning solution is ejected by gas outlet is with the angle drawing-off refinement of 5-60 °, high velocity jet air-flow is supplied to spinning head by air inlet, gas outlet outlet pressure is 0.2-1.2MPa, and temperature is room temperature; Spinning solution thread is through the electric field action of toroidal inductive electrode, solvent evaporates forms micro nanometer fiber, micro nanometer fiber is under high velocity jet air-flow and electrostatic field, being collected in distance spinning head 20-140cm place receives on lace curtaining, receiving lace curtaining is fixed on deflector roll, along with the rolling of deflector roll, receive the micro nanometer fiber felt that lace curtaining exports package.
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