CN108560065A - A kind of high temperature electrostatic spinning preparation method of PA6T/6 - Google Patents
A kind of high temperature electrostatic spinning preparation method of PA6T/6 Download PDFInfo
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- CN108560065A CN108560065A CN201810542617.4A CN201810542617A CN108560065A CN 108560065 A CN108560065 A CN 108560065A CN 201810542617 A CN201810542617 A CN 201810542617A CN 108560065 A CN108560065 A CN 108560065A
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- pa6t
- spinning
- electrostatic spinning
- spinning solution
- high temperature
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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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01D5/0076—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
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/80—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention provides a kind of high temperature electrostatic spinning preparation method of PA6T/6, and this method mainly includes the following steps that：Appropriate PA6T/6 and formic acid mixing are weighed first, dissolve to obtain the spinning solution that quality solubility is 14 ~ 20% by 80 ~ 98 DEG C of water-bath, spinning solution is secondly spinned into PA6T/6 fibers in 120 ~ 150 DEG C of hot environment by electrostatic spinning apparatus.The fusing point of PA6T/6 is high, and in forming process, processing temperature is often as high as 350 DEG C, to a certain extent reduces the molecular weight of PA6T/6, so that the reduction of the performances such as PA6T/6 performances such as crystallinity, mechanical performance, dimensional stability and resistance to chemical reagents.A kind of processing temperature of present invention offer significantly reduces and under the premise of not reducing PA6T/6 molecular weight, make the molding new methods of PA6T/6, and method and step provided by the invention is simple, it is easily operated, PA6T/6 fibers, which are made, has good tensile strength, toughness and modulus, while there is moderate elongation.
Description
Technical field
The present invention relates to the technical field of electrostatic spinning, more particularly to the high temperature electrostatic spinning preparation side of a kind of PA6T/6
Method.
Background technology
PA6T/6 is one that nylon 6T salt (terephthalic acid (TPA) hexamethylene diamine salt) is obtained with caprolactam by way of copolymerization
Class semiaromatic copolymer nylon.Such nylon resin had both maintained the good processing fluidity of amorphous nylon, while having water suction
The characteristics of rate is low, heat resistance and mechanical property significantly improve, is class of super heat-resistant resin, is widely used in machine-building, electricity
Heat-resisting, the wear-resisting and high intensity requirement special construction components such as road plate surface installation, weapon industry.
PA6T/6 is mainly by injection molding and extrusion forming at present, since the fusing point of PA6T/6 is up to 280~330 DEG C,
In forming process, processing temperature is often as high as 350 DEG C, to a certain extent reduces the molecular weight of PA6T/6, so that
The reduction of the performances such as PA6T/6 performances such as crystallinity, mechanical performance, dimensional stability and resistance to chemical reagents, it is certain using receiving
Limitation.
Electrostatic spinning process is the method that can directly, continuously prepare polymer nanofiber at present, have it is simple for process,
It easy to operate, the advantages that manufacturing speed is fast, is widely used in the fields such as medicine and environmental protection.Electrostatic spinning is as a kind of easy to be high
The New Processing for producing nanofiber of effect, nanofiber prepared therefrom have unique advantage, the fiber prepared
The advantages that small with diameter, internal surface area is big, and porosity is high, and mechanical property is good, in the side such as protection, filtering, matrices of composite material
Face has a good application prospect.However up to the present, in terms of preparing organic nanofibers, it is used for the high score of electrostatic spinning
Sub- kind is not enriched also, and the especially domestic research that PA6T/6 fibers are used to prepare to electrostatic spinning process is rarely reported.
Based on the above reason, it is necessary to which mousing out a kind of processing temperature significantly reduces and do not reducing PA6T/6 molecular weight
Under the premise of, make the molding new methods of PA6T/6, the method that electrostatic spinning process is especially used to prepare PA6T/6 fibers.
Invention content
To achieve the above object, the present invention provides a kind of high temperature electrostatic spinning preparation method of PA6T/6, include mainly with
Lower step：
（1）Sample dissolves：Appropriate PA6T/6 and formic acid mixing are weighed, then dissolves mixed liquor by 80 ~ 98 DEG C of water-bath
To spinning solution, the quality solubility of PA6T/6 is 14 ~ 20% in the spinning solution；
（2）Spinning fibre：Spinning solution is subjected to electrostatic spinning in the high temperature environment, setting electrostatic spinning apparatus voltage is 20 ~
30KV, it is 15 ~ 20cm to receive distance, and PA6T/6 fibers are made.
In a preferred embodiment, the step（1）The quality solubility of PA6T/6 is 16 ~ 18% in middle spinning solution；
In a preferred embodiment, the step（1）The quality solubility of PA6T/6 is 17% in middle spinning solution；
In a preferred embodiment, the step（2）The temperature of high temperature environment is 120 ~ 150 DEG C；
In a preferred embodiment, the step（2）The temperature of high temperature environment is 130 ~ 140 DEG C.
The excellent effect of the present invention is：
（1）A kind of processing temperature of present invention offer significantly reduces and under the premise of not reducing PA6T/6 molecular weight, makes PA6T/6
Molding new method is solved because of the excessively high reduction molecular weight of PA6T/6 forming temperatures, and the application of PA6T/6 is made to receive one
The problem of fixed limitation；
（2）The present invention solves the problems, such as that electrostatic spinning process is difficult to use in the preparation of PA6T/6 fibers, and having found to spin has
The solubility parameter and electrostatic spinning process parameter of the PA6T/6 fibers of superperformance；
（3）Method and step provided by the invention is simple, easily operated, and PA6T/6 fibers obtained have good tensile strength,
There is moderate diameter and diameter breadth coefficient simultaneously.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to being once described in detail.
Specific implementation mode
The present invention provides a kind of high temperature electrostatic spinning preparation method of PA6T/6, mainly includes the following steps that：
（1）Sample dissolves：Appropriate PA6T/6 and formic acid mixing are weighed, then dissolves mixed liquor by 80 ~ 98 DEG C of water-bath
To spinning solution, the quality solubility of PA6T/6 is 14 ~ 20% in the spinning solution；
（2）Spinning fibre：Spinning solution is subjected to electrostatic spinning in the high temperature environment, setting electrostatic spinning apparatus voltage is 20 ~
30KV, it is 15 ~ 20cm to receive distance, and PA6T/6 fibers are made.
PA6T/6：
PA6T/6 is a kind of half that nylon 6T salt (terephthalic acid (TPA) hexamethylene diamine salt) is obtained with caprolactam by way of copolymerization
Fragrant copolymer nylon.Such nylon resin had both maintained the good processing fluidity of amorphous nylon, at the same have water absorption rate it is low,
The characteristics of heat resistance and mechanical property significantly improve is class of super heat-resistant resin, is widely used in machine-building, circuit board table
Heat-resisting, the wear-resisting and high intensity requirement special construction component such as face installation, weapon industry.The fusing point of PA6T/6 is up to 280~330
DEG C, in forming process, processing temperature is often as high as 350 DEG C.
Electrostatic spinning：
Step（3）Described in electrostatic spinning be a kind of special fiber fabrication process, polymer solution or melt are in highfield
Middle carry out jet spinning.Under electric field action, the drop at syringe needle can be become conical (i.e. " taylor cone ") from spherical shape, and from circle
Extend to obtain fiber filaments in cone end.This mode can produce the polymer filaments of nanometer grade diameter.
Condition is used by the electrostatic spinning：It is 15 ~ 20cm that spinning, which receives distance,；Preferably, spinning receives distance
For 18 ~ 20cm；It is furthermore preferred that it is 19cm that spinning, which receives distance,.
Spinning voltage is 20 ~ 30 KV；Preferably, spinning voltage is 25 ~ 30 KV.
In a preferred embodiment, the step（2）The temperature of high temperature environment is 120 ~ 150 DEG C；
In a preferred embodiment, the step（2）The temperature of high temperature environment is 130 ~ 140 DEG C；
As a preferred embodiment, the step（1）The quality solubility of PA6T/6 is 16 ~ 18% in middle spinning solution；
As a preferred embodiment, the step（1）The quality solubility of PA6T/6 is 17% in middle spinning solution.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following embodiment is only used
In the invention will be further described, it should not be understood as limiting the scope of the invention, professional and technical personnel in the field
Some the nonessential modifications and adaptations made according to the content of foregoing invention, still fall within protection scope of the present invention.
In addition, if illustrated without other, it is raw materials used to be all commercially available.
Embodiment 1：
At room temperature, appropriate 3.6gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes
It obtains quality solubility and is 14% spinning solution after fully dissolving, then spinning solution is placed in electrostatic spinning apparatus and carries out Static Spinning
Silk, it is 120 DEG C which, which centers temperature, and setting voltage is 20KV, and it is 15cm to receive distance.It is received on the aluminium foil as cathode
Collect PA6T/6 fibers, finally fiber is tested for the property.
Embodiment 2：
At room temperature, appropriate 3.6gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes
It obtains quality solubility and is 14% spinning solution after fully dissolving, then spinning solution is placed in electrostatic spinning apparatus and carries out Static Spinning
Silk, it is 150 DEG C which, which centers temperature, and setting voltage is 25KV, and it is 16cm to receive distance.It is received on the aluminium foil as cathode
Collect PA6T/6 fibers, finally fiber is tested for the property.
Embodiment 3：
At room temperature, appropriate 5gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes it
Quality solubility is fully obtained after dissolving and is 18% spinning solution, then spinning solution is placed in electrostatic spinning apparatus and carries out electrostatic spinning,
It is 140 DEG C that the dress, which centers temperature, and setting voltage is 25KV, and it is 20cm to receive distance.It is collected on the aluminium foil as cathode
PA6T/6 fibers, are finally tested for the property fiber.
Embodiment 4：
At room temperature, appropriate 5gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes it
Quality solubility is fully obtained after dissolving and is 18% spinning solution, then spinning solution is placed in electrostatic spinning apparatus and carries out electrostatic spinning,
It is 150 DEG C that the dress, which centers temperature, and setting voltage is 30KV, and it is 18cm to receive distance.It is collected on the aluminium foil as cathode
PA6T/6 fibers, are finally tested for the property fiber.
Embodiment 5：
At room temperature, appropriate 4.5gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes
It obtains quality solubility and is 17% spinning solution after fully dissolving, then spinning solution is placed in electrostatic spinning apparatus and carries out Static Spinning
Silk, it is 130 DEG C which, which centers temperature, and setting voltage is 20KV, and it is 20cm to receive distance.It is received on the aluminium foil as cathode
Collect PA6T/6 fibers, finally fiber is tested for the property.
Embodiment 6：
At room temperature, appropriate 4.5gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes
It obtains quality solubility and is 17% spinning solution after fully dissolving, then spinning solution is placed in electrostatic spinning apparatus and carries out Static Spinning
Silk, it is 140 DEG C which, which centers temperature, and setting voltage is 30KV, and it is 20cm to receive distance.It is received on the aluminium foil as cathode
Collect PA6T/6 fibers, finally fiber is tested for the property.
Embodiment 7：
At room temperature, appropriate 7gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes it
Quality solubility is fully obtained after dissolving and is 20% spinning solution, then spinning solution is placed in electrostatic spinning apparatus and carries out electrostatic spinning,
It is 140 DEG C that the dress, which centers temperature, and setting voltage is 25KV, and it is 18cm to receive distance.It is collected on the aluminium foil as cathode
PA6T/6 fibers, are finally tested for the property fiber.
Embodiment 8：
At room temperature, appropriate 7gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes it
Quality solubility is fully obtained after dissolving and is 20% spinning solution, then spinning solution is placed in electrostatic spinning apparatus and carries out electrostatic spinning,
It is 145 DEG C that the dress, which centers temperature, and setting voltage is 30KV, and it is 18cm to receive distance.It is collected on the aluminium foil as cathode
PA6T/6 fibers, are finally tested for the property fiber.
Embodiment 9：
At room temperature, appropriate 4gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes it
Quality solubility is fully obtained after dissolving and is 16% spinning solution, then spinning solution is placed in electrostatic spinning apparatus and carries out electrostatic spinning,
It is 140 DEG C that the dress, which centers temperature, and setting voltage is 22KV, and it is 19cm to receive distance.It is collected on the aluminium foil as cathode
PA6T/6 fibers, are finally tested for the property fiber.
Embodiment 10：
At room temperature, appropriate 4gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes it
Quality solubility is fully obtained after dissolving and is 16% spinning solution, then spinning solution is placed in electrostatic spinning apparatus and carries out electrostatic spinning,
It is 150 DEG C that the dress, which centers temperature, and setting voltage is 28KV, and it is 20cm to receive distance.It is collected on the aluminium foil as cathode
PA6T/6 fibers, are finally tested for the property fiber.
Comparative example 1：
At room temperature, appropriate 4.5gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes
It obtains quality solubility and is 17% spinning solution after fully dissolving, then spinning solution is placed in electrostatic spinning apparatus and carries out Static Spinning
Silk, it is 110 DEG C which, which centers temperature, and setting voltage is 20KV, and it is 20cm to receive distance.After spinning starts, due to electrostatic
Device for spinning medium temperature is spent low, and solvent is difficult to volatilize, and spinning solution is solidified in syringe needle rapidly, and fiber cannot smoothly spray, in conduct
The PA6T/6 fibers being collected on the aluminium foil of cathode are few.
Comparative example 2：
At room temperature, appropriate 3.2gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes
It obtains quality solubility and is 13% spinning solution after fully dissolving, then spinning solution is placed in electrostatic spinning apparatus and carries out Static Spinning
Silk, it is 150 DEG C which, which centers temperature, and setting voltage is 25KV, and it is 16cm to receive distance.After spinning starts, due to spinning
The quality solubility of PA6T/6 is too low in liquid, and spinning solution can not form initial strength in syringe needle, cannot then generate continuous fiber,
The PA6T/6 fibers not being collected on the aluminium foil as cathode.
Comparative example 3：
At room temperature, appropriate 3.2gPA6T/6 and 30ml formic acid mixing is weighed, then mixed liquor, which is placed in 85 DEG C of water-baths, makes
It obtains quality solubility and is 13% spinning solution after fully dissolving, then spinning solution is placed in electrostatic spinning apparatus and carries out Static Spinning
Silk, it is 120 DEG C which, which centers temperature, and setting voltage is 20KV, and it is 15cm to receive distance.After spinning starts, due to electrostatic
Device for spinning medium temperature is spent low, and solvent is difficult to volatilize, and spinning solution is solidified in syringe needle rapidly, and fiber cannot smoothly spray, Er Qieyou
The quality solubility of PA6T/6 is too low in spinning solution, and spinning solution can not form initial strength in syringe needle, cannot then generate continuous
Fiber, the PA6T/6 fibers being collected on the aluminium foil as cathode are few.
Performance test：
1. average fibre diameter measures：
Pattern and fibre diameter use scanning electron microscope（VEGA3LMU, Tescan companies of Czech）Carry out Observe and measure；
2. the measurement of the tensile strength of fibre single thread（Bioassay standard uses GB 9997-88）：
Using JQ03new type Miniature tension instrument（Upper marine morning Digital Equipment Co., Ltd）It measures, the result of each sample is by 10
The average value of a this group of sample obtains；
3. diameter breadth coefficient（Coefficient of dispersion）.
Above-mentioned test result is shown in Table 1 the performance test results.
Example above-mentioned is merely illustrative, some features of the feature for explaining the disclosure, those skilled in the art
Present disclosure can be used for reference, technological parameter realization is suitably modified.In particular, it should be pointed out that all similar substitutions and modifications pair
It is it will be apparent that they are considered as being included in the present invention for those skilled in the art.The method of the present invention and application are
Be described through passing through preferred embodiment, related personnel obviously can not depart from the content of present invention, in spirit and scope to this
Methods and applications described in text are modified or suitably change and combine, to realize and apply the technology of the present invention.
Claims (5)
1. the high temperature electrostatic spinning preparation method of PA6T/6 a kind of, which is characterized in that adopt and be prepared by the following steps：
（1）Sample dissolves：Appropriate PA6T/6 and formic acid mixing are weighed, then dissolves mixed liquor by 80 ~ 98 DEG C of water-bath
To spinning solution, the quality solubility of PA6T/6 is 14 ~ 20% in the spinning solution；
（2）Spinning fibre：Spinning solution is subjected to electrostatic spinning in the high temperature environment, setting electrostatic spinning apparatus voltage is 20 ~
30kV, it is 15 ~ 20cm to receive distance, and PA6T/6 fibers are made.
2. the high temperature electrostatic spinning preparation method of PA6T/6 according to claim 1 a kind of, which is characterized in that the step
（1）The quality solubility of PA6T/6 is 16 ~ 18% in middle spinning solution.
3. the high temperature electrostatic spinning preparation method of PA6T/6 according to claim 2 a kind of, which is characterized in that the step
（1）The quality solubility of PA6T/6 is 17% in middle spinning solution.
4. the high temperature electrostatic spinning preparation method of PA6T/6 according to claim 1 a kind of, which is characterized in that the step
（2）The temperature of high temperature environment is 120 ~ 150 DEG C.
5. the high temperature electrostatic spinning preparation method of PA6T/6 according to claim 1 a kind of, which is characterized in that the step
（2）The temperature of high temperature environment is 130 ~ 140 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810542617.4A CN108560065A (en) | 2018-05-31 | 2018-05-31 | A kind of high temperature electrostatic spinning preparation method of PA6T/6 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810542617.4A CN108560065A (en) | 2018-05-31 | 2018-05-31 | A kind of high temperature electrostatic spinning preparation method of PA6T/6 |
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| CN108560065A true CN108560065A (en) | 2018-09-21 |
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