CN110325673A - Nanofiber manufacturing method and device - Google Patents
Nanofiber manufacturing method and device Download PDFInfo
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- CN110325673A CN110325673A CN201880013029.XA CN201880013029A CN110325673A CN 110325673 A CN110325673 A CN 110325673A CN 201880013029 A CN201880013029 A CN 201880013029A CN 110325673 A CN110325673 A CN 110325673A
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- nanofiber
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- 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
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- 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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- 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
- D01D5/04—Dry spinning methods
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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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The present invention provides a kind of nanofiber manufacturing method and device with good ratio defective product and good efficiency manufacture nanofiber.In the nanofiber manufacturing method, the solution that nano-fiber material is dissolved in the state of solvent and electrification is sprayed from the front end for the nozzle being arranged with the posture of front end upward, to manufacture nanofiber, which has liquid step and trapping step.Out in liquid step, solution is sprayed from the nozzle under the atmosphere that front end is disposed in the solvent comprising nano-fiber material.It traps in step, is that the polar collector opposite with solution induces the solution sprayed from nozzle to electrification, thus traps nanofiber.
Description
Technical field
The present invention relates to a kind of nanofiber manufacturing method and devices.
Background technique
Side as manufacture for example with several nm more than and less than the so-called nanofiber of the nanometer grade diameter of 1000nm
Method, it is known to Electrospinning.Electrospinning is also referred to electrostatic spinning (electrospinning) method, using with nozzle,
The electrospinning device (also referred to electrostatic spinning apparatus) of collector and power supply carries out.In electrospinning device, by power supply to
Apply voltage between nozzle and collector, such as nozzle electrification is made to be negative, collector electrification is made to be positive.If being applied with voltage
Under state, the raw material (hereinafter referred to as nano-fiber material) for spraying nanofiber from the front end of nozzle are dissolved in solvent and form
Solution, then the solution is moved to collector by Coulomb force, is captured on collector as nanofiber.
There is the device for the top that nozzle is disposed in collector in electrospinning device.The electrospinning device of the type
In, solution forms block in the front end of nozzle sometimes.The block includes solvent, falls in the nanofiber accumulated on collector sometimes
Collection face.In this case, it needs to remove to be attached in the nanofiber of accumulation and falls above-mentioned piece of position, therefore, product
Rate is impaired.Therefore, just like the side recorded in Japanese Unexamined Patent Publication 2012-167409 bulletin and International Publication No. 2014/057927
Method, that is, the solution sprayed from the nozzle being arranged with the posture of front end upward is induced to the collector for the top for being disposed in nozzle,
Thus it is trapped as nanofiber.
Also, also just like the method recorded in Japanese Unexamined Patent Publication 2009-074224 bulletin, that is, soaked in nozzle and collector
Stain sprays solution in the state of the undissolved bath foam of nano-fiber material, from nozzle.
Summary of the invention
The invention technical task to be solved
However, the method recorded in Japanese Unexamined Patent Publication 2012-167409 bulletin and International Publication No. 2014/057927
In, although the ratio defective product of nanofiber is good, the front end of nozzle is blocked by block.When the front end blocking of nozzle, in order to from nozzle
Front end remove above-mentioned piece, manufacture is stopped, and manufacture efficiency is poor.The method recorded in Japanese Unexamined Patent Publication 2009-074224 bulletin
In, nozzle is impregnated in the undissolved bath foam of nano-fiber material, therefore with Japanese Unexamined Patent Publication 2012-167409 bulletin and the world
The method for disclosing No. 2014/057927 is identical, the front end blocking of nozzle.
The purpose of the present invention is to provide a kind of nanometers with good ratio defective product and good efficiency manufacture nanofiber
Fibre manufacture and device.
For solving the means of technical task
In nanofiber manufacturing method of the invention, nanometer is sprayed from the front end for the nozzle being arranged with the state of front end upward
Fibrous material is dissolved in the solution of solvent and the state of electrification, to manufacture nanofiber, which has
Liquid step and trapping step out.Spray out in liquid step, under the atmosphere that front end is disposed in the solvent comprising nano-fiber material
Mouth sprays solution.It traps in step, is that the polar collector opposite with solution induces the solution sprayed from nozzle to electrification, by
This trapping nanofiber.
It is preferred that nozzle in the container for accommodating liquid solvent, is arranged with stretching out the state of front end from the liquid level in container,
By solvent gas made of the solvent gasification in container, front end is placed under atmosphere.
It is preferred that the distance between front end and liquid level are in the range of 2mm or more and 15mm or less.
It is preferred that at least 5 DEG C of low boiling point of the temperature of the solvent in container than solvent.
It is preferred that the angle of the nozzle relative to liquid level is in 45 ° or more and 90 ° or less of range.
Can be by spraying, forward end supplies solvent.
It is preferred that multiple nozzles ejections spaced apart from each other are molten out of range in 1mm or more and 20mm or less out in liquid step
Liquid.
It is preferred that the front end of multiple nozzles is identical direction.
It is preferred that any of the cellulose-based polymer of nano-fiber material and elastomer.It is preferred that nano-fiber material is
It is Triafol T when cellulose-based polymer.It is preferred that being acrylic elastomer when nano-fiber material is elastomer.
It is preferred that solvent is methylene chloride.
Nano-fiber manufacturing apparatus of the invention has nozzle, container, collector and voltage application portion.Nozzle is sprayed from front end
Nanofibers material is dissolved in solution made of solvent.The solvent of container receiving nano-fiber material.Collector is induced from spray
The solution that mouth sprays, traps as nanofiber.Voltage application portion is by applying the solution and collector that spray from front end
Voltage, charging solution and collector is opposite polarity.Nozzle is in container, with front end posture upward and from the liquid level of solvent
Stretch out the state setting of front end.
Invention effect
In accordance with the invention it is possible to manufacture nanofiber with good ratio defective product and good efficiency.
Detailed description of the invention
Fig. 1 is the synoptic diagram of non-woven fabric manufacturing equipment.
Fig. 2 is the synoptic diagram of nano-fiber manufacturing apparatus.
Specific embodiment
Fig. 1 is the synoptic diagram for implementing non-woven fabric manufacturing equipment 20 of the invention.Non-woven fabric manufacturing equipment 20 is for manufacturing
Nanofiber 11 and non-woven fabrics 10.Non-woven fabrics 10 such as can be used as non-dust cloth, filter cloth, with wound contact medical nonwoven
Cloth (referred to as spreading single (drape)) etc..
Non-woven fabrics 10 is made of nanofiber 11.Nanofiber 11 is using as the electrospinning of nanofiber manufacturing method
Method manufacture.The diameter of nanofiber 11 is in the range of 50nm or more and 2000nm or less, in present embodiment, substantially
400nm。
Non-woven fabric manufacturing equipment 20 has solution preparing portion 21, nano-fiber manufacturing apparatus 22 and the piping for connecting them
33。
Solution preparing portion 21 is used to prepare to be formed the solution 25 of nanofiber 11.Solution preparing portion 21 is by by nanofiber
Material 15 is dissolved in the solvent 31 of nano-fiber material to prepare (preparation) solution 25.The solution prepared by solution preparing portion 21
25, by piping 33, guide to nano-fiber manufacturing apparatus 22.
Nano-fiber manufacturing apparatus 22 carries out Electrospinning.In the example, nano-fiber manufacturing apparatus 22, which has, to be arranged to
Multiple nozzle 36a~36c of state spaced apart from each other.In explanation later, nozzle 36a, nozzle 36b, nozzle 36c are not distinguished
When, it is recorded as nozzle 36.One end of nozzle 36 is connect by piping 33 with solution preparing portion 21.As a result, from the another of nozzle 36
End sprays the solution 25 guided by solution preparing portion 21.The one end of nozzle 36 connecting with solution preparing portion 21 is referred to as " base
The other end of the ejection solution 25 of nozzle 36 is referred to as " front end " by end ".The solution 25 sprayed from the front end of nozzle 36 forms nanometer
Fiber 11.
In addition, the supporting mass 37 of strip is used in the accumulation of nanofiber 11 and the bearing of non-woven fabrics, along length in the example
Edge direction moves the supporting mass 37.About the detailed content of supporting mass 37, aftermentioned cross in Fig. 1 will be carried out using other attached drawings
To the width direction for being supporting mass 37, the paper longitudinal direction of Fig. 1 is the moving direction of supporting mass 37.Nozzle 36a~36c is arranged
At the state of the width direction arrangement along supporting mass 37.In the example, nozzle 36 is set as 3, but the number of nozzle 36 and unlimited
In this.In addition, being provided with the pump 38 for sending out solution 25 to nozzle 36 in each piping 33.By changing the revolving speed of pump 38, adjust
The flow of the solution 25 sprayed from nozzle 36.
With reference to Fig. 2, nano-fiber manufacturing apparatus 22 is illustrated.In Fig. 2, illustrate from the side nozzle 36a of Fig. 1
The case where, in order to avoid the complication of figure, for nozzle 36, only depicted nozzle 36a, is omitted the figure of nozzle 36b Yu nozzle 36c
Show.Nano-fiber manufacturing apparatus 22 has spinning chamber 45, the nozzle 36, container 46, cumulative portion 47, conductive member 48 and power supply
49 etc..
Spinning chamber 45 such as accommodate nozzle 36, container 46, cumulative portion 47 a part.In spinning chamber 45, in lower part
It is equipped with nozzle 36 and container 46, is equipped with cumulative portion 47 on top.Spinning chamber 45 prevents solvent by being configured to seal
Gas etc. leaks to the outside.Solvent gas is gas made of the solvent 31 of solution 25 gasifies.
Nozzle 36 is in container 46, with the posture setting of front end upward.That is, nozzle 36 is set as that the front end of solution 25 will be sprayed
Towards the state of the collector 58 for the top for being disposed in nozzle 36.The solution 25 sprayed from nozzle 36 is by being set to container 46
Opening, it is mobile to collector 58.Solution 25 is sprayed from the opening (hereinafter referred to as front opening) for the front end for being formed in nozzle 36
When, in front opening, substantially coniform taylor cone 53 is formed by solution 25.
The solvent 50 of the receiving nano-fiber material 15 of container 46.The solvent 50 is liquid.Gasified by solvent 50, nozzle 36
Front end be disposed in gaseous state include solvent 50 atmosphere under.Hereinafter, the solvent of the gaseous state is referred to as solvent gas
80.In addition, thering is the state of nozzle 36 to install to run through in the bottom of container 46 in this example, but for installing nozzle in container 46
36 method, however it is not limited to this.For example, it is also possible to the cardinal extremity of nozzle 36 is connected by the hose in the bottom through container 46,
Nozzle 36 is installed in container 46 via hose.In addition, as long as solvent 50 can dissolve nano-fiber material 15.As solvent
50, such as solvent identical with solvent 31 can be enumerated.
The piping 33 for the solvent 50 that guidance is sent out from pump 38 is connected on container 46.Container 46 is provided with detection solvent 50
Liquid level 52 horizontal liquid surface level sensor 54, according to the detection signal of liquid surface level sensor 54, control solvent 50 to
The injection rate of container 46 adjusts the height of the liquid level 52 in container 46.The height of liquid level 52 in container 46 is set below arranging
Height in the front end of the nozzle 36 of container 46.That is, nozzle 36 is in container 46, to stretch out front end from the liquid level 52 of solvent 50
State setting.
Also, container 46 is provided with the temperature sensor 56 of the temperature of detection solvent 50, according to the temperature sensor 56
Detection signal, pass through temperature regulation section it is (not shown) adjust container 46 in solvent 50 temperature.In addition, present embodiment
In, the temperature of the solvent 50 in container 46 is set as such as 5 DEG C of low boiling point than solvent 50.
Cumulative portion 47 has collector 58, collector rotating part 59, supporting mass supply unit 60 and supporting mass reeling end 61.Collection
Electrode 58 is used to induce the solution 25 sprayed from nozzle 36, traps as nanofiber 11, in present embodiment, after being captured in
On the supporting mass 37 stated.Collector 58 is made of the endless belt formed with made of metal ribbon.As long as collector 58 is by passing through use
The raw material that power supply 49 applies voltage and charges are formed, such as are set as stainless steel.Collector rotating part 59 is by a pair of rolls
62, roller 63 and motor 64 etc. are constituted.Collector 58 is horizontally hung and is around in a pair of rolls 62, roller 63.Have in the axis connection of a roller 62
It is disposed in the motor 64 of the outside of spinning chamber 45, rotates roller 62 with fixing speed.By the rotation, collector 58 is in roller 62
The mode recycled between roller 63 is mobile.In present embodiment, the movement speed of collector 58 is set as 10cm/ hours, but not
It is defined in this.
On collector 58, by supporting mass supply unit 60, it is fed with the supporting mass 37 being made of the aluminium flake of with shape.Supporting mass
37, for accumulating nanofiber 11, obtain as non-woven fabrics 10.Supporting mass supply unit 60, which has, sends out axis 60a.It is sending out
Axis 60a is equipped with supporting mass roller 65.Supporting mass roller 65 is batched by supporting mass 37 and is constituted in core 66.Supporting mass reeling end 61
With winding off spindle 67.Winding off spindle 67 in the core 68 installed, is batched by motor rotation (not shown) and is formed with non-woven fabrics 10
Supporting mass 37.In this way, the nano-fiber manufacturing apparatus 22 has the function of manufacturing nanofiber 11 and manufactures non-woven fabrics 10
Function implements the manufacture of nanofiber and non-woven fabrics based on Electrospinning.In addition, supporting mass 37 can also be placed in current collection
On pole 58, moved by the movement of collector 58.
Alternatively, it is also possible to directly carry out the accumulation of nanofiber 11 and the formation of non-woven fabrics 10, but root on collector 58
According to the raw material or the surface state of collector 58 etc. for forming collector 58, causes nanofiber 11 and non-woven fabrics 10 to attach, have
When be not easily stripped.Therefore, such as present embodiment, preferably the supporting mass 37 that nanofiber 11 and non-woven fabrics 10 are not easy to attach is guided
To collector 58, and nanofiber 11 is accumulated on the supporting mass 37.
Conductive member 48 is disposed in the lower section of container 46.Conductive member 48 and the nozzle 36 from the stretching of the lower section of container 46
Cardinal extremity electrical connection.
Power supply 49 is to apply voltage to nozzle 36 and collector 58, and thus making the electrification of nozzle 36 is the 1st polarity, and makes current collection
Pole 58 electrification be and the 1st opposite polarity polar 2nd polar voltage application portion.By in the nozzle 36 that has charged, thus
Solution 25 is charged, and is sprayed with the state of electrification from nozzle 36.Power supply 49 is connect with conductive member 48, via conductive member
48 pairs of nozzles 36 apply voltage.In addition, being not limited to this to the voltage application method of nozzle 36.For example, it is also possible to by spraying
Mouth 36 connects power supply 49 to apply voltage to nozzle 36.In present embodiment, so that the electrification of nozzle 36 is positive (+), make collector 58
Electrification is negative (-), but nozzle 36 and the polarity of collector 58 may be reversed.It is alternatively, it is also possible to flank collector 58 next
Current potential is set as 0.In present embodiment, the voltage for being applied to nozzle 36 and collector 58 is set as 30kV.By the electrification, from
Taylor cone 53, solution 25 are sprayed as spinning injection stream 69 to collector 58.In addition, in the example, by applying electricity to nozzle 36
It presses charge solution 25, but solution 25 can also be made to charge in piping 33, and the solution for the state charged 25 is guided
To nozzle 36.
The distance between nozzle 36 and collector 58 L1 are according in the type of nano-fiber material 15 and solvent 31, solution 25
Solvent 31 mass ratio etc., appropriate value is different, but in preferably 30mm or more and the range of 300mm or less, this embodiment party
180mm is set as in formula.
The voltage for being applied to nozzle 36 and collector 58 is preferably 2kV or more and 40kV hereinafter, from nanometer more carefully is formed
From the viewpoint of fiber 11, preferred voltage is as high as possible in the range.
Hereinafter, being illustrated to nanofiber manufacturing method.From the front end for the nozzle 36 being arranged with the posture of front end upward
The solution 25 that nano-fiber material 15 is dissolved in solvent 31 and the state of electrification is sprayed, to manufacture the Nanowire of nanofiber 11
It ties up in manufacturing method, comprising: go out liquid step, the spray under the atmosphere that front end is disposed in the solvent 50 comprising nano-fiber material 15
Mouth 36 sprays solution 25；And trapping step, it is sprayed to electrification with the induction of the collector 58 of 25 opposite polarity of solution from nozzle 36
Solution 25, thus trap nanofiber 11.Upward by the front end of nozzle 36 as described above, even if in solution 25 in nozzle
When block is formed in 36 front end, which will not fall on the nanofiber 11 accumulated on collector 58.Also, pass through nozzle 36
Front end is disposed under the atmosphere comprising solvent 50, is inhibited the above-mentioned piece of front end for being attached to nozzle 36, is prevented the front end of nozzle 36
Blocking.As a result, manufacturing nanofiber 11 with good ratio defective product and good efficiency.
Nozzle 36 is in the container 46 for accommodating liquid solvent 50, to stretch out the state of front end from the liquid level 52 in container 46
It is arranged.As a result, by solvent gas 80, the front end of nozzle 36 is placed under the atmosphere comprising solvent 50.Therefore, it is more reliably prevented from
The blocking of the front end of nozzle 36.
Alternatively, it is also possible to supply solvent 50 to the front end of nozzle 36 by spraying.When solvent 50 is sprayed, such as
It is preferred that by the solvent spray device amount etc. (not shown) for adjusting spraying solvent 50 being set as that the shape of taylor cone 53 will not be made
Etc. changed degree.The block of more preferably suppression solution 25 is attached to the front end of nozzle 36 as a result, is more reliably prevented from nozzle 36
Front end blocking.As a result, the manufacture efficiency of nanofiber 11 more improves.Also, in addition to the spraying of solvent 50 or replace solvent
50 be sprayed, can also supply solvent 50 to the front end of nozzle 36 with gaseous state.In addition, being arranged as by the front end of nozzle 36
Method under the atmosphere comprising solvent 50 can be selected suitably using the case where container 46 for accommodating liquid solvent 50 and by spraying
The case where solvent 50 it is any, in these, when using the container 46 for accommodating liquid solvent 50, the shape of taylor cone 53 will not be made
Shape changes, therefore more preferably.
The distance between the front end of nozzle 36 shown in FIG. 1 and liquid level 52 L2 preferably 2mm or more and 15mm it is below
In range.It is 2mm or more by distance L2, compared with when being less than 2mm, the solvent 50 of liquid is not above the front end of nozzle 36,
Therefore, more stably spinning by distance L2 is 15mm hereinafter, the concentration of solvent gas is high compared with when being greater than 15mm, because
This, more stably spinning.Distance L2 more preferably in the range of 2mm or more and 10mm or less, further preferably 3mm with
In the upper and range of 10mm or less.In addition, in present embodiment, such as it is set as 5mm.
The temperature of solvent 50 in container 46 is preferably than 5 DEG C of the low boiling point of solvent 50 or more, that is, than the low boiling point of solvent 50
At least 5 DEG C.This is because the temperature of solvent 50 is higher, more promote gasification, therefore, the temperature of the solvent 50 in container 46 is excessively
When close to boiling point, the solvent 50 in container 46 exhausts at once.Moreover, when the temperature of solvent 50 gets too close to boiling point, via nozzle
36 and the temperature of solution 25 is got higher, promote the gasification of solvent 31, damage the uniformity of the shape of nanofiber 11 sometimes.It is obtained
When the shape of the nanofiber 11 obtained is uneven, depending on the application, removal sometimes and desired variform part, knot
Fruit, ratio defective product are impaired.Therefore, from the viewpoint of ratio defective product, the temperature of preferred solvent 50 is sufficiently below boiling point.On the other hand,
From the viewpoint of efficiency, preferred solvent gas concentration is high, it is therefore preferable that the temperature of solvent 50 is high.Thus from more reliably mentioning
From the viewpoint of high yields and efficiency, at least 5 DEG C of low boiling point of the temperature of the solvent 50 in more preferable container 46 than solvent 50
And it is as high as possible.
The angle, θ of nozzle 36 relative to liquid level 52 is illustrated.Here, by the longitudinal direction of nozzle 36 is set as water
θ usually is set as 0 °, and θ when being set as vertically upward is set as 90 °.Nozzle 36 is 0 ° of 90 ° of < θ < therefore upward.The angle, θ is got over
Close to 90 °, in order to collector 58 it is mobile from the solution 25 that nozzle 36 sprays and required voltage becomes smaller.It is applied to nozzle 36
Voltage is smaller, more the gasification of the solvent 31 in the front end of inhibition nozzle 36, more inhibits the blocking of nozzle 36.Therefore, angle, θ is preferred
For in 45 ° or more and 90 ° or less of range, further preferably in 75 ° or more and 90 ° or less of range, most preferably
90°.In addition, angle, θ is for example set as 90 ° in present embodiment.
In addition, multiple nozzle 36a~36c are spaced from each other in the range of 1mm or more and 20mm or less in this example.By Fig. 1
Shown in the distance between each nozzle 36 when being set as L3, be 1mm or more by distance L3, compared with when being less than 1mm, inhibit spray
Electric discharge between mouth 36, thus steadily spinning are 20mm hereinafter, compared with when being greater than 20mm by distance L3, can make to set
Standby smallerization.Distance L3 is more preferably in the range of 3mm or more and 10mm or less.In addition, in present embodiment, distance L3
Such as it is set as 5mm.
The front end of multiple nozzle 36a~36c is preferably identical direction.About the direction " identical " of nozzle, in addition to each nozzle
36 angle, θ be identical situation other than, as long as at 0 ° or more and 45 ° hereinafter, as long as can be considered identical.Pass through multiple nozzles
The front end of 36a~36c is identical direction, can get mass area ratio more evenly, that is, the non-woven fabrics of thickness more evenly.Unit
Area quality refers to the quality of the per unit area of non-woven fabrics.Depending on the application, non-woven fabrics in uneven thickness is sometimes by part
Removal, and non-woven fabrics in homogeneous thickness can be used all, therefore ratio defective product is better.
By solution preparing portion 21, nano-fiber material 15 is dissolved in solvent 31, is thereby preparing for solution 25.
Nano-fiber material 15 is preferably cellulose-based polymer or elastomer.
Cellulose-based polymer as nano-fiber material 15 is preferably cellulose acylate, NC Nitroncellulose, ethyl
Any of cellulose, carboxymethylethylcellulose.As cellulose acylate, more preferable cellulose acetate, cellulose propionate
Element, cellulose butyrate, cellulose acetate propionate.As cellulose acetate, further preferred Triafol T and two acetic acid are fine
Dimension element.When as nano-fiber material 15 using cellulose-based polymer, particularly preferred Triafol T.
Also, the elastomer as nano-fiber material 15 is preferably acrylic elastomer, styrene series elastomer, alkene
Any of hydrocarbon system elastomer, vinyl chloride elastomer, amidocarbonic acid ester based elastomers and acid amides based elastomers.As nanometer
When fibrous material 15 is using elastomer, particularly preferred acrylic elastomer.
As solvent 31, can enumerate methanol, ethyl alcohol, isopropanol, butanol, benzyl alcohol, acetone, methyl ethyl ketone, cyclohexanone,
Methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl formate, Ethyl formate, hexane, hexamethylene, methylene chloride, chlorine
Imitative, carbon tetrachloride, benzene,toluene,xylene, dimethylformamide, N- methylpyrrole pyridine ketone, diethyl ether, dioxanes, tetrahydro furan
It mutters, 1- methoxy-2-propanol etc..These can be used alone, but also also mix together according to the type of nano-fiber material 15.
In these, more preferable methylene chloride (boiling point is 40 DEG C) in present embodiment, uses methylene chloride as solvent 31.
In the collector 58 of nozzle 36 and loopy moving, voltage is applied with by power supply 49.The electrification of nozzle 36 is work as a result,
For the 1st it is polar just, the electrification of collector 58 is polar negative as the 2nd.In nozzle 36, continuously it is fed with from solution preparing portion 21
Solution 25 is continuously fed with supporting mass 37 on mobile collector 58.Solution 25 is by nozzle 36, so that electrification is as the
1 it is polar just, and with the state of electrification from the front opening of nozzle 36 spray.
Trapping step is illustrated.The induction of collector 58 is sprayed from front opening with charging for the 1st polar state
Solution 25.Taylor cone 53 is formed in front opening as a result, sprays spinning injection stream 69 from the taylor cone 53 towards collector 58.
Electrification is the 1st polar spinning injection stream 69 towards during collector 58, repels caused by the charge by itself, is split into
Thin footpath.Thus nanofibers 11 are manufactured, and are captured on supporting mass 37.
The nanofiber 11 being captured is used as non-woven fabrics 10, is sent together with supporting mass 37 to supporting mass reeling end 61.Nonwoven
Cloth 10 is wound in core 68 with the state Chong Die with supporting mass 37.Core 68 from winding off spindle 67 after unloading, from supporting mass 37
Separate non-woven fabrics 10.The non-woven fabrics 10 so obtained is strip, later, such as can be cut into desired size.
In the example, the band of loopy moving is used as collector 58, but collector is not limited to band.For example, collection
Electrode can be fixed plate, also can be set to cylindric rotary body.When the current collection to be made of plate or cylinder
, it is preferable to use supporting mass 37 when pole, so as to easily separate non-woven fabrics from collector.In addition, when using rotary body, in rotary body
Circumferential surface form the non-woven fabrics of tubular being made of nanofiber, therefore, from the non-woven fabrics of rotary body extraction tubular after spinning,
And it is cut to desired size and shape, thus, it is possible to as non-woven cloth products.
Embodiment
[embodiment 1]~[embodiment 20]
In nano-fiber manufacturing apparatus 22, type, the type of solvent 50 and the quantity of nozzle 36 etc. of solvent 31 are changed, even
Continuous manufacture nanofiber 11 is as Examples 1 to 20.Used nano-fiber material 15 is recorded in the " nanofiber of table 1
Material " column.As nano-fiber material 15, when using cellulose acetate, it is recorded as on " nano-fiber material " column of table 1
" CA " when using elastomer, is recorded as " elastomer " on " nano-fiber material " column of table 1.Wherein, " CA " is taken using acetyl group
For the Triafol T of degree 2.87, the Kuraray Co., Ltd. system of " elastomer " used as acrylic elastomer
CLARITY (registered trademark).
As solvent 31, when using methylene chloride, it is recorded as " methylene chloride " on " solvent " column of table 1, uses n- methyl
When Pyrrolizidine ketone, " NMP " is recorded as on " solvent " column of table 1.
The presence or absence of container 46 is recorded in " the presence or absence of container " column of table 1.When having container 46, the type of solvent 50 is recorded in table
1 " type of solvent " column, the solvent 50 in container 46 and the temperature difference between the boiling point of solvent 50 are the (solvent in container 46
50 temperature)-(boiling point of solvent 50) be recorded in " temperature relative to the solvent in the container of the boiling point of solvent " column of table 1.
As solvent 50, when using methylene chloride, it is recorded as " methylene chloride " on " type of solvent " column of table 1, uses n- methyl pyrrole
When coughing up pyridine ketone, " NMP " is recorded as on " type of solvent " column of table 1.The presence or absence of the spraying " solvent for being recorded in table 1 of solvent 50
It is the presence or absence of spraying " column.The angle, θ of nozzle 36 is recorded in " angle of nozzle " column of table 1.The number of nozzle 36 is recorded in table 1
" number of nozzle " column.When being provided with multiple nozzles 36, the direction of the front end about each nozzle 36 is identical or different, note
Be loaded in " similarities and differences of the direction of each nozzle " column of table 1, the distance between each nozzle 36 be recorded in table 1 " between each nozzle away from
From " column.In addition, in " similarities and differences of the direction of each nozzle " column of table 1, multiple nozzles 36 be set as it is identical towards when, be recorded as " phase
Together ", in multiple nozzles 36 at least one be set as it is different towards when, be recorded as " difference ".The front end of nozzle 36 and the liquid in container 46
The distance between face is recorded in " the distance between spray nozzle front end and liquid level " column of table 1.In addition, the number of nozzle 36 is set as 1
It is a when manufacturing nanofiber 11, to be recorded in " similarities and differences of the direction of each nozzle " column and " the distance between each nozzle " column of table 1
For "-".
According to evaluation method below and benchmark evaluation ratio defective product and efficiency.
(1) ratio defective product
In the non-woven fabrics 10 be made of nanofiber 11 obtained, respectively evaluate non-woven fabrics 10 thickness uniformity with
The uniformity of the shape of nanofiber 11, according to each evaluation, with benchmark evaluation below ratio defective product.Thickness about non-woven fabrics 10
The uniformity of degree, from the sample for the square that accumulation is 100mm in the length that the non-woven fabrics 10 of supporting mass 37 cuts out one side, with connecing
Touch elcometer measures the thickness of the sample at 10 in the width direction, subtracts average value from the maximum value of these measured values,
It is evaluated according to the value that the numerical value is set as percentage divided by average value.The uniformity of shape about nanofiber 11,
From the sample for the square that accumulation is 10mm in the length that the non-woven fabrics 10 of supporting mass 37 cuts out one side, the sample is observed by visual observation
SEM (ScanningElectron Microscope (the scanning electron microscope)) images of product is evaluated.In addition, closing
In the shape of following nanofibers 11, " uniform " refers to, the thickness of nanofiber 11 is substantially permanent in the long side direction in SEM image
Fixed, " uneven " refers to, the thickness of nanofiber 11 changes in the long side direction in SEM image.Shape is non-uniform to be received
Rice fiber 11 confirms the round shape as drop or spherical for example in the midway of nanofiber 11.A, B, C are qualification, D
It is unqualified.As a result " ratio defective product " column shown in table 1.
A: for the uniformity of the thickness of non-woven fabrics within ± 10%, the shape of nanofiber is uniform.
B: the uniformity of the thickness of non-woven fabrics is more than ± 10%, but the shape of nanofiber is uniform, is not had in actual use
Problematic rank.
C: the shape of nanofiber is uneven, but the uniformity of the thickness of non-woven fabrics is within ± 10%, is actual use
The upper rank that there is no problem.
D: the uniformity of the thickness of non-woven fabrics is more than ± 10%, and the shape of nanofiber is uneven.
(2) efficiency
After continuous spinning 20 minutes, the presence or absence of block of solution 25 in the front end of visual confirmation nozzle 36 comes from nozzle
The spray mode of 36 solution 25, is evaluated according to following benchmark.A, B is qualification, and C is unqualified.As a result shown in table 1
" efficiency " column.
A: in the front end of nozzle without the block of attachment solution, the blocking of nozzle is not generated.
B: being attached with the block of minimal amount of solution in the front end of nozzle, but does not generate the blocking of nozzle.
C: solution is not sprayed from nozzle.
[table 1]
[comparative example 1]
The example being not under the atmosphere comprising solvent 50 as nozzle 36, manufactures Nanowire without using container 46
Dimension, using this as comparative example 1.Used nano-fiber material and solvent etc. are shown in table 1.Other conditions are set as and embodiment phase
Together.
According to method identical with embodiment and benchmark evaluation ratio defective product and efficiency.Evaluation result is shown in table 1.
Symbol description
10- non-woven fabrics, 11- nanofiber, 15- nano-fiber material, 21- solution preparing portion, 22- nanofiber manufacture dress
It sets, 25- solution, 31- solvent, 33- piping, 36- nozzle, 36a~36c- nozzle, 37- supporting mass, 38- pump, 45- spinning chamber,
46- container, 47- cumulative portion, 48- conductive member, 49- power supply, 50- solvent, 52- liquid level, 53- taylor cone, 54- liquid level pass
Sensor, 56- temperature sensor, 58- collector, 59- collector rotating part, 60- supporting mass supply unit, 60a- send out axis, 61- branch
Hold body reeling end, 62- roller, 63- roller, 64- motor, 65- supporting mass roller, 66- core, 67- winding off spindle, 68- core, 69- spinning
Injection stream, 80- solvent gas, the distance between L1- nozzle and collector, the distance between the front end of L2- nozzle and liquid level,
The distance between each nozzle of L3-, θ-nozzle angle.
Claims (13)
1. a kind of nanofiber manufacturing method sprays nano-fiber material from the front end for the nozzle being arranged with the posture of front end upward
It is dissolved in the solution of solvent and the state of electrification, to manufacture nanofiber, which is included
Liquid step out is sprayed from the nozzle under the atmosphere that the front end is disposed in the solvent comprising the nano-fiber material
The solution；And
Step is trapped, it is described molten to be that opposite with the solution polar collector induction is sprayed from the nozzle to electrification
Thus liquid traps nanofiber.
2. nanofiber manufacturing method according to claim 1, wherein
The nozzle is in the container of the solvent for accommodating liquid, to stretch out the front end from the liquid level in the container
State is arranged,
By solvent gas made of the solvent gasification in the container, the front end is placed under the atmosphere.
3. nanofiber manufacturing method according to claim 2, wherein
The distance between the front end and the liquid level are in the range of 2mm or more and 15mm or less.
4. nanofiber manufacturing method according to claim 2 or 3, wherein
At least 5 DEG C of low boiling point of the temperature of the solvent in the container than the solvent.
5. nanofiber manufacturing method according to any one of claim 2 to 4, wherein
The angle of the nozzle relative to the liquid level is in 45 ° or more and 90 ° or less of range.
6. nanofiber manufacturing method according to any one of claim 1 to 5, wherein
By spraying, the front end Xiang Suoshu supplies the solvent.
7. nanofiber manufacturing method according to any one of claim 1 to 6, wherein
In the liquid step out, multiple nozzles ejection institutes spaced apart from each other out of range in 1mm or more and 20mm or less
State solution.
8. nanofiber manufacturing method according to claim 7, wherein
The front end of multiple nozzles is identical direction.
9. nanofiber manufacturing method according to any one of claim 1 to 8, wherein
The nano-fiber material is any of cellulose-based polymer and elastomer.
10. nanofiber manufacturing method according to claim 9, wherein
The cellulose-based polymer is Triafol T.
11. nanofiber manufacturing method according to claim 9, wherein
The elastomer is acrylic elastomer.
12. nanofiber manufacturing method according to any one of claim 1 to 11, wherein
The solvent is methylene chloride.
13. a kind of nano-fiber manufacturing apparatus, has:
Nozzle sprays nano-fiber material from front end and is dissolved in solution made of solvent；
Container accommodates the solvent of the nano-fiber material；
Collector induces the solution sprayed from the nozzle, traps as nanofiber；And
Voltage application portion makes the solution by applying voltage to the solution and the collector that spray from the front end
It is opposite polarity with collector electrification,
The nozzle in the container, with front end posture upward and to stretch out the front end from the liquid level of the solvent
State setting.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017-031735 | 2017-02-23 | ||
| JP2017031735A JP6672198B2 (en) | 2017-02-23 | 2017-02-23 | Nanofiber manufacturing method and apparatus |
| PCT/JP2018/006145 WO2018155474A1 (en) | 2017-02-23 | 2018-02-21 | Nanofiber manufacturing method and device |
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| CN110325673A true CN110325673A (en) | 2019-10-11 |
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| CN201880013029.XA Pending CN110325673A (en) | 2017-02-23 | 2018-02-21 | Nanofiber manufacturing method and device |
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| JP (1) | JP6672198B2 (en) |
| KR (1) | KR102212977B1 (en) |
| CN (1) | CN110325673A (en) |
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| WO (1) | WO2018155474A1 (en) |
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| JP7214742B2 (en) * | 2018-09-06 | 2023-01-30 | 富士フイルム株式会社 | nonwoven fabric |
| JP7394579B2 (en) * | 2019-10-21 | 2023-12-08 | 花王株式会社 | Nanofiber sheet manufacturing equipment |
| JP7280369B2 (en) * | 2019-09-20 | 2023-05-23 | 富士フイルム株式会社 | Non-woven fabrics and filters |
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- 2018-02-21 KR KR1020197024446A patent/KR102212977B1/en active IP Right Grant
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2018155474A1 (en) | 2018-08-30 |
| JP6672198B2 (en) | 2020-03-25 |
| KR20190103444A (en) | 2019-09-04 |
| TW201831743A (en) | 2018-09-01 |
| JP2018135615A (en) | 2018-08-30 |
| KR102212977B1 (en) | 2021-02-04 |
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